Indian Patents. 257111:A LYOCELL THERMOREGULATORY FIBER AND A METHOD OF MAKING THEREOF

Title of Invention	A LYOCELL THERMOREGULATORY FIBER AND A METHOD OF MAKING THEREOF
Abstract	A lyocell fiber having thermoregulatory activity and a method of making thereof is disclosed. Micro-reservoirs are formed in the fibers having thermoregulatory activity.

Full Text	FORM - 2 THE PATENTS ACT, 1970 (39 OF 1970) AND THE PATENTS RULES, 2003 COMPLETE SPECIFICATION (See section 10; rule 13) A LYOCELL THERMOREGULATORY FIBER AND A METHOD OF MAKING THEREOF ADITYA BIRLA SCIENCE & TECHNOLOGY CO. LTD. an Indian Company of Aditya Birla Center, 2nd floor, C Wing, S. K. Ahire Marg, Mumbai 400 025, Maharashtra, India THE FOLLOWING SPECIFICATION PARTICULARLY DESCRIBES THE INVENTION AND THE MANNER IN WHICH IT IS TO BE PERFORMED. Field of the invention The present invention relates to textile fibers. Background of the invention The term "fiber" or "textile fiber" means a substance which is capable of being spun into a yarn or made into a fabric by bonding or by interlacing in a variety of methods including weaving, knitting, braiding, felting, twisting, or webbing, and which is the basic structural element of textile products. Fibers are classified on the basis of their length such as short fibers or staple fiber and long fibers or filament fiber. The fibers can also be classified on the basis of their origin such as natural fibers and man-made fibers. The term natural fibers means any fiber that exists as such in the natural state e.g. vegetable fibers or wood fibers. The other type of fibers is obtained from chemical substances. These are called man made fibers. They are rayon, polyester, nylon, acrylic (cashmilon) etc. For centuries, mankind has relied upon various plants and animals to provide raw materials for fabrics and clothing. In recent times, the industrialization and scientific advancement has provided several improved materials having far superior properties, particularly suitable for clothing. Lyocell is a manmade fiber derived from cellulose. Though it is related to rayon, lyocell is obtained by a solvent spinning technique. The solvent spinning technique, which is simpler and more environmentally sound, since it uses a non-toxic solvent chemical that can be recycled in the manufacturing process. 2 It is an extremely strong fabric with industrial uses such as in automotive filters, ropes, abrasive materials, bandages and protective suiting material. It is primarily found in the garment industry, particularly in women's clothing. Lyocell fibers are prepared by following process steps: The raw cellulose is dissolved into heated, pressurized vessel filled with an amine oxide solvent. After soaking for a short time in the solvent at high temperature under vacuum to remove excess water, the cellulose forms a clear solution and then it is filtered. The solution is then pumped through spinneret which is pierced with small holes to obtain long strands of fibers. The fibers are then immersed in another dilute solution of amine oxide. This helps to set the fiber strands. Then, they are washed with de-mineralized water. The lyocell fibers are then led to a drying area, where the water is evaporated from it. The strands are led to a finishing area, where the lubricant is applied. The dried, finished fibers are at this stage are called as a tow, which is a large untwisted bundle of continuous length filaments. The bundles of tow are taken to a crimper, a machine which compresses the fiber, giving it texture and bulk. The crimped fiber is then carded by mechanical carders, which perform an action like combing, to separate and order the strands. The carded strands are cut and baled for shipment to a fabric mill. The amine oxide used to dissolve the cellulose and set the fiber after spinning is recovered and re-used in the manufacturing process. From the spun or filament yarn, fabric is formed by knitting or weaving operations. Knitted fabrics can be made by using hooked needles to interlock one or more sets of yarns through a set of loops. The loops may be either loosely 3 or closely constructed, depending on the purpose of the fabric. Knitted fabrics can be used for hosiery, underwear, sweaters, slacks, suits, coats, rugs and other home furnishings. Knitting is performed using either weft or warp processes. Some typical preparations that are involved in the weaving operations are warping, slashing or sizing. Sizing agents are added to the yarn by solution or pad/dry techniques. Differences in raw materials, processing chemicals, fiber diameter, post treatments and blend ratios can be manipulated to produce a fiber having customized properties suitable for desired application. It is often desired that the lyocell fabrics possess typical properties such as thermal stability, ability to retain perfumes, antibacterial properties and the like. These properties are essential in several industrial as well as household applications. There has been a considerable interest in developing such materials. In order to impart various desirable properties to the fabric as mentioned above to the fabric, several additives are added. Such additives include antimicrobial agents, deodorizing agents, antistatic agents, perfumes. Besides such specific additives, generic additives for improving overall quality of the fabric, such as sizing agents, additives for increasing yarn softness and pliability are also added. Prior Art WO2008030648 discloses a temperature regulating, polymer containing fabric and a suspension formulation used in preparation of such fibers. The suspension comprises a solvent and plurality of microcapsules containing phase-change material. The suspension is used for incorporating the microcapsules in the 4 fabric. The microcapsules comprise a shell composed of acrylic acid and their derivatives and a core which is composed of a phase change material having a latent heat in a range between 80 J/g and 400 J/gm and a transition temperature in the range of 20°C-50°C. United States Patent Application no. 20070026228 discloses cellulosic fibers having enhanced reversible thermal properties and applications of such cellulosic fibers. The cellulosic fibers include a fiber body including a cellulosic material and a set of microcapsules dispersed in the cellulosic material. The set of microcapsules contain a phase change material having a latent heat of at least 40 J/g and a transition temperature in the range of 0°C-100°C. The phase change material provides thermal regulation based on absorption and release of the -latent .heat at the transition temperature. The cellulosic fibres are formed via a solution spinning process, and used in various products where thermal regulating properties are desired. WO2003062513 discloses a sheath core type fiber and fabric having thermal storage and release characteristics and the method of manufacturing the fiber as well as fabric. The fiber includes mixture of first polymer and a thermal stabilizing material which forms the core of the fiber and a polymer sheath forms the exterior of fiber and surrounds the core. The core and sheath polymers are selected from polyolefins, polyamides, polyesters, elastomeric polymers and combinations thereof. Earlier known processes of incorporating such additives, as reported in the above mentioned patents/applications, mainly involved conventional methods like spraying, encapsulating, solvent spinning the additives on the fabric. 5 However, these methods suffer from several disadvantages which include non¬uniform and improper adhesion of additives onto the fiber material, fading, waning and gradual washing out of the additives over a period of time and which further affects the feel and texture of the fabric. There is thus felt a need for a process of incorporating additives to fabric which overcomes these shortcomings. Objects of the Invention It is an object of this invention to provide thermoregulatory lyocell products, wherein at least one thermoregulatory constituent is incorporated into the body of the fiber. Another object of this invention is to provide a process of incorporating thermoregulatory constituents into lyocell fibers which ensures uniform distribution of the thermoregulatory constituent throughout the fiber length. Yet another object of this invention is to provide thermoregulatory lyocell fibers wherein the thermoregulatory constituents are retained in the lyocell product over a prolonged period of time. Yet another object of this invention is to provide a process of incorporating thermoregulatory constituents to lyocell fibers which does not affect the feel and texture of the fabric. Still another object of this invention is to provide a process of incorporating thermoregulatory constituents to lyocell fibers such that inherent properties of 6 the lyocell fibers such as fiber strength, linear density, tenacity, heat resistance, dyeability and drying properties are not altered. Definitions: As used in the present specification, the following words and phrases are generally intended to have the meanings as set forth below, except to the extent that the context in which they are used indicates otherwise. "Phase-change agent" means a substance having the ability to releases or absorbs heat whenever it undergoes change in its physical state. Enthalpy means heat content or total heat, including both sensible and latent heat. "Latent heat" means the heat energy needed to change the state of a substance (ie: from a solid to a liquid) but not it's temperature. "Flash point" means the temperature at which a substance gives off a sufficient amount of vapors to form an ignitable mixture with air. "Non-aqueous phase" means a melted mixture in liquid state which is water insoluble. "Aqueous phase" means substance dissolved in water. "Lyocell Polymer dope" means an intermediate material in the manufacture of lyocell rayon products that is used for preparation of fibers. 7 "Preform mass" means an intermediate material suitable for making fibers. Summary of the Invention In accordance with this invention there is provided a thermoregulatory lyocell formulation meant for manufacture of lyocell rayon products comprising: ■ at least one non-water-soluble thermoregulatory constituent having a melting point lying in a predetermined range of temperature said constituent being in the range of about 0.01 to 20% of the mass of the formulation, ■ at least one water soluble non-cationic surfactant having HLB value in the range of 9 to 40, in the range of range of 0.001 to 10% of the mass of the formulation, ■ cellulosic pulp in the range of about 3% to 35% of the mass of the formulation ■ NNMO in the range of about 60% to 80% of the mass of the formulation; and ■ water in the range of about 0% to 20 % with respect to the mass of the formulation. Typically, the thermoregulatory constituent is at least one selected from a group consisting of nonadecane, eicosane, heptadecane, octadecane, pentadecane, hexadecane, and other saturated hydrocarbons, decyl alcohol, lauryl alcohol, myristyl alcohol and other alphatic alcohols. Typically, the surfactant is at least one non-ionic surfactant selected from a group of non-ionic surfactants consisting of alkyl phenoxy ethoxylated non-ionic surfactants and ethoxylated alkyl alcohol surfactants, Polyethylene-block- 8 Poly propylene glycol-block-polyethylene glycol and Ethylenediamine tetrakis(propylene oxide-block-ethylene oxide) tetrol. Typically, the alkyl phenoxy ethoxylated non-ionic surfactant is at least one selected from a group consisting of Polyoxyethylene(8) isooctylphenyl ether, Nonylphenol polyethylene glycol ether, Polyoxyethylene(9) nonylphenyl ether, PoIyoxyethylene(lO) isooctylphenyl ether, Polyoxyethylene(12) nonylphenyl ether, Polyoxyethylene(12) isooctylphenyl ether, Polyoxyethylene(40) nonylphenyl ether, Polyoxyethylene(40) isooctylphenyl ether, Polyoxyethylene(lOO) nonylphenyl ether, Polyoxyethylene(150) dinonylphenyl ether, Surfonic N-95(Poly (oxy-1, 2-ethanediyl), alpha- (nonyl phenyl)-omega- hydroxyl-glycol ether) ( nonylphenol 9.5-mole ethoxylate) , Surfonic N-95(Poly (oxy-1, 2-ethanediyl), alpha- (nonyl phenyl)-omega-hydroxyl-glycol ether) ( nonylphenol 9.5-mole ethoxylate) , Surfonic N-120(nonylphenol 12-mole ethoxylate), Surfonic N-150 (nonylphenol 15-mole ethoxylate), Surfonic N-200 (nonylphenol 20-mole ethoxylate) , Surfonic N-300( nonylphenol 30-mole ethoxylate) , Surfonic N-400 nonylphenol 40-mole ethoxylate, Surfonic LF-7 (Alkyl polyoxyalkylene ether) , Surfonic LF-17 (ethoxylated and propoxylated linear primary 12-14 carbon number alcohol), Igepal CO-630 (nonylphenoxy poly(ethyleneoxy)ethanol,branched), Surfonic DNP-40 (dinonylphenol ethoxylate glycol ether). In accordance with one preferred embodiment of the invention, the HLB value of the surfactant is between 16 and 40. 