CN101379971A - Difenoconazole water dispersion granules and preparation technique thereof - Google Patents
Difenoconazole water dispersion granules and preparation technique thereof Download PDFInfo
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- CN101379971A CN101379971A CNA2008102018080A CN200810201808A CN101379971A CN 101379971 A CN101379971 A CN 101379971A CN A2008102018080 A CNA2008102018080 A CN A2008102018080A CN 200810201808 A CN200810201808 A CN 200810201808A CN 101379971 A CN101379971 A CN 101379971A
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Abstract
The invention discloses a difenoconazole water dispersible granule and a preparation technique thereof. The difenoconazole water dispersible granule is prepared by mixing the raw materials including 95% of difenoconazole, colophony graft polymer dispersant or acrylic polymer dispersant, naphthalene sulfonate, alpha-alkene sulfonate, ammonium sulphate, kaoline and white carbon black according to the proportion, and then the raw materials are ground in a dry way, granulated, dried and filtered. The water dispersible granule overcomes the harm of organic solvent in missible oil for the environment and the deficiencies of pulvis, so as to be easy to use, safe for the human beings and environment, and convenient to control the release and for orientation; as the used dispersant is multipolymer dispersant, the synergic action among radicals causes the dispersibility of the difenoconazole water dispersible granule to be superior to that of general micromolecule dispersant and homopolymer dispersant, so that the difenoconazole water dispersible granule prepared by the method has good dispersibility and rapid disintegration, and the suspension percentage in the water can reach 95.6%. In addition, the preparation technique has the advantages of simple operation, environmental protection and low cost, and is suitable for large-scale industrial production.
Description
Technical field
The present invention relates to a kind of pesticide water dispersible granules and preparation technology thereof, specifically, relates to a kind of difenoconazole water dispersible granule and preparation technology thereof.
Background technology
The tradition formulations of pesticide mainly are missible oil and pulvis.Missible oil mainly is that former medicine adds suitable emulsifiers dissolve and forms in organic solvents such as toluene or dimethylbenzene, is sprayed on the soil at a large amount of organic solvent of use, has caused very big influence to ecotope.Because production process is used a large amount of inflammable and explosive organic solvents, there are many potential safety hazards in missible oil in producing storage and transportation, brings harm for the people's lives and property safety.Pulvis is because particle is little, and easily drift in use, brings adverse effect to user and environment on every side.Water dispersible granules is a kind of novel formulation, is to use from natural world or synthetic filler to add suitable auxiliary agent, forms through the special process granulation, and this formulation has overcome the harm that missible oil with an organic solvent brings to environment in a large number, is easy to packing, metering, transportation, storage; Water-soluble because of water dispersible granules, also overcome some shortcomings of pulvis.Water dispersible granules is easy to use, and to the mankind and Environmental security, is easy to sustained release and orientation, so water dispersible granules is a kind of optimal selection that substitutes traditional missible oil and pulvis.
Difenoconazole belongs to triazole bactericidal agent; interior absorption is extremely strong; the main biosynthesis that suppresses the cell ergosterol; thereby destroy membrane structure and function; be mainly used in fruit tree and vegetable, wheat, potato, beans, crop such as melon; the sick poison of many fungies such as vegetables and melon and fruit I had good protection and therapeutic action, free from environmental pollution and agricultural product.Characteristics such as it is few to have consumption, and the lasting period is long, and is safe in utilization, good market prospects.A kind of " a kind of bactericidal composition that contains Difenoconazole and copper fungicide " disclosed among the Chinese patent literature CN101107932, above-mentioned water dispersible granules has overcome the environmental hazard of missible oil and the shortcoming of pulvis, be easy to use,, be easy to sustained release and orientation the mankind and Environmental security.But exist poor stability, cost height, disintegration slowly to reach dispersed weak point such as bad.
Summary of the invention
The purpose of this invention is to provide a kind of disintegration rapidly, good dispersion, suspensibility height, and environmentally safe, safe in utilization and prepare simple difenoconazole water dispersible granule and preparation technology thereof is to overcome the deficiency that above-mentioned prior art exists.
