Title of Invention	A PROCESS OF MAKING BALLOONS, AND PARTICULARLY, A COATING COMPOSITION FOR BALLOONS
Abstract	A process for making a coating composition for balloons comprising the steps of:- A)Making pigment slurry(premix) cintaining Titanium Dioxide,freeze thaw agent along with neutralizer,dispersant and an emulsifier. B)Subjecting the slurry so formed to a milling process to obtain an intermediate; and C)Blending the intermediate with a stabilizer, a modifier and a preservative.

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FORM-2 THE PATENTS ACT, 1970 (39 of 1970) & THE PATENTS RULES, 2003 COMPLETE Specification (See section 10 and rule 13) A PROCESS OF MAKING BALLOONS, AND PARTICULARLY, A COATING COMPOSITION FOR BALLOONS INDOFIL CHEMICALS CO. (a Division of MODIPON LTD.) an Indian Company of Nirlon House, Dr. Annie Besant Road, Mumbai 400 025, Maharashtra, India original 594/mum/2004 26-05-2004 THE FOLLOWING SPECIFICATION PARTICULARLY DESCRIBES THE INVENTION AND THE MANNER IN WHICH IT IS TO BE PERFORMED:- This invention relates to a process of making balloons, and particularly, a coating composition for balloons. BACKGROUND: The traditional process /practice for the preparation of balloons involves casting a natural latex dispersion in hollow molds and further dipping the mold in a slurry of titanium dioxide. This mold is finally dipped into an acetic acid solution for coagulation and if necessary, the process is repeated until the desired thickness of the balloon is obtained. Alternatively, the titanium oxide formulation is dispersed in the latex solution itself and the mold containing the latex solution is dipped in this dispersion. The mold is then dipped in an acid bath, most commonly glacial acetic acid bath for coagulation. For enhancing softening properties of the balloon, platicizers such as Turkey red oil are used. In both the cases, the balloon is then dried either under controlled conditions in an air-dried oven or under sunlight. In India, the operation is manual and has the following drawbacks documented below: 1. The balloon becomes hard after two to four months of manufacture 2. Yellowing of the white balloon 3. Color fades in case of dyed balloons in three to four months 4. Titanium dioxide slurry cannot be stored for more than forty eight hours 5. Titanium slurry tends to settle. This brings about variation in properties of the balloon with respect to dispersion, leveling, color, thickness 6. Titanium dioxide slurry being used as-is, is very costly This necessitated the development of alternative methods . 2 Methods of making balloons have been disclosed in various patents. GB594966 The patent discusses the process on improvements in the formulation of rubber and the like; however, none of the processes or formulation described in the specification did address the above problems. US 4634395 The Patent discusses a composition and method and apparatus for increasing the buoyant lifetime of a gas inflatable elastomeric balloon wherein a surface of a balloon is coated with an aqueous solution containing polyvinyl alcohol, and a water soluble plasticizer for polyvinyl alcohol such as glycerin, which coating is dried while the balloon is in the inflated condition. Treatment of a rubber latex balloon having an inflated diameter of about 15 cm to about 50 cm by the method of this invention claims to increase its buoyant lifetime about 600 percent without significantly changing the appearance of the balloon. US 5,383,806 The Patent describes the invention of a composition, method and apparatus for preserving the glossy, smooth exterior finish of a latex balloon wherein the exterior surface of the balloon is coated with an anionic aliphatic dispersion of polyester urethane material and dried. The method of application of the coating is discussed. The coating claims to significantly increase the lifetime of the balloon without significantly decreasing buoyancy US 4,002,590 The patent claims a coating composition for thick coating prepared by adding an aggregate to a coating liquid containing colloidal silica and formulations thereof with and dissolved and/or finely dispersed organic polymer, having an silicon oxide 2 /M.sub.2 O mole ratio substitutes with a monovalent alkali metal atom. The coating compositions are claimed for being especially suitable for coating of 1 - 20 kg/m.sup.2 in thickness and storable for a long