9 In accordance with one aspect of the invention, the thermoregulatory constituent, the solvent and the surfactant are processed to form micro-reservoirs which are embedded into the body of the formulation. Typically, the average mean size of the micro-reservoir is in the range of 5 nm to 2000 nm. The invention also extends to a thermoregulatory lyocell fiber, yarn and fabric manufactured from a formulation in accordance with this invention. In accordance with this invention there is also provided a process for preparation of a thermoregulatory lyocell formulation meant for manufacture of lyocell products comprising the following steps: • heating water-insoluble thermoregulatory constituent with a non-aqueous solvent followed by heating the resulting mixture between 25°C and 95°C to obtain a non-aqueous phase ; • dissolving and stirring a surfactant, optionally with a co-surfactant, in water to obtain an aqueous phase; • heating the aqueous-phase; • mixing the aqueous phase with the non-aqueous phase in the liquid state to form a admixture and homogenizing to obtain a micro-emulsion; • mixing together cellulosic pulp and NNMO solution to form a slurry; • dispersing the micro-emulsion in the slurry to obtain a preform mass wherein the thermoregulatory constituent is in the form of evenly dispersed micro-reservoirs; 10 • vaccumising the preform mass to remove water under 7 to 10 mm of Hg and temperature of over 90°C to obtain the formulation. Typically, the pH of the aqueous phase is in the range of 7 to 13. Typically, the amount of non-aqueous phase in the micro-emulsion is in the range of 0.1 to 40% of the mass of the micro-emulsion. Typically, the amount of surfactant in the micro-emulsion is in the range of 0.1 to 20% of the mass of the micro-emulsion. Typically, the proportion of thermoregulatory constituent in the lyocell product is in the range of 0.01 to 50% with respect to the mass of the lyocell product. Brief Description of the accompanying Drawings: The invention will be described in detail with reference to the accompanying drawings. In the accompanying drawing, Figure 1 illustrates the block diagram showing the method steps involved in the process in accordance with this invention. Figure 2 illustrates the cross-sectional view of thermoregulatory lyocell fibers prepared in accordance with this invention which shows uniform distribution of micro-reservoirs of thermoregulatory constituents entrapped across the length of the fibers. Detailed Description: 11 Lyocell fibers were the first viable manufactured fibers. The reason behind the most widespread use of these fibers lies in their versatility. Furthermore, these fibers also have peculiar ability to blend easily with many fibers which makes them the fibers of choice. Though fibers and fabrics made from them have many desirable properties, oftentimes, consumers expect performance characteristics beyond those for which fibers were designed. In order to meet with these increasing expectations, various thermoregulatory constituents are incorporated in the lyocell fibers. There has been a considerable interest in developing such materials. One of the additional desirable properties of lyocell fibers which has enormous demand is "thermoregulatory activity". Thermoregulatory constituents improve the thermal insulation of the lyocell fibers during changes in environmental temperature conditions. Thermoregulatory constituents are phase change materials which improve the thermal performance of clothing by absorbing or releasing heat when subjected to heating or cooling during a phase change. Thermoregulatory lyocell product abates the transient effect on a human body's heat loss when the person wearing such fabric is exposed to temperature swings resulting from change in environmental conditions. Typically, the thermoregulatory constituent is at least one selected from a group consisting of nonadecane, eicosane, heptadecane, octadecane, pentadecane, hexadecane and other saturated hydrocarbons, decyl alcohol, lauryl alcohol and myristyl alcohol and other aliphatic alcohols. 12 Thermoregulatory ability of the thermoregulatory constituents is governed by several factors which include melting point, quantity of the thermoregulatory constituent in the fabric, different combinations and proportions in which the thermoregulatory constituents are blended together, type of the polymer used in the fabric, thickness of the fabric, distribution of the thermoregulatory constituent in the fabric, and the process used for incorporating the thermoregulatory constituent in the fabric. Physicochemical characteristics of the thermoregulatory constituents that used, are provided herein below: Nonadecane:(Molecular formula: C19H40, CAS No: 629-92-5 EC No: 211-116-8 ) Appearance: white crystalline solid Melting point: 32 - 34 C Boiling point: 330 C Flashpoint: 168 C Eicosane (Molecular formula: C20H42 CAS No: 112-95-8 EINECS No: 204-018-1 Appearance: colourless crystals or wax-like solid Melting point: 36.7 C Boiling point: 342.7 C Heptadecane (n-heptadecane )Molecular formula: C17H36 CAS No: 629-78-7 EC No: 211-108-4 Appearance; colourless liquid or white solid Melting point: 21 C Boiling point: 302 C 13 Flash point: 148 C (closed cup) Octadecane Molecular formula: C18H38, CAS No: 593-45-3 EINECS No: 209-790-3 Appearance: white crystals or powder Melting point: 28-30 C Boiling point: 317 C Flashpoint: 165 C Myristyl alcohol: (Molecular formula: C]4H3oO)CASNo: 112-72-1, 27196-00-5 EC No: 204-000-3, 248-318-0 Appearance: white crystalline semi-solid Melting point37 - 39 C Boiling point: 277-288 C Flashpoint: 145 C Specific thermoformable properties of the fabric with respect to the desired temperature zones are adjusted by careful blend of the thermoregulatory constituents in specific proportions. The thermoregulatory constituent is selected such that it has a melting point that falls within the range of temperature in which thermal regulation is desired to be achieved. Thus, if thermal regulation is desired in the range of 21 -30 °C, then the melting point of the thermoregulatory constituent must fall within this range. Again if the fabric is to be used in climatic regions, where regulation is desired below 20 °C, then the thermoregulatory constituent having melting point below 20 °C is used. The thermoregulatory lyocell fabric acts as a transient thermal barrier by protecting the wearer of this fabric from the effects of cold or hot environments. When such thermoregulatory lyocell fabric is subjected to heating from the sun or a hot 14 environment, it will absorb transient heat as it changes phase from solid to liquid, and it will prevent the temperature of the fabric from rising by keeping it constant at the melting point temperature of the thermoregulatory constituent. Once thermoregulatory constituent has completely melted, its transient effect will cease and the temperature of the fabric will rise. In a similar manner, when a thermoregulatory fabric is subjected to a cold environment where the temperature is below its crystallization point, it will interrupt the cooling effect of the fabric structure by changing phase from liquid to solid, and the temperature of fabric will be kept constant at the crystallization point. Once all the thermoregulatory constituents have crystallized, the fabric temperature will drop, and the thermoregulatory constituents will have no effect on the fabric's thermal performance. Thus, the thermal performance of a thermoregulatory constituent is a function of phase change temperature, the amount of thermoregulatory constituent and the amount of energy it absorbs or releases during a phase change. In accordance with this invention there is provided a thermoregulatory lyocell formulation meant for manufacture of lyocell products comprising : ■ at least one non-water-soluble thermoregulatory constituent having a melting point lying in a predetermined range of temperature said constituent being in the range of about 0.01 to 20% of the mass of the formulation, ■ at least one water soluble non-cationic surfactant having HLB value in the range of 9 to 40, in the range of range of 0.001 to 10% of the mass of the formulation, ■ cellulosic pulp in the range of about 3% to 35% of the mass of the formulation 15 ■ NNMO in the range of about 60 to 80% of the mass of the formulation; and ■ water in the range of about 0% to 20 % with respect to the mass of the formulation. In accordance with the invention, thermoregulatory constituent is typically at least one selected from a group consisting of nonadecane, eicosane, heptadecane, octadecane and other satirdated hydrocarbons, myristyl alcohol and other aliphatic alcohols. The thermoregulatory constituent impart thermoregulation property to the fibers and ultimately to the fabric or garments made from these fibers. In accordance with this invention only water soluble non-ionic or anionic surfactant/co-surfactant is used. Typically, the non-ionic surfactant is selected from a group consisting of alkyl phenoxy ethoxylated non-ionic surfactants and ethoxylated alkyl alcohol surfactants, Polyethylene-block-Poly propylene glycol-block-polyethylene glycol and Ethylenediamine tetrakis(propylene oxide- block-ethyl ene oxide) tetrol. Typically, the alkyl phenoxy ethoxylated non-ionic surfactant is at least one selected from a group consisting of Polyoxyethylene(S) isooctylphenyl ether, Nonylphenol polyethylene glycol ether, Polyoxyethylene(9) nonylphenyl ether, Polyoxyethylene(lO) isooctylphenyl ether, Polyoxyethylene(12) nonylphenyl ether, Polyoxyethylene(12) isooctylphenyl ether, Polyoxyethylene(40) nonylphenyl ether, Polyoxyethylene(40) isooctylphenyl ether, Polyoxyethylene(lOO) nonylphenyl ether, Polyoxyethylene(150) dinonylphenyl ether, Surfonic N-95(Poly (oxy-1, 2-ethanediyl), alpha- (nonyl phenyl)-omega-hydroxyl-glycol ether) ( nonylphenol 9.5-mole ethoxylate) , Surfonic N-95(Poly (oxy-1, 2-ethanediyl), alpha- (nonyl phenyl)-omega-hydroxyl-glycol ether) ( nonylphenol 16 9.5-mole ethoxylate) , Surfonic N-120(nonyIphenol 12-mole ethoxylate) , Surfonic N-150 (nonylphenol 15-mole ethoxylate), Surfonic N-200 (nonylphenol 20-mole ethoxylate) , Surfonic N-300( nonylphenol 30-mole ethoxylate) , Surfonic N-400 nonylphenol 40-mole ethoxylate, Surfonic LF-7 (Alkyl polyoxyalkylene ether) , Surfonic LF-17 (ethoxylated and propoxylated linear primary 12-14 carbon number alcohol), Igepal CO-630 (nonylphenoxy poly(ethyleneoxy)ethanol,branched), Surfonic DNP-40 (dinonylphenol ethoxylate glycol ether). The non-ionic surfactant is selected such that the lipophilic portion of the non-ionic surfactant is compatible with the thermoregulatory constituent and the surfactant forms oil in water microemulsion. Surfactants with HLB values within the range of 9 to 40 are used. Preferably, non-ionic surfactants with HLB values more than 13 are used. In accordance with one preferred embodiment of the invention, the HLB value of the surfactant is between 16 and 40. In accordance with one aspect of the invention, the thermoregulatory constituent, the solvent and the surfactant are processed to form micro-reservoirs which are embedded into the body of the formulation. The thermoregulatory lyocell contains uniformly dispersed micro-reservoirs throughout the body of the fibers. The micro-reservoirs are discrete, nano-sized structures without any definite geometrical shape. Typically, the average mean size of the micro-reservoir is in the range of 5 nm to 2000 nm. 17 The invention also extends to a thermoregulatory lyocell fiber, yarn and fabric manufactured from a formulation in accordance with this invention. In accordance with this invention there is also provided a process for preparation of a thermoregulatory lyocell formulation meant for manufacture of lyocell products comprising the following steps: • heating a water-insoluble thermoregulatory constituent between 25°C and 95°C to obtain non-aqueous phase ; • dissolving and stirring a surfactant, optionally with a co-surfactant, in water to obtain an aqueous phase; • heating the aqueous-phase; • mixing the aqueous phase with the non-aqueous phase in the liquid state to form a admixture and homogenizing to obtain a micro-emulsion; • mixing together cellulosic pulp and NNMO solution to form a slurry; • dispersing the micro-emulsion in the slurry to obtain a preform mass wherein the thermoregulatory constituent is in the form of evenly dispersed micro-reservoirs; • vaccumising the preform mass to remove water under 7 to 10 mm of Hg. Typically, the pH of the aqueous phase is in the range of 7 to 13. Typically, the amount of non-aqueous phase in the micro-emulsion is in the range of 0.1 to 40% of the mass of the micro-emulsion. Typically, the amount of surfactant in the micro-emulsion is in the range of 0.1 to 20% of the mass of the micro-emulsion. .18 Typically, the proportion of thermoregulatory constituent in the lyocell product is in the range of 0.01 to 50% with respect to the mass of the lyocell product. Before arriving at the optimum concentration of the surfactant to be used, cloud point of the aqueous phase is determined. Typically, the melted non-aqueous phase containing thermoregulatory constituent in a non-aqueous solvent along with aqueous phase containing surfactants is emulsified using high speed mixers such as Ultraturrex or a mechanical emulsifier; a colloid mill; a high pressure homogenizer and an ultrasonic emulsifier to form a microemulsion. The micro-emulsion may contain further additional thermoregulatory constituents, if desired. The active ingredients are released from the micro-reservoir into the lyocell matrix. The structure of micro-reservoir, lyocell and surrounding conditions determine the release rate of the thermoregulatory constituent. The molecules of the volatile thermoregulatory constituents migrate from micro-reservoirs to the surrounding primarily by diffusion. The thermoregulatory constituent is released from the matrix in a controlled release manner. Conventional method for manufacture of lyocell involves following major steps: Step 1. Creating a solvent solution from wood pulp The wood pulp is obtained from a variety of sources, such as wood chips or even large rolls of paper that have been finely shredded, is the basic starting material for manufacture of lyocell fibers. In case of manufacture of lyocell no further 19 chemical treatment of the wood pulp is needed thereby making the process environment friendly. The wood pulp solution is produced in a straight solvation process by dissolving wood pulp at high temperatures and pressure in a recyclable non-toxic organic solvent solution of amine oxide, particularly N-methylmorpholine N-oxide,(NNMO). Lyocell is manufactured by a "closed loop" spinning process which conserves energy and water. Step 2. Spinning