CN110432265B - Pesticide water dispersible granule and preparation method thereof - Google Patents
Pesticide water dispersible granule and preparation method thereof Download PDFInfo
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- CN110432265B CN110432265B CN201910654215.8A CN201910654215A CN110432265B CN 110432265 B CN110432265 B CN 110432265B CN 201910654215 A CN201910654215 A CN 201910654215A CN 110432265 B CN110432265 B CN 110432265B
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/12—Powders or granules
- A01N25/14—Powders or granules wettable
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/34—Nitriles
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/44—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids
- A01N37/46—N-acyl derivatives
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
- A01N43/50—1,3-Diazoles; Hydrogenated 1,3-diazoles
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/10—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
- A01N47/12—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof containing a —O—CO—N< group, or a thio analogue thereof, neither directly attached to a ring nor the nitrogen atom being a member of a heterocyclic ring
- A01N47/14—Di-thio analogues thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/10—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
- A01N47/18—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof containing a —O—CO—N< group, or a thio analogue thereof, directly attached to a heterocyclic or cycloaliphatic ring
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
- A01N47/34—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the groups, e.g. biuret; Thio analogues thereof; Urea-aldehyde condensation products
Abstract
The invention belongs to the technical field of pesticide preparations, and provides a pesticide water dispersible granule and a preparation method thereof. A pesticide water dispersible granule comprises the following components in parts by weight: 15-70 parts of pesticide active ingredient, 5-10 parts of dispersing agent, 2-5 parts of wetting agent, 5.5-9 parts of disintegrating agent, 1-4 parts of binder and 2-10 parts of filler, wherein the dispersing agent is poloxamer, chitosan and citric acid in a mass ratio of 4: 1: 1.5. The preparation method comprises the steps of uniformly mixing the pesticide active ingredients, the dispersing agent and the disintegrating agent, crushing, mixing with the wetting agent and the binding agent which are dissolved by adding water to obtain a suspension, spray-drying the suspension, mixing with the filler, extruding, granulating, drying and the like. By the technical scheme, the problems of single formula and small application range of the water dispersible granule in the prior art are solved.
Description
Technical Field
The invention belongs to the technical field of pesticide preparations, and relates to a pesticide water dispersible granule and a preparation method thereof.
Background
The water dispersible granule is an environment-friendly new formulation of pesticide researched and developed in the 80 th of the 20 th century, and is developed on the basis of wettable powder and a suspending agent. The formulation reduces the pollution to the environment in the processing and using processes, is convenient for metering, packaging and transportation, reduces the use cost of farmers, and is a great trend in the current pesticide development.
At present, water dispersible granules mainly comprise raw material medicines, a dispersing agent, a wetting agent, a disintegrating agent, a binder, a filler and the like, the selection of an auxiliary agent is a key factor influencing the wettability, the disintegration and the suspension of the water dispersible granules, further influencing the retention amount and the retention time of a liquid medicine on the surface of a plant and the penetration capability of the liquid medicine on the epidermis of the plant, and influencing the biological activity of pesticides, the formula of the water dispersible granules in the prior art is single, and is sensitive to the change of raw materials, particularly the water dispersible granules are produced by the same raw material medicine of different manufacturers, and the performances of the water dispersible granules are greatly different, so that the research on the pesticide water dispersible granules with good applicability is necessary for improving the utilization rate of active ingredients of the pesticide.
Disclosure of Invention
The invention provides a pesticide water dispersible granule and a preparation method thereof, and solves the problems of single formula and small application range of the water dispersible granule in the prior art.
The technical scheme of the invention is realized as follows:
a pesticide water dispersible granule comprises the following components in parts by weight:
15-70 parts of pesticide active ingredients, 5-10 parts of dispersing agents, 2-5 parts of wetting agents, 5.5-9 parts of disintegrating agents, 1-4 parts of binders and 2-10 parts of fillers.
As a further technical scheme, the paint comprises the following components in parts by weight:
45 parts of pesticide active ingredients, 8 parts of dispersing agents, 4 parts of wetting agents, 7 parts of disintegrating agents, 2.5 parts of binding agents and 6 parts of fillers.
As a further technical scheme, the dispersing agent is poloxamer, chitosan and citric acid in a mass ratio of 4: 1: 1.5.
