CN111116499A - Triazolone water dispersible granule bactericide with crop resistance adjusting function and preparation method thereof - Google Patents

Triazolone water dispersible granule bactericide with crop resistance adjusting function and preparation method thereof Download PDF

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Publication number
CN111116499A
CN111116499A CN201811273602.9A CN201811273602A CN111116499A CN 111116499 A CN111116499 A CN 111116499A CN 201811273602 A CN201811273602 A CN 201811273602A CN 111116499 A CN111116499 A CN 111116499A
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triazolone
water dispersible
dispersible granule
sodium
sulfate
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彭昆
姜海鹏
刘志勇
严志超
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Jiangsu Sword Agrochemicals Co ltd
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Jiangsu Sword Agrochemicals Co ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D249/00Heterocyclic compounds containing five-membered rings having three nitrogen atoms as the only ring hetero atoms
    • C07D249/02Heterocyclic compounds containing five-membered rings having three nitrogen atoms as the only ring hetero atoms not condensed with other rings
    • C07D249/081,2,4-Triazoles; Hydrogenated 1,2,4-triazoles
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, 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
    • A01N25/12Powders or granules
    • A01N25/14Powders or granules wettable

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  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Pest Control & Pesticides (AREA)
  • Agronomy & Crop Science (AREA)
  • Plant Pathology (AREA)
  • Toxicology (AREA)
  • Engineering & Computer Science (AREA)
  • Dentistry (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention discloses a triazolone water dispersible granule bactericide with the function of adjusting crop resistance, which is characterized by comprising the following components: triazolone: 20-80 wt%, dispersant: 1-10 wt%, wetting agent: 1-10 wt%, disintegrating agent: 0.5-15 wt%, binder: 0.5-10 wt%, and the balance: and (4) filling. The triazolone water dispersible granule provided by the scheme of the invention is added with various different types of auxiliary agents, independently developed wetting agents, dispersing agents and disintegrating agents with optimal proportion, so that the triazolone water dispersible granule has the advantages of high active component content, small environmental pollution, high disintegration speed, good dispersibility, stable stability over time and heat storage performance and the like, and meanwhile, the activity of plants of crops can be improved, the absorption and utilization rate of effective components of the crops can be improved, and the stress resistance of the crops can be improved. The broad-spectrum bactericidal performance of the crops is excellent, and the safety is outstanding.

Description

Triazolone water dispersible granule bactericide with crop resistance adjusting function and preparation method thereof
Technical Field
The invention belongs to the technical field of plant sterilization medicaments, and particularly relates to a triazolone water dispersible granule bactericide which has a good sterilization effect and can properly adjust plant resistance and a preparation method thereof.
Background
Triazolone, chemical name: 1- (4-chlorophenoxy) -3, 3-dimethyl-1- (1,2, 4-triazole-1-yl) -2-butanone and triazolone is a systemic fungicide with high efficiency, low toxicity, low residue and broad spectrum, has special control effect on rust disease and powdery mildew of crops such as wheat, vegetables, fruit trees and the like, and is used for controlling wheat rust disease, powdery mildew, head smut of corn and sorghum, corn orchard spot disease and the like.
At present, triazolone is conventionally processed into wettable powder, missible oil or suspending agent for use. The wettable powder has serious dust drift in the actual use process, has great influence on human bodies and crops, uses a large amount of organic solvent in the production of missible oil, wastes resources, and pollutes the environment after being used, and the suspending agent cannot be processed into a high-content preparation due to the formulation characteristics. Therefore, the triazolone wettable powder and the suspending agent bring inconvenience in production, transportation and use in the application process.
The water dispersible granule is a novel preparation developed on the basis of wettable powder and a suspending agent. The dosage form overcomes the defects of wettable powder and suspending agent, has the advantages of environmental protection, safety and low cost, reduces the pollution to the environment in the processing and using processes, reduces the use cost of farmers, and is a great trend of the technical development of the prior pesticide preparation.