lyocell fiber from the solvent solution Before being formed into fibers, the lyocell polymer dope, is in a thick liquid state. In the spinning process this liquid is forced through a spinneret, which resembles a large shower head. The clear, viscous resultant solution is filtered and extruded into an aqueous bath of dilute amine oxide, and coagulated into fiber form. Step 3. Washing lyocell fiber to remove solvents The fiber is then washed before it is dried and twisted or spun into yarns, which are woven or knitted into fabrics and garments. Step 4. Drying fiber and producing yarns When the filament dries or solidifies, it forms what is called a continuous filament fiber. Many continuous filaments of specific thicknesses collected in a large bundle called a "tow". A tow may contain over a million continuous 20 filaments. The tow bundle is then crimped, is then mechanically cut into staple fibers, usually ranging in length from 1 to 6-1/2 inches, depending how they are to be used. Strands of continuous filament fibers are then twisted together to form a continuous filament yarn, which is then woven or knit into fabric. Step 5. Finishing to produce lyocell fabric The fabric is treated with an enzyme that attacks cellulose fibers. Home laundry detergents containing such enzymes are also used for treatment of the fabric for better finishing purposes. This enzyme dissolves the split-end hairs from the fiber surface. The fiber is then washed and agitated again. The resulting fabric is similar in texture and drape to sueded silk or sueded rayon found in fashion apparel. Fabrics processed this way can usually be machine washed and line dried successfully. Alternatively, the filaments so obtained are stretched to straighten out the fibers which are further blended using standard equipment. The blended fibers are laid in to a web followed by Consolidation of the web to obtain Non-woven Lyocell Fabric. The lyocell product made from the formulation in accordance with this invention contains uniformly dispersed micro-reservoirs throughout the mass which is shown in Fig. 2. 21 The thermoregulatory lyocell fibers contain the entrapped thermoregulatory constituent in releasable form. Microscopic examination of the micro-reservoirs in the lyocell fibers is shown in Fig 2. Thermoregulatory fabric improves the comfort of people irrespective of the fluctuations in the temperature of their surroundings on either side. Besides this, thermoregulatory fabric also improves the comfort of people as their body goes through a very active state (high metabolic production) to an inactive state on an intermittent basis in a cold environment. This feature is of particular relevance for outdoor sportsmen. The resultant lyocell fabric containing thermoregulatory constituent are tested. Linear Density (Denier) of the lyocell Fibers is determined by using standard ASTM Test Method (D 1577). The denier of the standard lyocell fiber (lyocell fiber without any thermoregulatory constituents) and anti-microbial enriched lyocell fiber remains the same. Thus addition of thermoregulatory constituents does not change the linear density of the lyocell fibers. Tensile strength and Young's modulus of lyocell fiber sample is tested on an Instron tensile testing machine as per the ASTM C1557-03 procedure at ambient temperature. Visual appearance of the thermoregulatory enriched fiber is evaluated by methods as prescribed in AATCC 124. As far as parameters like % Loss in Dry Tenacity and % loss in dry elongation are concerned, these remain the same in the thermoregulatory enriched lyocell fiber and the standard fiber. Incorporation of thermoregulatory constituent in accordance with this invention does not affect the visual appearance of the fiber. 22 Feel of the fiber: The thermoregulatory enriched lyocell fiber as prepared in accordance with this invention offers the same feel effect as is observed in case of plain lyocell fiber without any thermoregulatory constituent (Also referred as standard). Another important concern in textile industry is dye-ability of the fabric, which is tested by comparing the dyeability of the thermoregulatory constituent enriched fabric and the standard lyocell fabric. Dyeability of the thermoregulatory enriched lyocell fibers as prepared in accordance with this invention remains the same as that of the standard lyocell fiber. The invention will now be described with the help of the following non-limiting examples. Examples Example 1 Example 1A- Preparation of micro emulsion Myristyl alcohol (50gm) was heated until it melts to form a molten liquid. Surfonic N-400 nonylphenol 40-mole ethoxylate (surfactant) ( 5.6gm ) was dissolved and stirred in water 105ml to obtain 110.6gm of aqueous phase. The aqueous phase (110.6gm) and the molten liquid (50 gm) were homogenized in a high speed mixer (Ultraturrex) to obtain a micro-emulsion (160.6 gm ). Example 1 B- Preparation fiber and fabric Cellulosic pulp (839.4 gm) and 10600 gm of 50% NNMO solution were mixed to form lyocell slurry. The micro-emulsion as prepared in Example 1A was evenly dispersed in the slurry to obtain a preform mass. The homogenized preform mass was vaccumisied to remove water under 10 mm of Hg and at 23 temperature 110 °C to give Lyocell polymer dope (839.4 gm). The lyocell polymer dope was further spun in a spin bath of dilute NNMO solution, and coagulated into fiber form. The filaments so obtained were washed in water and dried at 100°C. The lyocell fiber thus obtained contained micro-reservoirs having the entrapped releasable thermoregulatory constituents. Although the micro reservoirs did not have any specific shape or size, they were found to be uniformly distributed throughout the body of the fiber. Example 2 Example 2A Preparation of micro emulsion Cetyl alcohol(50gm) was heated to from a molten liquid. Surfonic N-150 (nonylphenol 15-mole ethoxylate) (surfactant) (16.8 gm ) was dissolved and stirred in water 111.1ml to obtain 127. 9gm of clear aqueous phase The aqueous phase(127. 9gm ) and the molten liquid (50 gm) were homogenized in a high speed mixer (Ultraturrex) to obtain an thermoregulatory formulation in the form of micro-emulsion. (177.9 gm ) Example 2 B The micro-emulsion as prepared in Example 2A was added to lyocell slurry, vacuumised at high temperature to give lyocell Polymer Dope (containing 822. lgm cellulose) and was spun or extruded into various forms such as fiber or 24 film or cast into various shapes using the regeneration media as described in example 1. Example 3 Example 3 A Heptadecane (50gm) was heated to from a molten liquid. Surfonic N-150 (nonylphenol 15-mole ethoxylate) (surfactant) (16.8 gm ) was dissolved and stirred in water 111.1ml to obtain 127. 9gm of clear aqueous phase The aqueous phase(127. 9gm ) and the nolten liquid (50 gm) were homogenized in a high speed mixer (Ultraturrex) to obtain an thermoregulatory formulation in the form of micro-emulsion. (177.9 gm ) Example 3 B The micro-emulsion as prepared in Example 2A was added to lyocell slurry, vacuumised at high temperature to give lyocell Polymer Dope (contaiing 822.1 gm cellulose) and was spun or extruded into various forms such as fiber or film or cast into various shapes using the regeneration media as described in example 1. Example 4 Example 4 A Preparation of thermoregulatory formulation Heptadecane (35gm) myristyl alcohol (15gm) was heated to form a molten liquid. Surfonic N-30Q( nonylphenol 30-mole ethoxylate) (surfactant) (5.6gm) 25 was dissolved and stirred in water (105ml) to obtain 110.6 gm of clear aqueous phase The aqueous phase(110.6gm) and the molten liquid ( 50 gm) were homogenized in a high speed mixer (Ultraturrex) to obtain a micro-emulsion. Example 4 B The micro-emulsion as prepared in Example 4A was added to lyocell slurry, vacuumised at high temperature to give lyocell Polymer Dope (containing 839.4 gm cellulose) and was spun or extruded into various forms such as fiber or film or cast into various shapes using the regeneration media as described in example 1. Example 5 Example 5A Preparation of thermoregulatory formulation Nonadecane (750 gm) was heated to form a molten liquid. Surfonic N-200 (nonylphenol 20-mole ethoxylate) (surfactant) (50.4gm) was dissolved and stirred in water (1500ml) to obtain 1550 gm of clear aqueous phase The aqueous phase (1550 gm) and the molten liquid ( 750 gm) were homogenized in a high speed mixer (Ultraturrex) to obtain a micro-emulsion.(2.3kg) Example 5 B The micro-emulsion as prepared in Example 5A was added to lyocell slurry, vacuumised at high temperature to give lyocell Polymer Dope (containing 1.866Kg cellulose) and was spun or extruded into various forms such as fiber or 26 film or cast into various shapes using the regeneration media as described in example 1. Example 6 Example 6 A Preparation of thermoregulatory formulation Nonadecane (50gm) was melted to form a molten liquid. Surfonic N-200 (nonylphenol 20-mole ethoxylate) (surfactant) (11.2gm) was dissolved and stirred in water 210ml to obtain 221.2gm of clear aqueous phase. The aqueous phase(221.2gm) and the mixture lOOgm were homogenized in a high speed mixer (Ultraturrex) to obtain a micro-emulsion. (271.2gm) Example 6 B The micro-emulsion as prepared in Example 6A was added to lyocell slurry, vacuumised at high temperature to give lyocell Polymer Dope (containing 1.678Kg cellulose) and was spun or extruded into various forms such as fiber or film or cast into various shapes using the regeneration media as described in example 1. Example 7 Example 7 A Preparation of thermoregulatory formulation Eicosane 50 gm was melted to form a molten liquid. Surfonic N-300( nonylphenol 30-mole ethoxylate) (surfactant) (16.8gm) was dissolved and "*red in water 111.1ml to obtain 127.9gm of clear aqueous phase '^pus phase (127.9gm ) and the mixture 50gm were homogenized in a "xer (Ultraturrex) to obtain a micro-emulsion. (177.9gm ) 27 Example 7 B The micro-emulsion as prepared in Example 7 A was added to lyocell slurry, vacuumised at high temperature to give lyocell Polymer Dope (containing 822.1 gm cellulose) and was spun or extruded into various forms such as fiber or film or cast into various shapes using the regeneration media as described in example 1. Example 8 Example 8 A Preparation of thermoregulatory formulation Eicosane (25gm) and Nonadecane (25gm) were melted together to form a molten liquid. Surfonic N-300( nonylphenol 30-mole ethoxylate) (surfactant) (5.6 gm) was dissolved and stirred in water (105ml) to obtain (110.6 gm) of clear aqueous phase. The aqueous phase (110.6 gm) and the mixture (50 gm) were homogenized in a high speed mixer (Ultraturrex) to obtain a micro-emulsion. (160.6gm) Example 8 B The micro-emulsion as prepared in Example 8A was added to lyocell slurry, vacuumised at high temperature to give lyocell Polymer Dope (containing 839.4gm cellulose) and was spun or extruded into various forms such as fiber or film or cast into various shapes using the regeneration media as described in example 1. Example 9 Example 9A Preparation of micro emulsion 28 Nonadecane (50gm) was heated until it melts to form a molten liquid. Surfonic N-400 nonylphenol 40-mole ethoxylate (surfactant) ( 5.6gm ) was dissolved and stirred in water 105ml to obtain 110.6gm of aqueous phase. The aqueous phase (110.6gm) and the molten liquid (50 gm) were homogenized in a high speed mixer (Ultraturrex) to obtain a micro-emulsion (160.6 gm ). Example 9 B- Preparation fiber and fabric The micro-emulsion as prepared in Example 1A was added to lyocell slurry, vacuumised at high temperature to give lyocell Polymer Dope containing 839.4 gm cellulose and the resulting thermoregulatory enriched lyocell polymer dope was homogenized. The homogenized lyocell polymer dope and was spun or extruded into various forms such as fiber or film or cast into various shapes using the regeneration media as described in example 1. Example 10 Example 10 A Preparation of micro emulsion Myristyl alcohol (50gm ) was heated to from a molten liquid. Surfonic N-150 (nonylphenol 15-mole ethoxylate) (surfactant) (16.8 gm ) was dissolved and stirred in water 111.1ml to obtain 127. 9gm of clear aqueous phase The aqueous phase(127. 9gm ) and the molten liquid (50 gm) were homogenized in a high speed mixer (Ultraturrex) to obtain an thermoregulatory formulation . in the form of micro-emulsion. (177.9 gm ) Example 10 B 29 The micro-emulsion as prepared in Example 2A was added to lyocell slurry, vacuumised at high temperature to give lyocell Polymer Dope (containing 822. lgm cellulose) and was spun or extruded into various forms such as fiber or film or cast into various shapes using the regeneration media as described in example 1. Example 11 Example 11 A Eicosane(50gm ) was heated to from a molten liquid. Surfonic N-150 (nonylphenol 15-mole ethoxylate) (surfactant) (16.8 gm ) was dissolved and stirred in water 111.1ml to obtain 127. 9gm of clear aqueous phase The aqueous phase(127. 9gm ) and the molten liquid (50 gm) were homogenized in a high speed mixer (Ultraturrex) to obtain an thermoregulatory formulation in the form of micro-emulsion. (177.9 gm ) Example 11 B The micro-emulsion as prepared in Example 2A was added to lyocell slurry, vacuumised at high temperature to give lyocell Polymer Dope (containing 822.lgm cellulose) and was spun or extruded into various forms such as fiber or film or cast into various shapes using the regeneration media as described in example 1. Example 12 Example 12 A Preparation of thermoregulatory formulation 30 Heptadecane (50gm) was heated to form a molten liquid. Surfonic N-300( nonylphenol 30-mole ethoxylate) (surfactant) (5.6gm) was dissolved and stirred in water (105ml) to obtain 110.6 gm of clear aqueous phase The aqueous phase(l 10.6gm) and the molten liquid ( 50 gm) were homogenized in a high speed mixer (Ultraturrex) to obtain a micro-emulsion. Example 12 B The micro-emulsion as prepared in Example 4A was added to lyocell slurry, vacuumised at high temperature to give lyocell Polymer Dope (containing 839.4 gm cellulose) and was spun or extruded into various forms such as fiber or film or cast into various shapes using the regeneration media as described in example 1. Example 13 Example 13A Preparation of thermoregulatory formulation Nonadecane (500 gm) and hectadecane(250) were heated to form a molten liquid. Surfonic N-200 (nonylphenol 20-mole ethoxylate) (surfactant) (50.4gm) was dissolved and stirred in water (1500ml) to obtain 1550.4 gm of clear aqueous phase The aqueous phase(1550gm) and the molten liquid ( 750 gm) were homogenized in a high speed mixer (Ultraturrex) to obtain a micro- emulsion.