As a further technical scheme, the pesticide active ingredient is one or two of cyazofamid, mancozeb, metalaxyl, cymoxanil, carbendazim and chlorothalonil.
As a further technical scheme, the wetting agent is polyethylene glycol, polyethyleneimine and sodium polyacrylate in a mass ratio of 2: 1: 1.
As a further technical scheme, the disintegrating agent is one or more of sodium tripolyphosphate, sodium carboxymethyl starch and microcrystalline cellulose.
As a further technical scheme, the binder is one or more of carboxymethyl cellulose, polyvinyl alcohol, polyvinylpyrrolidone and sucrose.
As a further technical scheme, the filler is one or more of bentonite, kaolin, diatomite and white carbon black.
A preparation method of pesticide water dispersible granules comprises the following steps:
s1, weighing each component according to the formula of the pesticide water dispersible granule for later use;
s2, uniformly mixing the pesticide active ingredients, the dispersing agent and the disintegrating agent, and crushing to obtain mixed powder;
s3, dissolving the wetting agent and the binder with water, and mixing with the mixed powder to obtain a suspension;
s4, spray drying the suspension obtained in the step S3 to remove redundant water to obtain particles;
s5, uniformly mixing the particles obtained in the step S4 with a filler, extruding, granulating and drying to obtain the pesticide water dispersible granule.
As a further technical scheme, the weight ratio of water to wetting agent in step S3 is 45-55: 1.
the working principle and the beneficial effects of the invention are as follows:
1. according to the invention, the pesticide active ingredient is taken as a main material, the dispersant, the wetting agent, the disintegrating agent, the binder and the filler which are specific components are added, and the components are mutually cooperated, so that the suspension percentage of the prepared pesticide water dispersible granule is as high as 93.7%, the wetting time is as low as 52s, the disintegration time is as low as 42s, the suspension percentage, the wetting time and the disintegration time change after the prepared pesticide water dispersible granule is stored for 14 days in a (54 +/-2) DEG C constant temperature oven are small, and the pesticide water dispersible granule has good suspension, disintegration, wettability and heat storage stability, therefore, the retention amount of the pesticide water dispersible granule on the surface of a plant is improved, the retention time is prolonged, the biological activity of the pesticide active ingredient is improved, the utilization rate of the pesticide active ingredient is improved, the dosage is reduced, the cost is reduced.
2. According to the preparation method, the pesticide active ingredients, the dispersing agent and the disintegrating agent are uniformly mixed and then crushed, the mixture is mixed with the wetting agent and the binding agent which are dissolved by adding water to obtain the suspension, the suspension is subjected to spray drying and then is mixed with the filler, and the steps of extrusion granulation, drying and the like are carried out, so that the components in the pesticide water dispersible granule are dispersed more uniformly, the synergistic effect of the components is improved, and the dispersion stability of the pesticide water dispersible granule is further improved.
3. According to the invention, the components in the formula are cooperatively compatible, so that the prepared water dispersible granule has good suspension property, disintegration property, wettability and suspension stability aiming at different types of pesticide active ingredients and the compounding of two pesticide active ingredients, therefore, the formula is reasonable, the application range is wider, the applicability is stronger, and the water dispersible granule is suitable for popularization and application.
4. In the invention, the wetting agent is polyethylene glycol, polyethyleneimine and sodium polyacrylate in a mass ratio of 2.5: 1: 2, the polyethylene glycol, the polyethyleneimine and the sodium polyacrylate are compounded, so that the prepared pesticide water dispersible granule has good wettability and short wetting time, and the polyethylene glycol, the polyethyleneimine and the sodium polyacrylate have good water solubility, and are matched with the dispersant in the formula while the wettability is improved, so that the suspensibility, the disintegration and the heat storage stability of the pesticide water dispersible granule are improved.