period of time with an excellent stability, giving a cured coating having high water resistance, good weather resistance, high adhesive strength and no efflorescence in its surface. Balloons having improved resistance to oxidation. US 5,492,500 This patent explains the oxidation resistance of elastomeric balloons made from natural rubber being greatly improved by coating the exterior of the balloon with a film of uncured elastomer, preferably neoprene. The uncured elastomer coating is claimed to maintain the clarity of the inflated balloons. These balloons are claimed to be suitable for application as containers for gifts or in balloon sculpture. WO20040221 The patent is about processing of a medical balloon device to be used as a catheter and novel method of making and using the balloon is provided. In the method, a two-step forming process is provided, which overcomes the traditional brittleness exhibited by polymers when used below Tg. Selection criteria for polymeric materials that may yield medical balloons with desirable balloon strength and flexibility when processed according to the invention is also provided. None of these processes are useful for Indian conditions and are expensive. After application of serious thought process into experimentation through trial and error of various polymer compositions, the present invention was developed , which was an answer to all of the above problems. A principal feature of this invention is formulating titanium dioxide with a water dispersible acrylic polymer and fortified kaolin. The formulation, emparts softness properties, is alkaline in nature and is capable of being standardized. 4 BRIEF OUTLINE OF WORK CARRIED OUT : A. THE INGREDIENTS CONSTITUTED THE COMPOSITION OF PREMIX-1 (Pigment Slurry) ♦ Titanium Dioxide, which is basically used as an opacifier. ♦ Calcined clay, Wetting agent belonging to the class of poly hydroxy alcohols, used as a freeze thaw agent ♦ Neutralizer belonging to the class of amines ♦ Dispersant, basically belonging to class of polymethacrylates. ♦ Emulsifier from the alkyl aryl polyethoxylated phenol class ♦ Water The above ingredients, in a predetermined order, were subjected to high shear mixing for emulsification and homogenization under controlled conditions of temperature to form a premix. B. THIS PREMIX IS THEN SUBJECTED TO A SECOND UNIT OPERATION OF MILLING PROCESS FOR PREPARATION OF INTERMEDIATE-1 > The milling process involves use of a dyno-mill with a determined percentage loading of the grinding media. > Controlled conditions of air pressure for operation, seal flushing water pressure, compressed air output pressure and temperature of the unit operation are the critical parameters for the process. > After the required particle size of the intermediate formulation is attained, it is subjected to a third unit operation of blending C. INGREDIENTS FOR THE BLENDING OPERATION FOR PREPARATION OF FINAL PRODUCT 5 ♦ Intermediate 1 ♦ Dispersion stabilizer from the class of polymethacrylic acid ♦ Rheology Modifier which is an associative acrylic thickener ♦ Preservative and ♦ Water to obtain a formulation with a Total Solid content of 40 - 70% According to this invention there is therefore provided a process of making a coating composition for balloons comprising the steps of :- A) Making pigment slurry (premix) containing Titanium Dioxide, freeze thaw agent along with neutralizer, dispersant and an emulsifier; B) Subjecting the slurry so formed to a milling process to obtain an intermediate; and C) Blending the intermediate with a stabilizer, a modifier and a preservative. The Titanium Dioxide is used to make the balloon opaque. Typically, the freeze thaw agent is calcined clay (Kaolin). Alternatively, the freeze thaw agent is a wetting agent. Preferably, the freeze thaw agent is calcined clay and a wetting agent in combination. The wetting agent typically belongs to the class of polyhydroxy alcohols, such as Monoethylene Glycol. Preferably, the neutralizer belongs to the class of amines and is particularly, Triethanol Amine. The dispersant used belongs to the class of Polymethacrylates and is typically, Sodium Tripolyphosphate or Sodium Hexameta phosphate. The emulsifier is typically a non ionic surfactant, preferably belongs to the class of Polyethoxylated phenols and is preferred to be Ethylene Oxide condensate Nonyl phenol. The milling step is preferably carried