Title of Invention	AN IMPROVED PROCESS FOR THE PREPARATION OF SOLID ISOPROYL-N(3-CHLOROPHENYL) CARBAMATE
Abstract	An improved process for the preparation of solid isopropyl-N- (3-chlorophenyl) carbamate (CIPC) without the need for filling the molten CIPC into the drums directly in the plant during the last step of commercial production, for further transport, comprising of stirring of molten CIPC, between 100 - 5000 rpm at a temperature ranging between -20 to 35 °C, to initiate the solidification for semisolid mass; feeding the semi-solid mass on to a drum flakers maintained at -10 to 35°C with rpm between 1 - 60, to obtain flakes; maintaining the temperature of flakes between 5 - 25 ° C; grinding the flakes in a multi mill, with 1-5 mm sieve, at a temperature ranging from -5 to 25 °C; to obtain the solid isopropyl-N-(3-chlorophenyl) carbamate (CIPC) . This powder is optionally, compressed with a pressure of 15 to 300 kg/cm2 to form tablets, pellets, blocks/chunks of isopropyl-N-(3-cholorophenyl) carbamate.

Title of Invention

AN IMPROVED PROCESS FOR THE PREPARATION OF SOLID ISOPROYL-N(3-CHLOROPHENYL) CARBAMATE

Abstract

An improved process for the preparation of solid isopropyl-N- (3-chlorophenyl) carbamate (CIPC) without the need for filling the molten CIPC into the drums directly in the plant during the last step of commercial production, for further transport, comprising of stirring of molten CIPC, between 100 - 5000 rpm at a temperature ranging between -20 to 35 °C, to initiate the solidification for semisolid mass; feeding the semi-solid mass on to a drum flakers maintained at -10 to 35°C with rpm between 1 - 60, to obtain flakes; maintaining the temperature of flakes between 5 - 25 ° C; grinding the flakes in a multi mill, with 1-5 mm sieve, at a temperature ranging from -5 to 25 °C; to obtain the solid isopropyl-N-(3-chlorophenyl) carbamate (CIPC) . This powder is optionally, compressed with a pressure of 15 to 300 kg/cm2 to form tablets, pellets, blocks/chunks of isopropyl-N-(3-cholorophenyl) carbamate.

