CN102057910B - Difenoconazole and propiconazole suspending agent and preparation method thereof - Google Patents
Difenoconazole and propiconazole suspending agent and preparation method thereof Download PDFInfo
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- CN102057910B CN102057910B CN200910198943.9A CN200910198943A CN102057910B CN 102057910 B CN102057910 B CN 102057910B CN 200910198943 A CN200910198943 A CN 200910198943A CN 102057910 B CN102057910 B CN 102057910B
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Abstract
The invention discloses a difenoconazole and propiconazole suspending agent and a preparation method thereof. The difenoconazole and propiconazole suspending agent mainly comprises the following components in percentage by weight: 10 to 20 percent of difenoconazole, 10 to 20 percent of propiconazole, 2 to 6 percent of wetting dispersing agent, 5 to 15 percent of solvent, 2 to 10 percent of emulsifier, 2 to 10 percent of thickening agent, 0 to 10 percent of assistant and the balance of water. The invention also discloses a method for preparing the difenoconazole and propiconazole suspending agent. By compounding two pesticide active ingredients, namely the difenoconazole and the propiconazole into a stable suspending agent taking the water as a medium, the aims of saving resources, improving the preventing and controlling effects and contributing to environmental friendliness are fulfilled.
Description
Technical field
The present invention relates to a kind of biocide preparation of broad spectrum activity, relate in particular to a kind of Difenoconazole propiconazole suspension emulsion and preparation method thereof.
Background
Difenoconazole belongs to interior absorption sterilization, tool protection and therapeutic action.Fungicidal spectrum is wide, and blade face or seed treatment can improve output and the guaranteed quality of crop.To Ascomycetes, Basidiomycetes with partly know disease including Alternaria, Ascochyta, the mould genus of tail spore, Colletotrichum, ball Cuo Pseudomonas, Phoma, Ramularia, Septoria, Venturia, Erysiphaceae, Uredinales and some Seedborne pathogen have lasting protection and therapeutic action.
Propiconazole is a kind of interior absorption triazole bactericidal agent with protection and therapeutic action; can be absorbed by root, stem, leaf portion; and can be soon in plant strain body on conduction; control sac fungi; the disease that basidiomycetes and imperfect fungus cause; particularly to take-all, powdery mildew, rust, root rot, water rice bakanae disease, sigatoka has good control efficiency.
The Difenoconazole single dose that domestic market is sold is take missible oil EC and water dispersible granules WDG as main; The single dose of propiconazole is take missible oil EC as main, and the complex preparation of Difenoconazole and propiconazole is take missible oil EC as main, this quasi-tradition preparation (as missible oil) in a large number with an organic solvent with surfactant, not only wasted valuable resource, simultaneously also severe contamination environment for use.
Summary of the invention
The present invention is the problem existing in order to overcome prior art, and a kind of Difenoconazole propiconazole suspension emulsion providing and preparation method thereof, by a kind of stable suspension emulsion take water as medium that Difenoconazole, two kinds of pesticide activity components of propiconazole are re-dubbed, economize on resources, improve control efficiency and environmental object thereby reach.
To achieve these goals, Difenoconazole propiconazole suspension emulsion, be characterized in, mainly contain the component of following percentage by weight: Difenoconazole 10～20%, propiconazole 10～20%, wetting dispersing agent 2～6%, solvent 5～15%, emulsifier 2～10%, thickener 2～10%, adjuvant 0～10%, water surplus, supplying total weight percent is 100%.