out using a dyno mill and controlled condition of pressure and temperature to obtain an intermediate of requisite particle size. The 6 controlled condition of pressure comprises a air pressure for operation, seal flushing water pressure and compressed air output pressure. The stabilizer is a dispersion stablizer typically belongs to the class of Polymethacrylic Acid. The modifier is a rheology modifier and is a type of a associative acrylic thickener. The making of slurry and blending is carried out using water, preferably deionized water. The balloons are made of acrylic or styrene acrylic polymer emulsion. The balloons are made by a process comprising agitating acrylic emulsion in a resin kettle, step by step addition of pigment slurry, dispersing agent, acrylic thicker and adding a biocide after dispersing the whole material. The biocide [preservative] is typically formaldehyde or methyiisothiazolinone or chloromethylisothiazolinone. A preferable coating composition in accordance with this invention comprises Titanium Dioxide .. 15-30% Freeze Thaw Agent.. 20-40% Neutral izer.. 2-5% Dispersant.. 0.5-3% Emulsifier 0.2 -- 0.8% , Polymer emulsion .. 15-25% Acrylic Thickener.. 0.3-0.6% preservative 0.1 -0.5% Of total content of final composition. 7 The above ingredients, in a scheduled order are mixed to form the final product under controlled conditions of operation Examples EXAMPLE-1 PREMIX - PREPARATION OF INTERMEDIATE-I Basic raw materials & Manufacturing process of a Balloon Coating a) Titanium Dioxide (Rutile grade, Alumina & Zirconium coated) -282.0 Gms (15- 30% of final product) (Particle size - 0.28 u., Specific Gravity - 4.2) b) Calcined clay (15-30% of final product) - 282.0 Gms (Amino treated, pH @ 10% Solid- 9.0, Specific Gravity -2.6 Particle size- 0.8-1.5 microns) c) Wetting agent (Monoethylene Glycol) - 72.6 Gms ( 5-10% ) d) Neutralizing agent (Tri ethanol amine) -30.5 (2-5%) e) Dispersing agent (neutralized polymethacrylates/Sodium tri poly phosphate/ sodium hexa meta phosphate) - 9.54 ( 0.5 - 3%) f) Nonionic surfactant (40 moles ethylene Oxide condensate Nonyl Phenol, HLB values- 18) - 2.90 Grams ( 0.2-0.8%) g) Deionized Water (DIW) - 262.8 Grams Total weight- 942.34 Grams. MANUFACTURING PROCEDURE OF PIGMENT SLURRY 1. 202.8 Grams of De Ionized Water taken in Dyno Mill & turned on agitation to 2500 RPM. 2. 72.6 Grams of Monoethylene Glycol slowly added to the mill & rinse the container with 20 grams of DIW. 3. After 2 minutes 9.54 grams of dispersing agent added & rinse the container with 10 grams of DIW. 4. After that 282 grams of Titanium Dioxide slowly added to Disperser by 15 minutes. 8 5. 2.9 Grams of nonionic surfactant added & rinse the container with 10 grams of DIW. 6. After complete mixing 282 grams Calcined clay slowly added to the mill for about 20 minutes. 7. When dispersion is complete then 30.5 Grams of Tri ethanol amine added & rinse the container with 20 grams of DIW. 8. Disperse these materials for 3 - 4 hrs at 2500 RP M to get the desired particle size of slurry from 0.2 - 0.3 micron. Analysis Results of Intermediate - I(exp-2) Appearance - White liquid without foreign particles. Solid (%)- 61.4 Particle Size (d50) - 0.25 Micron (Shimadzu particle analyzer) STEP-2 PREPARATION OF FINAL PRODUCT Basic Raw Materials- a) Intermediate-1 (exp-2) - 800.00 Gms b) Binder (pure acryl ic/styrene acrylic emulsion of 50% solid) - 200.00 Gms (15 -25%) c) Dispersing agent (neutralized polymethacrylates)- 10.0 Gms (0.5 - 1.5%) d) Associative acrylic thickener (copolymer of ethyl acryl ate & met acrylic acid)-4.00 Gms (0.3 - 0.6%) e) Biocide (formaldehyde/ chloro methylisothiazolinone /methylisothiazolinone) -2.90 Gms (0.1 -0.5%) f) De Ionized Water - 10.00 Gms g) TOTAL-1026.9 Gms Manufacturing Procedure of Final Product a) 200.00 grams of acrylic emulsion taken in a Resin Kettle & turned on agitator (120 RPM). b) 800.00 Grams of Pigment slurry added to the kettle slowly over 10 minutes. 