Method for making microcapsules
专利摘要:
Microcapsules having a shell consisting of water-soluble polyvinyl alcohol and containing a liquid, water-in-soluble material are obtained by dispersing a liquid, water-insoluble phase of a substance, substance mixture or substance solution in an aqueous phase of polyvinyl alcohol obtained by partial hydrolysis of polyvinyl acetate and having a degree of hydrolysis of from 72 to 99 mol % and dehydrating the dispersion to obtain the capsules in powder form. 公开号:SU1075948A3 申请号:SU792730650 申请日:1979-02-07 公开日:1984-02-23 发明作者:Френш Хайнц;Хайнрих Рудольф;Альбрехт Конрад 申请人:Хехст Аг (Фирма); IPC主号:
专利说明:
cl with four::: 00 There is a method of encapsulating hydrophobic oily liquids using gelatin-gum arabic as a shell material. However, the microcapsules formed during this process are resistant to the action of water and slowly release their contents. Capsules of small size are obtained, the walls of which consist of several layers, the inner layer being, for example, polyvinyl alcohol, and the outer layer is gelatin. The capsules thus prepared are sufficiently dissolved only after many hours of treatment with water. There is also known a method of making powdered microencapsulated preparations which may contain oily liquids and which are obtained by drying by: spraying the film-forming polymer in the presence of a finely dispersed future capsule contents. As a polymer forming capsule walls, for example, polyacrylates, polyester and furan resins, polyurethanes based on polyurea, polyamides, vinyl acetate polymers, and cellulose derivatives 2 are used. However, with the exception of products derived from various cellulose derivatives, all other materials are poorly or completely insoluble in cold water. Even microcapsules prepared from cellulose derivatives swell very slowly and dissolve when dispersed in water. In addition, the swelling of cellulose microcapsules, when obtained by spraying, results in the clogging of spray nozzles. The closest to the invention is a method for producing microcapsules by dispersing a liquid water-insoluble core material in an aqueous solution based on polyvinyl alcohol with a degree of hydrolysis of 83-88 mol.% With stirring and drying (C. However, the shell of the resulting microcapsules, consisting of the polyvinyl alcohol SPVS reaction product) and ethylene glycol borate cyclic ether, is insoluble in water, which prevents the use of such microcapsules for protecting plants, which require the release of the core of the active substance at the right time. The purpose of the invention is to improve the solubility of the microcapsule shell. The goal is achieved by the method of producing microcapsules by dispersing a liquid water-insoluble core material in an aqueous solution based on polyvinyl 5 alcohol with a degree of hydrolysis of 8388 mol.% While stirring and drying, a water-insoluble pesticide selected from the group: 2- { 0,0-diethyl0-thionophosphoryl) -5-methyl-b-carbztoxypyrazolo-l, 5a3-pyrimidine (pyrazophos); 6,7,8,9,10,10-hexachlor-1,5,5a, 9a-tetrahydro-6,9-methano-2.4, 3-benzodioxatispin-3-oxide (endosulfan) j 5 2-Rtop-butyl-4,6-dinitrophenylacetate (dinosebacetate); 0,0-diethyl- (1-phenyl-1, 2,4-triazol-3-yl) -thionophosphate (triazophos) in the amount of 28.3736, 36% by weight of the dispersion in 20-25% Q nominal solution of polyvinyl alcohol. with viscosity of 374 cps, measured in 4% aqueous solution at 20 s, and sugiku carried out by spraying at 145-148 0 at the entrance and 50-55 0 at the height of the dryer. Example. 14O g of polyvinyl alcohol, obtained by partial saponification of polyvinyl acetate, with a viscosity of 3 cP (measured in a 4% aqueous solution at 20 ° C) and a degree of hydrolysis of 83 mol,%, is dissolved in 420 g of water (25% PVA solution) and with vigorous stirring, add 225 g of pyrazophos in 85 g to the resulting solution of t solution 1 tvor 5 methylnaf alina (35.63% by weight of the dispersion). The mixture is dispersed for 2 minutes in an apparatus with vigorous stirring at a stirring speed of about 5,000 rpm. 0 and then through a spray nozzle is introduced into the laboratory spray gun with a capacity of 3 kg / h of moisture. Spraying is carried out at a pressure of 3 MPa. Temperature 5 air inlet to the dryer 145l48-c, the temperature of the outgoing air before entering it in the cyclone 50-55 0. Air consumption 30. Q At the bottom of the cyclone, 405 g of dry, well-flowing, microcapsule powder is collected with a diameter of individual capsules of 1-20 microns and a bulk weight, respectively, bulk density c after shaking 33, respectively 38 g / 100 ml. The content of pyrazophos in the microcapsule is 45 wt.