Method of obtaining microcapsules of pesticides

FIELD: chemistry.

SUBSTANCE: invention relates to agriculture. Microcapsules of pesticides are obtained by mixing solution of sodium carboxymethylcellulose in cyclohexanol in presence of a surface-active substance with solution of pesticides in dimethylsulfoxide with further addition of ethanol after formation of solid phase.

EFFECT: invention makes it possible to simplify the process of obtaining microcapsules of preparation in water-soluble polymers, and increase weight output.

3 ex

 

The invention relates to the field of microencapsulation of pesticides.

Previously known methods for producing microcapsules of pesticides. Thus, in U.S. Pat. 2108036 Russian Federation IPC A01N 25/28, A01N 37/22 published 10.04.1998 describes how to obtain microencapsulated herbicide composition comprising acetochlor as the active ingredient and acceptable to him the antidote, enclosed in microcapsules obtained by the dispersion at room temperature, the active ingredient, and mixtures polymethylenepolyphenylisocyanate and isomeric 2,4 - and 2,6-tolylenediisocyanate taken in the ratio of 1.5-2:1 in an aqueous phase containing 1.0 to 1.5 wt.% protective colloid, preferably alkali metal lignosulfonate and 0.3 to 1.0 wt.% Surfactant, followed by heating the mixture up to 40-90°C and cooling to room temperature.

Disadvantages of the proposed method are dispersed in the aqueous phase, which complicates the process of production of microcapsules of drugs in polymers forming jellies in the aquatic environment at low concentrations in solution.

In Pat. 2089062 Russian Federation IPC A01N 25/28 published 10.09.1997 describes how to obtain microencapsulated pesticides according to the invention, based on the known method of microencapsulation, consisting of interfacial polycondensation polymethylenepolyphenylisocyanate and polyamine in the presence of a pesticide is about-active substances in the aquatic environment, containing surfactant, characterized in that the surfactant used ammonium salt of a partial ester of a copolymer of styrene and maleic anhydride (1:1) in an amount of 2-8 wt.% the number pesticide-active substances. As a pesticide, it is preferable to use metallacarboranes, propiconazol, diazinon.

The disadvantages of the invention to provide microcapsules by chemical method of interfacial polymerization, which consists of several stages, which makes the process long and complicates it, use as a surfactant compositions ammonium salt of a partial ester of a copolymer of styrene and maleic aldehyde in a certain ratio that can be replaced with a single connection, such as OS-20.

In Pat. WO/2010/137743 JP IPC A01N 25/28; A01N 51/00; A01P 7/04; B01J 13/16 published 02.12.2010 a method for the production of microcapsules containing pesticide compounds in the fatty acid ester, which delays the release timing of pesticide compounds in comparison with the conventional microcapsules. In the method of producing microcapsules includes:

1) maintaining a mixture of the pesticide compound with polyisocyanate from 20 to 60°C for 3 hours or more;

2) adding to the mixture of water containing polyols or polyamine, and preparations for the formation of liquid droplets in the water;

3) formation of a film of polyurethane or polyurea around the drops.

The disadvantages of pre the proposed method are the use of special equipment (rotary homogenizer), a multi-stage, which complicates the method of producing microcapsules and makes it long.

The closest method is the method proposed in U.S. Pat. 2165700 Russian Federation IPC A01N 25/28, A01N 53/00, A01N 57/00 published 27.04.2001 describes how to obtain microencapsulated insecticide, which is as follows: the solution mixture in an organic solvent composed of natural lipids and organophosphorus and/or a PYRETHROID insecticide in the weight ratio of 2-4:1, was dispersed in water to obtain the desired product. Using the proposed method allows to significantly simplify the process of encapsulation of insecticides and provides high quality insecticide preparation.

The disadvantage of the method proposed in U.S. Pat. 2165700 is a dispersion in water, which makes the proposed method applicable to the production of microcapsules of water-soluble drugs in water-soluble polymers.

The technical problem is to simplify the process of production of microcapsules of the drug in water-soluble polymers, increasing the yield by weight.

The solution of the technical problem is achieved by a method of producing microcapsules, characterized in that upon receipt of the microcapsules physico-chemical method for the deposition nerastvorim as precipitators are used cyclohexanol and ethanol, and the quality is as the shell of the microcapsules is sodium carboxymethyl cellulose, the retrieval process is carried out without special equipment.

A distinctive feature of the proposed method is the use of two precipitators - cyclohexanol and ethanol in obtaining microcapsules physico-chemical method for the deposition nerastvorim and sodium carboxymethyl cellulose as the shell of the microcapsules.

The result of the proposed method is to obtain microcapsules of pesticides at 25°C for 15 minutes.

Required for the reaction, the sodium carboxymethyl cellulose was industrial production.