9 c) After 2 minutes 10 grams of dispersing agent added to the kettle. d) After 2 minutes 4.00 Grams of acrylic thickener added to the kettle slowly over 10 minutes. e) Disperse the materials for 1 hour after that biocide added and mixed for another 5 minutes. f) Collected the materials and checked the properties. Analysis Results of Final Product) Appearance - White liquid & free from foreign particles. Solid (%)-60.1 PH - 9.0 Viscosity- 350 Ps (Brookfield RVT#5/20/25°C) Application - Using the above material 50 balloons were prepared. For making balloon the formulation made in accordance with example 2 was used 25% (20 -40% can be used) with natural latex & balloons were cast by pouring the dispersion in hollow molds, then these molds were dipped into an acetic acid solution after that the balloons were dried under sunlight. The balloons prepared were soft, non-tacky, uniformly opaque, no yellowing (for white balloons), more elastic than the balloons prepared by conventional method. The stability of slurry was also found to be 6-10 months compared to 48 hrs of conventional slurry. Again no external plasticizer was required for processing the balloon. EXAMPLE -2 PREMIX - PREPARATION OF INTERMEDIATE-I Basic raw materials & Manufacturing process of a Balloon Coating a) Titanium Dioxide (Rutile grade, Alumina & Zirconium coated) - 282.0 Gms (15- 30% of final product) (Particle size - 0.28 u., Specific Gravity - 4.2) b) Calcined clay (15-30% of final product) - 282.0 Gms (Vinyl treated, pH @ 10% Solid- 9.0, Specific Gravity -2.6 Particle size- 0.8-1.5 microns) 10 c) Wetting agent (Monoethylene Glycol) - 72.6 Gms ( 5-10% ) d) Neutralizing agent (Ammonia) -30.5 (2-5%) e) Dispersing agent (neutralized polymethacryiates/Sodium tri poly phosphate/ sodium hexa meta phosphate) - 9.54 ( 0.5 - 3%) f) Nonionic surfactant (40 moles ethylene Oxide condensate Nonyl Phenol, HLB values- 18) - 2.90 Grams ( 0.2-0.8%) g) Deionized Water (DIW) - 262.8 Grams Total weight - 942.34 Grams. MANUFACTURING PROCEDURE OF PIGMENT SLURRY 1. 202.8 Grams of De Ionized Water taken in Dyno Mill & turned on agitator to 2500 RPM. 2. 72.6 Grams of Monoethylene Glycol slowly added to the mill & rinse the container with 20 grams of DIW. 3. After 2 minutes 9.54 grams of dispersing agent added & rinse the container with 10 grams of DIW. 4. After that 282 grams of Titanium Dioxide slowly added to Disperser by 15 minutes. 5. 2.9 Grams of nonionic surfactant added & rinse the container with 10 grams of DIW. 6. After complete mixing 282 grams Calcined clay slowly added to the mill for about 20 minutes. 7. When dispersion is complete then 30.5 Grams of Ammonia added & rinse the container with 20 grams of DIW. 8. Disperse these materials for 3 - 4 hrs at 2500 RP M to get the desired particle size of slurry from 0.2 - 0.3 micron. Analysis Results of Intermediate - l(exp-2) Appearance - White liquid without foreign particles. Solid (%)- 60.4 Particle Size (d50) - 0.25 Micron (Shimadzu particle analyzer) STEP-2 PREPARATION OF FINAL PRODUCT Basic Raw Materials- a) Intermediate-1 (exp-2) - 800.00 Gms b) Binder (pure acrylic/styrene acrylic emulsion of 50% solid) - 200.00 Gms (15 -25%) c) Dispersing agent (neutralized polymethacrylates)- 10.0 Gms (0.5 - 1.5%) d) Associative acrylic thickener (copolymer of ethyl acryl ate & met acrylic acid)-4.00 Gms (0.3 - 0.6%) e) Biocide (formaldehyde/ chloro methylisothiazolinone /methylisothiazolinone) -2.90 Gms (0.1 -0.5%) f) De Ionized Water - 10.00 Gms g) TOTAL-1026.9 Gms Manufacturing Procedure of Final Product a) 200.00 grams of acrylic emulsion taken in a Resin Kettle & turned on agitator (120 RPM). b) 800.00 Grams of Pigment slurry added to the kettle slowly over 10 minutes. c) After 2 minutes 10 grams of dispersing agent added to the kettle. d) After 2 minutes 4.00 Grams of acrylic thickener added to the kettle slowly over 10 minutes. e) Disperse the materials for 1 hour after that biocide added and mixed for another 5 minutes. f) Collected the materials and checked the properties. Analysis Results of Final Product) Appearance - White liquid & free from foreign particles. Solid (%) - 60.0 PH - 8.9 Viscosity - 350 Ps (Brookfield RVT#5/20/25°C) Application - Using the above material 100 balloons were prepared. For making balloons 26% (20 - 40% can be used) of the formulation of example 2 was used with natural latex & the dispersion was cast in hollow molds, then these molds were 12 dipped into an acetic acid solution after that the balloons were dried under sunlight. The balloons prepared by using exp-2 were soft, non-tacky, uniformly opaque, without yellowing (for white balloons), more elastic than the balloons prepared by conventional method. The stability of slurry was also 6-10 months compared to 48 hrs of conventional slurry. Again no external plasticizer was required for processing