For achieving the above object, the technical solution used in the present invention is as follows:
Difenoconazole water dispersible granule of the present invention, form by following component and proportion of composing:
95% Difenoconazole 10～55%
Dispersant 4～8%
Naphthalene sulfonate 5～10%
Alpha-alkene sulfonate 4～10%
Ammonium sulfate 15～25%
Kaolin 15～50%
White carbon 2～10%
Above proportion of composing is a mass percent, and wherein dispersant is rosin graft copolymer dispersant or acrylics polymeric dispersant.
Described rosin graft copolymer dispersant is formed by radical polymerization by acrylic acid, SSS and rosin derivative, and the number average relative molecular weight of rosin graft copolymer is 12000～14000.
The monomer ratio of described rosin graft copolymer dispersant is as follows:
Acrylic acid 30～60%
SSS 20～50%
Rosin derivative 5～30%
Above proportioning is a mass percent, and three's sum is 100%; Wherein rosin derivative is the synthetic of maleopimaric acid acyl chlorides and hydroxyethyl methacrylate.
Described acrylics polymeric dispersant carries out free-radical polymerized forming by acrylic acid, SSS and hydroxyethyl methacrylate, and the number average relative molecular weight of terpolymer is 2000～40000.
The monomer ratio of described acrylics polymeric dispersant is as follows:
Acrylic acid 30～50%
SSS 20～40%
Hydroxyethyl methacrylate 10～40%
Above proportioning is a mass percent, and three's sum is 100%.
Described naphthalene sulfonate is a sodium naphthalene sulfonate.
The preparation technology of difenoconazole water dispersible granule of the present invention is as follows:
A) by each component raw material of proportioning weighing, stirring makes and mixes;
B) the said mixture material is carried out dry pulverization process;
C) material of collection after dry pulverization process, by extruder grain, dry then, screening gets final product.
Compared with prior art, beneficial effect of the present invention is as follows:
The present invention has overcome the harm that organic solvent brings to environment in the missible oil, has also overcome some shortcomings of pulvis, is easy to use, and to the mankind and Environmental security, is easy to sustained release and orientation; Because of used dispersant is a copolymer dispersant, synergy between group, make its dispersiveness be better than general little dispersal agent molecule and homopolymers dispersant, and physical and chemical stability is good, therefore by the good dispersion of the difenoconazole water dispersible granule of its preparation, disintegration is rapid, and the suspensibility in water can be up to 95.6%.In addition, that preparation technology of the present invention has is simple to operate, environmental protection and advantage with low cost, is fit to industrial scale production.
Embodiment
The present invention is described in further detail and completely below in conjunction with embodiment:
Embodiment 1
1) preparation of rosin graft copolymer dispersant
In there-necked flask, add the maleopimaric acid acyl chlorides of 16.7 mass parts, the hydroxyethyl methacrylate (HEMA) of 5.4 mass parts, the pyridine of 3.2 mass parts, toluene and a small amount of hydroquinones of 70 mass parts, logical N
2Protect, be heated to 100 ℃, insulation reaction 48h; Reaction finishes, and washes 3 times, and pressure reducing and steaming toluene obtains rosin derivative (MPAHEMA) then.
55 parts of deionized waters, 1 part of chain-transferring agent sodium hydrogensulfite, 15 parts of rosin derivatives (MPAHEMA) are joined in the four-hole boiling flask, while stirring heating; When the temperature in the four-hole boiling flask is raised to 70 ℃, add 21.6 parts of acrylic acid, 20 parts of SSSs and 2.1 parts of initiator ammonium persulfates, insulation reaction 3 hours; Naturally cool to room temperature, with sodium hydrate aqueous solution adjust pH to 7～8; The liquid of preparation is put into vacuum drying oven in 70 ℃ of dryings, promptly get the target dispersant.
2) preparation of difenoconazole water dispersible granule
11 part of 95% Difenoconazole, 4 parts of rosin graft copolymer dispersants, 5 parts of sodium naphthalene sulfonates, 10 parts of alpha-alkene sulfonates, 15 parts of ammonium sulfate, 45 parts of kaolin and 10 parts of white carbons are mixed; Dry pulverization process manufactures wetting powder; Wetting powder and 10 ml waters are added in the kneader simultaneously mediate, make plastic material; This material is sent into Squeezinggranulator carry out granulation; Dry, screening obtains water dispersible granules.