Full Text	FORM 2 THE PATENTS ACT, 1970 (39 of 1970) COMPLETE SPECIFICATION (See Section 10; Rule 13) AN IMPROVED PROCESS FOR THE PREPARATION OF SOLID ISOPROPYL-N-(3-CHLOROPHENYL) CARBAMATE We, UNITED PHOSPHORUS LIMITED, a company incorporated under the Companies Act, 1956 and having its registered office at 3-11, GIDC, Vapi-396 195, State of Gujarat, India and having its office at Uniphos House, 11th Road, C. D. Marg, Khar (West), Mumbai - 400 052, State of Maharashtra, India. The following specification particularly describes the invention and the manner in which it is to be performed: - Field of the invention This invention relates to an improved process for the preparation of solid isopropyl-N-(3-chlorophenyl) carbamate. The invention is disclosed in the context of an improved process for solidifying isopropyl-N-(3-chlorophenyl) carbamate during the final processing steps of a isopropyl-N-(3-chlorophenyl) carbamate manufacturing process and finally obtaining the solid small particles. Prior Art Isopropyl-N-(3-chlorophenyl) carbamate or Chlorpropham (CIPC) as it is more commonly known is used as a sprout inhibitor for storage of tubers, such as potatoes, for up to several months. Untreated tubers, in spite of storing in dark at low temperatures will generally sprout over time even in the absence of light. If the sprouting is allowed to continue unchecked, the tubers become commercially worthless. CIPC inhibits potato sprout development by interfering with spindle formation during cell division. Cell division is extremely important during the wound healing or curing period after potatoes are placed into storage. Wound healing requires the production of two to five new cell layers formed by cell division. If CIPC is applied to the potatoes before wound-healing process is complete, excessive losses due to tuber dehydration and disease can occur. CIPC may be applied any time after the wound healing process is complete but before the tubers break dormancy in early spring. In order to suppress the sprouting of a tuber, the tuber must be covered with a thin film of chlorpropham. CIPC is generally applied to the potatoes as an aerosol or as an emulsifiable concentrate. The emulsifiable concentrate is generally applied to the potatoes as a direct spray during the fresh packing operation. CIPC aerosols are generally applied to potatoes in bulk storage. The use of CIPC as a sprout inhibitor was first reported in 1952 by Marth. CIPC has a melting point of about 41°C, a vapourization temperature of about 246° C and a vapour 2 flash point of about 427°C. The ready evaporation of CIPC makes it of interest in the chemical treatment of food products, since only a small amount of residue may be left on the surface of treated food plants [American Potato Journal (1952), 29: 268 - 272]. Several methods have been developed for applying CIPC aerosols to potatoes in bulk storage. US Pat No. 4226179 to Sheldon, III et al. discloses a process whereby CIPC, either without solvent or with a relatively small amount of solvent, is atomized at a temperature of less than 121°C. The aerosol is formed in a fogger having a cylindrical mist chamber in which ultrasonic resonance nozzles atomize the chemical agent. The particles are carried by an airflow duct to a storage chamber containing potatoes. The aerosol condenses on the potatoes, thereby forming a growth inhibiting film thereon. US Pat No. 5723184 to Yamamoto, discloses a process whereby CIPC is heated to a molten state, pressurized, further heated and introduced into a heated air stream that is ducted to a storage chamber containing potatoes. US Pat No. 5935660 to Forsythe, et al. discloses a process similar to the afore-mentioned whereby solid CIPC is melted and then converted to an aerosol either by a pressurized hot air stream or by combustion gas stream. GB 2387797 to Hull John, et al. discloses a fogging machine comprising two separate chambers - one containing the solid CIPC and the other containing a heating device. The CIPC in the first chamber is heated by the heating device and then the heated CIPC is transferred to a fogging head by a pump. The fogging head has a vaporizer to provide vaporization of CIPC, which can then be applied to the potatoes. US Pat No. 4404016 to Zinninger, et al. describes a solution of CIPC prepared by dissolving it in monoethylene glycol and used as a spray for controlling tobacco sucker. FR 2778065 to De Vries rob George, discloses CIPC formulated with a vegetable oil for application to potatoes. 3 WO 2004071196 describes an aqueous composition for use as sprout inhibiting agent for potatoes, comprising chlorpropham and at least one surfactant, thereby avoiding the use of oils and/or solvents. US Publication No. 20030072855 to Robbs, Steven E.; et al., provides a process and apparatus for treating tubers in storage with CIPC dust, formed from larger chunks or blocks of solid CIPC, and inducting the particles into an air stream which transports the particles to a tuber storage shed. The major drawbacks of having aerosols are: 1. clogging of molten CIPC in transport or injector lines; 2. increased risk of scalding and burns to equipment operators, due to leakage of the scalding hot liquid CIPC or the need to repair application equipment containing liquid; 3. equipments require high temperatures and warm up time resulting in high costs; 4. heat stress subjected to the stored tubers/ vegetables; 5. CIPC is supplied commercially dissolved in organic solvents, which are non-eco friendly. Spraying and dusting cause heterogeneity and unevenness of application. [Study of potato sprout inhibitor treatments with chlorpropham, Mededelingen Faculteit Landbouwkundige en Toegepaste Biologische Wetenschappen (Universiteit Gent) (2002), 67(3), 431 - 439]. The use of CIPC in dust form requires the conversion of solid chunks into dust by pulverization. However, during pulverization the temperature may rise above 37 °C and CIPC can start melting. This hampers the formation of a free-flowing dust. The use of liquid CIPC for formulation at an industrial scale may result in spillages leading to accidents during handling. All of the above methods either convert liquid CIPC into aerosols or solid CIPC into dust and are cumbersome, time-consuming and require specialized equipments. At present, commercially manufacturing process for CIPC during the final processing step involves the filling of molten CIPC into the drums. The material over a period of 4 time, say more than 12 hours, becomes solid in drums. During further processing, this solid CIPC requires heating to again get the molten CIPC. This molten CIPC has to be poured, in required quantity, into smaller containers or die preparing pellets, blocks or chunks. These pellets, blocks or chunks are the presently available forms of CIPC in the market. These forms are suitable for further use during the treatment of tubers in storage chambers for sprout inhibition. Thus, the preparation of solid pellets, blocks or chunks from the commercially available CIPC in drums is a time-consuming process and only leads to added cost incurred due to re-processing. The above said, existing technology for converting liquid CIPC into its solid form comprises pouring molten CIPC at 70 °C in trays or blocks and allowing natural cooling of the material for more than 48 hours. However, solid CIPC produced in this manner is brittle and not thermo stable and the process is also cumbersome requiring large production area. Besides this, CIPC has super cooling property and hence, if kept in trays for solidification, it may take several hours to solidify even at low temperatures. The thermal conductivity of CIPC is poor and so solidification poses a major problem. What is needed is an improved for the preparation of solid isopropyl-N-(3-chlorophenyl) carbamate during the final processing stage of the CIPC manufacturing process, without filling of molten CIPC into drums; without re-heating the drums to obtain molten CIPC; with out pouring the molten CIPC into blocks or trays to form blocks or chunks; and which does not require the micronising of these blocks or chunks to get the small solid particles. Objects of Invention The present invention provides an improved process for the preparation of solid isopropyl-N-(3-chlorophenyl) carbamate. The present invention provides a commercial scale process for solidification of liquid CIPC. It further provides a process for preparing solid forms of CIPC, which may be used for generating pellets or tablets, blocks/chunks which in turn can be used to generate fumes to treat stored tubers and have better hardness and stability. The process includes the steps of forming small solid particles of 5 CIPC from the molten mass of CIPC during the last stage of its manufacturing process at commercial production level. Another object of the present invention is to provide an improved process for the preparation of solid isopropyl-N-(3-chlorophenyl) carbamate. Another object of the