the balloon. EXAMPLE -3 PREMIX - PREPARATION OF INTERMEDIATE! Basic raw materials & Manufacturing process of a Balloon Coating a)Titanium Dioxide (Rutile grade, Alumina & Zirconium coated) - 282.0 Gms (15-30% of final product) (Particle size - 0.32 p,, Specific Gravity - 4.2) b)Calcined clay (15-30% of final product) - 282.0 Gms (Vinyl treated, pH @ 10% Solid- 9.0,. Specific Gravity -2.6 Particle size- 0.8-1.5 microns) c)Wetting agent (Monoethylene Glycol) - 72.6 Gms ( 5-10% d)Neutralizing agent (Tri ethanol amine) -30.5 (2-5%) e)Dispersing agent (neutralized polymethacrylates/Sodium tri poly phosphate/ sodium hexa meta phosphate) - 9.54 ( 0.5 - 3%) f)Nonionic surfactant (40 moles ethylene Oxide condensate Nonyl Phenol, HLB values- 18) - 2.90 Grams ( 0.2-0.8%) g)Deionized Water (Dl W) - 262.8 Grams Total weight - 942.34 Grams. MANUFACTURING PROCEDURE OF PIGMENT SLURRY a) 202.8 Grams of De Ionized Water taken in Dyno Mill & turned on agitator to 2500 RPM. b) 72.6 Grams of Monoethylene Glycol slowly added to the mill & rinse the container with 20 grams of DIW. 13 c) After 2 minutes 9.54 grams of dispersing agent added & rinse the container with 10 grams of DIW. i. After that 282 grams of Titanium Dioxide slowly added to Disperser by 15 minutes, ii. 2.9 Grams of nonionic surfactant added & rinse the container with 10 grams of DIW. iii. After complete mixing 282 grams Calcined clay slowly added to the mill for about 20 minutes, iv. When dispersion is complete then 30.5 Grams of Triethanol amine added & rinse the container with 20 grams of DIW. v. Disperse these materials for 3 - 4 hrs at 2500 RP M to get the desired particle size of slurry from 0.2 ~0.3 micron. Analysis Results of Intermediate - I(exp-3) Appearance - White liquid without foreign particles. Solid (%)-60.3 Particle Size (d50) - 0.25 Micron (Shimadzu particle analyzer) STEP-2 PREPARATION OF FINAL PRODUCT Basic Raw Materials- a) Intermediate-1 (exp-2) - 800.00 Gms b) Binder (pure acryl ic/styrene acrylic emulsion of 50% solid) - 200.00 Gms (15 -25%) c) Dispersing agent (neutralized polymethacrylates)- 10.0 Gms (0.5 - 1.5%) d) Associative acrylic thickener (copolymer of ethyl acryl ate & met acrylic acid)-4.00 Gms (0.3 - 0.6%) h) Biocide (formaldehyde/ chloro methylisothiazolinone /methylisothiazolinone) -2.90 Gms (0.1-0.5%) e) De Ionized Water-10.00 Gms f) TOTAL-1026.9 Gms 14 Manufacturing Procedure of Final Product a) 200.00 grams of acrylic emulsion taken in a Resin Kettle & turned on agitator (120 RPM). b) 800.00 Grams of Pigment slurry added to the kettle slowly over 10 minutes. c) After 2 minutes 10 grams of dispersing agent added to the kettle. d) After 2 minutes 4.00 Grams of acrylic thickener added to the kettle slowly over 10 minutes. e) Disperse the materials for 1 hour after that biocide added and mixed for another 5 minutes. f) Collected the materials and checked the properties. Analysis Results of Final Product) Appearance - White liquid & free from foreign particles. Solid (%) - 60.0, pH - 9.1 Viscosity - 350 Ps (Brookfield RVT#5/20/25°C) Application - Using the above material 100 blue coloured balloons were prepared. For making balloon 26% (20 - 40% can be used) of the formulation was used with natural latex & cast in hollow molds, which were then dipped into an acetic acid solution after that the balloons were dried under sunlight. The balloons were soft, non-tacky, uniformly opaque, no discolouration, more elastic than the balloons prepared by conventional method. The stability of slurry was also 6-10 months compared to 48 hrs of conventional slurry. Again no external plasticizer was required for processing the balloon. EXAMPLE -4 PREMIX -PREPARATION OF INTERMEDIATE-I Basic raw materials & Manufacturing process of a Balloon Coating a) Titanium Dioxide (Rutile grade, Alumina & Zirconium coated) - 282.0 Gms (15- 30% of final product) (Particle size - 0.32 u., Specific Gravity - 4.2) b) Calcined clay (15-30% of final product) - 282.0 Gms 15 (Vinyl treated, pH @ 10% Solid- 9.0, Specific Gravity -2.6 Particle size- 0,8-1.5 microns) c) Wetting agent (Diethylene Glycol) - 72.6 Gms ( 5-10% ) d) Neutralizing agent (Tri ethanol amine) -30.5 (2-5%) e) Dispersing agent (neutralized polymethacrylates/Sodium tri poly phosphate/ sodium hexa meta phosphate) - 9.54 ( 0.5 - 3%) f) Nonionic surfactant (40 moles ethylene Oxide condensate Nonyl Phenol, HLB values- 18) - 2.90 Grams ( 0.2-0.8%) g) Deionized Water (DIW) - 262.8 Grams Total weight - 942.34 Grams. MANUFACTURING PROCEDURE OF PIGMENT SLURRY 1. 