CN112335675B

CN112335675B - Pesticide preparation containing fosthiazate and preparation method thereof

Info

Publication number: CN112335675B
Application number: CN202011307796.7A
Authority: CN
Inventors: 丁秀丽; 秦敦忠; 范文娟; 陆林华; 王雪松; 袁杰
Original assignee: Jiangsu Jinghe Interface Technology Co ltd
Current assignee: Nanjing Qingyu Biopharmaceutical Technology Co ltd
Priority date: 2020-11-20
Filing date: 2020-11-20
Publication date: 2022-07-12
Anticipated expiration: 2040-11-20
Also published as: CN112335675A

Abstract

The invention discloses a fosthiazate-containing pesticide preparation and a preparation method thereof, belonging to the field of pesticide preparations. According to the invention, the active substance containing the fosthiazate is prepared into the microcapsule, and further prepared into the water dispersible granule or granule containing the fosthiazate microcapsule, so that the inherent peculiar smell of the fosthiazate is shielded, the phytotoxicity on sensitive crops is avoided, and the compounding performance and the storage stability of the fosthiazate and other pesticides are improved.

Description

Pesticide preparation containing fosthiazate and preparation method thereof

Technical Field

The invention belongs to the field of pesticide preparations, and particularly relates to a fosthiazate-containing pesticide preparation and a preparation method thereof.

Background

The fosthiazate is a non-fumigation organophosphorus insecticide and nematicide, has strong contact activity, has obvious systemic poisoning and killing effects on various nematodes, insects and mites, has the main action mode of inhibiting the synthesis of acetylcholinesterase of target pests, has unique biological and physical and chemical properties so that the fosthiazate is suitable for application to soil, stems and leaves, and has broad-spectrum activity on plant parasitic nematodes, pests and mites. The fosthiazate also has high activity on a plurality of nematodes which have been generated with resistance by the traditional nematicides, and the nematodes which can be controlled comprise stem-leaf ectoparasitic nematodes on the overground part, root endoparasitic nematodes, semi-endoparasitic nematodes, ectoparasitic nematodes and the like on the underground part.

The fosthiazate raw pesticide has serious peculiar smell and strong corrosivity, presents certain acidity, is easy to cause crop phytotoxicity when being used alone, and is often used in combination with other medicaments. For example, Chinese patent application with the patent application number of 201610544379.1 discloses a fosthiazate-containing pesticide composition, which comprises, by weight, 0.1-30% of fosthiazate, 0.1-30% of nematicide, 0.1-15% of dispersant, 0.1-10% of wetting agent, 0.1-14% of binder and the balance of carrier to 100%; the preparation method comprises the specific production steps of uniformly mixing the active ingredients and other auxiliary agents, crushing by using an ultramicro jet mill, kneading, adding into a fluidized bed granulation dryer for granulation, drying and screening to prepare particles with corresponding weight percentage content, and compounding the fosthiazate and other nematicides in a certain proportion, so that the composition is suitable for preventing and treating crop nematode diseases caused by pathogenic nematodes, particularly crop root knot nematode diseases and cyst nematode diseases. However, the pesticide composition prepared by the method is easy to decompose and lose efficacy during storage.

In addition, in the prior art, fosthiazate is often coated in a capsule shell formed by high polymer materials as a capsule core, so that peculiar smell is shielded, the compatibility with other pesticides is improved, and the phytotoxicity to sensitive crops is reduced. For example, chinese patent application No. 201610007107.8 discloses a fosthiazate microcapsule suspension and a preparation method thereof, the microcapsule suspension comprises microcapsules and a suspending solvent system, wherein the microcapsules comprise a capsule core and a capsule wall; the capsule core is formed by fosthiazate; the capsule wall is formed by polyurea or polyurethane; the suspending solvent system comprises an organic solvent, an additive and water; the additive is at least one of an emulsifier, a dispersant, an antifreeze, a stabilizer, an acid-base regulator, a preservative, a defoamer and a viscosity regulator. The invention reduces the smell, prolongs the drug effect and improves the content of the preparation; the stabilizing agent is added in the preparation process, so that the decomposition of the fosthiazate can be effectively prevented, and the stability of the product is improved, so that the fosthiazate microcapsule suspending agent has high storage stability and slow release; reducing the phytotoxicity and being safe to crops. However, in the process of storage of the fosthiazate microcapsule suspending agent prepared by the method, the capsule wall of the microcapsule is still easy to corrode and damage, and the fosthiazate and the solvent in the capsule core are dissolved out, so that the problems of decomposition failure of the fosthiazate, oil precipitation, bottom formation, creaming, short storage period of the preparation and the like are caused, and serious phytotoxicity is caused to crops when the fosthiazate microcapsule suspending agent is applied.

In the microcapsules prepared by a chemical method and a physical and chemical method, some incompletely reacted isocyanates, amines, acrylates, resin prepolymers and aldehyde crosslinking agents can remain in a reaction liquid, or free high-molecular wall materials which are not combined on a microcapsule shell remain in a system when the microcapsules prepared by a physical method are adopted, and the existence of the substances influences the storage stability of a microcapsule product.

Disclosure of Invention

1. Problems to be solved

Aiming at the technical problems that in the prior art, a pesticide preparation containing fosthiazate is poor in compounding performance, unstable in quality, short in storage period, large in peculiar smell and easy to cause phytotoxicity to crops, the invention provides a pesticide preparation containing fosthiazate, wherein fosthiazate exists in the pesticide preparation in a microcapsule form, so that inherent peculiar smell of fosthiazate can be shielded, and the storage stability of the pesticide preparation containing fosthiazate is ensured;

meanwhile, the invention provides a preparation method of the fosthiazate-containing pesticide preparation, which comprises the steps of firstly preparing the active substance containing the fosthiazate into microcapsule suspension and filtering to obtain a capsule cake, and further preparing the capsule cake serving as a fosthiazate raw material into water dispersible granules or granules containing the fosthiazate microcapsules on the basis, so that the effective content of the fosthiazate is ensured.

2. Technical scheme

In order to solve the problems, the technical scheme adopted by the invention is as follows:

a pesticide preparation containing fosthiazate comprises an active ingredient, a wrapping material of the active ingredient and auxiliary ingredients, wherein the wrapping material of the active ingredient is a microcapsule capsule wall, and the active ingredient comprises fosthiazate or comprises fosthiazate and abamectin; the active ingredient is positioned in the microcapsule or positioned in the microcapsule and the auxiliary ingredient is positioned outside the microcapsule.

Further, the content of the active ingredient is at least 0.5 wt%, preferably 0.5-50 wt%; further preferably, if the pesticide preparation containing fosthiazate is water dispersible granules, the content of active ingredients is 5-50 wt%; if the pesticide preparation containing fosthiazate has a particle size, the content of the active ingredient is 0.5-15 wt%;

wherein if the active ingredients simultaneously comprise fosthiazate and avermectin, the content ratio of the fosthiazate to the avermectin is (1-99) to 1; more preferably, if the fosthiazate-containing pesticide preparation is a water dispersible granule, the content ratio of the two is (4-99): 1, and if the fosthiazate-containing pesticide preparation is a granule, the content ratio of the two is (1-10): 1.

Further, the content of the microcapsule is at least 0.6%; preferably the microcapsules are present in an amount of at least 6.1%; further preferably, the content of the microcapsule is 0.6-61.2%; more preferably, if the pesticide preparation containing fosthiazate is water dispersible granules, the content of the microcapsule is 6.1-61.2%; if the pesticide preparation containing fosthiazate is granules, the content of the microcapsule is 0.6-18.6%.

Further, the particle size of the microcapsule is 1-20 μm; the mass ratio of the capsule wall to the capsule core of the microcapsule is (1-6): 20, preferably (3-5): 20, and more preferably (3.2-4.04): 20.

Further, if the pesticide preparation containing fosthiazate is a water dispersible granule, the particle size of the microcapsule is 1-15 μm, the mass ratio of the capsule wall to the capsule core of the microcapsule is (1-4): 20, preferably (3-3.5): 20, and more preferably (3.2-3.34): 20;

when the fosthiazate-containing pesticide preparation is a granule, the particle size of the microcapsule is 3-20 μm, and the mass ratio of the capsule wall to the capsule core of the microcapsule is (3-6): 20, preferably (3.5-4.5): 20, and more preferably (3.58-4.04): 20.

Further, the pesticide preparation comprises the following components in percentage by mass:

0.1-160 parts of active component, preferably 0.5-140 parts, and more preferably 1-102 parts;

0.1-170 parts of solid powder, preferably 16-170 parts, and more preferably 64-167 parts;

the adhesive is polyethylene glycol aqueous solution and proper amount.