present invention is to provide an improved process for the preparation of solid from molten isopropyl-N-(3-chlorophenyl) carbamate that is commercially viable and effective for large scale conversion of liquid isopropyl-N-(3-chlorophenyl) carbamate into solid form. Yet another object of the present invention is to provide an improved process for the preparation of solid small particles of liquid isopropyl-N-(3-chlorophenyl) carbamate that provides solid forms which can be used directly for generating fumes to treat stored tubers. Yet another object of the present invention is to provide an improved process for the solidification of liquid isopropyl-N-(3-chlorophenyl) carbamate wherein further reprocessing is avoided thereby rendering it more economical and hassle-free. Still another object of the present invention is to provide an improved process for the solidification of liquid isopropyl-N-(3-chlorophenyl)carbamate that results into solid forms which are more thermo stable and have better hardness than existing solid forms. Yet another object of the present invention is to provide an improved process for the preparation of solid forms from the liquid isopropyl-N-(3-chlorophenyl) carbamate which are easier to handle and transport. Still yet another object of the present invention is to provide an improved process for the preparation of solid isopropyl-N-(3-chlorophenyl) carbamate without filling of molten CIPC into drums, blocks/chunks. 6 Still another object of the present invention is to provide an improved process for the preparation of solid isopropyl-N-(3-chlorophenyl) carbamate which does not require the re-heating the drums to obtain molten CIPC. Still yet another object of the present invention is to provide an improved process for the preparation of solid isopropyl-N-(3-chlorophenyl) carbamate which does not require the pouring of the molten CIPC into blocks or trays to form blocks or chunks. Still another object of the present invention is to provide an improved process for the preparation of solid isopropyl-N-(3-chlorophenyl) carbamate which does not require the micronising of blocks/chunks to get the small solid particles. Description of the Invention Accordingly, the present invention provides an improved process for the large scale preparation of solid isopropyl-N-(3-chlorophenyl) carbamate (CIPC) which yields solid CIPC that can be further converted into solid dosage forms such as tablets, pellets, blocks, chunks, etc. used for generating fumes to treat stored tubers. The instant invention includes the formation of small solid particles of CIPC at one site, by stirring the molten form of CIPC, available during the last stage of the commercial manufacturing process, to form semi-solid mass; feeding this mass on to drum flaker to obtain flakes; grinding these flakes in multimill to get the small solid particles which are less than the sieve used in the multimill. These particles are optionally compressed with a pressure of 15 to 300 Kg/cm2 to form tablets, pellets etc. This invention includes the proper stirring of the feed (molten) CIPC under controlled temperature and rpm (rotation per minutes) conditions; the semi-solid mass obtained after the stirring, is fed on to the drum flaker (running at constant rpm and controlled temperature condition) to get flakes; these flakes is later fed into the multimill, running under controlled temperature at constant rpm to provide the desirable size solid particles. 7 The CIPC is a waxy type of crystalline material, it is not effectively micronised in a high speed blended device. The temperature control is necessary during the complete process of making/preparing small solid particles as during grinding of flakes, rise in temperature occurs by the friction between flakes and blades. This needs to be avoided as increase in the temperature may be sufficient causes some melting at the surface of particles, finally results in agglomeration. This agglomeration may tend to minimize the grinding efficiency of multimill. Maintaining the temperature, throughout the process, provides the CIPC flakes which are more fragile and with reduced agglomeration. According to the present invention, an improved process for the preparation of solid isopropyl-N-(3-chlorophenyl) carbamate (CIPC) comprises: a. stirring of molten CIPC at 100 - 5000 rpm at a temperature ranging between -20 to 35 °C, till solidification is initiated to obtain semi-solid mass; b. feeding the semi-solid mass of step 1, on to a drum flaker maintained at -10 to 35°C with rpm between 1 - 60, to obtain flakes; c. maintaining the temperature of flakes, obtained in the step 2, between 5 - 25 ° C; d. grinding the flakes in a multi mill, with 1-5 mm sieve, at a temperature ranging from -5 to 25 °C; to obtain the solid isopropyl-N-(3-chlorophenyl) carbamate (CIPC). e. optionally, compressing the powder obtained in the above step at 15 to 300 kg/cm pressure to form tablets or pellets . The solid isopropyl-N-(3-chlorophenyl) carbamate (CIPC) obtained above may be compressed in solid forms i.e. tablets or pellets with 15 to 300 Kg/cm2 pressure. The solid forms i.e. tablets or pellets are packed in suitable containers and sold. The consumer can directly empty these in the fumigator and hence handling of CIPC can be avoided. Also, the solid forms thus produced have superior hardness and are thermostable over the existing solid CIPC forms available in the market. The process is simpler and space limitations do not hamper the production. The pellets thus prepared may also be used to make an EC formulation by just dissolving them in the required solvent. In a typical manufacturing process, a stirring vessel is coupled to a drum-flaker via a 8 transfer means. The stirring vessel is mounted below the vessel having molten CIPC finally in the commercial manufacturing process of CIPC. The stirring vessel is equipped with a prototype stirrer having a rpm (rotation per minute) variation of 100 to 5000 rpm controlled by an electrical rpm controlling system. The stirring vessel is also having a temperature control from -20 to 100° C. It shall be obvious that other types of temperature and rpm controlling system will serve equally well. Though not specifically shown, a vessel, a transfer means, valve, vent or any other container having the requisite output, may be substituted for the stirring vessel. The vessel has a feed chute into which molten CIPC is fed. The agitator of the vessel, stir the molten CIPC to initiate the solidification process. This semi-solid mass, as it exit through outlet port, comprises of a fraction of molten CIPC. A drum flaker, positioned adjacent to the outlet port. The drum flaker has a receiver where the semisolid mass drops from the outlet port of the vessel. The said receiver conveys the semi solid mass onto the roller of the drum flaker. The drum flaker is provided with a temperature control system, capable of maintaining a temperature of-10 to 50° C. The rollers are provided with a speed control system which can provide a movement of 1 to 100 rpm to rollers. The drum flaker finally provides the flakes which are free flowing. A multimill, positioned beneath the discharge/outlet port of drum flaker. The feed chute of multimill, into which the flakes were fed and supply these flakes to the grinding / working section of multimill. The multimill is having the arrangement to select the sieve of 1 to 5 mm or so and also have the controlled temperature arrangement from -20 to 60 °C. The ground solid particles comprised of particles having a major dimension of generally less then the sieve size selected. The said ground solid particles are sufficiently free flowing solid particles and can optionally be compressed with 15 to 300 Kg/cm2 pressure to form tablets, pellets, blocks/chunks etc. of required size, weight and /or shape. In present invention, the manufacturing process comprises the liquid CIPC, obtained at a temperature of 70 - 80 °C, is poured in a vessel equipped with cooling facility and a mechanical stirrer/agitator with rpm control. The stirring is maintained between 100 -5000 rpm, preferably 200 - 1000 rpm, and the temperature is maintained between -10 to 35°C, preferably 20 - 25 °C till the process of solidification is initiated. Thereafter this 9 semi-solid mass is fed on to a drum-fakers already maintained at 5 to 25 °C, preferably 15 to 20 °C, with roller movement maintained between 1-60 rpm, preferably 5-10 rpm, to get the flakes. These flakes, thus obtained, are then fed into the multimill having the required size sieve and its temperature maintained between -5 to 25 °C, preferably 5 to 15 °C. This temperature may be achieved by using a coolant either directly in contact with the CIPC flakes or indirectly by conventional methods known in the art. The coolants known in the art may be selected from liquid nitrogen, dry ice, chilled water, liquid helium, etc. A fine powder of CIPC is obtained. The fineness and particle size of the powder obtained depends