202.8 Grams of De Ionized Water taken in Dyno Mill & turned on agitator to 2500 RPM. 2. 72.6 Grams of Diethylene Glycol slowly added to the mill & rinse the container with 20 grams of DIW. 3. After 2 minutes 9.54 grams of dispersing agent added & rinse the container with 10 grams of DIW. 4. After that 282 grams of Titanium Dioxide slowly added to Disperser by 15 minutes. 5. 2.9 Grams of nonionic surfactant added & rinse the container with 10 grams of DIW. 6. After complete mixing 282 grams Calcined clay slowly added to the mill for about 20 minutes. 7. When dispersion is complete then 30.5 Grams of Triethanol amine added & rinse the container with 20 grams of DIW. 8. Disperse these materials for 3 - 4 hrs at 2500 RP M to get the desired particle size of slurry from 0.2 - 0.3 micron. Analysis Results of Intermediate - l(exp-2) Appearance- White liquid without foreign particles. Solid (%) - 60.3 Particle Size (d50) - 0.25 Micron 16 (Shimadzu particle analyzer) STEP-2 PREPARATION OF FINAL PRODUCT Basic Raw Materials- a) Intermediate-] (exp-2) - 800.00 Gms b) Binder (pure acrylic/styrene acrylic emulsion of 50% solid) - 200.00 Gms (15 -25%) c) Dispersing agent (neutralized polymethacrylates)- 10.0 Gms (0.5 - 1.5%) d) Associative acrylic thickener (copolymer of ethyl acryl ate & met acrylic acid)-4.00 Gms (0.3 - 0.6%) e) Biocide (formaldehyde/ chloro methylisothiazolinone /methylisothiazolinone) -2.90 Gms (0.1-0.5%) f) De Ionized Water - 10.00 Gms g) TOTAL-1026.9 Gms Manufacturing Procedure of Final Product a) 200.00 grams of acrylic emulsion taken in a Resin Kettle & turned on agitator (120 RPM). b) 800.00 Grams of Pigment slurry added to the kettle slowly over 10 minutes. c) After 2 minutes 10 grams of dispersing agent added to the kettle. d) After 2 minutes 4.00 Grams of acrylic thickener added to the kettle slowly over 10 minutes. e) Disperse the materials for 1 hour after that biocide added and mixed for another 5 minutes. f) Collected the materials and checked the properties. Analysis Results of Final Product) Appearance - White liquid & free from foreign particles. Solid (%) - 60.0 ,pH - 9.1 Viscosity - 350 Ps (Brookfield RVT#5/20/25°C) Application - Using the above material 100 red colored balloons. Red dye used for coloration. For making the balloons 26% (20 - 40% can be used) was dispersed with 17 natural latex & cast in hollow molds, which were then dipped into an acetic acid solution after that the balloons were dried under sunlight. The balloons were soft, non-tacky, uniformly opaque, no discolouration, more elastic than the balloons prepared by conventional method. The stability of slurry was 6-10 months compared to 48 hrs of conventional slurry. Again no external plasticizer was required for processing the balloon. EXAMPLE -5 PREMIX - PREPARATION OF INTERMEDIATE-I Basic raw materials & Manufacturing process of a Balloon Coating a) Titanium Dioxide (Rutile grade, Alumina & Zirconium coated) - 282.0 Gms (15- 30% of final product) (Particle size - 0.32 \x, Specific Gravity - 4.2) b) Calcined clay (15-30% of final product) - 282.0 Gms (Vinyl treated, pH @ 10% Solid- 9.0, Specific Gravity -2.6 Particle size- 0.8-1.5 microns) c) Wetting agent (Diethylene Glycol) - 72.6 Gms ( 5-10% ) cNeutralizing agent (Isopropyl amine) -30.5 (2-5%) d) Dispersing agent (neutralized polymethacrylates/Sodium tri poly phosphate/ sodium hexa meta phosphate) - 9.54 ( 0.5 - 3%) e) Nonionic surfactant (40 moles ethylene Oxide condensate Nonyl Phenol, HLB values- 18) - 2.90 Grams ( 0.2-0.8%) f) Deionized Water (DIW) - 262.8 Grams Total weight - 942.34 Grams. MANUFACTURING PROCEDURE OF PIGMENT SLURRY a. 202.8 Grams of De Ionized Water taken in Dyno Mill & turned on agitator to 2500 RPM. b. 72.6 Grams of Diethylene Glycol slowly added to the mill & rinse the container with 20 grams of DIW. 18 c. After 2 minutes 9.54 grams of dispersing agent added & rinse the container with 10 grams of DIW. d. After that 282 grams of Titanium Dioxide slowly added to Disperser by 15 minutes. e. 2.9 Grams of nonionic surfactant added & rinse the container with 10 grams of DIW. f. After complete mixing 282 grams Calcined clay slowly added to the mill for about 20 minutes. g. When dispersion is complete then 30.5 Grams of Isopropyl amine added & rinse the container