Further, if the pesticide preparation containing fosthiazate is water dispersible granules, the solid powder comprises the following components in parts by weight:

10-160 parts of active component, preferably 10-140 parts, and more preferably 10-102 parts;

60-170 parts of solid powder, preferably 64-170 parts, and more preferably 64-157 parts;

if the pesticide preparation containing fosthiazate is granules, the solid powder comprises the following components in parts by weight:

0.1-50 parts of active component, preferably 0.5-40 parts, and more preferably 1-31 parts;

100 to 170 parts of solid powder, preferably 130 to 170 parts, and more preferably 135 to 167 parts.

Further, the fineness of the solid powder is that 99.9% of the solid powder passes through 300-600 meshes;

the solid powder comprises the following components in parts by weight:

0.1-99 parts of inert carrier, preferably 1-90 parts; further preferably 5 to 79.23 parts;

0-90 parts of wetting dispersant, preferably 0-60 parts; further preferably 0 to 46 parts;

0-30 parts of abamectin, preferably 0-10 parts; further preferably 0 to 1.31 parts;

0-99.9 parts of fertilizer effect substances, preferably 0-99 parts; more preferably 0 to 94.5 parts.

Further, if the pesticide preparation containing the fosthiazate is a water dispersible granule, the fineness of the solid powder is 99.9% passing through 600 meshes, and if the pesticide preparation containing the fosthiazate is a granule, the fineness of the solid powder is 99.9% passing through 300 meshes.

50-99 parts of inert carrier, preferably 50-80 parts, and further preferably 53.5-79.23 parts;

10-90 parts of wetting dispersant, preferably 10-50 parts, and more preferably 20-46 parts;

0-3 parts of abamectin, preferably 0-1.31 parts; more preferably 0.6 to 1.31 parts.

Further, if the pesticide preparation containing fosthiazate is granules, the solid powder comprises the following components in parts by weight:

0.1-50 parts of inert carrier, preferably 5-30 parts, and more preferably 5-10 parts;

0-3 parts of abamectin, preferably 0-2.4 parts; further preferably 0.5 to 1.2 parts;

50 to 99 parts of fertilizer effect substances, and more preferably 90 to 94.5 parts.

Further, the inert carrier can be one or more selected from kaolin, white carbon black and diatomite;

the wetting dispersant can be one or more selected from sodium lignosulfonate, polycarboxylate, alkyl sulfate and alkyl naphthalene sulfonate formaldehyde condensate;

the fertilizer effect substance can be one or more selected from humic acid, seaweed powder and crab and shrimp shells.

Further, the wall forming material of the microcapsule can be one or more selected from polyurea, polylactic acid, polymethacrylate, melamine formaldehyde resin prepolymer or phenolic aldehyde modified urea formaldehyde resin prepolymer, and preferably melamine formaldehyde resin prepolymer.

The preparation method of the pesticide preparation containing fosthiazate comprises the following steps:

s1, preparing a microcapsule filter cake containing an active substance fosthiazate;

s2, preparing solid powder, and if necessary, adding a pH regulator to adjust the pH in the preparation process;

s3, mixing the microcapsule filter cake with solid powder, adding a binder aqueous solution, and extruding and granulating.

Further, in S1, the mixed liquid containing the active ingredient and the emulsifying dispersant is subjected to shearing treatment to form an oil-in-water emulsion; then, adding a wall forming material, forming a capsule wall by in-situ polymerization on an oil-water interface of the emulsion, and heating and curing to obtain microcapsule water suspension containing active substances; and finally, filtering to obtain a microcapsule filter cake.

Further, the emulsifying and dispersing agent can be one or more selected from sodium lignosulphonate, polycarboxylate and arabic gum.

Further, the following components are calculated according to the mass portion:

3-8 parts of an emulsifying dispersant; preferably 3.4-7 parts;

70-90 parts of active component; preferably 80-81 parts;

10-30 parts of wall forming material; preferably 19 to 21 parts.

3. Advantageous effects

Compared with the prior art, the invention has the beneficial effects that:

(1) compared with a single thiazole phosphine microcapsule suspension preparation sold in the market or other pesticide preparations directly containing a thiazole phosphine raw drug, the pesticide preparation containing the thiazole phosphine provided by the invention has the advantages that the thiazole phosphine exists in preparation particles in a form of being wrapped in the microcapsule, and the microcapsule is wrapped by solid powder (or abamectin-containing solid powder), so that the inherent peculiar smell of the thiazole phosphine can be shielded, and the phytotoxicity to sensitive crops can be avoided; the mixing compatibility of the fosthiazate and other substances can be improved, and the mixing difficulty of the fosthiazate and other substances is reduced; the physical stability of the pesticide preparation containing the fosthiazate during storage can be improved, and the lasting period of the fosthiazate can be prolonged; can well ensure the synergistic effect of various substances in the preparation, improve the control efficiency, prolong the lasting period and slow down the occurrence of drug resistance.

(2) According to the pesticide preparation containing fosthiazate, under the condition that the grain diameter of the microcapsule containing fosthiazate is determined, the mass ratio of the capsule wall to the capsule core of the microcapsule is required to be within a certain range, so that the stability and the pesticide effect of the pesticide preparation containing fosthiazate can be ensured simultaneously.

(3) According to the preparation method of the fosthiazate-containing pesticide preparation, firstly, active substances containing fosthiazate are prepared into the microcapsule suspending agent and filtered to obtain the cake, and on the basis, the cake is used as a fosthiazate raw material and further mixed with other solid powder materials for granulation to prepare the water dispersible granules or granules containing fosthiazate microcapsules, so that the inherent peculiar smell of fosthiazate can be shielded, and the phytotoxicity to sensitive crops is avoided; the mixing compatibility of the fosthiazate and other substances can be improved, and the mixing difficulty of the fosthiazate and other substances is reduced; but also can effectively ensure the effective content of the fosthiazate in the pesticide preparation containing the fosthiazate.

(3) According to the preparation method of the fosthiazate-containing pesticide preparation provided by the invention, the microcapsule containing the fosthiazate as the active ingredient is required to have a certain thickness of the capsule wall (microcapsule with a certain capsule wall/capsule core mass ratio), and then solid powder is further coated outside the microcapsule to prepare water dispersible granules or granules containing the fosthiazate, so that the prepared product has good storage stability and good pesticide effect.

(4) According to the preparation method of the fosthiazate-containing pesticide preparation, any organic solvent is prevented from being added in the preparation process, the pollution of the organic solvent to the environment is reduced, the quality problems of bag breaking, caking, dispersion, suspension rate reduction and the like caused by the fact that the organic solvent is extruded from the capsule core into solid powder due to extrusion in the processing process are avoided, the storage stability and the slow release performance of the fosthiazate-containing pesticide preparation in use are further guaranteed, and the bioavailability can be remarkably improved.

Detailed Description

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this disclosure relates.

Although any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present disclosure, the preferred methods and materials are described herein. For example, the inert carrier, the fertilizer, the wetting and dispersing agent, the wall forming material of the microcapsule, the emulsifying and dispersing agent, the binder, etc. may be selected in some embodiments, and any material similar or equivalent to the material selected herein may also be used.

As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.

Those who do not specify particular conditions herein, perform according to conventional conditions in the art or conditions suggested by those skilled in the art; the reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.

As used herein, the terms "about," "near," "approximately," and the like are also used for ease of description only to provide the flexibility associated with a given term, metric, or value. The degree of flexibility for a particular variable can be readily determined by one skilled in the art. Lengths, amounts, and other numerical data may be presented herein in a range format. It is to be understood that such a range format is used merely for convenience and brevity and should be interpreted flexibly to include not only the numerical values explicitly recited as the limits of the range, but also to include all the individual numerical values or sub-ranges encompassed within that range as if each numerical value and sub-range is explicitly recited. For example, a numerical range of about 1 to about 4.5 should be interpreted to include not only the explicitly recited limit values of 1 to about 4.5, but also include individual numbers (such as 2, 3, 4) and sub-ranges (such as 1 to 3, 2 to 4, etc.). The same principle applies to ranges reciting only one numerical value, such as "less than about 4.5," which should be construed to include all of the aforementioned values and ranges. Moreover, such an interpretation should apply regardless of the breadth of the range or feature being described.