The suspensibility of this water dispersible granules in water is 70.3%, and disintegration time is 8 minutes.
Embodiment 2
1) preparation of rosin graft copolymer dispersant
Described in embodiment 1.
2) preparation of difenoconazole water dispersible granule
11 part of 95% Difenoconazole, 6 parts of rosin graft copolymer dispersants, 7 parts of sodium naphthalene sulfonates, 7 parts of alpha-alkene sulfonates, 20 parts of ammonium sulfate, 43 parts of kaolin and 6 parts of white carbons are mixed; Dry pulverization process manufactures wetting powder; Wetting powder and 10 ml waters are added in the kneader simultaneously mediate, make plastic material; This material is sent into Squeezinggranulator carry out granulation; Dry, screening obtains water dispersible granules.
The suspensibility of this water dispersible granules in water is 88.9%, and disintegration time is 2 minutes.
Embodiment 3
1) preparation of rosin graft copolymer dispersant
Described in embodiment 1.
2) preparation of difenoconazole water dispersible granule
11 part of 95% Difenoconazole, 8 parts of rosin graft copolymer dispersants, 10 parts of sodium naphthalene sulfonates, 4 parts of alpha-alkene sulfonates, 25 parts of ammonium sulfate, 40 parts of kaolin and 2 parts of white carbons are mixed; Dry pulverization process manufactures wetting powder; Wetting powder and 10 ml waters are added in the kneader simultaneously mediate, make plastic material; This material is sent into Squeezinggranulator carry out granulation; Dry, screening obtains water dispersible granules.
The suspensibility of this water dispersible granules in water is 95.3%, and disintegration time is 1.8 minutes.
Embodiment 4
1) preparation of rosin graft copolymer dispersant
Described in embodiment 1.
2) preparation of difenoconazole water dispersible granule
22 part of 95% Difenoconazole, 4 parts of rosin graft copolymer dispersants, 8 parts of sodium naphthalene sulfonates, 7 parts of alpha-alkene sulfonates, 25 parts of ammonium sulfate, 30 parts of kaolin and 4 parts of white carbons are mixed; Dry pulverization process manufactures wetting powder; Wetting powder and 10 ml waters are added in the kneader simultaneously mediate, make plastic material; This material is sent into Squeezinggranulator carry out granulation; Dry, screening obtains water dispersible granules.
The suspensibility of this water dispersible granules in water is 79.2%, and disintegration time is 4 minutes.
Embodiment 5
1) preparation of rosin graft copolymer dispersant
Described in embodiment 1.
2) preparation of difenoconazole water dispersible granule
22 part of 95% Difenoconazole, 8 parts of rosin graft copolymer dispersants, 5 parts of sodium naphthalene sulfonates, 4 parts of alpha-alkene sulfonates, 20 parts of ammonium sulfate, 31 parts of kaolin and 10 parts of white carbons are mixed; Dry pulverization process manufactures wetting powder; Wetting powder and 10 ml waters are added in the kneader simultaneously mediate, make plastic material; This material is sent into Squeezinggranulator carry out granulation; Dry, screening obtains water dispersible granules.
The suspensibility of this water dispersible granules in water is 80.7%, and disintegration time is 2.5 minutes.
Embodiment 6
1) preparation of rosin graft copolymer dispersant
Described in embodiment 1.
2) preparation of difenoconazole water dispersible granule
22 part of 95% Difenoconazole, 6 parts of rosin graft copolymer dispersants, 10 parts of sodium naphthalene sulfonates, 10 parts of alpha-alkene sulfonates, 15 parts of ammonium sulfate, 35 parts of kaolin and 2 parts of white carbons are mixed; Dry pulverization process manufactures wetting powder; Wetting powder and 10 ml waters are added in the kneader simultaneously mediate, make plastic material; This material is sent into Squeezinggranulator carry out granulation; Dry, screening obtains water dispersible granules.
The suspensibility of this water dispersible granules in water is 85.0%, and disintegration time is 2 minutes.