upon the sieve used in multimill, which may be selected from 1 to 3 mm, preferably 1-3 mm. The fine powder obtained as per the process of this invention, may optionally be further converted into other solid dosage forms such as tablets, pellets, blocks/chunks etc. for selected dosages. This may be done by compressing the powder in desired quantity, in the required size mould and shapes, under pressure ranging from 15 - 300 kg/ cm preferably 100 - 150 kg/ cm . These tablet, pellets, blocks/chunks etc. may be directly used for further consumption. Even this powder can be directly packed and supplied for use for manufacturing tablets, pellets, blocks/chunks etc. even for direct use in apparatus used for treatment of stored tubers in small or large storage facilities. The solid forms thus produced are stable at temperatures up to 40° C whereas conventional solid CIPC is very brittle and melts at temperatures above 37° C. The CIPC pellets obtained by the process of this invention also have superior hardness and hence, do not melt at temperatures up to 40° C. As the solid CIPC produced by the method of the present invention has superior hardness the solid dosage forms can be directly packaged into suitable containers and sold. The end user can directly empty the contents into the fumigator and thereby avoid handling of the solid CIPC. The process of the present invention produces small pellets of CIPC so re-processing is not necessary. In this way the requirement for reprocessing like re-melting, building blocks/chunks, pulverizing is avoided thereby making the invented process very economical viable. The following examples are illustrative of the invention but not limitative of the scope thereof. 10 Example 1 500 gm of molten Chlorpropham (CIPC) at 70° C was transferred into a stainless steel vessel equipped with a mechanical stirrer having rpm controls. It was cooled to 30° C and stirring was maintained at 300 rpm. After 20 min of stirring process for solidification initiated to obtain semi-solid mass. This semi-solid mass was then fed on to a drum flakers moving at 10 rpm and maintained at a temperature of 15° G. Complete solidification occurred in the form of flakes immediately. The flakes thus obtained were ground at 10° C in a multi mill having a sieve with mesh size of 2 mm. The fine powder thus obtained was compressed at 100-kg/ cm into (20 x 10) mm pellets. Example 2 Same as in Example 1 except that the temperature of the molten Chlorpropham (CIPC) in the stainless steel vessel was lowered to 10° C. After 12 min of stirring, process of solidification (crystallization) initiated and semi-solid mass was seen. Complete solidification occurred in the mass on the drum flakers immediately. Example 3 Same as in Example 1 except that the temperature of the molten/liquid Chlorpropham (CIPC) in the stainless steel vessel was lowered to -8° C. After 4 min of stirring, process of solidification (crystallization) initiated and semi-solid mass was seen. Complete solidification occurred in the mass on the drum flakers immediately. Example 4 500 gm of molten/liquid Chlorpropham (CIPC) at 70° C was transferred into a stainless steel vessel. It was allowed to cool under natural conditions to 30° C without stirring. The process of solidification (Crystallization) initiated by the end of 10th hours and complete solidification occurred by 46 hours in the vessel itself. A lump of solid CIPC was obtained. 11 Example 5 500 gm of molten/liquid Chlorpropham (CIPC) at 70° C was transferred into a stainless steel vessel. It was allowed to cool at a temperature of -8° C, without stirring. The process of solidification (Crystallization) initiated by the end of 15 min and complete solidification occurred by 2 hours in the vessel itself. A lump of solid CIPC was obtained. Example 6 500 gm of molten/liquid Chlorpropham (CIPC) at 70° C was transferred into a stainless steel vessel equipped with a mechanical stirrer having rpm controls. It was cooled to 30° C and stirring was maintained at 100 rpm. After 35 min of stirring the process of solidification (crystallization) initiated. This semi-solid mass was then fed on to a drum flakers maintained at rpm of 10 and temperature of 15° C. Complete solidification occurred in the mass immediately on the drum flakers resulting into the flakes. The flakes thus obtained were ground at 10 °C in a multi mill having a sieve with mesh size of 2 mm. The fine powder thus obtained was compressed at 100 kg/ cm2 into (20 x 10) mm2 pellets. Example 7 Same as in Example 6 except that the temperature of the molten/liquid CIPC in the stainless steel vessel was lowered to -8° C. After 8 min of stirring the process of solidification (crystallization) initiated and semi-solid mass started to form in it. This semi-solid mass was then fed on to a drum flakers moving at 10 rpm and maintained at a temperature of 15° C. Complete solidification occurred in the mass on the drum flakers immediately resulting in the flakes. Example 8 Same as in Example 6 except that the stirring in the stainless steel reaction vessel was maintained at 1000 rpm. After 18 min of stirring the process of solidification (crystallization) was seen in it. This semi-solid mass was then fed on to a drum flakers moving with lOrpm and at a temperature of 15° C. Complete solidification occurred in the mass on the drum flakers immediately resulting in the flakes. 12 claim, 1. An improved process for the preparation of solid isopropyl-N- (3-chlorophenyl) carbamate (CIPC) comprising :- a. stirring of molten CIPC at 100 - 5000 rpm at a temperature ranging between -20 to 35° C, till solidification is initiated to obtain semi-solid mass; b. feeding the semi-solid mass of step 1, on to a drum flaker maintained at - 10 to 35° C with rpm between 1 - 60, to obtain flakes; c. maintaining the temperature of flakes, obtained in the step 2, between 5 - 25° C; d. grinding the flakes in a multi mill, with 1-5 mm sieve, at a temperature ranging from -5 to 25° C; to obtain the solid isopropyl-N-(3-chlorophenyl) carbamate (CIPC); e. optionally, compressing the powder obtained in the above step (d) at 15 to 300 kg/cm pressure to form tablets, pellets, blocks/chunks etc . 2. An improved process for the preparation of solid isopropyl-N- (3-chlorophenyl) carbamate (CIPC) as claimed in claim 1, wherein the molten CIPC is stirred at 200 to 1000 rpm. 3. An improved process for the preparation of solid isopropyl-N- (3-chlorophenyl) carbamate (CIPC) as claimed in claim 1, wherein the temperature during stirring of molten CIPC is maintained between 20 to 25° C. 4. An improved process for the preparation of solid isopropyl-N- (3-chlorophenyl) carbamate (CIPC) as claimed in claim 1, wherein the temperature of drum flakers is maintained between 15 - 20° C. 5. An improved process for the preparation of solid isopropyl-N- (3-chlorophenyl) carbamate (CIPC) as claimed in claim 1, wherein the roller of drum flakers is moving between 5-10 rpm. 13 6. An improved process for the preparation of solid isopropyl-N- (3-chlorophenyl) carbamate (CIPC) as claimed in claim 1, wherein the grinding of the flakes in multimill is done at a temperature from 5 - 15 °C. 7. An improved process for the preparation of solid isopropyl-N- (3-chlorophenyl) carbamate (CIPC) as claimed in claim 1, wherein the size of sieve used in the miltimill is from 1-3 mm. 8. An improved process for the preparation of solid isopropyl-N- (3-chlorophenyl) carbamate (CIPC) as claimed in claim 1, wherein the solid CIPC obtained is optionally compressed in the form of tablets, pellets, blocks/chunks etc. 9. An improved process for the preparation of solid isopropyl-N- (3-chlorophenyl) carbamate (CIPC) as claimed in claim 8, wherein the tablets, pellets, blocks/chunks etc. are obtained by using a pressure in the range of 100 - 200 kg/ cm . 10. An improved process for the preparation of solid isopropyl-N- (3-chlorophenyl) carbamate (CIPC) as substantially herein described in claims 1 - 9 and with reference to the aforesaid examples. 14 ABSTRACT An improved process for the preparation of solid isopropyl-N- (3-chlorophenyl) carbamate (CIPC) without the need for filling the molten CIPC into the drums directly in the plant during the last step of commercial production, for further transport, comprising of stirring of molten CIPC, between 100 - 5000 rpm at a temperature ranging between -20 to 35 °C, to initiate the solidification for semisolid mass; feeding the semi-solid mass on to a drum flakers maintained at -10 to 35°C with rpm between 1 - 60, to obtain flakes; maintaining the temperature of flakes between 5 - 25 ° C; grinding the flakes in a multi mill, with 1-5 mm sieve, at a temperature ranging from -5 to 25 °C; to obtain the solid isopropyl-N-(3-chlorophenyl) carbamate (CIPC) . This powder is optionally, compressed with a pressure of 15 to 300 kg/cm2 to form tablets, pellets, blocks/chunks of isopropyl-N-(3-cholorophenyl) carbamate. To, The Controller of Patents, Patent Office, Mumbai 15