It is noted that, when the active ingredient comprises only fosthiazate, the pesticide preparation containing fosthiazate provided herein has the active ingredient located inside the microcapsule and the auxiliary ingredient located outside the microcapsule; when the active ingredients of fosthiazate and avermectin are used, fosthiazate is arranged in the microcapsule, and the avermectin and the auxiliary ingredients are both arranged outside the microcapsule.

The active ingredients described herein are the pure contents of fosthiazate, avermectin (raw drug amount x ingredient ratio), not their raw drug contents.

Herein, the capsule wall is composed of a wall-forming material and an emulsion dispersant together.

In addition, the dosage form of the pesticide preparation containing fosthiazate provided by the invention can be water dispersible granules or granules; if the formulation is water dispersible granules, the pesticide preparation comprises an active component, solid powder and a binder; wherein the solid powder comprises an inert carrier, a pH regulator, a wetting dispersant or an inert carrier, abamectin, a pH regulator and a wetting dispersant; if the formulation is granules, the pesticide preparation comprises active components, solid powder and a binder; wherein the solid powder comprises an inert carrier, a fertilizer effect substance or an inert carrier, a fertilizer effect substance and abamectin.

In addition, the conventional extrusion granulation method of the water dispersible granule comprises the steps of preparing raw materials (raw pesticide, auxiliary agent and the like) into superfine wettable powder, adding the superfine wettable powder and a certain amount of water (or containing a binder) into a kneading machine for kneading to prepare a plastic material, wherein the water content is 15-20 wt%, and finally feeding the material into an extrusion granulator for granulation, drying and sieving to obtain a water dispersible granule product.

The conventional extrusion granulation method of the granules described herein is to knead the raw drug, the powdery carrier and water together, then to obtain the granule product through extrusion granulation, drying and screening. In the kneading process, the water addition amount is generally 16-22 wt%, and a proper amount of binder can also be added into the water.

Herein, the melamine formaldehyde resin prepolymer (50%) can be prepared according to the following method, or can be prepared by using a commercially available product, and the preparation method comprises the following steps:

the raw materials and the mixture ratio are that the mass ratio of melamine to formaldehyde is 1: 2.5;

adding an alkali solution into formaldehyde until the pH value is 8-9, then adding melamine, heating to 80 +/-2 ℃, carrying out condensation reaction on melamine-formaldehyde resin for 10-15min, and then adding deionized water to prepare a melamine-formaldehyde resin prepolymer solution with the mass concentration of 50%.

The invention is further described with reference to specific examples.

Example 1

The pesticide preparation containing fosthiazate in the embodiment is composed of microcapsules wrapped with fosthiazate and auxiliary components wrapped outside the microcapsules, and the dosage form is water dispersible granules; the preparation method comprises the following steps:

s1 preparation of a microcapsule cake containing an active substance

Dissolving 20.0g of Ultrazine NA (lignosulfonate) in 460g of water, adding 420g of fosthiazate raw drug (95.3%), shearing into oil-in-water emulsion with the average particle size of 2 mu m, then slowly adding 100g of melamine formaldehyde resin prepolymer (50%) into the emulsion under stirring, stirring and reacting for 1.5h at 30 +/-2 ℃, heating to 50 +/-2 ℃, continuing to react for 2h, cooling to room temperature, and carrying out centrifugal filtration to obtain 693g of fosthiazate microcapsule filter cake with the solid content of 70%, wherein the content of fosthiazate is 57.2% (the mass of the microcapsule wall is 16.7% of the mass of the capsule core, and the content of the microcapsule is 70% of the solid content in the filter cake).

S2 preparation of solid powder

200.0g of SP-27001 (polycarboxylate), 250.0g of Polyfon H, O (lignosulfonate), 10.0g of 10.0g K12 (alkyl sulfate), 5g of citric acid, 35g of white carbon black and 500g of calcined kaolin are uniformly mixed, and are subjected to superfine grinding to obtain 99.9% of solid powder passing through 600 meshes for later use. (wherein the wetting dispersant accounts for 46 percent, the inert filler accounts for 53.5 percent, and the ph regulator accounts for 0.5 percent).

S3 preparation of fosthiazate-containing water dispersible granules

87.5g of 57.2% fosthiazate microcapsule filter cake (with microcapsule content of 70%) obtained in the step 1 is uniformly mixed with 938.8g of solid powder obtained in the step 2, then a proper amount of 0.5% polyvinyl alcohol aqueous solution is added for uniform mixing, and the mixture is extruded, granulated, dried and screened to obtain fosthiazate water dispersible granules (with the thiazole phosphine microcapsule content of 6.1% and the solid powder content of 93.9%) with the particle size of 1 mm-1.7 mm and the fosthiazate content of 5%.

Example 2

s1 preparation of a microcapsule cake containing an active substance

Dissolving 20.0g of Ultrazine NA (lignosulfonate) in 460g of water, adding 420g of fosthiazate raw drug (95.3%), shearing into oil-in-water emulsion with the average particle size of 2 mu m, slowly adding 100g of melamine formaldehyde resin prepolymer (50%) into the emulsion under stirring, stirring and reacting at 30 +/-2 ℃ for 1.5h, heating to 50 +/-2 ℃ for further reacting for 2h, cooling to room temperature, and carrying out centrifugal filtration to obtain 693g of fosthiazate microcapsule filter cake with the solid content of 70%, wherein the content of fosthiazate is 57.2%. (the mass of the microcapsule wall is 16.7 percent of the mass of the capsule core, and the content of the microcapsule is equal to the solid content in the filter cake, namely 70 percent).

S2 preparation of solid powder

S3 preparation of fosthiazate-containing water dispersible granules

437.1g of 57.2% fosthiazate microcapsule filter cake (microcapsule content is 70%) obtained in the step 1 is uniformly mixed with 694g of solid powder obtained in the step 2, then a proper amount of 1% polyvinyl alcohol aqueous solution is added for uniform mixing, and the mixture is extruded, granulated, dried and screened to obtain fosthiazate water dispersible granules with grain diameter of 1 mm-1.7 mm and fosthiazate content of 25%. (the content of the fosthiazate microcapsules is 30.6 percent, and the solid powder is 69.4 percent).

Example 3

s1 preparation of a microcapsule cake containing an active substance

S2 preparation of solid powder

200.0g of SP-27001 (polycarboxylate), 250.0g of Polyfon H, O (lignosulfonate), 10.0g of 10.0g K12 (alkyl sulfate), 5g of citric acid, 35g of white carbon black and 500g of calcined kaolin are uniformly mixed, and are subjected to superfine grinding to obtain 99.9% of solid powder passing through 600 meshes for later use. (wherein the wetting dispersant accounts for 46 percent, the inert filler accounts for 53.5 percent, and the ph regulator accounts for 0.5 percent)

S3 preparation of fosthiazate-containing water dispersible granules

874.2g of the 57.2% fosthiazate microcapsule filter cake (solid content is 70%) obtained in the step 1 is uniformly mixed with 388g of the solid powder obtained in the step 2, then a proper amount of 2% polyvinyl alcohol aqueous solution is added for uniform mixing, and the mixture is extruded, granulated, dried and screened to obtain fosthiazate water dispersible granules (the content of the fosthiazate microcapsule is 61.2% and the solid powder is 38.8%) with the grain diameter of 1 mm-1.7 mm and the fosthiazate content is 50%.

Example 4

The pesticide preparation containing fosthiazate in the embodiment is composed of a microcapsule coated with fosthiazate and an auxiliary component coated outside the microcapsule and containing avermectin, wherein the content of the fosthiazate and the avermectin is respectively 4 wt% and 1 wt%, and the dosage form is water dispersible granules; the preparation method comprises the following steps:

s1 preparation of a microcapsule cake containing an active substance

Dissolving 12.0g of Reax 825E (lignosulfonate) and 5.0g of SP-27001 (polycarboxylate) in 463g of water, adding 420g of fosthiazate raw drug (95.3%), shearing into oil-in-water emulsion with the average particle size of 1 mu m, slowly adding 100g of melamine formaldehyde resin prepolymer (50%) into the emulsion while stirring, stirring and reacting for 1.5h at 30 +/-2 ℃, heating to 50 +/-2 ℃ for further reaction for 2h, cooling to room temperature, and centrifugally filtering to obtain 667.0g of fosthiazate microcapsule filter cake with the solid content of 73%, wherein the content of the fosthiazate is 60.0% (the mass of the microcapsule wall is 16% of the mass of the capsule core, and the content of the microcapsule is the same as the solid content in the filter cake, namely 73%).