5. In the invention, the dispersant is poloxamer, chitosan and citric acid in a mass ratio of 4: 1: 1.5, in the dispersing agent, poloxamer, chitosan and citric acid are mutually matched, so that the dispersing performance and the heat storage stability of the pesticide water dispersible granule are obviously improved. Poloxamer is a polyoxyethylene-polyoxypropylene-polyoxyethylene triblock copolymer, polyoxyethylene chains in molecular chains have relative hydrophilicity, so that active ingredients of pesticides can be well dispersed and stably suspended in aqueous solution, polyoxypropylene chains have relative lipophilicity, and can have good compatibility with the active ingredients of the pesticides, stable mutual structures are formed with the active ingredients of the pesticides, the suspension stability of the pesticide water dispersible granules is further enhanced, poloxamer and chitosan are assembled in water through hydrogen bonds to form stable molecular structures, the long chain structures in the chitosan increase steric hindrance, the acting force between a dispersing agent and the active ingredients of the pesticides is enhanced, the heat storage stability of the pesticide water dispersible granules is improved, the citric acid is added, an acid environment is created, the dissolution of the chitosan in water is promoted, and the interaction between the poloxamer and the chitosan is enhanced, in addition, the chitosan has good permeability, and can improve the penetrating capacity of the pesticide water dispersible granules on plant epidermis, thereby improving the biological activity of the pesticide, reducing the dosage, reducing the cost, improving the cost performance of the pesticide water dispersible granules and having strong practicability.
6. According to the preparation method of the dispersing agent, the poloxamer aqueous solution with the mass fraction of 20% is prepared firstly, the citric acid is added for dissolving, then the chitosan is added, the dispersing agent is obtained by freeze drying after full dissolution, and the specific preparation method can reserve the active ingredients in the dispersing agent to the maximum extent, so that the effect of the dispersing agent in the pesticide water dispersible granule can be fully exerted.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A pesticide water dispersible granule comprises the following components in parts by weight:
15 parts of pesticide active ingredient, 5 parts of dispersant, 2 parts of wetting agent, 5.5 parts of disintegrating agent, 1 part of binder and 2 parts of filler,
wherein the dispersant is poloxamer, chitosan and citric acid in a mass ratio of 4: 1: 1.5, the pesticide active ingredient is cyazofamid, the wetting agent is polyethylene glycol, polyethyleneimine and sodium polyacrylate in a mass ratio of 2: 1:1, the disintegrating agent is sodium tripolyphosphate, the binder is carboxymethyl cellulose, the filler is bentonite,
the preparation method comprises the following steps:
s1, weighing each component according to the formula for later use;
s2, uniformly mixing the pesticide active ingredients, the dispersing agent and the disintegrating agent, and crushing to obtain mixed powder;
s3, dissolving the wetting agent and the binder with water, and mixing with the mixed powder to obtain a suspension, wherein the weight ratio of the water to the wetting agent is 50: 1;
s4, spray drying the suspension obtained in the step S3 to remove redundant water to obtain particles;
s5, uniformly mixing the particles obtained in the step S4 with a filler, extruding, granulating and drying to obtain the pesticide water dispersible granule.
Example 2
A pesticide water dispersible granule comprises the following components in parts by weight:
70 parts of pesticide active ingredients, 10 parts of dispersing agents, 5 parts of wetting agents, 9 parts of disintegrating agents, 4 parts of binding agents and 10 parts of fillers,
wherein the dispersant is poloxamer, chitosan and citric acid in a mass ratio of 4: 1: 1.5, the pesticide active ingredient is cyazofamid, the wetting agent is polyethylene glycol, polyethyleneimine and sodium polyacrylate in a mass ratio of 2: 1:1, the disintegrating agent is sodium tripolyphosphate, the binder is carboxymethyl cellulose, the filler is bentonite,
the weight ratio of water to wetting agent in step S3 was 55: 1, the rest of the preparation steps are the same as example 1.
Example 3
A pesticide water dispersible granule comprises the following components in parts by weight:
45 parts of pesticide active ingredient, 8 parts of dispersant, 4 parts of wetting agent, 7 parts of disintegrant, 2.5 parts of binder and 6 parts of filler,
wherein the dispersant is poloxamer, chitosan and citric acid in a mass ratio of 4: 1: 1.5, the pesticide active ingredient is cyazofamid, the wetting agent is polyethylene glycol, polyethyleneimine and sodium polyacrylate in a mass ratio of 2: 1:1, the disintegrating agent is sodium tripolyphosphate, the binder is carboxymethyl cellulose, the filler is bentonite,
the weight ratio of water to wetting agent in step S3 was 45: 1, the rest of the preparation steps are the same as example 1.