Above-mentioned Difenoconazole propiconazole suspension emulsion, wherein, described wetting dispersing agent is selected naphthalenesulfonic acid-formaldehyde condensate, triphenyl vinyl phenol polyethenoxy ether class and derivative eater, fatty alcohol polyethenoxy ether class, alkylphenol polyoxyethylene class, macromolecule EO-PO block copolymer, lignosulfonates, alkylphenol-polyethenoxy formaldehyde condensation products sulphate, alkylphenol polyoxyethylene formaldehyde condensation products sulphate phosphate, styrene phenol formaldehyde resin polyoxyethylene ether phosphate salt, styryl phenol polyethenoxy polyethenoxy ether, alkyl naphthalene formaldehyde condensate sulfonates, macromolecule is dredged a dress copolymer of type, two kinds or three kinds of above being used in combination in polymerization of carboxylic acid salt.
Above-mentioned Difenoconazole propiconazole suspension emulsion, wherein, described solvent is selected from the one in toluene, dimethylbenzene, aliphatic solvent oil, cyclohexanone, methylated vegetable oil, mineral oil, aromatic solvent naphtha, 1-METHYLPYRROLIDONE, carrene, methyl-sulfoxide, benzinum.
Above-mentioned Difenoconazole propiconazole suspension emulsion, wherein, described emulsifier is selected macromolecule EO-PO block copolymer, Nonyl pheno (NP series), alkylphenol-polyethenoxy polyethers and sulphate thereof or phosphoric acid fat, fatty alcohol-polyoxyethylene ether (AEO series), polyoxyethylene nonylphenol ether phosphate, alkylphenol polyoxyethylene formaldehyde condensation products sulphate phosphate, styrene phenol formaldehyde resin polyoxyethylene ether phosphate salt, styryl phenol polyethenoxy polyethenoxy ether, this dish SPAN series, one or more kinds of being used in combination in soil temperature TWEEN series.
Above-mentioned Difenoconazole propiconazole suspension emulsion, wherein, described thickener is selected from the one or more kinds of combinations in xanthans, cellulose ether and derivative thereof, polyethylene glycol, PVAC polyvinylalcohol, aluminium-magnesium silicate, bentonite, kaolin, diatomite, white carbon, polyvinyl alcohol, gelatin, gum Arabic.
Above-mentioned Difenoconazole propiconazole suspension emulsion, wherein, described adjuvant is selected from one or more the combination in antifreeze, PH conditioning agent, sterilization antiseptic, defoamer; Wherein:
Described antifreeze is selected from the one in ethylene glycol, propane diols, glycerine, PEG400, isopropyl alcohol, urea; It accounts for 0～10% of total weight percent;
Described PH acid-base modifier is selected from the one in glacial acetic acid, hydrochloric acid, citric acid, ammoniacal liquor, monoethanolamine, triethanolamine, NaOH; Institute's expense is that the pH value of final products is adjusted in stability range;
A kind of its that described sterilization antiseptic is selected from formaldehyde, potassium sorbate, Sodium Benzoate, formaldehyde, isothiazolinone accounts for 0.1～0.5% of total weight percent;
Described defoamer is selected from the one in silicon defoamer, polyethers defoamer, higher alcohols, tributyl phosphate, polysiloxane defoamers, and it accounts for 0.5～2% of total weight percent.
Above-mentioned Difenoconazole propiconazole suspension emulsion, wherein, described water is deionized water or distilled water.
The preparation method of Difenoconazole propiconazole suspension emulsion, is characterized in, according to raw material components described above and ratio, comprises the following steps:
Step 1: add wetting dispersing agent, silicone defoaming agent mixing and stirring in deionized water, then after dropping into difenoconazole technical material and being uniformly dispersed, carry out serialization sand milling by horizontal sand mill, sand milling temperature is controlled at below 40 ℃, granularity stops sand milling after reaching claimed range, obtains the suspending agent of Difenoconazole;
Step 2: propiconazole is dissolved in solvent, obtains oil phase after stirring; The difenoconazole suspending agent that emulsifier, step 1 are prepared joins in deionization and stirs evenly and obtain water; The oil phase configuring poured in water and open high speed homogenizing, forming stable suspension emulsion;
Step 3: open and stir in the Difenoconazole propiconazole suspension emulsion preparing, then add antifreeze, thickener, bactericide, stir, make Difenoconazole propiconazole suspension emulsion finished product.