S2 preparation of solid powder

11.0g of abamectin original drug (97.5 percent), 50.0g of Agrilan 700 (polycarboxylate), 100.0g of Reax AG (lignosulfonate), 50.0g of Morwet D-425 (alkyl naphthalene sulfonate formaldehyde condensate) and 789.0g of diatomite are uniformly mixed, and are subjected to superfine grinding to obtain 99.9 percent of 1.07 percent of abamectin powder passing through a 600-mesh screen for later use. (wherein the wetting dispersant accounts for 20%, the inert filler accounts for 78.9%, and the abamectin original drug accounts for 1.1%).

S3 preparation of fosthiazate-containing water dispersible granules

83.4g of fosthiazate microcapsule filter cake (solid content is 73%) with 60% of fosthiazate microcapsule filter cake obtained in the step 1 is uniformly mixed with 939.1g of ultrafine powder of 1.07% of abamectin obtained in the step 2, then a proper amount of 0.5% of polyvinyl alcohol aqueous solution is added for uniform mixing, and the mixture is extruded, granulated, dried and sieved to obtain fosthiazate abamectin water dispersible granules (the content of fosthiazate microcapsule is 6.1% and the solid powder is 93.9%) with the particle size of 1 mm-1.7 mm and the active substance content of 5%.

Example 5

The pesticide preparation containing fosthiazate in the embodiment is composed of a microcapsule coated with fosthiazate and an auxiliary component coated outside the microcapsule and containing avermectin, wherein the content of the fosthiazate and the avermectin is 27.0 wt% and 0.5 wt%, and the dosage form is water dispersible granules; the preparation method comprises the following steps:

s1 preparation of a microcapsule cake containing an active substance

Dissolving 12.0g of Reax 825E (lignosulfonate) and 5.0g of SP-27001 (polycarboxylate) in 463g of water, adding 420g of fosthiazate raw drug (95.3%), shearing into oil-in-water emulsion with the average particle size of 5 mu m, slowly adding 100g of melamine formaldehyde resin prepolymer (50%) into the emulsion while stirring, stirring and reacting for 1.5h at 30 +/-2 ℃, heating to 50 +/-2 ℃ for further reaction for 2h, cooling to room temperature, and centrifugally filtering to obtain 667.0g of fosthiazate microcapsule filter cake with the solid content of 73%, wherein the content of the fosthiazate is 60.0% (the mass of the microcapsule wall is 16% of the mass of the capsule core, and the content of the microcapsule is the same as the solid content in the filter cake, namely 73%).

S2 preparation of solid powder

7.7g of abamectin original drug (97.5 percent), 50.0g of Agrilan 700 (polycarboxylate), 100.0g of Reax AG (lignosulfonate), 50.0g of Morwet D-425 (alkyl naphthalene sulfonate formaldehyde condensate) and 792.3g of diatomite are uniformly mixed, and are subjected to superfine grinding to obtain 99.9 percent of abamectin powder which passes through 600 meshes and is 0.75 percent for later use. (wherein the wetting dispersant accounts for 20%, the inert filler accounts for 79.23%, and the abamectin technical accounts for 0.77%).

S3 preparation of fosthiazate-containing water dispersible granules

450g of 60% fosthiazate microcapsule filter cake (solid content is 73%) obtained in the step 1 is uniformly mixed with 671.5g of 0.75% avermectin powder obtained in the step 2, then a proper amount of 1% polyvinyl alcohol aqueous solution is added and uniformly mixed, and the fosthiazate-avermectin water dispersible granule with the particle size of 1 mm-1.7 mm and the active substance content of 27.5% is obtained through extrusion granulation, drying and screening. (the content of the fosthiazate microcapsules is 32.9 percent, and the solid powder is 67.1 percent).

Example 6

The pesticide preparation containing fosthiazate in the embodiment is composed of a microcapsule coated with fosthiazate and an auxiliary component coated outside the microcapsule and containing avermectin, wherein the content of the fosthiazate and the avermectin is 49.5 wt% and 0.5 wt%, and the dosage form is water dispersible granules; the preparation method comprises the following steps:

s1 preparation of a microcapsule cake containing an active substance

Dissolving 12.0g of Reax 825E (lignosulfonate) and 5.0g of SP-27001 (polycarboxylate) in 463g of water, adding 420g of fosthiazate raw drug (95.3%), shearing into oil-in-water emulsion with the average particle size of 15 mu m, slowly adding 100g of melamine formaldehyde resin prepolymer (50%) into the emulsion while stirring, stirring and reacting for 1.5h at 30 +/-2 ℃, heating to 50 +/-2 ℃ for further reaction for 2h, cooling to room temperature, and centrifugally filtering to obtain 667.0g of fosthiazate microcapsule filter cake with the solid content of 73%, wherein the content of the fosthiazate is 60.0% (the mass of the microcapsule wall is 16% of the mass of the capsule core, and the content of the microcapsule is the same as the solid content in the filter cake, namely 73%).

S2 preparation of solid powder

13.1g of abamectin technical material (97.5 percent), 50.0g of Agrilan 700 (polycarboxylate), 100.0g of Reax AG (lignosulfonate), 50.0g of Morwet D-425 (alkyl naphthalene sulfonate formaldehyde condensate), 50g of white carbon black and 736.9g of diatomite are uniformly mixed and subjected to superfine grinding to obtain 1.28 percent of abamectin powder which passes through 600 meshes and is reserved. (wherein the wetting dispersant accounts for 20%, the inert filler accounts for 78.69%, and the abamectin technical accounts for 1.31%).

S3 preparation of fosthiazate-containing water dispersible granules

825g of the 60% fosthiazate microcapsule filter cake (with the solid content of 73%) obtained in the step 1 is uniformly mixed with 397.7g of the 1.28% avermectin ultrafine powder obtained in the step 2, then a proper amount of 1% polyvinyl alcohol aqueous solution is added and uniformly mixed, and then extrusion granulation, drying and screening are carried out to obtain the fosthiazate avermectin water dispersible granule (with the fosthiazate microcapsule content of 60.2% and the solid powder content of 39.8%) with the particle size of 1 mm-1.7 mm and the active substance content of 50%.

Example 7

The pesticide preparation containing fosthiazate in the embodiment is composed of microcapsules coated with fosthiazate and auxiliary components coated outside the microcapsules, and the dosage form is granules; the preparation method comprises the following steps:

s1 preparation of a microcapsule cake containing an active substance

Dissolving 10.0g 10.0g E414 (Arabic gum) and 15.0g carboxymethylcellulose sodium in 463g water, adding 420g fosthiazate raw drug (95.3%), shearing into oil-in-water emulsion with the average particle size of 7 mu m, then slowly adding 100g melamine formaldehyde resin prepolymer (50%) into the emulsion while stirring, stirring and reacting for 1.5h at 30 +/-2 ℃, heating to 50 +/-2 ℃ for further reacting for 2h, cooling to room temperature, and centrifugally filtering to obtain 738.8g fosthiazate microcapsule filter cake with the solid content of 67%, wherein the fosthiazate content is 54.1% (the microcapsule wall mass is 17.9% of the capsule core mass, and the microcapsule content is the same as the solid content in the filter cake, namely 67%).

S2 preparation of solid powder

Uniformly mixing 700g of humic acid, 200g of crab and shrimp shells and 100g of clay, and crushing the mixture through a 300-mesh sieve to obtain organic fertilizer powder for later use; (fertilizer effect substance 90%, inert filler 10%).

S3 preparation of granules containing fosthiazate

And (3) uniformly mixing 9.3g of the 54.1% fosthiazate microcapsule filter cake (with the solid content of 67%) obtained in the step (1) with 993.8g of the organic fertilizer powder obtained in the step (2), adding a proper amount of 5% polyvinyl alcohol aqueous solution, uniformly mixing, extruding, granulating, drying and screening to obtain fosthiazate granules with the grain size of 1-10 mm and the fosthiazate content of 0.5%. (the using amount of the fosthiazate microcapsules is 0.62 percent, and the solid powder is 99.38 percent).

Example 8

s1 preparation of a microcapsule cake containing an active substance

S2 preparation of solid powder

S3 preparation of granules containing fosthiazate

138.6g of the 54.1% fosthiazate microcapsule filter cake (with the solid content of 67%) obtained in the step 1 and 907.1g of the organic fertilizer powder obtained in the step 2 are uniformly mixed, a proper amount of 5% polyvinyl alcohol aqueous solution is added for uniform mixing, and after extrusion granulation, drying and screening, fosthiazate granules with the grain size of 1mm-10mm and the fosthiazate content of 7.5% are obtained. (the using amount of the fosthiazate microcapsules is 9.3 percent, and the solid powder is 90.7 percent).