In addition, the existing plant bactericidal drugs in the market have great harm to plants after being used, so that the plants cannot be well produced, and the quality and the yield of crops are influenced. Therefore, it is required to develop a novel bactericide and a preparation method thereof, which can exert a good bactericidal effect on plants, reduce the growth damage to the plants, and have a certain effect of adjusting the resistance of crops to improve the growth quality of the crops.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to develop the triazolone water dispersible granule which is environment-friendly, safe, low in cost and easy to use, aiming at the defects of environmental pollution, harm to human health, phytotoxicity, high use cost and the like in the prior art. Another object of the present invention is to provide a method for preparing the triazolone water dispersible granule.
The technical scheme is as follows: the invention relates to a triazolone water dispersible granule bactericide with crop resistance regulation function, which comprises the following components: triazolone: 20-80 wt%, dispersant: 1-10 wt%, wetting agent: 1-10 wt%, disintegrating agent: 0.5-15 wt%, binder: 0.5-10 wt%, and the balance: and (4) filling.
Further, in order to improve the dispersing effect of the medicament, the dispersing agent is selected from at least two of sodium lignosulfonate, calcium lignosulfonate, alkylphenol polyoxyethylene ether formaldehyde condensate, naphthalene sulfonate formaldehyde condensate, p-methoxy fatty amide benzene sulfonic acid, tristyrene polyoxyethylene ether, fatty alcohol polyoxyethylene ether, polymer carboxylate, methylene dinaphthalene sodium sulfonate, styrene polyoxyethylene ether phosphate and salt thereof, and alkylphenol polyoxyethylene formaldehyde condensate sulfate.
Further, as a preferred embodiment, the dispersant is calcium lignosulfonate, p-methoxy fatty amido benzene sulfonic acid and alkylphenol polyoxyethylene formaldehyde condensate sulfate in a mass ratio of 5-7: 1: 1-2 mixture.
Further, in order to improve the wetting effect of the formula of the invention in use, the preparation method of the wetting agent comprises the following steps:
(11) mixing the components in a mass ratio of 1: mixing 0.5-1.5 parts of sodium dodecyl sulfate and dioctyl sodium sulfosuccinate, heating to 60-65 ℃, and performing high-speed shearing and stirring for 0.5-1 h by using a shearing machine under the condition of 2500-3500 r/min;
(12) adding a mixture of 1: 1-2 of sodium lauryl sulfate and alkyl naphthalene sulfonate, wherein the mass ratio of the sodium lauryl sulfate to the sodium dodecyl sulfate is 1: 0.8 to 1.2; adjusting the temperature to 68-72 ℃, and carrying out high-speed shearing and stirring for 0.5-1 h by using a shearing machine under the condition of 2500-3500 r/min;
(13) and (3) under the condition of heat preservation, carrying out superfine grinding on the material prepared in the step (12) by using a jet mill, sequentially stirring and mixing the material with fumed silica, attapulgite and organobentonite, uniformly mixing, and carrying out superfine grinding by using the jet mill again to obtain the wetting agent.
Further, the disintegrating agent is selected from one or more of ammonium sulfate, sodium sulfate, urea, sodium carbonate, sodium chloride, calcium chloride, starch, potassium carbonate, sodium bicarbonate, potassium bicarbonate or potassium nitrate.
Further, the disintegrant sodium sulfate, starch and ammonium sulfate are mixed according to the mass ratio of 1: 0.5-1.5: 1-2.
Further, in order to ensure that the medicament has good bactericidal effect, reduce the damage to crops and improve the resistance of the crops, the binder is selected from one or more of carboxymethyl cellulose, carboxyethyl cellulose, sodium carboxymethyl starch, polyethylene glycol, polyvinyl alcohol, glucose or lactose.
Further, the filler is selected from one or more of kaolin, diatomite, light calcium carbonate, white carbon black, attapulgite, bentonite or starch.