Embodiment 7
1) preparation of rosin graft copolymer dispersant
Described in embodiment 1.
2) preparation of difenoconazole water dispersible granule
32 part of 95% Difenoconazole, 8 parts of rosin graft copolymer dispersants, 10 parts of sodium naphthalene sulfonates, 10 parts of alpha-alkene sulfonates, 15 parts of ammonium sulfate, 15 parts of kaolin and 10 parts of white carbons are mixed; Dry pulverization process manufactures wetting powder; Wetting powder and 10 ml waters are added in the kneader simultaneously mediate, make plastic material; This material is sent into Squeezinggranulator carry out granulation; Dry, screening obtains water dispersible granules.
The suspensibility of this water dispersible granules in water is 85.6%, and disintegration time is 3.5 minutes.
Embodiment 8
1) preparation of rosin graft copolymer dispersant
Described in embodiment 1.
2) preparation of difenoconazole water dispersible granule
44 part of 95% Difenoconazole, 6 parts of rosin graft copolymer dispersants, 7 parts of sodium naphthalene sulfonates, 7 parts of alpha-alkene sulfonates, 15 parts of ammonium sulfate, 15 parts of kaolin and 6 parts of white carbons are mixed; Dry pulverization process manufactures wetting powder; Wetting powder and 10 ml waters are added in the kneader simultaneously mediate, make plastic material; This material is sent into Squeezinggranulator carry out granulation; Dry, screening obtains water dispersible granules.
The suspensibility of this water dispersible granules in water is 82.9%, and disintegration time is 4 minutes.
Embodiment 9
1) preparation of rosin graft copolymer dispersant
Described in embodiment 1.
2) preparation of difenoconazole water dispersible granule
55 part of 95% Difenoconazole, 4 parts of rosin graft copolymer dispersants, 5 parts of sodium naphthalene sulfonates, 4 parts of alpha-alkene sulfonates, 15 parts of ammonium sulfate, 15 parts of kaolin and 2 parts of white carbons are mixed; Dry pulverization process manufactures wetting powder; Wetting powder and 10 ml waters are added in the kneader simultaneously mediate, make plastic material; This material is sent into Squeezinggranulator carry out granulation; Dry, screening obtains water dispersible granules.
The suspensibility of this water dispersible granules in water is 63.4%, and disintegration time is 3 minutes.
Embodiment 10
1) preparation of acrylics polymeric dispersant
1000 parts of deionized waters, 4 parts of chain-transferring agent sodium hydrogensulfites, 100 parts of SSSs are joined in the four-hole boiling flask, while stirring heating; When the temperature in the four-hole boiling flask is raised to 70 ℃, add 105 parts of acrylic acid, 95 parts of hydroxyethyl methacrylates and 13 parts of initiator ammonium persulfates, insulation reaction 2.5 hours; Naturally cool to room temperature, with sodium hydrate aqueous solution adjust pH to 7～8; The liquid of preparation is put into vacuum drying oven in 70 ℃ of dryings, promptly get the target dispersant.
2) preparation of difenoconazole water dispersible granule
20 part of 95% Difenoconazole, 4 parts of acrylics polymeric dispersants, 5 parts of sodium naphthalene sulfonates, 4 parts of alpha-alkene sulfonates, 15 parts of ammonium sulfate, 50 parts of kaolin and 2 parts of white carbons are mixed; Dry pulverization process manufactures wetting powder; Wetting powder and 10 ml waters are added in the kneader simultaneously mediate, make plastic material; This material is sent into Squeezinggranulator carry out granulation; Dry, screening obtains water dispersible granules.
The suspensibility of this water dispersible granules in water is 75.3%, and disintegration time is 8 minutes.
Embodiment 11
1) preparation of acrylics polymeric dispersant
Described in embodiment 10.
2) preparation of difenoconazole water dispersible granule
20 part of 95% Difenoconazole, 6 parts of acrylics polymeric dispersants, 8 parts of sodium naphthalene sulfonates, 7 parts of alpha-alkene sulfonates, 25 parts of ammonium sulfate, 28 parts of kaolin and 6 parts of white carbons are mixed; Dry pulverization process manufactures wetting powder; Wetting powder and 10 ml waters are added in the kneader simultaneously mediate, make plastic material; This material is sent into Squeezinggranulator carry out granulation; Dry, screening obtains water dispersible granules.