Example 9

s1 preparation of a microcapsule cake containing an active substance

S2 preparation of solid powder

S3 preparation of granules containing fosthiazate

277.3g of 54.1% fosthiazate microcapsule filter cake (with 67% of solid content) obtained in the step 1 is uniformly mixed with 814.2g of organic fertilizer powder obtained in the step 2, a proper amount of 5% polyvinyl alcohol aqueous solution is added for uniform mixing, and after extrusion granulation, drying and screening, fosthiazate granules (with the grain size of 1mm-10mm and the fosthiazate content of 15%) are obtained (with the fosthiazate microcapsule dosage of 18.6% and the solid powder of 81.4%).

Example 10

The pesticide preparation containing fosthiazate in the embodiment is composed of a microcapsule coated with fosthiazate and an auxiliary component coated outside the microcapsule and containing avermectin, wherein the content of the fosthiazate and the avermectin is 0.5 wt% and 0.5 wt%, and the preparation form is granules; the preparation method comprises the following steps:

s1 preparation of a microcapsule cake containing an active substance

30.0g of Borresperse NA (lignosulfonate) and 5.0g of carboxymethylcellulose sodium are dissolved in 463g of water, 420g of fosthiazate raw drug (95.3%) is added, the mixture is sheared into oil-in-water emulsion with the average particle size of 20 mu m, then 100g of melamine formaldehyde resin prepolymer (50%) is slowly added into the emulsion under stirring, the mixture is stirred and reacted for 1.5h at the temperature of 30 +/-2 ℃, the temperature is increased to 50 +/-2 ℃ for continuous reaction for 2h, the temperature is reduced to room temperature, and centrifugal filtration is carried out to obtain 737.2g of fosthiazate microcapsule filter cake with the solid content of 68.5%, wherein the content of the fosthiazate is 54.3% (the mass of the microcapsule wall is 20.2% of the mass of the capsule core, and the content of the microcapsule is the same as the solid content in the filter cake, namely 68.5%).

S2 preparation of solid powder

Uniformly mixing 700g of humic acid, 244.8g of seaweed powder, 50g of kaolin and 5.2g of abamectin raw drug (97.5 percent), crushing and sieving by using a 300-mesh sieve to obtain 0.51 percent of abamectin organic fertilizer powder for later use; (the fertilizer effect substance is 94.48 percent, the inert filler is 5 percent, and the abamectin technical is 0.52 percent).

S3 preparation of granules containing fosthiazate

9.2g of the 54.3% fosthiazate microcapsule filter cake (with the solid content of 68.5%) obtained in the step 1 and 993.7g of the 5.1% avermectin organic fertilizer powder obtained in the step 2 are uniformly mixed, a proper amount of 5% polyvinyl alcohol aqueous solution is added for uniform mixing, and after extrusion granulation, drying and screening, fosthiazate avermectin (0.5% + 0.5%) granules with the particle size of 1mm-10mm and the active substance content of 1% are obtained. (the using amount of the fosthiazate microcapsules is 0.63 percent, and the solid powder is 99.37 percent).

Example 11

The pesticide preparation containing fosthiazate in the embodiment is composed of a microcapsule coated with fosthiazate and an auxiliary component coated outside the microcapsule and containing avermectin, wherein the content of the fosthiazate and the avermectin is 5 wt% and 0.5 wt%, and the dosage form is granules; the preparation method comprises the following steps:

s1 preparation of a microcapsule cake containing an active substance

Dissolving 10.0g 10.0g E414 (Arabic gum) and 15.0g carboxymethylcellulose sodium in 463g water, adding 420g fosthiazate raw drug (95.3%), shearing into oil-in-water emulsion with the average particle size of 3 mu m, then slowly adding 100g melamine formaldehyde resin prepolymer (50%) into the emulsion with stirring, stirring and reacting for 1.5h at 30 +/-2 ℃, heating to 50 +/-2 ℃, continuing to react for 2h, cooling to room temperature, and centrifugally filtering to obtain 738.8g fosthiazate microcapsule filter cake with the solid content of 67%, wherein the fosthiazate content is 54.1% (the microcapsule wall mass is 20.2% of the capsule core mass, and the microcapsule content is the same as the solid content in the filter cake, namely 68.5%).

S2 preparation of solid powder

Uniformly mixing 700g of humic acid, 238.0g of seaweed powder, 50g of kaolin and 5.4g of abamectin original drug (97.5 percent), crushing and sieving by using a 300-mesh sieve to obtain 0.53 percent of abamectin organic fertilizer powder for later use; (the fertilizer effect substance is 98.96 percent, the inert filler is 5 percent, and the abamectin technical is 0.54 percent).

S3 preparation of granules containing fosthiazate

92.1g of fosthiazate microcapsule filter cake (solid content is 68.5%) with 54.3% obtained in the step 1 is uniformly mixed with 943.4g of avermectin organic fertilizer powder with 5.3% obtained in the step 2, a proper amount of 5% polyvinyl alcohol aqueous solution is added for uniform mixing, and after extrusion granulation, drying and screening, fosthiazate avermectin (5% + 0.5%) granules with the grain diameter of 1mm-10mm and the active substance content of 5.5% are obtained. (the using amount of the fosthiazate microcapsules is 0.63 percent, and the solid powder is 99.37 percent).

Example 12

The pesticide preparation containing fosthiazate in the embodiment is composed of a microcapsule coated with fosthiazate and an auxiliary component coated outside the microcapsule and containing avermectin, wherein the content of the fosthiazate and the avermectin is 10 wt% and 1 wt%, and the dosage form is granules; the preparation method comprises the following steps:

s1 preparation of a microcapsule cake containing an active substance

Dissolving 10.0g 10.0g E414 (Arabic gum) and 15.0g carboxymethylcellulose sodium in 463g water, adding 420g fosthiazate raw drug (95.3%), shearing into oil-in-water emulsion with the average particle size of 20 mu m, then slowly adding 100g melamine formaldehyde resin prepolymer (50%) into the emulsion with stirring, stirring and reacting for 1.5h at 30 +/-2 ℃, heating to 50 +/-2 ℃, continuing to react for 2h, cooling to room temperature, and centrifugally filtering to obtain 738.8g fosthiazate microcapsule filter cake with the solid content of 67%, wherein the fosthiazate content is 54.1% (the microcapsule wall mass is 20.2% of the capsule core mass, and the microcapsule content is the same as the solid content in the filter cake, namely 68.5%).

S2 preparation of solid powder

Uniformly mixing 700g of humic acid, 238.2g of seaweed powder, 50g of kaolin and 11.8g of abamectin raw pesticide (97.5 percent), crushing and sieving by using a 300-mesh sieve to obtain 1.15 percent of abamectin organic fertilizer powder for later use; (93.82 percent of fertilizer effect substance, 5 percent of inert filler and 1.18 percent of abamectin original drug).

S3 preparation of granules containing fosthiazate

184.2g of the 54.3% fosthiazate microcapsule filter cake (with the solid content of 68.5%) obtained in the step 1 and 873.8g of the 1.15% avermectin organic fertilizer powder obtained in the step 2 are uniformly mixed, a proper amount of 5% polyvinyl alcohol aqueous solution is added for uniform mixing, and after extrusion granulation, drying and screening, fosthiazate avermectin (10% + 1%) granules with the particle size of 1mm-10mm and the active substance content of 11% are obtained. (fosthiazate microcapsule content 12.62%, solid powder 87.38%).

Comparative example 1

The pesticide preparation containing fosthiazate in the embodiment is a microcapsule which is wrapped by the fosthiazate and is the same as the microcapsule in the embodiment 9, and the preparation form is as follows:

the preparation method comprises the following steps:

s1 preparation of microcapsule suspensions containing active substances

Dissolving 10.0g E414 (Arabic gum) and 15.0g of sodium carboxymethylcellulose in 463g of water, adding 420g of fosthiazate raw drug (95.3%), shearing into oil-in-water emulsion with the average particle size of 7 mu m, slowly adding 100g of melamine formaldehyde resin prepolymer (50%) into the emulsion while stirring, stirring and reacting for 1.5h at 30 +/-2 ℃, heating to 50 +/-2 ℃, continuing to react for 2h, and cooling to room temperature to obtain a fosthiazate microcapsule suspension (the content of fosthiazate is 40%) for later use.