The invention also provides a preparation method of the triazolone water dispersible granule bactericide, which comprises the following steps:
(21) accurately weighing the triazolone original drug and the disintegrant, and uniformly mixing in a mixer, wherein the temperature is controlled to be 20-30 ℃ in the process;
(22) micronizing the uniformly mixed material by a jet mill to obtain mother powder, wherein the temperature needs to be controlled below 25 ℃ in the process;
(23) mixing the superfine powder with dispersant, wetting agent and filler;
(24) and (2) carrying out ultrafine grinding on the uniformly mixed material by using a jet mill, kneading the uniformly mixed material with water and a binder, then granulating, drying at the temperature of 55-65 ℃ until the water content is less than or equal to 2.5 wt%, screening, and obtaining the triazolone water dispersible granule bactericide after passing inspection.
Has the advantages that: the triazolone water dispersible granule provided by the scheme of the invention is added with various different types of auxiliary agents, independently developed wetting agents, dispersing agents and disintegrating agents with optimal proportion, so that the triazolone water dispersible granule has the advantages of high active component content, small environmental pollution, high disintegration speed, good dispersibility, stable stability over time and heat storage performance and the like, and meanwhile, the activity of plants of crops can be improved, the absorption and utilization rate of effective components of the crops can be improved, and the stress resistance of the crops can be improved. The broad-spectrum bactericidal performance of the crops is excellent, and the safety is outstanding.
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FIG. 1 is a process flow diagram of an embodiment of the present invention.
Detailed Description
The technical solution of the present invention is described in detail by the following examples, but the scope of the present invention is not limited to the examples.
Example 1: accurately weighing 25 wt% of triazolone original drug, 10 wt% of disintegrant and 0.5 wt% of potassium nitrate, and uniformly mixing in a mixer, wherein the temperature is controlled at 20-35 ℃. And (3) carrying out superfine grinding on the uniformly mixed material by using a jet mill to obtain mother powder, wherein the temperature is controlled below 25 ℃ in the process. Mixing the superfine ground mother powder with 6.5 wt% of calcium lignosulfonate, 1 wt% of p-methoxy fatty amido benzenesulfonic acid, 1.5 wt% of alkylphenol polyoxyethylene formaldehyde condensate sulfate, 2.0 wt% of wetting agent, 1.5 wt% of caproic acid diethylaminoacetate and filler kaolin. And (2) carrying out superfine grinding on the uniformly mixed material by using a jet mill, kneading the uniformly mixed material with water and 0.5 wt% of carboxymethyl cellulose serving as a binder, then granulating, drying at the temperature of between 55 and 65 ℃ below zero until the moisture content is less than or equal to 2.5 wt%, screening, and obtaining the required triazolone water dispersible granule after passing inspection. Screening qualified materials for detection, and returning unqualified materials to the pulverizer for remixing and pulverizing; through detection, the content of the active ingredient triazolone is 15.22 wt%, and the water content: 1.0 wt%, pH 9.72, wet sieve test (passing 75 μm sieve) 98% or more, dispersibility: 90%, abrasion resistance: 96%, suspension percentage: 95%, permanent foaming (1 min): 20ml, wetting time: 10 seconds, dust: 1.0 percent, and qualified heat storage stability.
The preparation method of the wetting agent in this example is as follows:
(11) mixing the components in a mass ratio of 1: mixing sodium dodecyl sulfate 1 with dioctyl sodium sulfosuccinate, heating to 60-65 ℃, and performing high-speed shearing and stirring for 0.8h by using a shearing machine under the condition of 3000 r/min;
(12) adding a mixture of 1: 1.5 of sodium lauryl sulfate and alkyl naphthalene sulfonate, wherein the mass ratio of the sodium lauryl sulfate to the sodium dodecyl sulfate is 1: 1; adjusting the temperature to 68-70 ℃, and carrying out high-speed shearing and stirring for 0.5h by using a shearing machine under the condition of 3200 r/min;
(13) and (3) under the condition of heat preservation, carrying out superfine grinding on the material prepared in the step (12) by using a jet mill, sequentially stirring and mixing the material with fumed silica, attapulgite and organobentonite, uniformly mixing, and carrying out superfine grinding by using the jet mill again to obtain the wetting agent.