with 20 grams of DIW. h. Disperse these materials for 3 - 4 hrs at 2500 RP M to get the desired particle size of slurry from 0.2 - 0.3 micron. Analysis Results of Intermediate - I(exp-2) Appearance- White liquid without foreign particles. Solid (%) - 60.3 Particle Size (d50) - 0.25 Micron (Shimadzu particle analyzer) STEP-2 PREPARATION OF FINAL PRODUCT Basic Raw Materials- a) Intermediate-1 (exp-2) - 800.00 Gms b) Binder (pure acrylic/styrene acrylic emulsion of 50% solid) - 200.00 Gms (15 -25%) c) Dispersing agent (neutralized polymethacrylates)- 10.0 Gms (0.5 - 1.5%) d) Associative acrylic thickener (copolymer of ethyl acryl ate & met acrylic acid)-4.00 Gms (0.3 - 0.6%) g) Biocide (formaldehyde/ chloro methylisothiazolinone /methylisothiazolinone) -2.90 Gms (0.1 -0.5%) e) De Ionized Water - 10.00 Gms f) TOTAL-1026.9 Gms 19 Manufacturing Procedure of Final Product a) 200.00 grams of acrylic emulsion taken in a Resin Kettle & turned on agitator (120 RPM). b) 800.00 Grams of Pigment slurry added to the kettle slowly over 10 minutes. c) After 2 minutes 10 grams of dispersing agent added to the kettle. d) After 2 minutes 4.00 Grams of acrylic thickener added to the kettle slowly over 10 minutes. e) Disperse the materials for 1 hour after that biocide added and mixed for another 5 minutes. f) Collected the materials and checked the properties. Analysis Results of Final Product) Appearance - White liquid & free from foreign particles. Solid (%) - 60.0, PH - 9.1, Viscosity - 350 Ps (Brookfield RVT#5/20/25°C) Application - Using the above material we have prepared 100 red colored balloons. Red dye used for coloration. For making balloon 26% was dispersed in natural latex & castin hollow molds, treated as above The balloons were soft, non-tacky, uniformly opaque, no discolouration, more elastic than the balloons prepared by conventional method. The stability of slurry was 6-10 months compared to 48 hrs of conventional slurry. Again no external plasticizer was required for processing the balloon. Thus it can be seen that The formulation in accordance with this invention displayed remarkably improved application oriented results. The following were the findings of the formulation with respect to application at the customer"s end: 1. Uniform Dispersion thus ruling out inconsistencies with regards to color, thickness. Leveling, variation. 20 2. The product, unlike titanium dioxide slurry can be stored for a minimum of three months 3. In case of colored balloons, marked improvement was found in retention of color as against use of titanium dioxide slurry 4. Yellowing of the white balloons was retarded to a drastic extent 5. The balloon was soft and non-tacky 6. Elongation ( measured as tensile strength) is far superior to the balloons prepared using existing formulation 7. No special requirement was felt for a adding any piasticizer after the processing of balloon 8. The formulation is substantially cheaper than the existing product used. . It was observed that synergism in the various properties of the formulation was brought out which otherwise would not have been exhibiting all of the above properties. The product stability and lessening of the yellowing of the white balloons and improvement in tensile strength were unexpected properties displayed by the formulation. 21 We Claim: 1) A process of making a coating composition for balloons comprising the steps of :- A)Making pigment slurry (premix) containing Titanium Dioxide, freezing cum thawing agent along with neutralizer, dispersant and an emulsifier; B)Subjecting the slurry so formed to a milling process to obtain an intermediate; and QBlending the intermediate with a stabilizer, a modifier and a preservative. 2) A process of making a coating composition for balloons as claimed in Claim 1, wherein Titanium Dioxide is used to make the balloon opaque. 3) A process of making a coating composition for balloons as claimed in claim 1, wherein the freeze thaw agent is calcined clay (Kaolin). 4) A process of making a coating composition for balloons as claimed in Claim 1, wherein freeze thaw agent is a wetting agent. 5) A process of making a coating composition for balloons as claimed in Claim 1 wherein the freeze thaw agent is calcined clay and a wetting agent in combination. 6) A process of making a coating composition for balloons as claimed in Claim 5 wherein the wetting agent belongs to the class of polyhydroxy alcohols. 