S2 preparation of suspending agent containing fosthiazate microcapsules

2g of xanthan gum (suspension thickening aid) is dissolved in 500g of water, 40g of propylene glycol (antifreeze agent), 10g of sodium benzoate (preservative) and 375g of the fosthiazate microcapsule suspension (fosthiazate content 40%) are added, and the mixture is stirred and mixed uniformly to obtain the medicament of the comparative example 1, namely the 15% fosthiazate microcapsule suspension.

Compared with the embodiment of the invention, the comparative example 1 lacks the solid powder accounting for 81.4 percent of the preparation amount, and the solid powder is added and mixed according to the proportion for application in the pharmacodynamic test to accurately reflect the difference of the invention and the prior art.

The composition and preparation of the solid powder were the same as those of example 9.

Comparative example 2

The pesticide preparation containing fosthiazate in the embodiment is composed of microcapsules coated with fosthiazate and auxiliary components coated outside the microcapsules, and the dosage form is granules; basically, the method is the same as the method in example 9 except that:

s1 preparation of microcapsule suspensions containing active substances

Dissolving 10.0g E414 (Arabic gum) and 15.0g of sodium carboxymethylcellulose in 463g of water, adding 420g of fosthiazate raw drug (95.3%), shearing into oil-in-water emulsion with the average particle size of 7 mu m, slowly adding 100g of melamine formaldehyde resin prepolymer (50%) into the emulsion under stirring, stirring and reacting for 1.5h at 30 +/-2 ℃, heating to 50 +/-2 ℃, continuing to react for 2h, and cooling to room temperature to obtain a fosthiazate microcapsule suspension (the content of fosthiazate is 40%, and the solid content is 49.5% for later use).

S2 preparation of solid powder, same as in example 9.

S3 preparation of granules containing fosthiazate

814.2g of solid powder is uniformly dispersed in 800 g of water, 375g of microcapsule suspension and a proper amount of 5% polyvinyl alcohol aqueous solution are added, the mixture is uniformly stirred and dispersed, and granules with the grain diameter of 1 mm-1.7 mm are collected by spraying, drying and granulating, so that 15% fosthiazate water dispersible granules (the usage amount of fosthiazate microcapsules is 18.6%, and the solid powder is 81.4%) are obtained.

Comparative example 3

The pesticide preparation containing fosthiazate in the embodiment is composed of microcapsules coated with fosthiazate and auxiliary components coated outside the microcapsules, and the dosage form is granules; essentially the same as example 9, except that:

s1 preparation of microcapsule suspensions containing active substances

S2 preparation of solid powder, same as in example 9.

S3 preparation of granules containing fosthiazate

814.2g of solid powder is evenly dispersed in 800 g of water, then 375g of microcapsule suspension and a proper amount of 5 percent polyvinyl alcohol aqueous solution are added, the mixture is evenly stirred and dispersed, and granules with the grain diameter of 1mm to 10mm are collected by spray drying granulation and screening, thus obtaining 15 percent fosthiazate granules (the usage amount of the fosthiazate microcapsules is 18.6 percent, and the solid powder is 81.4 percent).

Example 13

The pesticide preparation containing fosthiazate in the embodiment is composed of a microcapsule coated with fosthiazate and an auxiliary component coated outside the microcapsule and containing abamectin, wherein the content of the fosthiazate is 50 wt%, and the dosage form is water dispersible granules; the specific preparation method of the pesticide preparation containing fosthiazate in this example is basically the same as that of example 3, and the only difference is that:

in step S1, the mass of the prepared microcapsule wall is 3% of the mass of the capsule core, specifically:

dissolving 5.0g of UltrazineNA (lignosulfonate) in 559.8g of water, adding 420g of fosthiazate raw drug (95.3%), shearing into oil-in-water emulsion with the average particle size of 2 mu m, then slowly adding 15.2g of melamine formaldehyde resin prepolymer (50%) into the emulsion under stirring, stirring and reacting for 1.5h at 30 +/-2 ℃, heating to 50 +/-2 ℃, continuing to react for 2h, cooling to room temperature, and centrifugally filtering to obtain 712.6g of fosthiazate microcapsule filter cake with the solid content of 60.7%, wherein the content of fosthiazate is 56.1%.

Step S2 is the same as in example 3;

s3 preparation of fosthiazate-containing water dispersible granules

891.3g of 56.1% fosthiazate microcapsule filter cake (solid content is 60.7%) obtained in the step 1 is uniformly mixed with 459.0g of solid powder obtained in the step 2, then a proper amount of 2% polyvinyl alcohol aqueous solution is added and uniformly mixed, and granules with the grain diameter of 1 mm-1.7 mm are obtained through extrusion granulation, drying and screening, so that 50% fosthiazate water dispersible granules (the content of the fosthiazate microcapsule is 54.1% and the solid powder is 45.9%) are obtained.

Example 14

in step S1, the mass of the prepared microcapsule wall is 10% of the mass of the capsule core, specifically:

dissolving 15g of Ultrazine NA (lignosulfonate) in 511g of water, adding 420g of fosthiazate raw drug (95.3%), shearing into oil-in-water emulsion with the average particle size of 2 mu m, slowly adding 54g of melamine formaldehyde resin prepolymer (50%) into the emulsion under stirring, stirring at 30 +/-2 ℃ for reaction for 1.5h, heating to 50 +/-2 ℃ for continuous reaction for 2h, cooling to room temperature, and performing centrifugal filtration to obtain 731g of fosthiazate microcapsule filter cake with the solid content of 63.2%, wherein the content of fosthiazate is 54.7%.

Step S2 is the same as in example 3;

s3 preparation of fosthiazate-containing water dispersible granules

914.1g of 54.7% fosthiazate microcapsule filter cake (solid content: 63.2%) obtained in the step 1 is uniformly mixed with 422.3g of solid powder obtained in the step 2, then a proper amount of 2% polyvinyl alcohol aqueous solution is added and uniformly mixed, and granules with the grain diameter of 1 mm-1.7 mm are obtained through extrusion granulation, drying and screening, so that 50% fosthiazate water dispersible granules (the content of the fosthiazate microcapsule: 57.8% and the solid powder: 42.2%) are obtained.

Example 15

in step S1, the mass of the prepared microcapsule wall is 20% of the mass of the capsule core, specifically:

dissolving 20g of Ultrazine NA (lignosulfonate) in 432g of water, adding 420g of fosthiazate raw drug (95.3%), shearing into oil-in-water emulsion with the average particle size of 2 mu m, slowly adding 128g of melamine formaldehyde resin prepolymer (50%) into the emulsion under stirring, stirring at 30 +/-2 ℃ for reaction for 1.5h, heating to 50 +/-2 ℃ for continuous reaction for 2h, cooling to room temperature, and performing centrifugal filtration to obtain 723g of fosthiazate microcapsule filter cake with the solid content of 69.7%, wherein the content of fosthiazate is 55.3%.

Step S2 is the same as in example 3;

s3 preparation of fosthiazate-containing water dispersible granules

904.2g of the 55.3% fosthiazate microcapsule filter cake (solid content is 69.7%) obtained in the step 1 is uniformly mixed with 369.8g of the solid powder obtained in the step 2, then a proper amount of 2% polyvinyl alcohol aqueous solution is added and uniformly mixed, and granules with the grain diameter of 1 mm-1.7 mm are obtained through extrusion granulation, drying and screening, so that 50% fosthiazate water dispersible granules (the content of the fosthiazate microcapsule is 50% and the solid powder is 37.0%) are obtained.

Example 16

The pesticide preparation containing fosthiazate in the embodiment is composed of microcapsules coated with fosthiazate and auxiliary components coated outside the microcapsules, wherein the content of the fosthiazate is 15 wt%, and the dosage form is granules; the specific preparation method of the pesticide preparation containing fosthiazate in this example is basically the same as that of example 9, and the only difference is that:

in step S1, the mass of the prepared microcapsule wall is 15% of the mass of the capsule core, specifically:

dissolving 10g E414 (Arabic gum) and 15g of sodium carboxymethylcellulose in 479g of water, adding 420g of fosthiazate raw drug (95.3%), shearing into oil-in-water emulsion with the average particle size of 7 mu m, slowly adding 76g of melamine formaldehyde resin prepolymer (50%) into the emulsion while stirring, stirring and reacting at 30 +/-2 ℃ for 1.5h, heating to 50 +/-2 ℃ for further reacting for 2h, cooling to room temperature, and performing centrifugal filtration to obtain 750g of fosthiazate microcapsule filter cake with the solid content of 64.4%, wherein the fosthiazate content is 53.3% (the capsule wall mass of the microcapsule is 15% of the capsule core mass, and the microcapsule content is the same as the solid content in the filter cake, namely 64.4%);

step S2 is the same as in example 9;

s3 preparation of granules containing fosthiazate

281.4g of the 53.3% fosthiazate microcapsule filter cake (with the solid content of 64.4%) obtained in the step 1 and 818.8g of the organic fertilizer powder obtained in the step 2 are uniformly mixed, a proper amount of 5% polyvinyl alcohol aqueous solution is added for uniform mixing, and after extrusion granulation, drying and screening, fosthiazate granules (with the content of the fosthiazate microcapsule of 18.2% and the solid powder of 81.8%) with the grain size of 1mm-10mm 15% are obtained.