Example 2: accurately weighing 80 wt% of triazolone original drug, 1 wt% of disintegrant and 0.5 wt% of potassium carbonate, and uniformly mixing in a mixer, wherein the temperature is controlled at 20-30 ℃. And (3) carrying out superfine grinding on the uniformly mixed material by using a jet mill to obtain mother powder, wherein the temperature is controlled below 25 ℃ in the process. Mixing the superfine ground mother powder with 5 wt% of calcium lignosulfonate, 1 wt% of p-methoxy fatty amido benzenesulfonic acid, 1 wt% of alkylphenol polyoxyethylene formaldehyde condensate sulfate, 7.0 wt% of wetting agent, 0.05 wt% of brassinolide and filler kaolin. And (2) carrying out superfine grinding on the uniformly mixed material by using a jet mill, kneading the uniformly mixed material with water and 0.5 wt% of polyvinyl alcohol serving as a binder, then granulating, drying at 55-65 ℃ until the water content is less than or equal to 2.5 wt%, screening, and obtaining the required triazolone water dispersible granule after passing inspection. (screening qualified materials for detection, returning unqualified materials to the crusher for re-mixing and crushing) the content of the active ingredient triazolone is 30.24%, the water content is less than or equal to 3.0%, the pH value is 9.26, the content of the active ingredient triazolone is more than or equal to 98% in a wet screening test (passing through a 75 mu m screen), the dispersity is more than or equal to 80%, the wear resistance is more than or equal to 90%, the suspension rate is more than or equal to 90%, the lasting foamability (1min) is less than or equal to 60ml, the wetting time is less than or equal to 30 seconds, the dust is less than or equal.
The preparation method of the wetting agent in this example is as follows:
(11) mixing the components in a mass ratio of 1: mixing 0.5 of sodium dodecyl sulfate and sodium dioctyl sulfosuccinate, heating to 60-65 ℃, and carrying out high-speed shearing and stirring for 1h by using a shearing machine under the condition of 2500 r/min;
(12) adding a mixture of 1: 2, wherein the mass ratio of the sodium lauryl sulfate to the sodium dodecyl sulfate is 1: 0.8; adjusting the temperature to 70-72 ℃, and carrying out high-speed shearing and stirring for 1h by using a shearing machine under the condition of 2500 r/min;
(13) and (3) under the condition of heat preservation, carrying out superfine grinding on the material prepared in the step (12) by using a jet mill, sequentially stirring and mixing the material with fumed silica, attapulgite and organobentonite, uniformly mixing, and carrying out superfine grinding by using the jet mill again to obtain the wetting agent.
Example 3: accurately weighing 50 wt% of triazolone original drug, 15 wt% of disintegrant and 1.5 wt% of ammonium sulfate, and uniformly mixing in a mixer, wherein the temperature is controlled at 20-30 ℃. And (3) carrying out superfine grinding on the uniformly mixed material by using a jet mill to obtain mother powder, wherein the temperature is controlled below 25 ℃ in the process. Mixing the superfine ground mother powder with 7 wt% of calcium lignosulphonate, 1 wt% of p-methoxy fatty amido benzenesulfonic acid, 2 wt% of alkylphenol polyoxyethylene formaldehyde condensate sulfate, 4.0 wt% of wetting agent, 0.05 wt% of brassinolide and filler attapulgite. And (2) carrying out superfine grinding on the uniformly mixed material by using a jet mill, kneading the uniformly mixed material with water and 0.5 wt% of binder glucose, then granulating, drying at 55-65 ℃ until the moisture content is less than or equal to 2.5 wt%, screening, and obtaining the required triazolone water dispersible granule after passing inspection. (screening qualified materials for detection, returning unqualified materials to the crusher for re-mixing and crushing) detecting that the content of the active ingredient triazolone is 50.37%, the water content is less than or equal to 3.0%, the pH value is 9.46, a wet screening test (passing through a 75 mu m screen) is more than or equal to 98%, the dispersity is more than or equal to 80%, the wear resistance is more than or equal to 90%, the suspension rate is more than or equal to 90%, the lasting foamability (1min) is less than or equal to 60ml, the wetting time is less than or equal to 30 seconds, the dust is less than or equal to 3.0%, and the.