Full Text

FORM 2
THE PATENTS ACT, 1970
(39 of 1970)
COMPLETE SPECIFICATION
(See Section 10; Rule 13)
AN IMPROVED PROCESS FOR THE PREPARATION OF SOLID ISOPROPYL-N-(3-CHLOROPHENYL) CARBAMATE
We, UNITED PHOSPHORUS LIMITED, a company incorporated under the Companies Act, 1956 and having its registered office at 3-11, GIDC, Vapi-396 195, State of Gujarat, India and having its office at Uniphos House, 11th Road, C. D. Marg, Khar (West), Mumbai - 400 052, State of Maharashtra, India.
The following specification particularly describes the invention and the manner in which it is to be performed: -

Field of the invention
This invention relates to an improved process for the preparation of solid isopropyl-N-(3-chlorophenyl) carbamate. The invention is disclosed in the context of an improved process for solidifying isopropyl-N-(3-chlorophenyl) carbamate during the final processing steps of a isopropyl-N-(3-chlorophenyl) carbamate manufacturing process and finally obtaining the solid small particles.
Prior Art
Isopropyl-N-(3-chlorophenyl) carbamate or Chlorpropham (CIPC) as it is more commonly known is used as a sprout inhibitor for storage of tubers, such as potatoes, for up to several months. Untreated tubers, in spite of storing in dark at low temperatures will generally sprout over time even in the absence of light. If the sprouting is allowed to continue unchecked, the tubers become commercially worthless.
CIPC inhibits potato sprout development by interfering with spindle formation during cell division. Cell division is extremely important during the wound healing or curing period after potatoes are placed into storage. Wound healing requires the production of two to five new cell layers formed by cell division. If CIPC is applied to the potatoes before wound-healing process is complete, excessive losses due to tuber dehydration and disease can occur. CIPC may be applied any time after the wound healing process is complete but before the tubers break dormancy in early spring. In order to suppress the sprouting of a tuber, the tuber must be covered with a thin film of chlorpropham. CIPC is generally applied to the potatoes as an aerosol or as an emulsifiable concentrate. The emulsifiable concentrate is generally applied to the potatoes as a direct spray during the fresh packing operation. CIPC aerosols are generally applied to potatoes in bulk storage.
The use of CIPC as a sprout inhibitor was first reported in 1952 by Marth. CIPC has a melting point of about 41°C, a vapourization temperature of about 246° C and a vapour
2

flash point of about 427°C. The ready evaporation of CIPC makes it of interest in the chemical treatment of food products, since only a small amount of residue may be left on the surface of treated food plants [American Potato Journal (1952), 29: 268 - 272]. Several methods have been developed for applying CIPC aerosols to potatoes in bulk storage.
US Pat No. 4226179 to Sheldon, III et al. discloses a process whereby CIPC, either without solvent or with a relatively small amount of solvent, is atomized at a temperature of less than 121°C. The aerosol is formed in a fogger having a cylindrical mist chamber in which ultrasonic resonance nozzles atomize the chemical agent. The particles are carried by an airflow duct to a storage chamber containing potatoes. The aerosol condenses on the potatoes, thereby forming a growth inhibiting film thereon.
US Pat No. 5723184 to Yamamoto, discloses a process whereby CIPC is heated to a molten state, pressurized, further heated and introduced into a heated air stream that is ducted to a storage chamber containing potatoes. US Pat No. 5935660 to Forsythe, et al. discloses a process similar to the afore-mentioned whereby solid CIPC is melted and then converted to an aerosol either by a pressurized hot air stream or by combustion gas stream.
GB 2387797 to Hull John, et al. discloses a fogging machine comprising two separate chambers - one containing the solid CIPC and the other containing a heating device. The CIPC in the first chamber is heated by the heating device and then the heated CIPC is transferred to a fogging head by a pump. The fogging head has a vaporizer to provide vaporization of CIPC, which can then be applied to the potatoes.
US Pat No. 4404016 to Zinninger, et al. describes a solution of CIPC prepared by dissolving it in monoethylene glycol and used as a spray for controlling tobacco sucker.
FR 2778065 to De Vries rob George, discloses CIPC formulated with a vegetable oil for application to potatoes.
3

WO 2004071196 describes an aqueous composition for use as sprout inhibiting agent for potatoes, comprising chlorpropham and at least one surfactant, thereby avoiding the use of oils and/or solvents.
US Publication No. 20030072855 to Robbs, Steven E.; et al., provides a process and apparatus for treating tubers in storage with CIPC dust, formed from larger chunks or blocks of solid CIPC, and inducting the particles into an air stream which transports the particles to a tuber storage shed.
The major drawbacks of having aerosols are:
1. clogging of molten CIPC in transport or injector lines;
2. increased risk of scalding and burns to equipment operators, due to leakage of the scalding hot liquid CIPC or the need to repair application equipment containing liquid;
3. equipments require high temperatures and warm up time resulting in high costs;
4. heat stress subjected to the stored tubers/ vegetables;
5. CIPC is supplied commercially dissolved in organic solvents, which are non-eco friendly.
Spraying and dusting cause heterogeneity and unevenness of application. [Study of potato sprout inhibitor treatments with chlorpropham, Mededelingen Faculteit Landbouwkundige en Toegepaste Biologische Wetenschappen (Universiteit Gent) (2002), 67(3), 431 - 439]. The use of CIPC in dust form requires the conversion of solid chunks into dust by pulverization. However, during pulverization the temperature may rise above 37 °C and CIPC can start melting. This hampers the formation of a free-flowing dust. The use of liquid CIPC for formulation at an industrial scale may result in spillages leading to accidents during handling.
All of the above methods either convert liquid CIPC into aerosols or solid CIPC into dust and are cumbersome, time-consuming and require specialized equipments.
At present, commercially manufacturing process for CIPC during the final processing step involves the filling of molten CIPC into the drums. The material over a period of
4