Example 17

in step S1, the mass of the prepared microcapsule wall is 25% of the mass of the capsule core, specifically:

dissolving 10g E414 (Arabic gum) and 15g of sodium carboxymethylcellulose in 395g of water, adding 420g of fosthiazate raw drug (95.3%), shearing into oil-in-water emulsion with the average particle size of 7 mu m, slowly adding 160g of melamine formaldehyde resin prepolymer (50%) into the emulsion under stirring, stirring at 30 +/-2 ℃ for reaction for 1.5h, heating to 50 +/-2 ℃ for continuous reaction for 2h, cooling to room temperature, and carrying out centrifugal filtration to obtain 729.2g of fosthiazate microcapsule filter cake with the solid content of 72%, wherein the content of the fosthiazate is 54.9% (the mass of the microcapsule wall is 25% of the mass of the capsule core, and the content of the microcapsule is the same as the solid content in the filter cake, namely 72%);

step S2 is the same as in example 9;

s3 preparation of granules containing fosthiazate

273.2g of 54.1% fosthiazate microcapsule filter cake (solid content 72%) obtained in the step 1 and 803.3g of organic fertilizer powder obtained in the step 2 are uniformly mixed, a proper amount of 5% polyvinyl alcohol aqueous solution is added for uniform mixing, and after extrusion granulation, drying and screening, fosthiazate granules (the content of fosthiazate microcapsules is 19.7% and the solid powder content is 80.3%) with the grain size of 1mm-10mm 15% are obtained.

Example 18

in step S1, the prepared microcapsule has a wall mass of 35% of the core mass, specifically:

dissolving 15.0g 15.0g E414 (Arabic gum) and 30.0g carboxymethylcellulose sodium in 331g of water, adding 420g of fosthiazate raw drug (95.3%), shearing into oil-in-water emulsion with the average particle size of 7 mu m, then slowly adding 204g of melamine formaldehyde resin prepolymer (50%) into the emulsion under stirring, stirring and reacting for 1.5h at 30 +/-2 ℃, heating to 50 +/-2 ℃, continuing to react for 2h, cooling to room temperature, and centrifugally filtering to obtain 808.1g of fosthiazate microcapsule filter cake with the solid content of 71%, wherein the content of fosthiazate is 49.5% (the mass of the microcapsule wall is 35% of the mass of the capsule core, and the content of the microcapsule is the same as the solid content in the filter cake, namely 71%).

Step S2 is the same as in example 9;

s3 preparation of granules containing fosthiazate

303.0g of the fosthiazate microcapsule filter cake (solid content 71%) obtained in the step 1 and 784.8g of the organic fertilizer powder obtained in the step 2 are uniformly mixed, a proper amount of 5% polyvinyl alcohol aqueous solution is added to be uniformly mixed, and after extrusion granulation, drying and screening, fosthiazate granules (the content of the fosthiazate microcapsule is 21.5% and the solid powder is 78.5%) with the grain size of 1mm-10mm 15% are obtained.

Example 19

Compared with the conventional fosthiazate preparation, the fosthiazate pesticide preparation provided by the invention has the advantages that the quality and the storage stability of the fosthiazate preparation are obviously improved. The differences in the fosthiazate pesticide formulations and the methods of preparation thereof of the present invention are illustrated by comparing the test results of the main quality control items of the fosthiazate formulations of the examples of the present invention with those of commercial or conventionally prepared fosthiazate formulations.

Table 1 shows the test results of the main quality control items of the examples and comparative examples of the present invention, and the suspension percentage and the thermal storage decomposition rate in Table 1 were measured according to GB/T14825-2006 or GB/T19136-2003, respectively.

CK1-6 and CK13-15 in Table 1 are water dispersible granules prepared by a conventional extrusion granulation method, and active ingredients, a dispersion wetting aid, a filler, a binder and the like are the same as those in the corresponding examples;

CK7-12 and CK16-18 are granules prepared by a conventional extrusion granulation method, and active ingredients, a dispersing wetting auxiliary agent, a fertilizer effect substance, a filler, a binder and the like are the same as those in the corresponding examples;

comparative example 1 is a microcapsule suspension prepared by the prior art, comparative examples 2 and 3 are water dispersible granules and granules prepared by spray granulation, the components contain non-solid substances in the reaction liquid for preparing the microcapsule, and other components are the same as those in example 9.

TABLE 1 main quality control items of water dispersible granule containing fosthiazate

Compared with the prior art, the pesticide preparation containing fosthiazate provided by the invention has the advantages that the storage stability of the preparation is obviously improved, the heat storage decomposition rate of the active ingredients is obviously lower than that of a control medicament, the suspension rate of the fosthiazate water dispersible granule provided by the embodiments 1-6 of the invention is obviously higher than that of the control medicament, and the heat storage decomposition rate is obviously lower than that of the control medicament, taking the embodiment 5 as an example, the suspension rate of fosthiazate in the embodiment 5 of the invention is 95.7%, the suspension rate of abamectin is 87.6%, the heat storage decomposition rate of fosthiazate is 4.1%, and the suspension rate of abamectin is 3.2% (the suspension rate of fosthiazate in the control medicament CK5 is 78.9%, the suspension rate of abamectin is 77.4%, the heat storage decomposition rate of fosthiazate is 14.2%, and the suspension rate of abamectin is 77.5%); the fosthiazate granules provided by examples 7 to 12 of the present invention have good storage stability relative to a control agent, and example 9 is taken as an example, the thermal storage decomposition rate of example 9 of the present invention is 4.3% (CK9, comparative example 1, comparative example 2, and comparative example 3 is 40.1%).

According to the fosthiazate-containing water dispersible granule, the mass ratio of the capsule wall to the capsule core is preferably 5-30% and is lower than 5%, the mass of the granule is obviously influenced, example 13 (the mass ratio of the capsule wall to the capsule core is 3%, the suspension rate is 67%, and the heat storage decomposition rate is 13.7%) is equivalent to that of CK13 (the suspension rate is 65%, and the heat storage decomposition rate is 13.9%), and the mass ratio of the capsule wall to the capsule core is obviously lower than that of example 3 (the suspension rate is 89.5%, and the heat storage decomposition rate is 4.5%) within the range of 5-30%; in the granules containing fosthiazate of the present invention, the mass ratio of capsule wall to capsule core is preferably 17.9 to 20.2%, and when the mass ratio is less than 5%, the mass is significantly affected, and example 16 (mass ratio of capsule wall to capsule core is 15%, and heat storage decomposition rate is 17.6%) is slightly superior to control CK13 (heat storage decomposition rate is 20.4%), and is significantly lower than example 9 (heat storage decomposition rate is 4.3%) when the mass ratio of capsule wall to capsule core is 17.9 to 20.2%.

The following field efficacy tests show that the fosthiazate water dispersible granules provided by the embodiments 1 to 6 or the fosthiazate granules provided by the embodiments 7 to 12 can control the harm of nematodes in seedling stage and even whole growth stage of the crop, and the crop yield is obviously improved. The control medicament used in the test is fosthiazate water dispersible granules or fosthiazate granules prepared by a conventional method, and the active ingredients, the dispersing wetting auxiliary, the fertilizer effect substances, the fillers, the bonding agents and the like are the same as the corresponding examples. The dosages of the field efficacy test are shown in table 2.

TABLE 2 field drug effect test Agents and dosages

The composition and preparation method of the fertilizer powder are the same as those of the solid powder in example 9, the using ratio of the fosthiazate to the fertilizer powder is the same as that of example 9, namely the fosthiazate (folded powder): the fertilizer powder is 15: 81.4, 200g of fosthiazate CS (15%) is mixed with 162.8g of the fertilizer powder for use, before application, 200g of 15% fosthiazate CS and 162.8g of the fertilizer powder are mixed to be prepared into particles, and after most of moisture is dried in the air, the particles are spread.