The preparation method of the wetting agent in this example is as follows:
(11) mixing the components in a mass ratio of 1: mixing 1.5 parts of sodium dodecyl sulfate and sodium dioctyl sulfosuccinate, heating to 60-65 ℃, and carrying out high-speed shearing and stirring for 0.5h by using a shearing machine under the condition of 3500 r/min;
(12) adding a mixture of 1: 1.5 of sodium lauryl sulfate and alkyl naphthalene sulfonate, wherein the mass ratio of the sodium lauryl sulfate to the sodium dodecyl sulfate is 1: 1.2; adjusting the temperature to 70-72 ℃, and carrying out high-speed shearing and stirring for 1h by using a shearing machine under the condition of 3500 r/min;
(13) and (3) under the condition of heat preservation, carrying out superfine grinding on the material prepared in the step (12) by using a jet mill, sequentially stirring and mixing the material with fumed silica, attapulgite and organobentonite, uniformly mixing, and carrying out superfine grinding by using the jet mill again to obtain the wetting agent.
As noted above, while the present invention has been shown and described with reference to certain preferred embodiments, it is not to be construed as limited thereto. Various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (9)

1. A triazolone water dispersible granule bactericide with the function of adjusting crop resistance is characterized by comprising the following components: triazolone: 20-80 wt%, dispersant: 1-10 wt%, wetting agent: 1-10 wt%, disintegrating agent: 0.5-15 wt%, binder: 0.5-10 wt%, and the balance: and (4) filling.
2. The triazolone water dispersible granule fungicide with crop resistance regulation according to claim 1, characterized in that: the dispersing agent is selected from at least two of sodium lignosulfonate, calcium lignosulfonate, alkylphenol polyoxyethylene ether formaldehyde condensate, naphthalenesulfonate formaldehyde condensate, p-methoxy fatty amido benzenesulfonic acid, triphenylethylene-polyoxyethylene ether, fatty alcohol-polyoxyethylene ether, polymer carboxylate, sodium methylene dinaphthalene sulfonate, styrene-polyoxyethylene ether phosphate and salt thereof, and alkylphenol polyoxyethylene formaldehyde condensate sulfate.
3. The triazolone water dispersible granule fungicide with crop resistance regulation according to claim 2, characterized in that: the dispersing agent is calcium lignosulfonate, p-methoxy fatty amido benzenesulfonic acid and alkylphenol polyoxyethylene formaldehyde condensate sulfate, and the mass ratio of the dispersing agent to the calcium lignosulfonate to the p-methoxy fatty amido benzenesulfonic acid to the alkylphenol polyoxyethylene formaldehyde condensate sulfate is 5-7: 1: 1-2 mixture.
4. The triazolone water dispersible granule fungicide with crop resistance regulation according to claim 1, characterized in that: the preparation method of the wetting agent comprises the following steps:
(11) mixing the components in a mass ratio of 1: mixing 0.5-1.5 parts of sodium dodecyl sulfate and dioctyl sodium sulfosuccinate, heating to 60-65 ℃, and performing high-speed shearing and stirring for 0.5-1 h by using a shearing machine under the condition of 2500-3500 r/min;
(12) adding a mixture of 1: 1-2 of sodium lauryl sulfate and alkyl naphthalene sulfonate, wherein the mass ratio of the sodium lauryl sulfate to the sodium dodecyl sulfate is 1: 0.8 to 1.2; adjusting the temperature to 68-72 ℃, and carrying out high-speed shearing and stirring for 0.5-1 h by using a shearing machine under the condition of 2500-3500 r/min;
(13) and (3) under the condition of heat preservation, carrying out superfine grinding on the material prepared in the step (12) by using a jet mill, sequentially stirring and mixing the material with fumed silica, attapulgite and organobentonite, uniformly mixing, and carrying out superfine grinding by using the jet mill again to obtain the wetting agent.