(2.3kg) Example 13 B The micro-emulsion as prepared in Example 5A was added to lyocell slurry, vacuumised at high ■ temperature to give lyocell Polymer Dope (containing 31 1.866Kg cellulose) and was spun or extruded into various forms such as fiber or film or cast into various shapes using the regeneration media as described in example 1. Example 14 Example 14 A Preparation of thermoregulatory formulation Nonadecane (40gm) and heptadecane (10)gm were melted to form a molten liquid. Surfonic N-200 (nonylphenol 20-mole ethoxylate) (surfactant) (11.2gm) was dissolved and stirred in water 210ml to obtain 221.2gm of clear aqueous phase. The aqueous phase(221.2gm) and the mixture lOOgm were homogenized in a highspeed mixer (Ultraturrex) to obtain a micro-emulsion. (321.2gm ) Example 14 B The micro-emulsion as prepared in Example 6A was added to lyocell slurry, vacuumised at high temperature to give lyocell Polymer Dope (containing 1.678Kg cellulose ) and was spun or extruded into various forms such as fiber or film or cast into various shapes using the regeneration media as described in example 1. Example 15 Example 15 A Preparation of thermoregulatory formulation Myristyl alcohol (30gm ) and heptadecane(20gm) were melted to form a molten liquid. Surfonic N-300( nonylphenol 30-mole ethoxylate) (surfactant) (16.8gm) 32 was dissolved and stirred in water 111.1ml to obtain 127.9gm of clear aqueous phase The aqueous phase (127.9gm ) and the mixture 50gm were homogenized in a high speed mixer (Ultraturrex) to obtain a micro-emulsion. (177.9gm) Example 15 B The micro-emulsion as prepared in Example 7A was added to lyocell slurry, vacuumised at high temperature to give lyocell Polymer Dope (contaiing 822.1 gm cellulose) and was spun or extruded into various forms such as fiber or film or cast into various shapes using the regeneration media as described in example 1. Example 16 Example 16 A Preparation of thermoregulatory formulation Eicosane (25gm) and Hectadecane (25gm) were melted together to form a molten liquid. Surfonic N-300( nonylphenol 30-mole ethoxylate) (surfactant) (5.6 gm) was dissolved and stirred in water (105ml) to obtain (110.6 gm) of clear aqueous phase. The aqueous phase (110.6 gm) and the mixture (50 gm) were homogenized in a high speed mixer (Ultraturrex) to obtain a micro-emulsion. (160.6gm ) Example 16 B The micro-emulsion as prepared in Example 8A was added to lyocell slurry, vacuumised at high temperature to give lyocell Polymer Dope (containing 839.4gm celllulosej and was spun or extruded into various forms such as fiber 33 or film or cast into various shapes using the regeneration media as described in example 1. Testing procedures: The thermoregulatory lyocell products as prepared in the above examples (1 to 10) were tested by using following test procedures: 1) Linear Density (Denier) of the lyocell Fibers was determined by using standard ASTM Test Method (D 1577). The denier of the standard lyocell fiber (without any thermoregulatory constituents) and anti-microbial lyocell fibers as prepared in accordance with example IB was found to be uniform(1.5 denier) irrespective of the type and quantity of the thermoregulatory constituent. 2) Tensile strength and Young's modulus of lyocell fiber samples were tested on an Instron tensile testing machine as per the ASTM CI557-03 procedure at ambient temperature. 3) Emulsion stability: The stability of micro-emulsions as prepared in the above examples, was evaluated by keeping the same under observation in measuring cylinders for 3 days. During this period no phase separation was observed. 4) Feel of the fabric: The lyocell fabrics as prepared in the above examples and standard fabric (lyocell fabric without thermoregulatory constituents), were randomly given to twenty subjects and they were asked to evaluate the texture and feel of the fiber. The test fiber material was interchanged several times amongst the human subjects. Collective results as submitted by the human subjects confirmed that nobody could distinguish between the 34 thermoregulatory lyocell fabrics prepared in accordance with the Examples provided above and the standard fabric. 5) Dyeability: The thermoregulatory lyocell fabrics as prepared in the above examples and the standard fabric as described above were dyed uniformly with reactive dyes. No noticeable difference as to the Dyeability of the two respective lyocell fabrics, with and without thermoregulatory constituent was reported. 6) Visual appearance of the thermoregulatory lyocell fiber was evaluated by methods as prescribed in AATCC 124. As far as parameters like % Loss in Dry Tenacity and % loss in dry elongation are concerned, these remained the same( lyocell fiber and the standard fiber 7) Determination of enthalpy of the fabric specimen: the thermoregulatory properties of the specimen fabrics/fibers as prepared in examples 1 to 10 were evaluated by measuring respective enthalpies of the specimen. The enthalpies were measured using DSC(Differential scanning calorimetry) technique. The recorded enthalpies of the fiber and fabric obtained in examples 1 to 10 are provided in the Table 1. 35 Table 1 Specimen No. enthalpy J/g Fiber enthalpy J/g Fabric 1 4.3 4.29 2 5.4 5.38 3 6.6 6.63 4 6 5.98 5 37 36.3 6 4.3 4.1 7 8.4 8.41 8 7.2 7.19 9 6.5 6.4 10 5.2 5.24 11 8.4 8.35 12 6.5 6.55 13 34.1 34.6 14 3.1 3.0 15 5.5 5.6 16 6.5 6.5 8. Thermoregulatory testing: Free flowing robes made to fit the physique of twenty human volunteers, selected at random between ages 16 to 56, were made from undyed 36 thermoregulatory Lyocell fabric prepared in accordance with this invention. Simultaneously, identical robes with same design weer also made from undyed standard fabric (Lyocell fabric without any thermo regulatory constituents). A temperature monitored room was selected where the temperature could be precisely controlled. The temperature in the room was set at 21°C. The twenty human volunteers were requested to wear the robes and assemble in the room and be there in the room for a period of 30 min. They were made to randomly wear either a standard robe (robe made from standard fabric) or a robe made from the fabric of this invention. But they were not informed about the type of the robe that was being worn. After 30 minutes, a\\ the volunteers were asked to step out into the outside non-air-conditioned environment, where the tempreature was 280c and they were asked to abserve and note the time where they felt warm in the area covered by the robe. Thereafter, all the volunteers switched their robes, ie: The volunteer given a robe of standard fabric, was allotted a robe made from the fabric of this invention and vise-a-versa. They were again asked to go back irto the room and remain there for 30 min. and again step out into the external environment and again observe and note the time when they started feeling warm. The volunteers were then asked to give an evaluation of the time required to feel the warmth in both the instances. The results of the experiments were as follows. Seventeen volunteers opined that they felt warm in the standard fabric, at least on an average of 3 minutes quicker than the fabric of this invention. Two volunteers could not sense significant difference in time and one volunteer recorded an earlier feeling of warmth in case of the fabric of this invention. 37 In case of direct comparison between the robes, 17 volunteers opined that they felt cooler and more comfortable wearing a ward-robe made from the fabric of this invention. Three volunteers expressed no significant difference between the two. There was no volunteer who provided any reverse finding. Similar test was conducted in which the volunteers were made to go from a hotter external environment at 30 C to an air-conditioned environment maintained at 21 C. All of the volunteers expressed that they felt warmer and more comfortable in the robe made from the fabric of this invention and the reported response time for feeling cold was on an average 3 min. longer. It is thus concluded that the fabric made in accordance with this invention exhibits thermoregulatory effect in either situation, ie when there is a rise in temperature and when there is a fall in the temperature. While considerable emphasis has been placed herein on the specific steps of the preferred embodiment, it will be appreciated that many alterations can be made and that many modifications can be made in the preferred embodiment without departing from the principles of the invention. These and other changes in the preferred embodiment as well as other embodiments of the invention will be apparent to those skilled in the art from the disclosure herein, whereby it is to be distinctly understood that the foregoing descriptive matter is to be interpreted merely as illustrative of the invention and not as a limitation. 38 We Claim-. 1. A thermoregulatory lyocell formulation meant for manufacture of lyocell products comprising : ■ at least one non-water-soluble thermoregulatory constituent having a melting point lying in a predetermined range of temperature said constituent being in the range of about 0.01 to 20% of the mass of the formulation, ■ at least one water soluble non-cationic surfactant having HLB value in the range of 9 to 40, in the range of range of 0.001 to 10% of the mass of the formulation, ■ cellulosic pulp in the range of about 3% to 35% of the mass of the tbrmuiat'ibn ■ NNMO in the range of about 60 to 80% of the mass of the formulation; and ■ water in the range of about 0% to 20 % with respect to the mass of the formulation. 2. A formulation as claimed in claim 8, wherein the thermoregulatory constituent is at least one selected from a group consisting of nonadecane, eicosane, heptadecane, octadecane, pentadecane, hexadecane, decyl alcohol, lauryl alcohol and myristyl alcohol. 3. A formulation as claimed in claim 1, wherein the surfactant is at least one non-ionic surfactant selected from a group of non-ionic surfactants consisting of alkyl phenoxy ethoxylated non-ionic surfactants and ethoxylated alkyl alcohol, Polyethylene-block-Poly propylene glycol-block-polyethylene 39 glycol and Ethylenediamine tetrakis(propylene oxide-block-ethylene oxide) tetrol. A formulation as claimed in claim 8, wherein the alkyl phenoxy ethoxylated non-ionic surfactant is at least one selected from a group consisting of Polyoxyethylene(8) isooctylphenyl ether, Nonylphenol polyethylene glycol ether, Polyoxyethylene(9) nonylphenyl ether, Polyoxyethy lene(10) isooctylphenyl ether, Polyoxyethylene(12) nonylphenyl ether, Polyoxyethylene(12) isooctylphenyl ether, Polyoxyethylene(40) nonylphenyl ether, Polyoxyethylene(40) isooctylphenyl ether, Polyoxyethylene( 100) nonylphenyl ether, Polyoxyethylene(150) dinonylphenyl ether, Surfonic N- 95(Poly (oxy-1, 2-ethanediyl), alpha- (nonyl phenyl)-omega-hydroxyl-glycol ether) ( nonylphenol 9.5-mole ethoxylate) , Surfonic N-95(Poly (oxy-1, 2- ethanediyl), alpha- (nonyl phenyl)-omega-hydroxyl-glycol ether) ( nonylphenol 9.5-mole ethoxylate) , Surfonic N-120(nonylphenol 12-mole ethoxylate) , Surfonic N-150 (nonylphenol 15-mole ethoxylate), Surfonic N-200 (nonylphenol 20-mole ethoxylate) , Surfonic N-300( nonylphenol 30-mole ethoxylate) , Surfonic N-400 nonylphenol 40-mole ethoxylate, Surfonic LF-7 (Alkyl polyoxyalkylene ether) , Surfonic LF-17 (ethoxylated and propoxylated linear primary 12-14 carbon number alcohol), Igepal CO-630 (nonylphenoxy poly(ethyleneoxy)ethanoI,branched), Surfonic DNP-40 (dinonylphenol ethoxylate glycol ether). 4. A formulation as claimed in claim 1, wherein the preferred HLB value of the surfactant is between 16 and 40. 40 5. A formulation as claimed in claim 1, wherein the average mean size of the micro-reservoir is in the range of 5 nm to 2000 run. 6. A thermoregulatory lyocell fiber manufactured from a formulation as claimed in claim 1. 7. A thermoregulatory lyocell yarn manufactured from a formulation as claimed in claim 1. 8. A thermoregulatory lyocell fabric manufactured from a formulation as claimed in claim 1. 9. A process of preparation of a thermoregulatory lyocell formulation meant for manufacture of lyocell products comprising the following steps : • heating a water-insoluble thermoregulatory constituent between 25°C and 95°C to obtain a non-aqueous phase ; • dissolving and stirring a surfactant, optionally with a co-surfactant, in water to obtain an aqueous phase; • heating the aqueous-phase; • mixing the aqueous phase with the non-aqueous phase in the liquid state to form a admixture and homogenizing to obtain a micro-emulsion; • mixing together cellulosic pulp and NNMO solution to form a slurry; • dispersing the micro-emulsion in the slurry to obtain a preform mass wherein the antimicrobial constituent is in the form of evenly dispersed micro-reservoirs; 41 vaccumismg the preform mass to remove water under 7 to 10 mm of Hg and a temperature over 90°C to obtain the formulation. Dated this 3rd day of My, 2008. Mohan Dewan of R. K. Dewan and Co. Applicants' Patent Attorney 42