time, say more than 12 hours, becomes solid in drums. During further processing, this solid CIPC requires heating to again get the molten CIPC. This molten CIPC has to be poured, in required quantity, into smaller containers or die preparing pellets, blocks or chunks. These pellets, blocks or chunks are the presently available forms of CIPC in the market. These forms are suitable for further use during the treatment of tubers in storage chambers for sprout inhibition. Thus, the preparation of solid pellets, blocks or chunks from the commercially available CIPC in drums is a time-consuming process and only leads to added cost incurred due to re-processing.
The above said, existing technology for converting liquid CIPC into its solid form comprises pouring molten CIPC at 70 °C in trays or blocks and allowing natural cooling of the material for more than 48 hours. However, solid CIPC produced in this manner is brittle and not thermo stable and the process is also cumbersome requiring large production area. Besides this, CIPC has super cooling property and hence, if kept in trays for solidification, it may take several hours to solidify even at low temperatures. The thermal conductivity of CIPC is poor and so solidification poses a major problem.
What is needed is an improved for the preparation of solid isopropyl-N-(3-chlorophenyl) carbamate during the final processing stage of the CIPC manufacturing process, without filling of molten CIPC into drums; without re-heating the drums to obtain molten CIPC; with out pouring the molten CIPC into blocks or trays to form blocks or chunks; and which does not require the micronising of these blocks or chunks to get the small solid particles.
Objects of Invention
The present invention provides an improved process for the preparation of solid isopropyl-N-(3-chlorophenyl) carbamate. The present invention provides a commercial scale process for solidification of liquid CIPC. It further provides a process for preparing solid forms of CIPC, which may be used for generating pellets or tablets, blocks/chunks which in turn can be used to generate fumes to treat stored tubers and have better hardness and stability. The process includes the steps of forming small solid particles of
5

CIPC from the molten mass of CIPC during the last stage of its manufacturing process at commercial production level.
Another object of the present invention is to provide an improved process for the preparation of solid isopropyl-N-(3-chlorophenyl) carbamate.
Another object of the present invention is to provide an improved process for the preparation of solid from molten isopropyl-N-(3-chlorophenyl) carbamate that is commercially viable and effective for large scale conversion of liquid isopropyl-N-(3-chlorophenyl) carbamate into solid form.
Yet another object of the present invention is to provide an improved process for the preparation of solid small particles of liquid isopropyl-N-(3-chlorophenyl) carbamate that provides solid forms which can be used directly for generating fumes to treat stored tubers.
Yet another object of the present invention is to provide an improved process for the solidification of liquid isopropyl-N-(3-chlorophenyl) carbamate wherein further reprocessing is avoided thereby rendering it more economical and hassle-free.
Still another object of the present invention is to provide an improved process for the solidification of liquid isopropyl-N-(3-chlorophenyl)carbamate that results into solid forms which are more thermo stable and have better hardness than existing solid forms.
Yet another object of the present invention is to provide an improved process for the preparation of solid forms from the liquid isopropyl-N-(3-chlorophenyl) carbamate which are easier to handle and transport.
Still yet another object of the present invention is to provide an improved process for the preparation of solid isopropyl-N-(3-chlorophenyl) carbamate without filling of molten CIPC into drums, blocks/chunks.
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Still another object of the present invention is to provide an improved process for the preparation of solid isopropyl-N-(3-chlorophenyl) carbamate which does not require the re-heating the drums to obtain molten CIPC.
Still yet another object of the present invention is to provide an improved process for the preparation of solid isopropyl-N-(3-chlorophenyl) carbamate which does not require the pouring of the molten CIPC into blocks or trays to form blocks or chunks.
Still another object of the present invention is to provide an improved process for the preparation of solid isopropyl-N-(3-chlorophenyl) carbamate which does not require the micronising of blocks/chunks to get the small solid particles.
Description of the Invention
Accordingly, the present invention provides an improved process for the large scale preparation of solid isopropyl-N-(3-chlorophenyl) carbamate (CIPC) which yields solid CIPC that can be further converted into solid dosage forms such as tablets, pellets, blocks, chunks, etc. used for generating fumes to treat stored tubers.
The instant invention includes the formation of small solid particles of CIPC at one site, by stirring the molten form of CIPC, available during the last stage of the commercial manufacturing process, to form semi-solid mass; feeding this mass on to drum flaker to obtain flakes; grinding these flakes in multimill to get the small solid particles which are less than the sieve used in the multimill. These particles are optionally compressed with a pressure of 15 to 300 Kg/cm2 to form tablets, pellets etc.
This invention includes the proper stirring of the feed (molten) CIPC under controlled temperature and rpm (rotation per minutes) conditions; the semi-solid mass obtained after the stirring, is fed on to the drum flaker (running at constant rpm and controlled temperature condition) to get flakes; these flakes is later fed into the multimill, running under controlled temperature at constant rpm to provide the desirable size solid particles.
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The CIPC is a waxy type of crystalline material, it is not effectively micronised in a high speed blended device. The temperature control is necessary during the complete process of making/preparing small solid particles as during grinding of flakes, rise in temperature occurs by the friction between flakes and blades. This needs to be avoided as increase in the temperature may be sufficient causes some melting at the surface of particles, finally results in agglomeration. This agglomeration may tend to minimize the grinding efficiency of multimill. Maintaining the temperature, throughout the process, provides the CIPC flakes which are more fragile and with reduced agglomeration.
According to the present invention, an improved process for the preparation of solid isopropyl-N-(3-chlorophenyl) carbamate (CIPC) comprises:
a. stirring of molten CIPC at 100 - 5000 rpm at a temperature ranging between -20
to 35 °C, till solidification is initiated to obtain semi-solid mass;
b. feeding the semi-solid mass of step 1, on to a drum flaker maintained at -10 to
35°C with rpm between 1 - 60, to obtain flakes;
c. maintaining the temperature of flakes, obtained in the step 2, between 5 - 25 ° C;
d. grinding the flakes in a multi mill, with 1-5 mm sieve, at a temperature ranging
from -5 to 25 °C; to obtain the solid isopropyl-N-(3-chlorophenyl) carbamate
(CIPC).
e. optionally, compressing the powder obtained in the above step at 15 to 300
kg/cm pressure to form tablets or pellets .
The solid isopropyl-N-(3-chlorophenyl) carbamate (CIPC) obtained above may be compressed in solid forms i.e. tablets or pellets with 15 to 300 Kg/cm2 pressure. The solid forms i.e. tablets or pellets are packed in suitable containers and sold. The consumer can directly empty these in the fumigator and hence handling of CIPC can be avoided. Also, the solid forms thus produced have superior hardness and are thermostable over the existing solid CIPC forms available in the market. The process is simpler and space limitations do not hamper the production. The pellets thus prepared may also be used to make an EC formulation by just dissolving them in the required solvent.
In a typical manufacturing process, a stirring vessel is coupled to a drum-flaker via a
8