7) A process of making a coating composition for balloons as Claimed in Claim 6 wherein the wetting agent is Monoethylene Glycol. 8) A process of making a coating composition for balloons as claimed in Claim 1 wherein the neutralizer belongs to the class of amines. 22 9) A process of making a coating composition for balloons as claimed in Claim 8 wherein the amine is Triethanol Amine. 10) A process of making a coating composition for balloons as claimed in Claim 1 wherein the dispersant used belongs to the class of Polymethacrylates. 11) A process of making a coating composition for balloons as claimed in Claim 10 wherein the dispersant is Sodium Tripolyphosphates. 12) A process of making a coating composition for balloons as claimed in Claim 11 wherein the dispersant is Sodium Hexameta phosphate. 13) A process of making a coating composition for balloons as claimed in Claim 1 wherein the emulsifier is a non ionic surfactant. 14) A process of making a coating composition for balloons as claimed in Claim 13 wherein the emulsifier used belongs to the class of Polyethoxylated phenols. 15) A process of making a coating composition for balloons as claimed in Claim 14 wherein the emulsifier is Ethylene Oxide condensate Nonyl phenol. 16) A process of making a coating composition for balloons as claimed in Claim 1 wherein the milling step is carried out using a dyno mill and controlled condition of pressure and temperature to obtain an intermediate of requisite particle size. 17) A process of making a coating composition for balloons as claimed in Claim 16, wherein the controlled condition of pressure comprises a air pressure for operation, seal flushing water pressure and compressed air output pressure. 23 18) A process of making a coating composition for balloons as claimed in Claim 1 in which the stabilizer is a dispersion stablizer belonging to the class of Polymethacrylic Acid. 19) A process of making a coating composition for balloons as claimed in Claim 1 wherein the modifier is a rheology modifier and is a type of a associative acrylic thickener. 20) A process of making a Coating composition for balloons as claimed in Claim 1, wherein the making of slurry and blending is carried out using water. 21) A process of making a Coating composition for balloons as claimed in Claim 20, wherein water is deionized water. 22) A process of making a Coating composition for balloons as claimed in Claim 1, wherein the balloons are made of acrylic or styrene acrylic polymer emulsion. 23) A process of making a coating composition for balloons as claimed , in Claim 22 wherein the balloons are made by a process comprising agitating acrylic emulsion in a resin kettle, step by step addition of pigment slurry, dispersing agent, acrylic thicker and adding a biocide after dispersing the whole material. 24) A process of making a coating composition for balloons Claim 23 wherein the biocide is formaldehyde. 25) A process of making a coating composition for balloons as Claimed in claim 23 wherein the biocide is methylisothiazolinone. 26)A process of making a coating composition for balloons as claimed in Claim 23, wherein the biocide is chlororriethylisothiazolinone. 24 27) A coating composition for making balloons, said coating composition made according to any of the preceding claims, comprising Titanium Dioxide .. 15-30% Freeze Thaw Agent.. 20-40% Neutralizer.. 2-5% Dispersant. 0.5-3% Emulsifier 0.2-0.8% Polymer emulsion .. 15-25% Acrylic Thickener.. 0.3-0.6% preservative 0.1-0.5% Of total content of final composition. 28) Balloons obtained by the process as claim in any of the preceding claims. 29)A Process for making the balloon coating composition substantially as herein described with reference to the examples. Mohan Dewan of R K Dewan & Co Applicants" Patent Attorney 25

Documents:

597-mum-2004-cancelled pages(08-06-2007).pdf

597-mum-2004-claims(granted)-(08-06-2007).doc

597-mum-2004-claims(granted)-(08-06-2007).pdf

597-mum-2004-correspondence(08-06-2007).pdf

597-mum-2004-correspondence(ipo)-(18-02-2008).pdf

597-mum-2004-form 1(26-05-2004).pdf

597-mum-2004-form 13(16-04-2008).pdf

597-mum-2004-form 18(09-10-2006).pdf

597-mum-2004-form 2(granted)-(08-06-2007).doc

597-mum-2004-form 2(granted)-(08-06-2007).pdf

597-mum-2004-form 3(26-05-2004).pdf

597-mum-2004-form 5(18-05-2005).pdf

597-mum-2004-power of attorney(26-05-2004).pdf