Full Text

FORM - 2
THE PATENTS ACT, 1970
(39 OF 1970)
AND
THE PATENTS RULES, 2003
COMPLETE SPECIFICATION (See section 10; rule 13)

A LYOCELL THERMOREGULATORY FIBER AND A METHOD OF
MAKING THEREOF
ADITYA BIRLA SCIENCE & TECHNOLOGY CO. LTD.
an Indian Company of Aditya Birla Center, 2nd floor, C Wing, S. K. Ahire Marg, Mumbai 400 025,
Maharashtra, India
THE FOLLOWING SPECIFICATION PARTICULARLY DESCRIBES THE INVENTION AND THE MANNER IN WHICH IT IS TO BE PERFORMED.

Field of the invention
The present invention relates to textile fibers.
Background of the invention
The term "fiber" or "textile fiber" means a substance which is capable of being spun into a yarn or made into a fabric by bonding or by interlacing in a variety of methods including weaving, knitting, braiding, felting, twisting, or webbing, and which is the basic structural element of textile products.
Fibers are classified on the basis of their length such as short fibers or staple fiber and long fibers or filament fiber. The fibers can also be classified on the basis of their origin such as natural fibers and man-made fibers. The term natural fibers means any fiber that exists as such in the natural state e.g. vegetable fibers or wood fibers. The other type of fibers is obtained from chemical substances. These are called man made fibers. They are rayon, polyester, nylon, acrylic (cashmilon) etc.
For centuries, mankind has relied upon various plants and animals to provide raw materials for fabrics and clothing. In recent times, the industrialization and scientific advancement has provided several improved materials having far superior properties, particularly suitable for clothing.
Lyocell is a manmade fiber derived from cellulose. Though it is related to rayon, lyocell is obtained by a solvent spinning technique. The solvent spinning technique, which is simpler and more environmentally sound, since it uses a non-toxic solvent chemical that can be recycled in the manufacturing process.
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It is an extremely strong fabric with industrial uses such as in automotive filters,
ropes, abrasive materials, bandages and protective suiting material. It is
primarily found in the garment industry, particularly in women's clothing.
Lyocell fibers are prepared by following process steps:
The raw cellulose is dissolved into heated, pressurized vessel filled with an
amine oxide solvent.
After soaking for a short time in the solvent at high temperature under vacuum
to remove excess water, the cellulose forms a clear solution and then it is
filtered.
The solution is then pumped through spinneret which is pierced with small holes
to obtain long strands of fibers. The fibers are then immersed in another dilute
solution of amine oxide. This helps to set the fiber strands. Then, they are
washed with de-mineralized water.
The lyocell fibers are then led to a drying area, where the water is evaporated
from it. The strands are led to a finishing area, where the lubricant is applied.
The dried, finished fibers are at this stage are called as a tow, which is a large
untwisted bundle of continuous length filaments. The bundles of tow are taken
to a crimper, a machine which compresses the fiber, giving it texture and bulk.
The crimped fiber is then carded by mechanical carders, which perform an
action like combing, to separate and order the strands. The carded strands are cut
and baled for shipment to a fabric mill.
The amine oxide used to dissolve the cellulose and set the fiber after spinning is
recovered and re-used in the manufacturing process.
From the spun or filament yarn, fabric is formed by knitting or weaving operations. Knitted fabrics can be made by using hooked needles to interlock one or more sets of yarns through a set of loops. The loops may be either loosely
3

or closely constructed, depending on the purpose of the fabric. Knitted fabrics can be used for hosiery, underwear, sweaters, slacks, suits, coats, rugs and other home furnishings. Knitting is performed using either weft or warp processes.
Some typical preparations that are involved in the weaving operations are warping, slashing or sizing. Sizing agents are added to the yarn by solution or pad/dry techniques. Differences in raw materials, processing chemicals, fiber diameter, post treatments and blend ratios can be manipulated to produce a fiber having customized properties suitable for desired application. It is often desired that the lyocell fabrics possess typical properties such as thermal stability, ability to retain perfumes, antibacterial properties and the like. These properties are essential in several industrial as well as household applications. There has been a considerable interest in developing such materials. In order to impart various desirable properties to the fabric as mentioned above to the fabric, several additives are added. Such additives include antimicrobial agents, deodorizing agents, antistatic agents, perfumes. Besides such specific additives, generic additives for improving overall quality of the fabric, such as sizing agents, additives for increasing yarn softness and pliability are also added.
Prior Art
WO2008030648 discloses a temperature regulating, polymer containing fabric and a suspension formulation used in preparation of such fibers. The suspension comprises a solvent and plurality of microcapsules containing phase-change material. The suspension is used for incorporating the microcapsules in the
4

fabric. The microcapsules comprise a shell composed of acrylic acid and their derivatives and a core which is composed of a phase change material having a latent heat in a range between 80 J/g and 400 J/gm and a transition temperature in the range of 20°C-50°C.
United States Patent Application no. 20070026228 discloses cellulosic fibers having enhanced reversible thermal properties and applications of such cellulosic fibers. The cellulosic fibers include a fiber body including a cellulosic material and a set of microcapsules dispersed in the cellulosic material. The set of microcapsules contain a phase change material having a latent heat of at least 40 J/g and a transition temperature in the range of 0°C-100°C. The phase change material provides thermal regulation based on absorption and release of the -latent .heat at the transition temperature. The cellulosic fibres are formed via a solution spinning process, and used in various products where thermal regulating properties are desired.
WO2003062513 discloses a sheath core type fiber and fabric having thermal storage and release characteristics and the method of manufacturing the fiber as well as fabric. The fiber includes mixture of first polymer and a thermal stabilizing material which forms the core of the fiber and a polymer sheath forms the exterior of fiber and surrounds the core. The core and sheath polymers are selected from polyolefins, polyamides, polyesters, elastomeric polymers and combinations thereof.
Earlier known processes of incorporating such additives, as reported in the above mentioned patents/applications, mainly involved conventional methods like spraying, encapsulating, solvent spinning the additives on the fabric.
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However, these methods suffer from several disadvantages which include non¬uniform and improper adhesion of additives onto the fiber material, fading, waning and gradual washing out of the additives over a period of time and which further affects the feel and texture of the fabric.
There is thus felt a need for a process of incorporating additives to fabric which overcomes these shortcomings.
Objects of the Invention
It is an object of this invention to provide thermoregulatory lyocell products, wherein at least one thermoregulatory constituent is incorporated into the body of the fiber.
Another object of this invention is to provide a process of incorporating thermoregulatory constituents into lyocell fibers which ensures uniform distribution of the thermoregulatory constituent throughout the fiber length.
Yet another object of this invention is to provide thermoregulatory lyocell fibers wherein the thermoregulatory constituents are retained in the lyocell product over a prolonged period of time.
Yet another object of this invention is to provide a process of incorporating thermoregulatory constituents to lyocell fibers which does not affect the feel and texture of the fabric.
Still another object of this invention is to provide a process of incorporating thermoregulatory constituents to lyocell fibers such that inherent properties of
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the lyocell fibers such as fiber strength, linear density, tenacity, heat resistance, dyeability and drying properties are not altered.
Definitions:
As used in the present specification, the following words and phrases are
generally intended to have the meanings as set forth below, except to the extent that the context in which they are used indicates otherwise.
"Phase-change agent" means a substance having the ability to releases or absorbs heat whenever it undergoes change in its physical state.
Enthalpy means heat content or total heat, including both sensible and latent heat.
"Latent heat" means the heat energy needed to change the state of a substance (ie: from a solid to a liquid) but not it's temperature.
"Flash point" means the temperature at which a substance gives off a sufficient amount of vapors to form an ignitable mixture with air.
"Non-aqueous phase" means a melted mixture in liquid state which is water insoluble.
"Aqueous phase" means substance dissolved in water.
"Lyocell Polymer dope" means an intermediate material in the manufacture of lyocell rayon products that is used for preparation of fibers.
7

"Preform mass" means an intermediate material suitable for making fibers.
Summary of the Invention
In accordance with this invention there is provided a thermoregulatory lyocell formulation meant for manufacture of lyocell rayon products comprising:
■ at least one non-water-soluble thermoregulatory constituent having a melting point lying in a predetermined range of temperature said constituent being in the range of about 0.01 to 20% of the mass of the formulation,
■ at least one water soluble non-cationic surfactant having HLB value in the range of 9 to 40, in the range of range of 0.001 to 10% of the mass of the formulation,
■ cellulosic pulp in the range of about 3% to 35% of the mass of the formulation
■ NNMO in the range of about 60% to 80% of the mass of the formulation; and
■ water in the range of about 0% to 20 % with respect to the mass of the formulation.
Typically, the thermoregulatory constituent is at least one selected from a group consisting of nonadecane, eicosane, heptadecane, octadecane, pentadecane, hexadecane, and other saturated hydrocarbons, decyl alcohol, lauryl alcohol, myristyl alcohol and other alphatic alcohols.
Typically, the surfactant is at least one non-ionic surfactant selected from a group of non-ionic surfactants consisting of alkyl phenoxy ethoxylated non-ionic surfactants and ethoxylated alkyl alcohol surfactants, Polyethylene-block-
8

Poly propylene glycol-block-polyethylene glycol and Ethylenediamine tetrakis(propylene oxide-block-ethylene oxide) tetrol.
Typically, the alkyl phenoxy ethoxylated non-ionic surfactant is at least one
selected from a group consisting of Polyoxyethylene(8) isooctylphenyl ether,
Nonylphenol polyethylene glycol ether, Polyoxyethylene(9) nonylphenyl ether,
PoIyoxyethylene(lO) isooctylphenyl ether, Polyoxyethylene(12) nonylphenyl
ether, Polyoxyethylene(12) isooctylphenyl ether, Polyoxyethylene(40)
nonylphenyl ether, Polyoxyethylene(40) isooctylphenyl ether,
Polyoxyethylene(lOO) nonylphenyl ether, Polyoxyethylene(150) dinonylphenyl
ether, Surfonic N-95(Poly (oxy-1, 2-ethanediyl), alpha- (nonyl phenyl)-omega-
hydroxyl-glycol ether) ( nonylphenol 9.5-mole ethoxylate) , Surfonic N-95(Poly
(oxy-1, 2-ethanediyl), alpha- (nonyl phenyl)-omega-hydroxyl-glycol ether) (
nonylphenol 9.5-mole ethoxylate) , Surfonic N-120(nonylphenol 12-mole
ethoxylate), Surfonic N-150 (nonylphenol 15-mole ethoxylate), Surfonic N-200
(nonylphenol 20-mole ethoxylate) , Surfonic N-300( nonylphenol 30-mole
ethoxylate) , Surfonic N-400 nonylphenol 40-mole ethoxylate, Surfonic LF-7
(Alkyl polyoxyalkylene ether) , Surfonic LF-17 (ethoxylated and propoxylated
linear primary 12-14 carbon number alcohol), Igepal CO-630 (nonylphenoxy
poly(ethyleneoxy)ethanol,branched), Surfonic DNP-40 (dinonylphenol
ethoxylate glycol ether).
In accordance with one preferred embodiment of the invention, the HLB value
of the surfactant is between 16 and 40.
9

In accordance with one aspect of the invention, the thermoregulatory constituent, the solvent and the surfactant are processed to form micro-reservoirs which are embedded into the body of the formulation.
Typically, the average mean size of the micro-reservoir is in the range of 5 nm to 2000 nm.
The invention also extends to a thermoregulatory lyocell fiber, yarn and fabric manufactured from a formulation in accordance with this invention.
In accordance with this invention there is also provided a process for preparation of a thermoregulatory lyocell formulation meant for manufacture of lyocell products comprising the following steps:
• heating water-insoluble thermoregulatory constituent with a non-aqueous solvent followed by heating the resulting mixture between 25°C and 95°C to obtain a non-aqueous phase ;
• dissolving and stirring a surfactant, optionally with a co-surfactant, in water to obtain an aqueous phase;
• heating the aqueous-phase;
• mixing the aqueous phase with the non-aqueous phase in the liquid state to form a admixture and homogenizing to obtain a micro-emulsion;
• mixing together cellulosic pulp and NNMO solution to form a slurry;
• dispersing the micro-emulsion in the slurry to obtain a preform mass wherein the thermoregulatory constituent is in the form of evenly dispersed micro-reservoirs;
10

• vaccumising the preform mass to remove water under 7 to 10 mm of Hg and temperature of over 90°C to obtain the formulation.
Typically, the pH of the aqueous phase is in the range of 7 to 13.
Typically, the amount of non-aqueous phase in the micro-emulsion is in the range of 0.1 to 40% of the mass of the micro-emulsion.
Typically, the amount of surfactant in the micro-emulsion is in the range of 0.1 to 20% of the mass of the micro-emulsion.
Typically, the proportion of thermoregulatory constituent in the lyocell product is in the range of 0.01 to 50% with respect to the mass of the lyocell product.
Brief Description of the accompanying Drawings:
The invention will be described in detail with reference to the accompanying drawings.
In the accompanying drawing, Figure 1 illustrates the block diagram showing the method steps involved in the process in accordance with this invention.
Figure 2 illustrates the cross-sectional view of thermoregulatory lyocell fibers prepared in accordance with this invention which shows uniform distribution of micro-reservoirs of thermoregulatory constituents entrapped across the length of the fibers.
Detailed Description:
11

Lyocell fibers were the first viable manufactured fibers. The reason behind the
most widespread use of these fibers lies in their versatility. Furthermore, these
fibers also have peculiar ability to blend easily with many fibers which makes
them the fibers of choice.
Though fibers and fabrics made from them have many desirable properties,
oftentimes, consumers expect performance characteristics beyond those for
which fibers were designed. In order to meet with these increasing expectations,
various thermoregulatory constituents are incorporated in the lyocell fibers.
There has been a considerable interest in developing such materials.
One of the additional desirable properties of lyocell fibers which has enormous
demand is "thermoregulatory activity".
Thermoregulatory constituents improve the thermal insulation of the lyocell fibers during changes in environmental temperature conditions. Thermoregulatory constituents are phase change materials which improve the thermal performance of clothing by absorbing or releasing heat when subjected to heating or cooling during a phase change.
Thermoregulatory lyocell product abates the transient effect on a human body's heat loss when the person wearing such fabric is exposed to temperature swings resulting from change in environmental conditions.
Typically, the thermoregulatory constituent is at least one selected from a group consisting of nonadecane, eicosane, heptadecane, octadecane, pentadecane, hexadecane and other saturated hydrocarbons, decyl alcohol, lauryl alcohol and myristyl alcohol and other aliphatic alcohols.
12