According to the related method of pesticide field efficacy test criteria of the people's republic of China, cucumber greenhouses with the same crop varieties and basically consistent fertilizer and water management and underground pest occurrence conditions are respectively selected, different treatment cells are divided, blank control is set for each treatment, and the pesticide is applied according to the test scheme shown in the table 3. The application mode is that the embodiment 1 to the embodiment 6 and the comparison CK1 to CK6 are that the seedling stage is watered and the root is irrigated, the embodiment 7 to the embodiment 18 and the comparison CK7 to CK18 and the comparison example 1 to 3 are that the hole ditch is directly broadcast before sowing or before seedling transplanting. Blank control is set in each test field, normal water and fertilizer management is carried out, nematode damage conditions are investigated 30 days, 60 days and 90 days after pesticide application, mu harvesting amount is counted, and the control effect of root-knot nematodes and the mu yield in each treatment area are shown in table 3.

TABLE 3 root-knot nematode control Effect and mu yield in each treatment area

The control effect of the preparation obtained in the embodiment of the invention is not obviously different from that of a control medicament in 30 days after the preparation, but is obviously better than that of the control medicament in 60 days and 90 days after the preparation. Compared with a control medicament, the preparation prepared by the embodiment of the invention has good slow release performance (taking the embodiment 9 as an example, the control effect of 71.1% after 30 days (the control effect of CK9 is 68.5%), the control effect of 60 days after the preparation is 80.5% (the control effect of CK9 is 70.2%, the control effect of 63.2% in comparison example 1, the control effect of 67.7% in comparison example 2 and the control effect of 55.4% in comparison example 3), the control effect of 90 days after the preparation is 93.3% (the control effect of CK9 is 50.4%, the control effect of 51.3% in comparison example 1 and the control effect of 46.3% in comparison example 2 and the control effect of 44.0% in comparison example 3), the slow release effect is very obvious), the bioavailability can be obviously improved, the nematocidal effect of fosthiazate is fully exerted, the yield of cucumber per mu is improved by 40% (the yield per mu of 16785 kg in the embodiment 9, the yield of CK9 is 11986 kg, the yield per mu in comparison example 1 is 12658 kg, the yield per mu of comparative example 2 is 12330 kg and the yield per mu of comparative example 3 is 11547 kg).

The water dispersible granule containing fosthiazate disclosed by the invention has the advantages that the mass ratio of the capsule wall to the capsule core is 16-16.7% by an optimal selection method, and the control effect is obviously influenced when the mass of the capsule wall and the capsule core exceeds the range, in example 13 (the mass ratio of the capsule wall to the capsule core is 3%, the control effect in 30 days is 66.4%, the control effect in 60 days is 60.3%, the control effect in 90 days is 45.3%, and the yield per mu of cucumber is 12143 kg) the water dispersible granule is equivalent to that of control CK13 (the control effect in 30 days is 67.7%, the control effect in 60 days is 60.2%, the control effect in 90 days is 42.7%, and the yield per mu of cucumber is 12007 kg), and the water dispersible granule is obviously lower than that the mass ratio of the capsule wall to the capsule core is 5-30% (the control effect in 30 days is 70.2%, the control effect in 60 days is 80.2%, the control effect in 90 days is 91.8%, and the yield per mu of cucumber is 16322 kg); example 15 (the mass ratio of the capsule wall to the capsule core is 20%, the control effect in 30 days is 51.3%, the control effect in 60 days is 66.1%, the control effect in 90 days is 74.1%, and the cucumber yield per mu is 12085 kg) is equivalent to that of control CK13 (the control effect in 30 days is 67.7%, the control effect in 60 days is 67.4%, the control effect in 90 days is 46.3%, and the cucumber yield per mu is 12699 kg), and is significantly lower than that of the capsule wall and the capsule core in the range of 5-30% (the control effect in 30 days is 70.2%, the control effect in 60 days is 80.2%, the control effect in 90 days is 91.8%, and the cucumber yield per mu is 16322 kg); in the granules containing fosthiazate, the mass ratio of the capsule wall to the capsule core is 17.9-20.2% preferably, and the control effect is significantly influenced when the mass ratio of the capsule wall to the capsule core exceeds the range, in example 16 (the mass ratio of the capsule wall to the capsule core is 15%, the control effect in 30 days is 70.2%, the control effect in 60 days is 80.2%, the control effect in 90 days is 91.8%, and the yield per mu of cucumber is 16322 kg) is equivalent to that of control CK16 (the control effect in 30 days is 69.6%, the control effect in 60 days is 70.6%, the control effect in 90 days is 51.9%, and the yield per mu of cucumber is 12001 kg), and the mass ratio of the capsule wall to the capsule core is significantly lower than that in example 9 (the mass ratio of the capsule wall to the capsule core is 17.9-20.2%) (the control effect in 30 days is 71.1%, the control effect in 60 days is 80.5%, the control effect in 90 days is 93.3%, and the yield per mu of cucumber is 16785 kg); example 18 (35% of capsule wall and capsule core by mass, 55.5% of 30-day control effect, 63.5% of 60-day control effect, 50.3% of 90-day control effect, and 11785 kg of cucumber yield per mu) is slightly lower than control CK18 (65.6% of 30-day control effect, 70.3% of 60-day control effect, 51.9% of 90-day control effect, and 12625 kg of cucumber yield per mu), and is significantly lower than example 9 (71.1% of 30-day control effect, 80.5% of 60-day control effect, 93.3% of 90-day control effect, and 16785 kg of cucumber yield per mu) in which the mass ratio of capsule wall and capsule core is 17.9-20.2%.

Claims

1. A pesticide preparation containing fosthiazate comprises an active ingredient and an auxiliary ingredient, and is characterized in that: the active ingredients comprise fosthiazate or fosthiazate and abamectin; the auxiliary component is solid powder; the content of the active ingredients is 0.5-50 wt%;

the active ingredient fosthiazate is positioned inside the microcapsule, and the active ingredient abamectin and the solid powder are positioned outside the microcapsule;

the content of the microcapsule is 0.6-61.2%;

the pesticide preparation is water dispersible granules or granules;

the wall forming material of the microcapsule is one or more than one of polyurea, polylactic acid, polymethacrylate, melamine formaldehyde resin prepolymer and phenolic aldehyde modified urea formaldehyde resin prepolymer;

if the pesticide preparation containing fosthiazate is water dispersible granules, the particle size of the microcapsule is 1-15 mu m, the mass ratio of the capsule wall to the capsule core of the microcapsule is 16-16.7%, and the solid powder comprises an inert carrier and a wetting dispersant;

if the pesticide preparation containing fosthiazate is granules, the particle size of the microcapsule is 3-20 mu m, the mass ratio of the capsule wall to the capsule core of the microcapsule is 17.9-20.2%, and the solid powder comprises an inert carrier;

s2, preparing solid powder;

2. The pesticidal formulation containing fosthiazate according to claim 1, characterized in that: the active ingredients comprise fosthiazate and abamectin at the content ratio of (1-99) to (1-2.62).

3. The pesticidal formulation containing fosthiazate according to claim 2, characterized in that: the content ratio of the active components fosthiazate and abamectin is 84 (1-2.62).

4. The pesticidal formulation containing fosthiazate according to claim 1, characterized in that: the pesticide preparation comprises the following components in parts by weight:

1-102 parts of a microcapsule filter cake containing an active ingredient;

64-167 parts of solid powder.

5. The fosthiazate-containing pesticidal formulation according to claim 4, characterized in that: the fineness of the solid powder is that 99.9% of the solid powder passes through 300-600 meshes;

the solid powder comprises the following components in parts by weight:

0.1-99 parts of an inert carrier;

0-90 parts of wetting dispersant;

0-30 parts of abamectin;

0-99.9 parts of fertilizer effect substances.

6. The pesticidal formulation containing fosthiazate according to claim 1, characterized in that:

if the pesticide preparation containing fosthiazate is water dispersible granules, the solid powder comprises the following components in parts by weight:

0.1-99 parts of an inert carrier;

10-90 parts of a wetting dispersant;

0-30 parts of abamectin;

0.1-99 parts of an inert carrier;

0-30 parts of abamectin;

50-99 parts of fertilizer effect substances.

7. The fosthiazate-containing pesticidal formulation according to any one of claims 1 to 6, wherein:

the S1 specifically includes: shearing a mixed solution containing an active substance and an emulsifying dispersant to form an oil-in-water emulsion;

then, adding a wall forming material, carrying out in-situ polymerization on an oil-water interface of the emulsion to form a capsule wall, and heating and curing to obtain a microcapsule suspension containing an active substance;

and finally, filtering to obtain a microcapsule filter cake.