The preparation method of Difenoconazole propiconazole suspension emulsion, is characterized in, according to raw material components described above and ratio, comprises the following steps:
Step 1: add wetting dispersing agent, silicone defoaming agent mixing and stirring in deionized water, then after dropping into difenoconazole technical material and being uniformly dispersed, carry out serialization sand milling by horizontal sand mill, sand milling temperature is controlled at below 40 ℃, granularity stops sand milling after reaching claimed range, obtains the suspending agent of Difenoconazole;
Step 2: propiconazole is dissolved in solvent, obtains oil phase after stirring; Emulsifier is joined in deionization and stirs evenly and obtain water; The oil phase configuring, to entering in water and opening high speed homogenizing, is formed to propiconazole emusion in water, reach after requirement until propiconazole emusion in water granularity, the difenoconazole suspending agent that then adds step 1 to prepare, stirs, and obtains suspension emulsion;
Step 3: open and stir in the Difenoconazole propiconazole suspension emulsion preparing, then add antifreeze, thickener, bactericide, stir, make Difenoconazole propiconazole suspension emulsion finished product.
The preparation method of above-mentioned Difenoconazole propiconazole suspension emulsion, wherein, it is average grain diameter 0.5 μ m～1.5 μ m that the aqueous emulsion granularity described in step 2 reaches requirement.
The preparation method of above-mentioned Difenoconazole propiconazole suspension emulsion, wherein, it is average grain diameter 1 μ m～5 μ m that the suspending agent granularity described in step 1 reaches requirement.
Because the present invention has adopted above technical scheme, the technique effect of its generation is obvious:
1, suspension emulsion of the present invention is combined in two pesticide activity components in same formulation, and biological control effect can be complementary, prevents and treats pedigree thereby expanded; When use, can avoid the problem of the mixed immiscible property of single dose bucket, improve agricultural production efficiency;
2, the present invention, take water as continuous media, to the producer and user's safety, has environmental-protection function to environment; Making water is that continuous media also can effectively reduce excitant and the toxicity to skin and eyes;
3, the present invention does not use or reduces the usage amount of organic solvent (as: toluene, xylene), has avoided inflammable, explosive and poisoning problem in production; Packing, storage and freight are reduced, save production cost.
Embodiment
The present invention is by Difenoconazole and two kinds of active ingredients of propiconazole, add relevant wetting dispersing agent, solvent, emulsifier, thickener, adjuvant, by the formulations of pesticide compounded technology of water baseization, prepare the environment-friendly type preparation Difenoconazole propiconazole suspension emulsion SE take water as medium.Difenoconazole and propiconazole belong to the interior absorption triazole bactericidal agent with protection and treatment, wherein:
Difenoconazole physicochemical property: benzene product are colorless solid, 76 ℃ of fusing points, 220 ℃/4Pa of boiling point, vapour pressure 120nPa (20 ℃).Dissolubility (20 ℃): water 3.3 mg/litre, are soluble in organic solvent.≤ 300 ℃ stable, and in soil, mobility is little, slow degradation.
Propiconazole physicochemical property: former medicine outward appearance is faint yellow sticky silk fabric liquid, 180 ℃ of boiling points (13.3Pa), vapour pressure (20 ℃) 0.133mPa, index of refraction 1.5468, proportion (20 ℃) 1.27g/cm3.In water, solvability is 110mg/L, is soluble in organic solvent.320 ℃ following stable, more stable to light, is hydrolyzed not obvious.More stable in acidity, alkaline medium, not corroding metal.
Difenoconazole propiconazole suspension emulsion of the present invention, mainly contain the component of following percentage by weight: Difenoconazole 10～20%, propiconazole 10～20%, wetting dispersing agent 2～6%, solvent 5～15%, emulsifier 2～10%, thickener 2～10%, adjuvant 0～10%, water surplus, supplying total weight percent is 100%.