Thermoregulatory ability of the thermoregulatory constituents is governed by several factors which include melting point, quantity of the thermoregulatory constituent in the fabric, different combinations and proportions in which the thermoregulatory constituents are blended together, type of the polymer used in the fabric, thickness of the fabric, distribution of the thermoregulatory constituent in the fabric, and the process used for incorporating the thermoregulatory constituent in the fabric.
Physicochemical characteristics of the thermoregulatory constituents that used, are provided herein below:
Nonadecane:(Molecular formula: C19H40, CAS No: 629-92-5 EC No: 211-116-8 ) Appearance: white crystalline solid Melting point: 32 - 34 C Boiling point: 330 C Flashpoint: 168 C
Eicosane (Molecular formula: C20H42 CAS No: 112-95-8
EINECS No: 204-018-1 Appearance: colourless crystals or wax-like solid
Melting point: 36.7 C
Boiling point: 342.7 C
Heptadecane (n-heptadecane )Molecular formula: C17H36
CAS No: 629-78-7 EC No: 211-108-4 Appearance; colourless liquid or white
solid
Melting point: 21 C
Boiling point: 302 C
13

Flash point: 148 C (closed cup)
Octadecane Molecular formula: C18H38, CAS No: 593-45-3 EINECS No: 209-790-3 Appearance: white crystals or powder Melting point: 28-30 C Boiling point: 317 C Flashpoint: 165 C
Myristyl alcohol: (Molecular formula: C]4H3oO)CASNo: 112-72-1, 27196-00-5 EC No: 204-000-3, 248-318-0 Appearance: white crystalline semi-solid Melting point37 - 39 C Boiling point: 277-288 C Flashpoint: 145 C
Specific thermoformable properties of the fabric with respect to the desired temperature zones are adjusted by careful blend of the thermoregulatory constituents in specific proportions. The thermoregulatory constituent is selected such that it has a melting point that falls within the range of temperature in which thermal regulation is desired to be achieved. Thus, if thermal regulation is desired in the range of 21 -30 °C, then the melting point of the thermoregulatory constituent must fall within this range. Again if the fabric is to be used in climatic regions, where regulation is desired below 20 °C, then the thermoregulatory constituent having melting point below 20 °C is used. The thermoregulatory lyocell fabric acts as a transient thermal barrier by protecting the wearer of this fabric from the effects of cold or hot environments. When such thermoregulatory lyocell fabric is subjected to heating from the sun or a hot
14

environment, it will absorb transient heat as it changes phase from solid to liquid, and it will prevent the temperature of the fabric from rising by keeping it constant at the melting point temperature of the thermoregulatory constituent. Once thermoregulatory constituent has completely melted, its transient effect will cease and the temperature of the fabric will rise. In a similar manner, when a thermoregulatory fabric is subjected to a cold environment where the temperature is below its crystallization point, it will interrupt the cooling effect of the fabric structure by changing phase from liquid to solid, and the temperature of fabric will be kept constant at the crystallization point. Once all the thermoregulatory constituents have crystallized, the fabric temperature will drop, and the thermoregulatory constituents will have no effect on the fabric's thermal performance.
Thus, the thermal performance of a thermoregulatory constituent is a function of phase change temperature, the amount of thermoregulatory constituent and the amount of energy it absorbs or releases during a phase change.
In accordance with this invention there is provided a thermoregulatory lyocell formulation meant for manufacture of lyocell products comprising :
■ at least one non-water-soluble thermoregulatory constituent having a melting point lying in a predetermined range of temperature said constituent being in the range of about 0.01 to 20% of the mass of the formulation,
■ at least one water soluble non-cationic surfactant having HLB value in the range of 9 to 40, in the range of range of 0.001 to 10% of the mass of the formulation,
■ cellulosic pulp in the range of about 3% to 35% of the mass of the formulation
15

■ NNMO in the range of about 60 to 80% of the mass of the formulation; and
■ water in the range of about 0% to 20 % with respect to the mass of the formulation.
In accordance with the invention, thermoregulatory constituent is typically at least one selected from a group consisting of nonadecane, eicosane, heptadecane, octadecane and other satirdated hydrocarbons, myristyl alcohol and other aliphatic alcohols.
The thermoregulatory constituent impart thermoregulation property to the fibers and ultimately to the fabric or garments made from these fibers.
In accordance with this invention only water soluble non-ionic or anionic
surfactant/co-surfactant is used. Typically, the non-ionic surfactant is selected
from a group consisting of alkyl phenoxy ethoxylated non-ionic surfactants and
ethoxylated alkyl alcohol surfactants, Polyethylene-block-Poly propylene
glycol-block-polyethylene glycol and Ethylenediamine tetrakis(propylene oxide-
block-ethyl ene oxide) tetrol. Typically, the alkyl phenoxy ethoxylated non-ionic
surfactant is at least one selected from a group consisting of
Polyoxyethylene(S) isooctylphenyl ether, Nonylphenol polyethylene glycol
ether, Polyoxyethylene(9) nonylphenyl ether, Polyoxyethylene(lO)
isooctylphenyl ether, Polyoxyethylene(12) nonylphenyl ether,
Polyoxyethylene(12) isooctylphenyl ether, Polyoxyethylene(40) nonylphenyl ether, Polyoxyethylene(40) isooctylphenyl ether, Polyoxyethylene(lOO) nonylphenyl ether, Polyoxyethylene(150) dinonylphenyl ether, Surfonic N-95(Poly (oxy-1, 2-ethanediyl), alpha- (nonyl phenyl)-omega-hydroxyl-glycol ether) ( nonylphenol 9.5-mole ethoxylate) , Surfonic N-95(Poly (oxy-1, 2-ethanediyl), alpha- (nonyl phenyl)-omega-hydroxyl-glycol ether) ( nonylphenol
16

9.5-mole ethoxylate) , Surfonic N-120(nonyIphenol 12-mole ethoxylate) ,
Surfonic N-150 (nonylphenol 15-mole ethoxylate), Surfonic N-200
(nonylphenol 20-mole ethoxylate) , Surfonic N-300( nonylphenol 30-mole
ethoxylate) , Surfonic N-400 nonylphenol 40-mole ethoxylate, Surfonic LF-7
(Alkyl polyoxyalkylene ether) , Surfonic LF-17 (ethoxylated and propoxylated
linear primary 12-14 carbon number alcohol), Igepal CO-630 (nonylphenoxy
poly(ethyleneoxy)ethanol,branched), Surfonic DNP-40 (dinonylphenol
ethoxylate glycol ether).
The non-ionic surfactant is selected such that the lipophilic portion of the non-ionic surfactant is compatible with the thermoregulatory constituent and the surfactant forms oil in water microemulsion. Surfactants with HLB values within the range of 9 to 40 are used. Preferably, non-ionic surfactants with HLB values more than 13 are used.
In accordance with one preferred embodiment of the invention, the HLB value of the surfactant is between 16 and 40.
In accordance with one aspect of the invention, the thermoregulatory constituent, the solvent and the surfactant are processed to form micro-reservoirs which are embedded into the body of the formulation. The thermoregulatory lyocell contains uniformly dispersed micro-reservoirs throughout the body of the fibers. The micro-reservoirs are discrete, nano-sized structures without any definite geometrical shape.
Typically, the average mean size of the micro-reservoir is in the range of 5 nm to 2000 nm.
17

The invention also extends to a thermoregulatory lyocell fiber, yarn and fabric manufactured from a formulation in accordance with this invention.
In accordance with this invention there is also provided a process for preparation of a thermoregulatory lyocell formulation meant for manufacture of lyocell products comprising the following steps:
• heating a water-insoluble thermoregulatory constituent between 25°C and 95°C to obtain non-aqueous phase ;
• dissolving and stirring a surfactant, optionally with a co-surfactant, in water to obtain an aqueous phase;
• heating the aqueous-phase;
• mixing the aqueous phase with the non-aqueous phase in the liquid state to form a admixture and homogenizing to obtain a micro-emulsion;
• mixing together cellulosic pulp and NNMO solution to form a slurry;
• dispersing the micro-emulsion in the slurry to obtain a preform mass wherein the thermoregulatory constituent is in the form of evenly dispersed micro-reservoirs;
• vaccumising the preform mass to remove water under 7 to 10 mm of Hg.
Typically, the pH of the aqueous phase is in the range of 7 to 13.
Typically, the amount of non-aqueous phase in the micro-emulsion is in the range of 0.1 to 40% of the mass of the micro-emulsion.
Typically, the amount of surfactant in the micro-emulsion is in the range of 0.1 to 20% of the mass of the micro-emulsion.
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Typically, the proportion of thermoregulatory constituent in the lyocell product is in the range of 0.01 to 50% with respect to the mass of the lyocell product.
Before arriving at the optimum concentration of the surfactant to be used, cloud point of the aqueous phase is determined.
Typically, the melted non-aqueous phase containing thermoregulatory constituent in a non-aqueous solvent along with aqueous phase containing surfactants is emulsified using high speed mixers such as Ultraturrex or a mechanical emulsifier; a colloid mill; a high pressure homogenizer and an ultrasonic emulsifier to form a microemulsion. The micro-emulsion may contain further additional thermoregulatory constituents, if desired.
The active ingredients are released from the micro-reservoir into the lyocell matrix. The structure of micro-reservoir, lyocell and surrounding conditions determine the release rate of the thermoregulatory constituent. The molecules of the volatile thermoregulatory constituents migrate from micro-reservoirs to the surrounding primarily by diffusion. The thermoregulatory constituent is released from the matrix in a controlled release manner.
Conventional method for manufacture of lyocell involves following major steps:
Step 1. Creating a solvent solution from wood pulp
The wood pulp is obtained from a variety of sources, such as wood chips or even large rolls of paper that have been finely shredded, is the basic starting material for manufacture of lyocell fibers. In case of manufacture of lyocell no further
19

chemical treatment of the wood pulp is needed thereby making the process environment friendly.
The wood pulp solution is produced in a straight solvation process by dissolving wood pulp at high temperatures and pressure in a recyclable non-toxic organic solvent solution of amine oxide, particularly N-methylmorpholine N-oxide,(NNMO).
Lyocell is manufactured by a "closed loop" spinning process which conserves energy and water.
Step 2. Spinning lyocell fiber from the solvent solution
Before being formed into fibers, the lyocell polymer dope, is in a thick liquid state. In the spinning process this liquid is forced through a spinneret, which resembles a large shower head.
The clear, viscous resultant solution is filtered and extruded into an aqueous bath of dilute amine oxide, and coagulated into fiber form.
Step 3. Washing lyocell fiber to remove solvents
The fiber is then washed before it is dried and twisted or spun into yarns, which are woven or knitted into fabrics and garments.
Step 4. Drying fiber and producing yarns
When the filament dries or solidifies, it forms what is called a continuous filament fiber. Many continuous filaments of specific thicknesses collected in a large bundle called a "tow". A tow may contain over a million continuous
20

filaments. The tow bundle is then crimped, is then mechanically cut into staple fibers, usually ranging in length from 1 to 6-1/2 inches, depending how they are to be used.
Strands of continuous filament fibers are then twisted together to form a continuous filament yarn, which is then woven or knit into fabric.
Step 5. Finishing to produce lyocell fabric
The fabric is treated with an enzyme that attacks cellulose fibers. Home laundry detergents containing such enzymes are also used for treatment of the fabric for better finishing purposes. This enzyme dissolves the split-end hairs from the fiber surface. The fiber is then washed and agitated again. The resulting fabric is similar in texture and drape to sueded silk or sueded rayon found in fashion apparel. Fabrics processed this way can usually be machine washed and line dried successfully.
Alternatively, the filaments so obtained are stretched to straighten out the fibers which are further blended using standard equipment. The blended fibers are laid in to a web followed by Consolidation of the web to obtain Non-woven Lyocell Fabric.
The lyocell product made from the formulation in accordance with this invention contains uniformly dispersed micro-reservoirs throughout the mass which is shown in Fig. 2.
21

The thermoregulatory lyocell fibers contain the entrapped thermoregulatory
constituent in releasable form. Microscopic examination of the micro-reservoirs
in the lyocell fibers is shown in Fig 2.
Thermoregulatory fabric improves the comfort of people irrespective of the
fluctuations in the temperature of their surroundings on either side.
Besides this, thermoregulatory fabric also improves the comfort of people as
their body goes through a very active state (high metabolic production) to an
inactive state on an intermittent basis in a cold environment. This feature is of
particular relevance for outdoor sportsmen.
The resultant lyocell fabric containing thermoregulatory constituent are tested. Linear Density (Denier) of the lyocell Fibers is determined by using standard ASTM Test Method (D 1577). The denier of the standard lyocell fiber (lyocell fiber without any thermoregulatory constituents) and anti-microbial enriched lyocell fiber remains the same. Thus addition of thermoregulatory constituents does not change the linear density of the lyocell fibers.
Tensile strength and Young's modulus of lyocell fiber sample is tested on an Instron tensile testing machine as per the ASTM C1557-03 procedure at ambient temperature.
Visual appearance of the thermoregulatory enriched fiber is evaluated by methods as prescribed in AATCC 124. As far as parameters like % Loss in Dry Tenacity and % loss in dry elongation are concerned, these remain the same in the thermoregulatory enriched lyocell fiber and the standard fiber. Incorporation of thermoregulatory constituent in accordance with this invention does not affect the visual appearance of the fiber.
22