The suspensibility of this water dispersible granules in water is 88.2%, and disintegration time is 5 minutes.
Embodiment 12
1) preparation of acrylics polymeric dispersant
Described in embodiment 10.
2) preparation of difenoconazole water dispersible granule
20 part of 95% Difenoconazole, 8 parts of acrylics polymeric dispersants, 10 parts of sodium naphthalene sulfonates, 10 parts of alpha-alkene sulfonates, 20 parts of ammonium sulfate, 22 parts of kaolin and 10 parts of white carbons are mixed; Dry pulverization process manufactures wetting powder; Wetting powder and 10 ml waters are added in the kneader simultaneously mediate, make plastic material; This material is sent into Squeezinggranulator carry out granulation; Dry, screening obtains water dispersible granules.
The suspensibility of this water dispersible granules in water is 85.2%, and disintegration time is 1.8 minutes.
Embodiment 13
1) preparation of acrylics polymeric dispersant
Described in embodiment 10.
2) preparation of difenoconazole water dispersible granule
10 part of 95% Difenoconazole, 6 parts of acrylics polymeric dispersants, 8 parts of sodium naphthalene sulfonates, 7 parts of alpha-alkene sulfonates, 20 parts of ammonium sulfate, 43 parts of kaolin and 6 parts of white carbons are mixed; Dry pulverization process manufactures wetting powder; Wetting powder and 10 ml waters are added in the kneader simultaneously mediate, make plastic material; This material is sent into Squeezinggranulator carry out granulation; Dry, screening obtains water dispersible granules.
The suspensibility of this water dispersible granules in water is 88.2%, and disintegration time is 1.8 minutes.
Embodiment 14
1) preparation of acrylics polymeric dispersant
Described in embodiment 10.
2) preparation of difenoconazole water dispersible granule
35 part of 95% Difenoconazole, 6 parts of acrylics polymeric dispersants, 8 parts of sodium naphthalene sulfonates, 7 parts of alpha-alkene sulfonates, 15 parts of ammonium sulfate, 25 parts of kaolin and 4 parts of white carbons are mixed; Dry pulverization process manufactures wetting powder; Wetting powder and 10 ml waters are added in the kneader simultaneously mediate, make plastic material; This material is sent into Squeezinggranulator carry out granulation; Dry, screening obtains water dispersible granules.
The suspensibility of this water dispersible granules in water is 95.6%, and disintegration time is 2.5 minutes.
Embodiment 15
1) preparation of acrylics polymeric dispersant
Described in embodiment 10.
2) preparation of difenoconazole water dispersible granule
55 part of 95% Difenoconazole, 4 parts of acrylics polymeric dispersants, 5 parts of sodium naphthalene sulfonates, 4 parts of alpha-alkene sulfonates, 15 parts of ammonium sulfate, 15 parts of kaolin and 2 parts of white carbons are mixed; Dry pulverization process manufactures wetting powder; Wetting powder and 10 ml waters are added in the kneader simultaneously mediate, make plastic material; This material is sent into Squeezinggranulator carry out granulation; Dry, screening obtains water dispersible granules.
The suspensibility of this water dispersible granules in water is 68.1%, and disintegration time is 7 minutes.
Claims (7)
1. a difenoconazole water dispersible granule is characterized in that, is made up of following component and proportion of composing:
95% Difenoconazole 10～55%
Dispersant 4～8%
Naphthalene sulfonate 5～10%
Alpha-alkene sulfonate 4～10%
Ammonium sulfate 15～25%
Kaolin 15～50%
White carbon 2～10%
Above proportion of composing is a mass percent, and wherein dispersant is rosin graft copolymer dispersant or acrylics polymeric dispersant.
2. difenoconazole water dispersible granule according to claim 1, it is characterized in that, described rosin graft copolymer dispersant is formed by radical polymerization by acrylic acid, SSS and rosin derivative, and the number average relative molecular weight of rosin graft copolymer is 12000～14000.