The form that is emulsion particle due to suspension emulsion Central Plains pharmaceutically active ingredient is distributed in whole system, can use the former medicine of some dissolution with solvents solids or dilute the former medicine of full-bodied liquid.Can cause suspension emulsion under these solvent actions in, there is the phenomenon that oiling dissolves on the part solia particle surface of solid dispersed phase, and causes and the problem of Ostwald ripening (generate crystallization and crystal is grown up) finally cause the unstable of suspension emulsion.The present invention effectively avoids the appearance of above-mentioned phenomenon by screening suitable wetting dispersing agent.Wetting dispersing agent of the present invention is selected naphthalenesulfonic acid-formaldehyde condensate, triphenyl vinyl phenol polyethenoxy ether class and derivative eater, fatty alcohol polyethenoxy ether class, alkylphenol polyoxyethylene class, macromolecule EO-PO block copolymer, lignosulfonates, alkylphenol-polyethenoxy formaldehyde condensation products sulphate, alkylphenol polyoxyethylene formaldehyde condensation products sulphate phosphate, styrene phenol formaldehyde resin polyoxyethylene ether phosphate salt, styryl phenol polyethenoxy polyethenoxy ether, alkyl naphthalene formaldehyde condensate sulfonates, macromolecule is dredged a dress copolymer of type, two kinds or three kinds of above being used in combination in polymerization of carboxylic acid salt.
Because in suspension emulsion, the former medicine of propiconazole exists in whole suspension system with the form of emulsion particle, under this former medicine normal temperature, is high viscosity liquid shape, so will screen a kind of thinner (solvent), for effectively reducing the viscosity of propiconazole, prepare more stable emulsion system.And this thinner (solvent) should be water insoluble or has micro-solvability in water.The propiconazole emulsion particle making should be stable at the temperature of production and product duration of storage, can not have crystallization.Simultaneously thinner (solvent) has high flash-point, the safety when guaranteeing to prepare.Solvent of the present invention is selected from the one in toluene, dimethylbenzene, aliphatic solvent oil, cyclohexanone, methylated vegetable oil, mineral oil, aromatic solvent naphtha, 1-METHYLPYRROLIDONE, carrene, methyl-sulfoxide, benzinum, can reach stable effect.
Because suspension emulsion is that disperse phase (comprising: solia particle and emulsion particle) stable and uniform is dispersed among the medium take water as continuous phase, because emulsion dispersion belongs to unsettled system on thermodynamics, easily cause coacervation or emulsion attached collection breakdown of emulsion in solid dispersed phase of system.So the emulsifier of the present invention's screening can effectively be avoided this point, obtains stable suspension emulsion.Emulsifier of the present invention is selected macromolecule EO-PO block copolymer, Nonyl pheno (NP series), alkylphenol-polyethenoxy polyethers and sulphate thereof or phosphoric acid fat, fatty alcohol-polyoxyethylene ether (AEO series), polyoxyethylene nonylphenol ether phosphate, alkylphenol polyoxyethylene formaldehyde condensation products sulphate phosphate, styrene phenol formaldehyde resin polyoxyethylene ether phosphate salt, styryl phenol polyethenoxy polyethenoxy ether, this dish SPAN series, one or more kinds of being used in combination in soil temperature TWEEN series.
Thickener of the present invention is selected from the one or more kinds of combinations in xanthans, cellulose ether and derivative thereof, polyethylene glycol, PVAC polyvinylalcohol, aluminium-magnesium silicate, bentonite, kaolin, diatomite, white carbon, polyvinyl alcohol, gelatin, gum Arabic.