%, Residual moisture to, 5 wt.%. 0 Example2. 140 g of polyvinyl alcohol of the type indicated in Example 1 is dissolved in 420 g of water (25% PVA solution) and in the resulting solution in those indicated in Example 1 5 conditions dispersed heated to a solution of 200 g of endosulfan in 120 g of methylnaphthalene (36.36% by weight of the dispersion). After drying the dispersion in a spray dryer under the same conditions as in Example 1, 410 g of a dry, well-flowing microcapsule powder with individual capsules 1-20 µm in diameter and an empty cap, weighing 29 g, respectively, are obtained. / 100 ml. The content of eido sulfan in the microencapsulated product is 42% by weight, the residual moisture 0.5% by weight. Froze 240 g of polyvinyl alcohol with a viscosity of 4 cp (measured in 4% aqueous solution with) and a degree of hydrolysis of 88 mol.% Are dissolved in 960 ml of water (20% solution) and dispersed in the resulting solution. As indicated in Example 1, a solution of 280 g of dinosebacetate in 200 g of 4-methylcyclohexanone (28.57% by weight of the dispersion). After drying the dispersion in a spray dryer under the same conditions as in pretter 1, 655 g of dry are obtained. bulk powder micrrcapsules with mass1 | by weight 39, respectively, the bulk density after shaking 44 g / 100 ml. The content of dinosebacetate in a micro; encapsulated product is 36.% by weight, the residual moisture is 0.5% by weight. Example 4. 210 g of polyvinyl alcohol specified in the example. 3 types. dissolved in 800 g of water (20.79% solution of PVA) and in the resulting In solution under the same conditions as in Example 1, a solution of 300 g of triazofos is dispersed in 100 g of methylnaphthalene (28.37% by weight of the dispersion). After drying the dispersion 5 in the spray dryer under the same conditions as in Example 1, 550 g of dry, xopcxdo bulk powder with a bulk weight of 32 and a corresponding bulk density after shaking 37 g / 100 ml are obtained. The content of triazophos in the microencapsulated product is 48% by weight, the residual moisture is 40.5% by weight. TiMcaM thus, the invention poses to obtain microcapsules, obaschalaschke improved solubility, which means that they use a {at 4 and 9e markings.
权利要求:
Claims (4) [1] DREAMS FOR PRODUCING MICROCapsules by dispersing a liquid, water-insoluble material of the core with an aqueous solution based on polyvinyl alcohol with a degree of hydrolysis of 83-88 mol% with stirring and drying, characterized in that, in order to improve the solubility of the shell of the microcapsules, water-insoluble is subjected to dispersion at 5 ° C. selected from the group: [2] 2- (0,0 diethylthionophosphoryl) -5-methyl-6carbethoxypyraeo- {1,5 <j} -pyrimidine; 6,7,8,9,10,10-hexachloro-1, T, 5 °, 9-tetrahydro-6.9-methano-2.4, [3] 3-benzodioxathiopin-3-oceanide; 2- * tor-butyl- [4] 4,6-dinitrophenyl acetate; 0,0-diethyl (1-phenyl-1,2,4-trnazol-3-yl) * thioiophosphate, in the amount of 28.37-36.36% by weight of the dispersion in a 20-25% solution of polyvinyl alcohol with a viscosity 3-4 cP, measured in a 4% aqueous solution at 20 ° C, and drying is carried out by spraying at 145148 ° C at the inlet and 50-55 ° C at the outlet of the dryer. ... at
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同族专利:
公开号 | 公开日 JPS54113420A|1979-09-05| FR2416053A1|1979-08-31| PT69189A|1979-03-01| AR221079A1|1980-12-30| TR20916A|1983-01-01| FR2416053B1|1986-12-05| ES477361A1|1979-07-01| US4244836A|1981-01-13| DD141462A5|1980-05-07| IL56592A|1982-01-31| CH642567A5|1984-04-30| DE2805106A1|1979-08-16| HU181882B|1983-11-28| IL56592D0|1979-05-31| NL7900958A|1979-08-09| IT1110108B|1985-12-23| CA1129263A|1982-08-10| IT7919912D0|1979-02-05| GB2013610B|1982-08-18| PH14906A|1982-01-29| ATA82379A|1981-12-15| BR7900708A|1979-09-04| AT367654B|1982-07-26| BE874006A|1979-08-07| MX5897E|1984-08-22| GB2013610A|1979-08-15|
引用文献:
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申请号 | 申请日 | 专利标题 DE19782805106|DE2805106A1|1978-02-07|1978-02-07|MICROCAPSULES MADE OF POLYVINYL ALCOHOL WITH LIQUID, WATER-INSOLUBLE FILLING MATERIAL AND PROCESS FOR THEIR PRODUCTION| 相关专利
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