5. The triazolone water dispersible granule fungicide with crop resistance regulation according to claim 1, characterized in that: the disintegrating agent is one or more selected from ammonium sulfate, sodium sulfate, urea, sodium carbonate, sodium chloride, calcium chloride, starch, potassium carbonate, sodium bicarbonate, potassium bicarbonate or potassium nitrate.
6. The triazolone water dispersible granule fungicide with crop resistance regulation according to claim 5, characterized in that: the disintegrating agent is prepared from sodium sulfate, starch and ammonium sulfate according to a mass ratio of 1: 0.5-1.5: 1-2.
7. The triazolone water dispersible granule fungicide with crop resistance regulation according to claim 1, characterized in that: the binder is selected from one or more of carboxymethyl cellulose, carboxyethyl cellulose, sodium carboxymethyl starch, polyethylene glycol, polyvinyl alcohol, glucose or lactose.
8. The triazolone water dispersible granule fungicide with crop resistance regulation according to claim 1, characterized in that: the filler is selected from one or more of kaolin, diatomite, light calcium carbonate, white carbon black, attapulgite, bentonite or starch.
9. A preparation method of the triazolone water dispersible granule bactericide as claimed in claim 1, characterized by comprising the following steps:
(21) accurately weighing the triazolone original drug and the disintegrant, and uniformly mixing in a mixer, wherein the temperature is controlled to be 20-30 ℃ in the process;
(22) micronizing the uniformly mixed material by a jet mill to obtain mother powder, wherein the temperature needs to be controlled below 25 ℃ in the process;
(23) mixing the superfine powder with dispersant, wetting agent and filler;
(24) and (2) carrying out ultrafine grinding on the uniformly mixed material by using a jet mill, kneading the uniformly mixed material with water and a binder, then granulating, drying at the temperature of 55-65 ℃ until the water content is less than or equal to 2.5 wt%, screening, and obtaining the triazolone water dispersible granule bactericide after passing inspection.
CN201811273602.9A 2018-10-30 2018-10-30 Triazolone water dispersible granule bactericide with crop resistance adjusting function and preparation method thereof Pending CN111116499A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101044852A (en) * 2006-03-29 2007-10-03 河北省农林科学院植物保护研究所 Compound bactericidal agent for prevention and control of wheat fungi diseases, and its application
CN101632355A (en) * 2009-08-31 2010-01-27 桂林集琦生化有限公司 Pesticide water dispersible granule containing organic silicon surface active agent and preparation method thereof
CN104585166A (en) * 2015-02-09 2015-05-06 四川国光农化股份有限公司 Triazolone water dispersible granules capable of increasing heat storage suspension rate and stability and production method
CN111109267A (en) * 2018-10-30 2020-05-08 江苏剑牌农化股份有限公司 Metconazole water dispersible granule with crop growth regulating effect and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101044852A (en) * 2006-03-29 2007-10-03 河北省农林科学院植物保护研究所 Compound bactericidal agent for prevention and control of wheat fungi diseases, and its application
CN101632355A (en) * 2009-08-31 2010-01-27 桂林集琦生化有限公司 Pesticide water dispersible granule containing organic silicon surface active agent and preparation method thereof
CN104585166A (en) * 2015-02-09 2015-05-06 四川国光农化股份有限公司 Triazolone water dispersible granules capable of increasing heat storage suspension rate and stability and production method
CN111109267A (en) * 2018-10-30 2020-05-08 江苏剑牌农化股份有限公司 Metconazole water dispersible granule with crop growth regulating effect and preparation method thereof

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