EXAMPLE 1 Obtaining the microcapsules metolachlor in the sodium carboxymethyl cellulose, the ratio of 1:3

To 6 g of 5% solution of sodium carboxymethyl cellulose in cyclohexanol add 0.01 g of the drug E472c as surfactants. The resulting mixture was put on a magnetic stirrer and include mixing. 0.1 g of metolachlor dissolved in 0.5 ml DMSO and transferred to a solution of sodium carboxymethylcellulose in cyclohexanol. After the formation after the formation of metolachlor independent solid phase very slowly added dropwise 3 ml of ethanol and 1 ml of distilled water. The resulting suspension of microcapsules is filtered by the filter SCHOTT 16 class then washed with acetone, dried in a desiccator over calcium chloride.

Received 0,255 g of the microcapsules. The yield was 64%.

p> EXAMPLE 2 Obtaining microcapsules of propiconazole + tebuconazole in the sodium carboxymethyl cellulose, the ratio of 1:3

To 6 g of 5% solution of sodium carboxymethyl cellulose in cyclohexanol add 0.01 g of the drug E472c as surfactants. The resulting mixture was put on a magnetic stirrer and include mixing. 0.1 g of propiconazole + tebuconazole dissolved in 0.5 ml DMSO and transferred to a solution of sodium carboxymethylcellulose in cyclohexanol. After the formation after the formation of propiconazole + tebuconazole independent solid phase very slowly added dropwise 3 ml of ethanol and 1 ml of distilled water. The resulting suspension of microcapsules is filtered by the filter SCHOTT 16 class then washed with acetone, dried in a desiccator over calcium chloride.

Received 0,210 g of the microcapsules. The yield was 53%.

EXAMPLE 3 Obtaining microcapsules of clopyralid in the sodium carboxymethyl cellulose, the ratio of 1:3

To 6 g of 5% solution of sodium carboxymethyl cellulose in cyclohexanol add 0.01 g of the drug Is as surfactants. The resulting mixture was put on a magnetic stirrer and include mixing. 0.1 g of clopyralid dissolved in 0.5 ml DMSO and transferred to a solution of sodium carboxymethylcellulose in cyclohexanol. After the formation after the formation of clopyralid self-TV is rdeu phase very slowly added dropwise 3 ml of ethanol and 1 ml of distilled water. The resulting suspension of microcapsules is filtered by the filter SCHOTT 16 class then washed with acetone, dried in a desiccator over calcium chloride.

Received 0,255 g of the microcapsules. The yield was 64%.

Thus, the obtained microcapsules physico-chemical method for the deposition nerastvorim using cyclohexanol and ethanol as precipitators, which increases output. The process is simple to perform and lasts for 15 minutes, requires no special equipment.

The proposed method is suitable for the agricultural industry due to ease of implementation and adaptability.

The method of producing microcapsules of pesticides, characterized in that the solution of sodium carboxymethyl cellulose in the cyclohexanol in the presence of a surfactant is mixed with a solution of pesticides in dimethyl sulfoxide followed after the formation of the solid phase by the addition of ethanol.



 

Same patents:

FIELD: medicine, pharmaceutics.

SUBSTANCE: invention relates to method of obtaining microcapsules of medication of cephalosporin group in konjac gum. In accordance with claimed method cephalosporin powder, preliminarily dissolved in dimethylformamide, and surface-active substance are added to konjac gum solution in isopropyl alcohol, with addition of carbinol after formation of independent solid phase by cephalosporin. Obtained suspension of microcapsules is filtered, washed with acetone and dried in dessicator.

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4 ex

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4 ex

FIELD: veterinary medicine.

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1 tbl

FIELD: medicine, pharmaceutics.

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4 ex

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7 ex

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8 ex

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3 ex

FIELD: medicine, pharmaceutics.

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48 ex

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4 ex

FIELD: chemistry.

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7 ex

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2 ex

FIELD: chemistry.

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7 ex

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,

where R1, R3, R5, R7 independently denote methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, sec-butylene, tert-butyl; R2, R4, R6, R8 independently denote hydrogen, methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, sec-butyl, tert-butyl; R9, R10 denote hydrogen or hydroxymethyl; including oligomeric forms of compounds (I), where the number of moles of compounds (I) ranges from 2 to 10; and the microcapsules have average diameter from 0.3 to 25 mcm when using a conventional laser diffraction analyser to measure particle size with preliminary conventional dissolution in water while stirring. The invention also describes a method of producing an agrochemical composition of a typical encapsulated suspension, containing said microcapsules, and versions of using said microcapsules.

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12 cl, 12 ex, 13 dwg

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20 cl, 11 ex, 4 dwg

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1 tbl, 10 ex

FIELD: chemistry.

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23 cl, 2 ex, 1 tbl

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21 cl, 1 tbl, 10 ex

FIELD: agriculture.

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13 cl, 4 ex

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17 cl, 3 ex

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5 cl, 4 ex

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3 cl, 2 tbl, 11 ex

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