transfer means. The stirring vessel is mounted below the vessel having molten CIPC finally in the commercial manufacturing process of CIPC. The stirring vessel is equipped with a prototype stirrer having a rpm (rotation per minute) variation of 100 to 5000 rpm controlled by an electrical rpm controlling system. The stirring vessel is also having a temperature control from -20 to 100° C. It shall be obvious that other types of temperature and rpm controlling system will serve equally well. Though not specifically shown, a vessel, a transfer means, valve, vent or any other container having the requisite output, may be substituted for the stirring vessel.
The vessel has a feed chute into which molten CIPC is fed. The agitator of the vessel, stir the molten CIPC to initiate the solidification process. This semi-solid mass, as it exit through outlet port, comprises of a fraction of molten CIPC. A drum flaker, positioned adjacent to the outlet port. The drum flaker has a receiver where the semisolid mass drops from the outlet port of the vessel. The said receiver conveys the semi solid mass onto the roller of the drum flaker. The drum flaker is provided with a temperature control system, capable of maintaining a temperature of-10 to 50° C. The rollers are provided with a speed control system which can provide a movement of 1 to 100 rpm to rollers. The drum flaker finally provides the flakes which are free flowing. A multimill, positioned beneath the discharge/outlet port of drum flaker. The feed chute of multimill, into which the flakes were fed and supply these flakes to the grinding / working section of multimill. The multimill is having the arrangement to select the sieve of 1 to 5 mm or so and also have the controlled temperature arrangement from -20 to 60 °C. The ground solid particles comprised of particles having a major dimension of generally less then the sieve size selected. The said ground solid particles are sufficiently free flowing solid particles and can optionally be compressed with 15 to 300 Kg/cm2 pressure to form tablets, pellets, blocks/chunks etc. of required size, weight and /or shape.
In present invention, the manufacturing process comprises the liquid CIPC, obtained at a temperature of 70 - 80 °C, is poured in a vessel equipped with cooling facility and a mechanical stirrer/agitator with rpm control. The stirring is maintained between 100 -5000 rpm, preferably 200 - 1000 rpm, and the temperature is maintained between -10 to 35°C, preferably 20 - 25 °C till the process of solidification is initiated. Thereafter this
9

semi-solid mass is fed on to a drum-fakers already maintained at 5 to 25 °C, preferably 15 to 20 °C, with roller movement maintained between 1-60 rpm, preferably 5-10 rpm, to get the flakes. These flakes, thus obtained, are then fed into the multimill having the required size sieve and its temperature maintained between -5 to 25 °C, preferably 5 to 15 °C. This temperature may be achieved by using a coolant either directly in contact with the CIPC flakes or indirectly by conventional methods known in the art. The coolants known in the art may be selected from liquid nitrogen, dry ice, chilled water, liquid helium, etc. A fine powder of CIPC is obtained. The fineness and particle size of the powder obtained depends upon the sieve used in multimill, which may be selected from 1 to 3 mm, preferably 1-3 mm. The fine powder obtained as per the process of this invention, may optionally be further converted into other solid dosage forms such as tablets, pellets, blocks/chunks etc. for selected dosages. This may be done by compressing the powder in desired quantity, in the required size mould and shapes, under pressure ranging from 15 - 300 kg/ cm preferably 100 - 150 kg/ cm . These tablet, pellets, blocks/chunks etc. may be directly used for further consumption. Even this powder can be directly packed and supplied for use for manufacturing tablets, pellets, blocks/chunks etc. even for direct use in apparatus used for treatment of stored tubers in small or large storage facilities.
The solid forms thus produced are stable at temperatures up to 40° C whereas conventional solid CIPC is very brittle and melts at temperatures above 37° C. The CIPC pellets obtained by the process of this invention also have superior hardness and hence, do not melt at temperatures up to 40° C. As the solid CIPC produced by the method of the present invention has superior hardness the solid dosage forms can be directly packaged into suitable containers and sold. The end user can directly empty the contents into the fumigator and thereby avoid handling of the solid CIPC. The process of the present invention produces small pellets of CIPC so re-processing is not necessary. In this way the requirement for reprocessing like re-melting, building blocks/chunks, pulverizing is avoided thereby making the invented process very economical viable.
The following examples are illustrative of the invention but not limitative of the scope thereof.
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Example 1
500 gm of molten Chlorpropham (CIPC) at 70° C was transferred into a stainless steel vessel equipped with a mechanical stirrer having rpm controls. It was cooled to 30° C and stirring was maintained at 300 rpm. After 20 min of stirring process for solidification initiated to obtain semi-solid mass. This semi-solid mass was then fed on to a drum flakers moving at 10 rpm and maintained at a temperature of 15° G. Complete solidification occurred in the form of flakes immediately. The flakes thus obtained were ground at 10° C in a multi mill having a sieve with mesh size of 2 mm. The fine powder thus obtained was compressed at 100-kg/ cm into (20 x 10) mm pellets.
Example 2
Same as in Example 1 except that the temperature of the molten Chlorpropham (CIPC) in the stainless steel vessel was lowered to 10° C. After 12 min of stirring, process of solidification (crystallization) initiated and semi-solid mass was seen. Complete solidification occurred in the mass on the drum flakers immediately.
Example 3
Same as in Example 1 except that the temperature of the molten/liquid Chlorpropham (CIPC) in the stainless steel vessel was lowered to -8° C. After 4 min of stirring, process of solidification (crystallization) initiated and semi-solid mass was seen. Complete solidification occurred in the mass on the drum flakers immediately.
Example 4
500 gm of molten/liquid Chlorpropham (CIPC) at 70° C was transferred into a stainless steel vessel. It was allowed to cool under natural conditions to 30° C without stirring. The process of solidification (Crystallization) initiated by the end of 10th hours and complete solidification occurred by 46 hours in the vessel itself. A lump of solid CIPC was obtained.
11