Feel of the fiber: The thermoregulatory enriched lyocell fiber as prepared in accordance with this invention offers the same feel effect as is observed in case of plain lyocell fiber without any thermoregulatory constituent (Also referred as standard).
Another important concern in textile industry is dye-ability of the fabric, which is tested by comparing the dyeability of the thermoregulatory constituent enriched fabric and the standard lyocell fabric. Dyeability of the thermoregulatory enriched lyocell fibers as prepared in accordance with this invention remains the same as that of the standard lyocell fiber.
The invention will now be described with the help of the following non-limiting
examples.
Examples Example 1
Example 1A- Preparation of micro emulsion
Myristyl alcohol (50gm) was heated until it melts to form a molten liquid. Surfonic N-400 nonylphenol 40-mole ethoxylate (surfactant) ( 5.6gm ) was dissolved and stirred in water 105ml to obtain 110.6gm of aqueous phase. The aqueous phase (110.6gm) and the molten liquid (50 gm) were homogenized in a high speed mixer (Ultraturrex) to obtain a micro-emulsion (160.6 gm ).
Example 1 B- Preparation fiber and fabric
Cellulosic pulp (839.4 gm) and 10600 gm of 50% NNMO solution were mixed to form lyocell slurry. The micro-emulsion as prepared in Example 1A was evenly dispersed in the slurry to obtain a preform mass. The homogenized preform mass was vaccumisied to remove water under 10 mm of Hg and at
23

temperature 110 °C to give Lyocell polymer dope (839.4 gm). The lyocell polymer dope was further spun in a spin bath of dilute NNMO solution, and coagulated into fiber form.
The filaments so obtained were washed in water and dried at 100°C. The lyocell fiber thus obtained contained micro-reservoirs having the entrapped releasable thermoregulatory constituents. Although the micro reservoirs did not have any specific shape or size, they were found to be uniformly distributed throughout the body of the fiber.
Example 2
Example 2A
Preparation of micro emulsion
Cetyl alcohol(50gm) was heated to from a molten liquid.
Surfonic N-150 (nonylphenol 15-mole ethoxylate) (surfactant) (16.8 gm ) was
dissolved and stirred in water 111.1ml to obtain 127. 9gm of clear aqueous
phase
The aqueous phase(127. 9gm ) and the molten liquid (50 gm) were homogenized
in a high speed mixer (Ultraturrex) to obtain an thermoregulatory formulation
in the form of micro-emulsion. (177.9 gm )
Example 2 B
The micro-emulsion as prepared in Example 2A was added to lyocell slurry, vacuumised at high temperature to give lyocell Polymer Dope (containing 822. lgm cellulose) and was spun or extruded into various forms such as fiber or
24

film or cast into various shapes using the regeneration media as described in example 1.
Example 3
Example 3 A
Heptadecane (50gm) was heated to from a molten liquid.
Surfonic N-150 (nonylphenol 15-mole ethoxylate) (surfactant) (16.8 gm ) was
dissolved and stirred in water 111.1ml to obtain 127. 9gm of clear aqueous
phase
The aqueous phase(127. 9gm ) and the nolten liquid (50 gm) were homogenized
in a high speed mixer (Ultraturrex) to obtain an thermoregulatory formulation
in the form of micro-emulsion. (177.9 gm )
Example 3 B
The micro-emulsion as prepared in Example 2A was added to lyocell slurry, vacuumised at high temperature to give lyocell Polymer Dope (contaiing 822.1 gm cellulose) and was spun or extruded into various forms such as fiber or film or cast into various shapes using the regeneration media as described in example 1.
Example 4
Example 4 A
Preparation of thermoregulatory formulation
Heptadecane (35gm) myristyl alcohol (15gm) was heated to form a molten
liquid. Surfonic N-30Q( nonylphenol 30-mole ethoxylate) (surfactant) (5.6gm)
25

was dissolved and stirred in water (105ml) to obtain 110.6 gm of clear aqueous phase
The aqueous phase(110.6gm) and the molten liquid ( 50 gm) were homogenized in a high speed mixer (Ultraturrex) to obtain a micro-emulsion.
Example 4 B
The micro-emulsion as prepared in Example 4A was added to lyocell slurry,
vacuumised at high temperature to give lyocell Polymer Dope (containing 839.4
gm cellulose) and was spun or extruded into various forms such as fiber or film
or cast into various shapes using the regeneration media as described in example
1.
Example 5
Example 5A
Preparation of thermoregulatory formulation
Nonadecane (750 gm) was heated to form a molten liquid. Surfonic N-200 (nonylphenol 20-mole ethoxylate) (surfactant) (50.4gm) was dissolved and stirred in water (1500ml) to obtain 1550 gm of clear aqueous phase The aqueous phase (1550 gm) and the molten liquid ( 750 gm) were homogenized in a high speed mixer (Ultraturrex) to obtain a micro-emulsion.(2.3kg)
Example 5 B
The micro-emulsion as prepared in Example 5A was added to lyocell slurry, vacuumised at high temperature to give lyocell Polymer Dope (containing 1.866Kg cellulose) and was spun or extruded into various forms such as fiber or
26

film or cast into various shapes using the regeneration media as described in example 1.
Example 6
Example 6 A
Preparation of thermoregulatory formulation
Nonadecane (50gm) was melted to form a molten liquid. Surfonic N-200
(nonylphenol 20-mole ethoxylate) (surfactant) (11.2gm) was dissolved and
stirred in water 210ml to obtain 221.2gm of clear aqueous phase.
The aqueous phase(221.2gm) and the mixture lOOgm were homogenized in a
high speed mixer (Ultraturrex) to obtain a micro-emulsion. (271.2gm)
Example 6 B
The micro-emulsion as prepared in Example 6A was added to lyocell slurry, vacuumised at high temperature to give lyocell Polymer Dope (containing 1.678Kg cellulose) and was spun or extruded into various forms such as fiber or film or cast into various shapes using the regeneration media as described in example 1.
Example 7
Example 7 A
Preparation of thermoregulatory formulation
Eicosane 50 gm was melted to form a molten liquid. Surfonic N-300( nonylphenol 30-mole ethoxylate) (surfactant) (16.8gm) was dissolved and "*red in water 111.1ml to obtain 127.9gm of clear aqueous phase
'^pus phase (127.9gm ) and the mixture 50gm were homogenized in a "xer (Ultraturrex) to obtain a micro-emulsion. (177.9gm )
27

Example 7 B
The micro-emulsion as prepared in Example 7 A was added to lyocell slurry,
vacuumised at high temperature to give lyocell Polymer Dope (containing 822.1
gm cellulose) and was spun or extruded into various forms such as fiber or film
or cast into various shapes using the regeneration media as described in example
1.
Example 8
Example 8 A
Preparation of thermoregulatory formulation
Eicosane (25gm) and Nonadecane (25gm) were melted together to form a
molten liquid. Surfonic N-300( nonylphenol 30-mole ethoxylate) (surfactant)
(5.6 gm) was dissolved and stirred in water (105ml) to obtain (110.6 gm) of
clear aqueous phase.
The aqueous phase (110.6 gm) and the mixture (50 gm) were homogenized in a
high speed mixer (Ultraturrex) to obtain a micro-emulsion. (160.6gm)
Example 8 B
The micro-emulsion as prepared in Example 8A was added to lyocell slurry, vacuumised at high temperature to give lyocell Polymer Dope (containing 839.4gm cellulose) and was spun or extruded into various forms such as fiber or film or cast into various shapes using the regeneration media as described in example 1.
Example 9
Example 9A Preparation of micro emulsion
28

Nonadecane (50gm) was heated until it melts to form a molten liquid. Surfonic N-400 nonylphenol 40-mole ethoxylate (surfactant) ( 5.6gm ) was dissolved and stirred in water 105ml to obtain 110.6gm of aqueous phase. The aqueous phase (110.6gm) and the molten liquid (50 gm) were homogenized in a high speed mixer (Ultraturrex) to obtain a micro-emulsion (160.6 gm ).
Example 9 B- Preparation fiber and fabric
The micro-emulsion as prepared in Example 1A was added to lyocell slurry, vacuumised at high temperature to give lyocell Polymer Dope containing 839.4 gm cellulose and the resulting thermoregulatory enriched lyocell polymer dope was homogenized. The homogenized lyocell polymer dope and was spun or extruded into various forms such as fiber or film or cast into various shapes using the regeneration media as described in example 1.
Example 10
Example 10 A
Preparation of micro emulsion
Myristyl alcohol (50gm ) was heated to from a molten liquid.
Surfonic N-150 (nonylphenol 15-mole ethoxylate) (surfactant) (16.8 gm ) was
dissolved and stirred in water 111.1ml to obtain 127. 9gm of clear aqueous
phase
The aqueous phase(127. 9gm ) and the molten liquid (50 gm) were homogenized
in a high speed mixer (Ultraturrex) to obtain an thermoregulatory formulation .
in the form of micro-emulsion. (177.9 gm )
Example 10 B
29

The micro-emulsion as prepared in Example 2A was added to lyocell slurry, vacuumised at high temperature to give lyocell Polymer Dope (containing 822. lgm cellulose) and was spun or extruded into various forms such as fiber or film or cast into various shapes using the regeneration media as described in example 1.
Example 11
Example 11 A
Eicosane(50gm ) was heated to from a molten liquid.
Surfonic N-150 (nonylphenol 15-mole ethoxylate) (surfactant) (16.8 gm ) was
dissolved and stirred in water 111.1ml to obtain 127. 9gm of clear aqueous
phase
The aqueous phase(127. 9gm ) and the molten liquid (50 gm) were
homogenized in a high speed mixer (Ultraturrex) to obtain an thermoregulatory
formulation in the form of micro-emulsion. (177.9 gm )
Example 11 B
The micro-emulsion as prepared in Example 2A was added to lyocell slurry, vacuumised at high temperature to give lyocell Polymer Dope (containing 822.lgm cellulose) and was spun or extruded into various forms such as fiber or film or cast into various shapes using the regeneration media as described in example 1.
Example 12
Example 12 A
Preparation of thermoregulatory formulation
30

Heptadecane (50gm) was heated to form a molten liquid. Surfonic N-300( nonylphenol 30-mole ethoxylate) (surfactant) (5.6gm) was dissolved and stirred in water (105ml) to obtain 110.6 gm of clear aqueous phase The aqueous phase(l 10.6gm) and the molten liquid ( 50 gm) were homogenized in a high speed mixer (Ultraturrex) to obtain a micro-emulsion.
Example 12 B
The micro-emulsion as prepared in Example 4A was added to lyocell slurry,
vacuumised at high temperature to give lyocell Polymer Dope (containing 839.4
gm cellulose) and was spun or extruded into various forms such as fiber or film
or cast into various shapes using the regeneration media as described in example
1.
Example 13
Example 13A
Preparation of thermoregulatory formulation
Nonadecane (500 gm) and hectadecane(250) were heated to form a molten
liquid. Surfonic N-200 (nonylphenol 20-mole ethoxylate) (surfactant) (50.4gm)
was dissolved and stirred in water (1500ml) to obtain 1550.4 gm of clear
aqueous phase
The aqueous phase(1550gm) and the molten liquid ( 750 gm) were
homogenized in a high speed mixer (Ultraturrex) to obtain a micro-
emulsion.(2.3kg)
Example 13 B
The micro-emulsion as prepared in Example 5A was added to lyocell slurry,
vacuumised at high ■ temperature to give lyocell Polymer Dope (containing
31

1.866Kg cellulose) and was spun or extruded into various forms such as fiber or film or cast into various shapes using the regeneration media as described in example 1.
Example 14
Example 14 A
Preparation of thermoregulatory formulation
Nonadecane (40gm) and heptadecane (10)gm were melted to form a molten
liquid. Surfonic N-200 (nonylphenol 20-mole ethoxylate) (surfactant) (11.2gm)
was dissolved and stirred in water 210ml to obtain 221.2gm of clear aqueous
phase.
The aqueous phase(221.2gm) and the mixture lOOgm were homogenized in a
highspeed mixer (Ultraturrex) to obtain a micro-emulsion. (321.2gm )
Example 14 B
The micro-emulsion as prepared in Example 6A was added to lyocell slurry, vacuumised at high temperature to give lyocell Polymer Dope (containing 1.678Kg cellulose ) and was spun or extruded into various forms such as fiber or film or cast into various shapes using the regeneration media as described in example 1.
Example 15
Example 15 A
Preparation of thermoregulatory formulation
Myristyl alcohol (30gm ) and heptadecane(20gm) were melted to form a molten
liquid. Surfonic N-300( nonylphenol 30-mole ethoxylate) (surfactant) (16.8gm)
32

was dissolved and stirred in water 111.1ml to obtain 127.9gm of clear aqueous phase
The aqueous phase (127.9gm ) and the mixture 50gm were homogenized in a high speed mixer (Ultraturrex) to obtain a micro-emulsion. (177.9gm)
Example 15 B
The micro-emulsion as prepared in Example 7A was added to lyocell slurry,
vacuumised at high temperature to give lyocell Polymer Dope (contaiing 822.1
gm cellulose) and was spun or extruded into various forms such as fiber or film
or cast into various shapes using the regeneration media as described in example
1.
Example 16
Example 16 A
Preparation of thermoregulatory formulation
Eicosane (25gm) and Hectadecane (25gm) were melted together to form a
molten liquid. Surfonic N-300( nonylphenol 30-mole ethoxylate) (surfactant)
(5.6 gm) was dissolved and stirred in water (105ml) to obtain (110.6 gm) of
clear aqueous phase.
The aqueous phase (110.6 gm) and the mixture (50 gm) were homogenized in a
high speed mixer (Ultraturrex) to obtain a micro-emulsion. (160.6gm )
Example 16 B
The micro-emulsion as prepared in Example 8A was added to lyocell slurry, vacuumised at high temperature to give lyocell Polymer Dope (containing 839.4gm celllulosej and was spun or extruded into various forms such as fiber
33