Example 4
A pesticide water dispersible granule comprises the following components in parts by weight:
45 parts of pesticide active ingredient, 5 parts of dispersing agent, 2 parts of wetting agent, 6 parts of disintegrating agent, 2.5 parts of binder and 2 parts of filler, wherein the dispersing agent is poloxamer, chitosan and citric acid in a mass ratio of 4: 1: 1.5, the pesticide active components are cymoxanil and mancozeb with the mass ratio of 8: 1, the wetting agent is polyethylene glycol, polyethyleneimine and sodium polyacrylate in a mass ratio of 2: 1:1, the disintegrating agent is sodium carboxymethyl starch, the binder is polyvinyl alcohol, the filler is kaolin,
the preparation method is the same as that of example 1.
Example 5
A pesticide water dispersible granule comprises the following components in parts by weight:
38 parts of pesticide active ingredient, 8 parts of dispersing agent, 4 parts of wetting agent, 7 parts of disintegrating agent, 2.5 parts of binder and 6 parts of filler, wherein the dispersing agent is poloxamer, chitosan and citric acid in a mass ratio of 4: 1: 1.5, the pesticide active ingredients are metalaxyl and mancozeb with the mass ratio of 24: 5, the wetting agent is polyethylene glycol, polyethyleneimine and sodium polyacrylate in a mass ratio of 2: 1:1, disintegrating agent is a mixture of sodium tripolyphosphate and sodium carboxymethyl starch in a mass ratio of 1:1, binder is sucrose, filler is white carbon black,
the preparation method is the same as that of example 1.
Example 6
A pesticide water dispersible granule comprises the following components in parts by weight:
20 parts of pesticide active ingredients, 8 parts of a dispersing agent, 4 parts of a wetting agent, 7 parts of a disintegrating agent, 2.5 parts of a binder and 8.5 parts of a filler, wherein the dispersing agent is poloxamer, chitosan and citric acid in a mass ratio of 4: 1: 1.5, the pesticide active ingredients are cyazofamid and cymoxanil with the mass ratio of 1: 4, the wetting agent is polyethylene glycol, polyethyleneimine and sodium polyacrylate in a mass ratio of 2: 1:1, the disintegrating agent is a mixture of sodium tripolyphosphate and microcrystalline cellulose with the mass ratio of 1:1, the binder is a mixture of carboxymethyl cellulose and polyvinyl alcohol with the mass ratio of 1:1, the filler is bentonite,
the preparation method is the same as that of example 1.
Example 7
A pesticide water dispersible granule comprises the following components in parts by weight:
45 parts of pesticide active ingredient, 8 parts of dispersing agent, 4 parts of wetting agent, 7 parts of disintegrating agent, 2.5 parts of binder and 6 parts of filler, wherein the dispersing agent is poloxamer, chitosan and citric acid in a mass ratio of 4: 1: 1.5, the pesticide active ingredient is carbendazim, the wetting agent is polyethylene glycol, polyethyleneimine and sodium polyacrylate in a mass ratio of 2: 1:1, the disintegrating agent is sodium carboxymethyl starch, the binder is polyvinyl alcohol, the filler is kaolin,
the preparation method is the same as that of example 1.
The preparation method of the dispersant in the embodiment 1-7 comprises the following steps: dissolving poloxamer in a certain amount of water to obtain a poloxamer aqueous solution with a concentration of 20%, adding citric acid into the poloxamer aqueous solution, adding chitosan after dissolving, mixing uniformly, and freeze-drying to obtain the dispersing agent.
Comparative example 1
A pesticide water dispersible granule comprises the following components in parts by weight:
45 parts of pesticide active ingredient, 5 parts of dispersing agent, 2 parts of wetting agent, 6 parts of disintegrating agent, 2.5 parts of binding agent and 2 parts of filler, wherein the dispersing agent is poloxamer, and the pesticide active ingredient is cymoxanil and mancozeb with the mass ratio of 8: 1, the wetting agent is polyethylene glycol, polyethyleneimine and sodium polyacrylate in a mass ratio of 2: 1:1, the disintegrating agent is sodium carboxymethyl starch, the binder is polyvinyl alcohol, the filler is kaolin,
the preparation method is the same as that of example 1.