Example 5
500 gm of molten/liquid Chlorpropham (CIPC) at 70° C was transferred into a stainless steel vessel. It was allowed to cool at a temperature of -8° C, without stirring. The process of solidification (Crystallization) initiated by the end of 15 min and complete solidification occurred by 2 hours in the vessel itself. A lump of solid CIPC was obtained.
Example 6
500 gm of molten/liquid Chlorpropham (CIPC) at 70° C was transferred into a stainless steel vessel equipped with a mechanical stirrer having rpm controls. It was cooled to 30° C and stirring was maintained at 100 rpm. After 35 min of stirring the process of solidification (crystallization) initiated. This semi-solid mass was then fed on to a drum flakers maintained at rpm of 10 and temperature of 15° C. Complete solidification occurred in the mass immediately on the drum flakers resulting into the flakes. The flakes thus obtained were ground at 10 °C in a multi mill having a sieve with mesh size of 2 mm. The fine powder thus obtained was compressed at 100 kg/ cm2 into (20 x 10) mm2 pellets.
Example 7
Same as in Example 6 except that the temperature of the molten/liquid CIPC in the stainless steel vessel was lowered to -8° C. After 8 min of stirring the process of solidification (crystallization) initiated and semi-solid mass started to form in it. This semi-solid mass was then fed on to a drum flakers moving at 10 rpm and maintained at a temperature of 15° C. Complete solidification occurred in the mass on the drum flakers immediately resulting in the flakes.
Example 8
Same as in Example 6 except that the stirring in the stainless steel reaction vessel was maintained at 1000 rpm. After 18 min of stirring the process of solidification (crystallization) was seen in it. This semi-solid mass was then fed on to a drum flakers moving with lOrpm and at a temperature of 15° C. Complete solidification occurred in the mass on the drum flakers immediately resulting in the flakes.
12

claim,
1. An improved process for the preparation of solid isopropyl-N- (3-chlorophenyl)
carbamate (CIPC) comprising :-
a. stirring of molten CIPC at 100 - 5000 rpm at a temperature ranging
between -20 to 35° C, till solidification is initiated to obtain semi-solid
mass;
b. feeding the semi-solid mass of step 1, on to a drum flaker maintained at -
10 to 35° C with rpm between 1 - 60, to obtain flakes;
c. maintaining the temperature of flakes, obtained in the step 2, between 5 -
25° C;
d. grinding the flakes in a multi mill, with 1-5 mm sieve, at a temperature
ranging from -5 to 25° C; to obtain the solid isopropyl-N-(3-chlorophenyl)
carbamate (CIPC);
e. optionally, compressing the powder obtained in the above step (d) at 15 to
300 kg/cm pressure to form tablets, pellets, blocks/chunks etc .
2. An improved process for the preparation of solid isopropyl-N- (3-chlorophenyl)
carbamate (CIPC) as claimed in claim 1, wherein the molten CIPC is stirred at 200 to 1000 rpm.
3. An improved process for the preparation of solid isopropyl-N- (3-chlorophenyl)
carbamate (CIPC) as claimed in claim 1, wherein the temperature during stirring of molten CIPC is maintained between 20 to 25° C.
4. An improved process for the preparation of solid isopropyl-N- (3-chlorophenyl)
carbamate (CIPC) as claimed in claim 1, wherein the temperature of drum flakers is maintained between 15 - 20° C.
5. An improved process for the preparation of solid isopropyl-N- (3-chlorophenyl)
carbamate (CIPC) as claimed in claim 1, wherein the roller of drum flakers is moving between 5-10 rpm.
13

6. An improved process for the preparation of solid isopropyl-N- (3-chlorophenyl)
carbamate (CIPC) as claimed in claim 1, wherein the grinding of the flakes in multimill is done at a temperature from 5 - 15 °C.
7. An improved process for the preparation of solid isopropyl-N- (3-chlorophenyl)
carbamate (CIPC) as claimed in claim 1, wherein the size of sieve used in the miltimill is from 1-3 mm.
8. An improved process for the preparation of solid isopropyl-N- (3-chlorophenyl)
carbamate (CIPC) as claimed in claim 1, wherein the solid CIPC obtained is optionally compressed in the form of tablets, pellets, blocks/chunks etc.
9. An improved process for the preparation of solid isopropyl-N- (3-chlorophenyl)
carbamate (CIPC) as claimed in claim 8, wherein the tablets, pellets, blocks/chunks etc. are obtained by using a pressure in the range of 100 - 200 kg/ cm .
10. An improved process for the preparation of solid isopropyl-N- (3-chlorophenyl)
carbamate (CIPC) as substantially herein described in claims 1 - 9 and with reference to the aforesaid examples.

14

ABSTRACT
An improved process for the preparation of solid isopropyl-N- (3-chlorophenyl) carbamate (CIPC) without the need for filling the molten CIPC into the drums directly in the plant during the last step of commercial production, for further transport, comprising of stirring of molten CIPC, between 100 - 5000 rpm at a temperature ranging between -20 to 35 °C, to initiate the solidification for semisolid mass; feeding the semi-solid mass on to a drum flakers maintained at -10 to 35°C with rpm between 1 - 60, to obtain flakes; maintaining the temperature of flakes between 5 - 25 ° C; grinding the flakes in a multi mill, with 1-5 mm sieve, at a temperature ranging from -5 to 25 °C; to obtain the solid isopropyl-N-(3-chlorophenyl) carbamate (CIPC) . This powder is optionally, compressed with a pressure of 15 to 300 kg/cm2 to form tablets, pellets, blocks/chunks of isopropyl-N-(3-cholorophenyl) carbamate.
To,
The Controller of Patents,
Patent Office,
Mumbai
15

Documents:

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Patent Number

278067

Indian Patent Application Number

913/MUM/2005

PG Journal Number

52/2016

Publication Date

16-Dec-2016

Grant Date

09-Dec-2016

Date of Filing

05-Aug-2005

Name of Patentee

UPL LIMITED,

Applicant Address

UNIPHOS HOUSE, 11TH ROAD, C.D. MARG, KHAR (WEST), MUMBAI-400 052

Inventors:

#	Inventor's Name	Inventor's Address
1	JADHAV PRAKASH MAHADEV	12, Hasayavadhan Society, Tejpal Scheme No: 4, Vile Parle (Eest) Mumbai-400057
2	SHROFF JAIDEV RAJNIKANT	4-B, Summer Palace, Nargis Dutt Road, Pali Hill, Bandar (West ) Mumbai- 400 050

PCT International Classification Number

Nil

PCT International Application Number

N/A

PCT International Filing date

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1			NA