or film or cast into various shapes using the regeneration media as described in example 1.
Testing procedures:
The thermoregulatory lyocell products as prepared in the above examples (1 to 10) were tested by using following test procedures:
1) Linear Density (Denier) of the lyocell Fibers was determined by using
standard ASTM Test Method (D 1577).
The denier of the standard lyocell fiber (without any thermoregulatory constituents) and anti-microbial lyocell fibers as prepared in accordance with example IB was found to be uniform(1.5 denier) irrespective of the type and quantity of the thermoregulatory constituent.
2) Tensile strength and Young's modulus of lyocell fiber samples were tested on an Instron tensile testing machine as per the ASTM CI557-03 procedure at ambient temperature.
3) Emulsion stability: The stability of micro-emulsions as prepared in the above examples, was evaluated by keeping the same under observation in measuring cylinders for 3 days. During this period no phase separation was observed.
4) Feel of the fabric: The lyocell fabrics as prepared in the above examples and standard fabric (lyocell fabric without thermoregulatory constituents), were randomly given to twenty subjects and they were asked to evaluate the texture and feel of the fiber. The test fiber material was interchanged several times amongst the human subjects. Collective results as submitted by the human subjects confirmed that nobody could distinguish between the
34

thermoregulatory lyocell fabrics prepared in accordance with the Examples provided above and the standard fabric.
5) Dyeability: The thermoregulatory lyocell fabrics as prepared in the above examples and the standard fabric as described above were dyed uniformly with reactive dyes. No noticeable difference as to the Dyeability of the two respective lyocell fabrics, with and without thermoregulatory constituent was reported.
6) Visual appearance of the thermoregulatory lyocell fiber was evaluated by
methods as prescribed in AATCC 124. As far as parameters like % Loss in
Dry Tenacity and % loss in dry elongation are concerned, these remained the
same( lyocell fiber and the standard fiber
7) Determination of enthalpy of the fabric specimen: the thermoregulatory
properties of the specimen fabrics/fibers as prepared in examples 1 to 10 were
evaluated by measuring respective enthalpies of the specimen. The enthalpies
were measured using DSC(Differential scanning calorimetry) technique. The
recorded enthalpies of the fiber and fabric obtained in examples 1 to 10 are
provided in the Table 1.
35

Table 1

Specimen
No. enthalpy J/g Fiber enthalpy J/g Fabric
1 4.3 4.29
2 5.4 5.38
3 6.6 6.63
4 6 5.98
5 37 36.3
6 4.3 4.1
7 8.4 8.41
8 7.2 7.19
9 6.5 6.4
10 5.2 5.24
11 8.4 8.35
12 6.5 6.55
13 34.1 34.6
14 3.1 3.0
15 5.5 5.6
16 6.5 6.5
8. Thermoregulatory testing:
Free flowing robes made to fit the physique of twenty human volunteers, selected at random between ages 16 to 56, were made from undyed
36

thermoregulatory Lyocell fabric prepared in accordance with this invention. Simultaneously, identical robes with same design weer also made from undyed standard fabric (Lyocell fabric without any thermo regulatory constituents).
A temperature monitored room was selected where the temperature could be precisely controlled. The temperature in the room was set at 21°C. The twenty human volunteers were requested to wear the robes and assemble in the room and be there in the room for a period of 30 min. They were made to randomly wear either a standard robe (robe made from standard fabric) or a robe made from the fabric of this invention. But they were not informed about the type of the robe that was being worn. After 30 minutes, a\\ the volunteers were asked to step out into the outside non-air-conditioned environment, where the tempreature was 280c and they were asked to abserve and note the time where they felt warm in the area covered by the robe.
Thereafter, all the volunteers switched their robes, ie: The volunteer given a robe of standard fabric, was allotted a robe made from the fabric of this invention and vise-a-versa. They were again asked to go back irto the room and remain there for 30 min. and again step out into the external environment and again observe and note the time when they started feeling warm. The volunteers were then asked to give an evaluation of the time required to feel the warmth in both the instances.
The results of the experiments were as follows.
Seventeen volunteers opined that they felt warm in the standard fabric, at least on an average of 3 minutes quicker than the fabric of this invention.
Two volunteers could not sense significant difference in time and one volunteer recorded an earlier feeling of warmth in case of the fabric of this invention.
37

In case of direct comparison between the robes, 17 volunteers opined that they
felt cooler and more comfortable wearing a ward-robe made from the fabric of
this invention.
Three volunteers expressed no significant difference between the two. There
was no volunteer who provided any reverse finding.
Similar test was conducted in which the volunteers were made to go from a
hotter external environment at 30 C to an air-conditioned environment
maintained at 21 C. All of the volunteers expressed that they felt warmer and
more comfortable in the robe made from the fabric of this invention and the
reported response time for feeling cold was on an average 3 min. longer.
It is thus concluded that the fabric made in accordance with this invention exhibits thermoregulatory effect in either situation, ie when there is a rise in temperature and when there is a fall in the temperature.
While considerable emphasis has been placed herein on the specific steps of the preferred embodiment, it will be appreciated that many alterations can be made and that many modifications can be made in the preferred embodiment without departing from the principles of the invention. These and other changes in the preferred embodiment as well as other embodiments of the invention will be apparent to those skilled in the art from the disclosure herein, whereby it is to be distinctly understood that the foregoing descriptive matter is to be interpreted merely as illustrative of the invention and not as a limitation.
38

We Claim-.
1. A thermoregulatory lyocell formulation meant for manufacture of lyocell
products comprising :
■ at least one non-water-soluble thermoregulatory constituent having a melting point lying in a predetermined range of temperature said constituent being in the range of about 0.01 to 20% of the mass of the formulation,
■ at least one water soluble non-cationic surfactant having HLB value in the range of 9 to 40, in the range of range of 0.001 to 10% of the mass of the formulation,
■ cellulosic pulp in the range of about 3% to 35% of the mass of the tbrmuiat'ibn
■ NNMO in the range of about 60 to 80% of the mass of the formulation; and
■ water in the range of about 0% to 20 % with respect to the mass of the formulation.

2. A formulation as claimed in claim 8, wherein the thermoregulatory constituent is at least one selected from a group consisting of nonadecane, eicosane, heptadecane, octadecane, pentadecane, hexadecane, decyl alcohol, lauryl alcohol and myristyl alcohol.
3. A formulation as claimed in claim 1, wherein the surfactant is at least one non-ionic surfactant selected from a group of non-ionic surfactants consisting of alkyl phenoxy ethoxylated non-ionic surfactants and ethoxylated alkyl alcohol, Polyethylene-block-Poly propylene glycol-block-polyethylene
39

glycol and Ethylenediamine tetrakis(propylene oxide-block-ethylene oxide)
tetrol.
A formulation as claimed in claim 8, wherein the alkyl phenoxy ethoxylated
non-ionic surfactant is at least one selected from a group consisting of
Polyoxyethylene(8) isooctylphenyl ether, Nonylphenol polyethylene glycol
ether, Polyoxyethylene(9) nonylphenyl ether, Polyoxyethy lene(10)
isooctylphenyl ether, Polyoxyethylene(12) nonylphenyl ether,
Polyoxyethylene(12) isooctylphenyl ether, Polyoxyethylene(40) nonylphenyl
ether, Polyoxyethylene(40) isooctylphenyl ether, Polyoxyethylene( 100)
nonylphenyl ether, Polyoxyethylene(150) dinonylphenyl ether, Surfonic N-
95(Poly (oxy-1, 2-ethanediyl), alpha- (nonyl phenyl)-omega-hydroxyl-glycol
ether) ( nonylphenol 9.5-mole ethoxylate) , Surfonic N-95(Poly (oxy-1, 2-
ethanediyl), alpha- (nonyl phenyl)-omega-hydroxyl-glycol ether) ( nonylphenol
9.5-mole ethoxylate) , Surfonic N-120(nonylphenol 12-mole ethoxylate) ,
Surfonic N-150 (nonylphenol 15-mole ethoxylate), Surfonic N-200
(nonylphenol 20-mole ethoxylate) , Surfonic N-300( nonylphenol 30-mole
ethoxylate) , Surfonic N-400 nonylphenol 40-mole ethoxylate, Surfonic LF-7
(Alkyl polyoxyalkylene ether) , Surfonic LF-17 (ethoxylated and propoxylated
linear primary 12-14 carbon number alcohol), Igepal CO-630 (nonylphenoxy
poly(ethyleneoxy)ethanoI,branched), Surfonic DNP-40 (dinonylphenol
ethoxylate glycol ether).
4. A formulation as claimed in claim 1, wherein the preferred HLB value of the surfactant is between 16 and 40.
40

5. A formulation as claimed in claim 1, wherein the average mean size of the
micro-reservoir is in the range of 5 nm to 2000 run.
6. A thermoregulatory lyocell fiber manufactured from a formulation as
claimed in claim 1.
7. A thermoregulatory lyocell yarn manufactured from a formulation as claimed in claim 1.
8. A thermoregulatory lyocell fabric manufactured from a formulation as claimed in claim 1.
9. A process of preparation of a thermoregulatory lyocell formulation meant for manufacture of lyocell products comprising the following steps :

• heating a water-insoluble thermoregulatory constituent between 25°C and 95°C to obtain a non-aqueous phase ;
• dissolving and stirring a surfactant, optionally with a co-surfactant, in water to obtain an aqueous phase;
• heating the aqueous-phase;
• mixing the aqueous phase with the non-aqueous phase in the liquid state to form a admixture and homogenizing to obtain a micro-emulsion;
• mixing together cellulosic pulp and NNMO solution to form a slurry;
• dispersing the micro-emulsion in the slurry to obtain a preform mass wherein the antimicrobial constituent is in the form of evenly dispersed micro-reservoirs;
41

vaccumismg the preform mass to remove water under 7 to 10 mm of Hg and a temperature over 90°C to obtain the formulation.
Dated this 3rd day of My, 2008.

Mohan Dewan
of R. K. Dewan and Co.
Applicants' Patent Attorney
42

Documents:

1392-mum-2008-abstract.doc

1392-mum-2008-abstract.pdf

1392-MUM-2008-ANNEXURE TO FORM 3(26-9-2012).pdf

1392-MUM-2008-CLAIMS(AMENDED)-(26-9-2012).pdf

1392-mum-2008-claims.doc

1392-mum-2008-claims.pdf

1392-MUM-2008-CORRESPONDENCE(13-04-2010).pdf

1392-mum-2008-correspondence(18-7-2008).pdf

1392-MUM-2008-CORRESPONDENCE(24-7-2009).pdf

1392-MUM-2008-CORRESPONDENCE(6-8-2013).pdf

1392-mum-2008-correspondence.pdf

1392-mum-2008-description(complete).doc

1392-mum-2008-description(complete).pdf

1392-mum-2008-drawing.pdf

1392-MUM-2008-EP DOCUMENT(26-9-2012).pdf

1392-mum-2008-form 1(18-7-2008).pdf

1392-MUM-2008-FORM 1(6-8-2013).pdf

1392-MUM-2008-FORM 1(MARKED COPY)-(6-8-2013).pdf

1392-mum-2008-form 1.pdf

1392-MUM-2008-FORM 13(6-8-2013).pdf

1392-MUM-2008-FORM 18(24-7-2009).pdf

1392-mum-2008-form 2(title page)-(3-7-2008).pdf

1392-mum-2008-form 2(title page).pdf

1392-mum-2008-form 2.doc

1392-mum-2008-form 2.pdf

1392-MUM-2008-FORM 26(26-9-2012).pdf

1392-MUM-2008-FORM 3(13-04-2010).pdf

1392-mum-2008-form 3(3-7-2008).pdf

1392-mum-2008-form 3.pdf

1392-MUM-2008-MARKED COPY(26-9-2012).pdf

1392-MUM-2008-REPLY TO EXAMINATION REPORT(26-9-2012).pdf

1392-MUM-2008-SPECIFICATION(AMENDED)-(26-9-2012).pdf

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Patent Number

257111

Indian Patent Application Number

1392/MUM/2008

PG Journal Number

36/2013

Publication Date

06-Sep-2013

Grant Date

03-Sep-2013

Date of Filing

03-Jul-2008

Name of Patentee

ADITYA BIRLA SCIENCE & TECHNOLOGY CO. LTD.

Applicant Address

ADITYA BIRLA CENTRE, 2ND FLOOR, C WING, S.K. AHIRE MARG, MUMBAI - 400 025

Inventors:

#	Inventor's Name	Inventor's Address
1	KAPOOR BIR	ADITYA BIRLA CENTRE, 2ND FLOOR, C WING, S.K. AHIRE MARG, MUMBAI-400 025,
2	LODHA PREETI	ADITYA BIRLA CENTRE, 2ND FLOOR, C WING, S.K. AHIRE MARG, MUMBAI-400 025,
3	MAHAJAN TUSHAR	ADITYA BIRLA CENTRE, 2ND FLOOR, C WING, S.K. AHIRE MARG, MUMBAI-400 025,

PCT International Classification Number

C08K5/01

PCT International Application Number

N/A

PCT International Filing date

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1	NIL	1900-09-01	India