3. difenoconazole water dispersible granule according to claim 2 is characterized in that, the monomer ratio of described rosin graft copolymer dispersant is as follows:
Acrylic acid 30～60%
SSS 20～50%
Rosin derivative 5～30%
Above proportioning is a mass percent, and three's sum is 100%; Wherein rosin derivative is the synthetic of maleopimaric acid acyl chlorides and hydroxyethyl methacrylate.
4. difenoconazole water dispersible granule according to claim 1, it is characterized in that, described acrylics polymeric dispersant carries out free-radical polymerized forming by acrylic acid, SSS and hydroxyethyl methacrylate, and the number average relative molecular weight of terpolymer is 2000～40000.
5. difenoconazole water dispersible granule according to claim 4 is characterized in that, the monomer ratio of described acrylics polymeric dispersant is as follows:
Acrylic acid 30～50%
SSS 20～40%
Hydroxyethyl methacrylate 10～40%
Above proportioning is a mass percent, and three's sum is 100%.
6. difenoconazole water dispersible granule according to claim 1 is characterized in that, described naphthalene sulfonate is a sodium naphthalene sulfonate.
7. the preparation technology of the described difenoconazole water dispersible granule of claim 1 is characterized in that, concrete steps are as follows:
A) by each component raw material of proportioning weighing, stirring makes and mixes;
B) the said mixture material is carried out dry pulverization process;
C) material of collection after dry pulverization process, by extruder grain, dry then, screening gets final product.
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| CNA2008102018080A CN101379971A (en) | 2008-10-27 | 2008-10-27 | Difenoconazole water dispersion granules and preparation technique thereof |
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| CNA2008102018080A CN101379971A (en) | 2008-10-27 | 2008-10-27 | Difenoconazole water dispersion granules and preparation technique thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102132699A (en) * | 2010-01-21 | 2011-07-27 | 中化化工科学技术研究总院 | Paclobutrazol water dispersible granules/tablets and preparation method thereof |
| CN101632361B (en) * | 2009-08-18 | 2012-07-04 | 江苏丰登农药有限公司 | Difenoconazole emulsible powder |
| CN105594743A (en) * | 2014-11-17 | 2016-05-25 | 武汉凌科达科技有限公司 | Pesticide composition preparation method |
| CN105637835A (en) * | 2013-10-25 | 2016-06-01 | 统一有限责任两合公司 | Clusters of polynomials for data points |
| CN105638726A (en) * | 2014-11-17 | 2016-06-08 | 武汉凌科达科技有限公司 | A pesticide composition |
| CN106305730A (en) * | 2016-08-20 | 2017-01-11 | 广东中迅农科股份有限公司 | Difenoconazole containing water dispersible granule and preparation method thereof |
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2008
- 2008-10-27 CN CNA2008102018080A patent/CN101379971A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101632361B (en) * | 2009-08-18 | 2012-07-04 | 江苏丰登农药有限公司 | Difenoconazole emulsible powder |
| CN102132699A (en) * | 2010-01-21 | 2011-07-27 | 中化化工科学技术研究总院 | Paclobutrazol water dispersible granules/tablets and preparation method thereof |
| CN102132699B (en) * | 2010-01-21 | 2013-09-04 | 中化化工科学技术研究总院 | Paclobutrazol water dispersible granules/tablets and preparation method thereof |
| CN105637835A (en) * | 2013-10-25 | 2016-06-01 | 统一有限责任两合公司 | Clusters of polynomials for data points |
| CN105637835B (en) * | 2013-10-25 | 2020-03-20 | 统一有限责任两合公司 | Method and communication terminal for telecommunication |
| US10681090B2 (en) | 2013-10-25 | 2020-06-09 | Unify Gmbh & Co. Kg | Method for telecommunication and communication terminal |
| CN105594743A (en) * | 2014-11-17 | 2016-05-25 | 武汉凌科达科技有限公司 | Pesticide composition preparation method |
| CN105638726A (en) * | 2014-11-17 | 2016-06-08 | 武汉凌科达科技有限公司 | A pesticide composition |
| CN106305730A (en) * | 2016-08-20 | 2017-01-11 | 广东中迅农科股份有限公司 | Difenoconazole containing water dispersible granule and preparation method thereof |
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