Comparative example 2
A pesticide water dispersible granule comprises the following components in parts by weight:
45 parts of pesticide active ingredient, 5 parts of dispersant, 2 parts of wetting agent, 6 parts of disintegrant, 2.5 parts of binder and 2 parts of filler, wherein the dispersant is chitosan, and the pesticide active ingredient is cymoxanil and mancozeb with the mass ratio of 8: 1, the wetting agent is polyethylene glycol, polyethyleneimine and sodium polyacrylate in a mass ratio of 2: 1:1, the disintegrating agent is sodium carboxymethyl starch, the binder is polyvinyl alcohol, the filler is kaolin,
the preparation method is the same as that of example 1.
Comparative example 3
A pesticide water dispersible granule comprises the following components in parts by weight:
45 parts of pesticide active ingredient, 5 parts of dispersing agent, 2 parts of wetting agent, 6 parts of disintegrating agent, 2.5 parts of binder and 2 parts of filler, wherein the dispersing agent is poloxamer and chitosan in a mass ratio of 4: 1, the pesticide active ingredients are cymoxanil and mancozeb with the mass ratio of 8: 1, the wetting agent is polyethylene glycol, polyethyleneimine and sodium polyacrylate in a mass ratio of 2: 1:1, the disintegrating agent is sodium carboxymethyl starch, the binder is polyvinyl alcohol, and the filler is kaolin; the preparation method of the dispersant comprises the following steps: dissolving poloxamer in a certain amount of water to obtain a poloxamer aqueous solution with the concentration of 20%, adding chitosan into the poloxamer aqueous solution, uniformly mixing, and freeze-drying to obtain a dispersing agent;
the preparation method is the same as that of example 1.
Comparative example 4
A pesticide water dispersible granule comprises the following components in parts by weight:
45 parts of pesticide active ingredient, 8 parts of dispersing agent, 4 parts of wetting agent, 7 parts of disintegrating agent, 2.5 parts of binder and 6 parts of filler, wherein the dispersing agent is poloxamer, chitosan and citric acid in a mass ratio of 4: 1: 1.5, the pesticide active components are cymoxanil and mancozeb with the mass ratio of 8: 1, the wetting agent is polyethylene glycol, polyethyleneimine and sodium polyacrylate in a mass ratio of 2: 1:1, the disintegrating agent is sodium carboxymethyl starch, the binder is polyvinyl alcohol, the filler is kaolin, the preparation method of the dispersing agent is that poloxamer is dissolved in a certain amount of water to prepare poloxamer aqueous solution with the concentration of 20 percent, citric acid is added into the poloxamer aqueous solution, chitosan is added after the dissolution, the mixture is evenly mixed and dried in vacuum at 60 ℃ to obtain the dispersing agent,
the preparation method is the same as that of example 1.
The following performance tests were carried out on the pesticide water dispersible granules prepared in examples 1 to 7 and comparative examples 1 to 3:
1. suspension percentage: testing the suspension rate of the sample according to a method specified in GB/T14825-2006 pesticide suspension rate determination method;
2. wettability: using a graduated cylinder test, 1.0g of sample was quickly poured into a graduated cylinder containing 500mL of 342mg/L of hard water without agitation, and the time to 99% of the sample sinking to the bottom of the cylinder was recorded.
3. Disintegration property: a graduated cylinder test method is adopted, 90mL of distilled water is added into a 100mL stoppered measuring cylinder, a 0.5g granule sample is added at 25 ℃, the middle part of the measuring cylinder is clamped, the cylinder opening is stoppered, the measuring cylinder rotates around the center at the speed of 8r/min until the sample is completely disintegrated in water, and the disintegration time is recorded.
4. Heat storage stability: according to the specification of GB/T19136-2003 'stability for thermal storage of pesticide', about 5g of sample is sealed in a 50ml ampoule bottle, placed in a constant temperature oven at (54 +/-2) ° C and taken out after being stored for 14 days, and the suspension rate, wettability and disintegrability of the sample are measured according to the methods in 1, 2 and 3, and the test results are shown in the following table:
table 1 Performance test results of pesticide water dispersible granules prepared in examples 1-7 and comparative examples 1-3
As can be seen from Table 1, compared with the pesticide water dispersible granules prepared in comparative examples 1 to 4, the pesticide water dispersible granules prepared in examples 1 to 7 of the invention have high suspension rate, short wetting time and short disintegration time, the suspension rate is as high as 93.7%, the wetting time is as low as 52s, the disintegration time is as low as 42s, and the changes of the suspension rate, the wetting time and the disintegration time after being stored for 14 days in a constant-temperature oven at (54 +/-2) DEG C are small, so that the pesticide water dispersible granules prepared in the invention have good suspension property, disintegration property, wettability and heat storage stability. The prepared pesticide water dispersible granule has good suspension property, disintegration property, wettability and heat storage stability for different types of pesticide active ingredients and the mixture of the two pesticide active ingredients, and the water dispersible granule prepared by the invention has stronger applicability to different types of pesticide active ingredients, so that the water dispersible granule has wider application range and is suitable for popularization and application.
Compared with example 4, the dispersant of the pesticide water dispersible granule in the comparative example 1 is only poloxamer, the dispersant of the pesticide water dispersible granule in the comparative example 2 is only chitosan, the dispersant of the pesticide water dispersible granule in the comparative example 3 is only poloxamer and chitosan, and the dispersant of the pesticide water dispersible granule in the comparative example 4 is completely mixed and then dried in vacuum at 60 ℃, so that compared with example 4, the pesticide water dispersible granule in the comparative example 1 has longer disintegration time, poorer heat storage stability, relatively lower suspension rate and relatively longer wetting time; the pesticide water dispersible granule of the comparative example 2 has poorer suspension rate, longer wetting time, longer disintegration time and poorer heat storage stability; the pesticide water dispersible granule of the comparative example 3 has relatively poorer suspension rate, relatively longer wetting time and disintegration time and relatively poorer heat storage stability; the pesticide water dispersible granule of the comparative example 4 is poorer in heat storage stability, poorer in suspension rate and longer in wetting time and disintegration time, which means that poloxamer, chitosan and citric acid in the dispersing agent are matched with each other, so that the dispersing performance and the heat storage stability of the pesticide water dispersible granule are remarkably improved, and the active ingredients in the dispersing agent can be retained to the maximum extent by adopting a freeze drying mode in the preparation method of the dispersing agent, so that the efficacy of the dispersing agent in the pesticide water dispersible granule can be fully exerted.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. The pesticide water dispersible granule is characterized by comprising the following components in parts by weight:
15-70 parts of pesticide active ingredient, 5-10 parts of dispersing agent, 2-5 parts of wetting agent, 5.5-9 parts of disintegrating agent, 1-4 parts of binder and 2-10 parts of filler,
the dispersing agent is poloxamer, and the mass ratio of chitosan to citric acid is 4: 1: 1.5, dissolving poloxamer in a certain amount of water to obtain a 20% poloxamer aqueous solution, adding citric acid into the poloxamer aqueous solution, adding chitosan after dissolving, mixing uniformly, freeze-drying to obtain the dispersing agent,
the wetting agent is polyethylene glycol, polyethyleneimine and sodium polyacrylate in a mass ratio of 2: 1: 1.
2. The pesticide water dispersible granule as claimed in claim 1, which is characterized by comprising the following components in parts by weight:
45 parts of pesticide active ingredients, 8 parts of dispersing agents, 4 parts of wetting agents, 7 parts of disintegrating agents, 2.5 parts of binding agents and 6 parts of fillers.
3. The pesticide water dispersible granule according to claim 1, wherein the pesticide active ingredient is one or two of cyazofamid, mancozeb, metalaxyl, cymoxanil, carbendazim and chlorothalonil.
4. The pesticide water dispersible granule according to claim 1, wherein the disintegrating agent is one or more of sodium tripolyphosphate, sodium carboxymethyl starch and microcrystalline cellulose.
5. The pesticide water dispersible granule according to claim 1, wherein the binder is one or more of carboxymethyl cellulose, polyvinyl alcohol, polyvinylpyrrolidone and sucrose.
6. The pesticide water dispersible granule according to claim 1, wherein the filler is one or more of bentonite, kaolin, diatomite and white carbon black.
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