Described adjuvant is selected from one or more the combination in antifreeze, PH conditioning agent, sterilization antiseptic, defoamer; Wherein: described antifreeze is selected from the one in ethylene glycol, propane diols, glycerine, PEG400, isopropyl alcohol, urea; It accounts for 0～10% of total weight percent; Described PH acid-base modifier is selected from the one in glacial acetic acid, hydrochloric acid, citric acid, ammoniacal liquor, monoethanolamine, triethanolamine, NaOH; Institute's expense is that the pH value of final products is adjusted in stability range; A kind of its that described sterilization antiseptic is selected from formaldehyde, potassium sorbate, Sodium Benzoate, formaldehyde, isothiazolinone accounts for 0.1～0.5% of total weight percent; Described defoamer is selected from the one in silicon defoamer, polyethers defoamer, higher alcohols, tributyl phosphate, polysiloxane defoamers, and it accounts for 0.5～2% of total weight percent.
Described water is deionized water or distilled water.
The present invention has adopted a kind of low cost, is convenient to preparation method and the process route of the suspension emulsion of suitability for industrialized production.In suspension emulsion of the present invention, the former medicine of Difenoconazole exists in whole suspension system with the form of solia particle, this former medicine belongs to the former medicine of low melting point (76 ℃ of fusing points), the general method of pulverizing has dry pulverization process and wet pulverizing, the broken way of the former medicinal powder of solid adopting in the present invention, select the broken difenoconazole technical material of wet method hypothermia grait abrasive dust, obtain the suspension system of solia particle, be then deployed into suspension emulsion with the emulsion system of propiconazole.
Now further describe the technology of the present invention by following instantiation in order better to illustrate.Described embodiment is only exemplary, not in order to limit the present invention.The technical staff in the technical field of the invention, without departing from the spirit and scope of the present invention, can be used for a variety of modifications and variations.Therefore, protection scope of the present invention is with being as the criterion that claims were defined.
Embodiment mono-:
The first step: by 25g deionized water and Nekal BX 1.0g (the wetting dispersing agent product of BASF AG's Negel), MD-T 3.0g (the dispersant product of Nantong Lian Nong company Pluronic PE 6800), silicone defoaming agent 0.5g mixing and stirring, then after the difenoconazole technical material that drops into 10g is uniformly dispersed, carry out serialization sand milling by horizontal sand mill, sand milling temperature is controlled at below 40 ℃, granularity reaches and stops sand milling after claimed range (actual measurement average grain diameter 1.5 μ m), obtain the suspending agent SC of Difenoconazole.
Second step: the propiconazole of 10g is dissolved in the esterification soybean oil of 5g (commercial material), obtains oil phase after stirring; To in the deionization of the Pluronic PE6800 of 2.0g (emulsifier production of the PO-EO of BASF AG block copolymer), 28.4g, stir evenly (water); The oil phase configuring, to entering water and opening high speed homogenizing, is formed to stable O/W emulsion, and granularity reaches and stops homogenizing after claimed range (actual measurement average grain diameter 0.5 μ m～1.5 μ m) obtains the aqueous emulsion EW of propiconazole.
The 3rd step: add the propiconazole emusion in water EW 45.4g preparing in the difenoconazole suspending agent SC 39.5g preparing, open simultaneously and stir (maintaining 200 turn/min), then add ethylene glycol 5.0g, 10g xanthans (2%) aqueous solution, bactericide KF88 0.1g (isothiazolinone compounds), stir, the average granula 1.43 μ m of final products make 20% Difenoconazole propiconazole suspension emulsion SE.
Embodiment bis-,
The first step: by 24g deionized water and Igepal BC/100 1.0g (the wetting dispersing agent product of Rhodia), dispersant MD 3.0g (Nantong Lian Nong company alkylphenol-polyethenoxy polyethers phosphoric acid lipid product), silicone defoaming agent 1g mixing and stirring, then after the difenoconazole technical material that drops into 15g is uniformly dispersed, carry out serialization sand milling by horizontal sand mill, sand milling temperature is controlled at below 40 ℃, granularity reaches and stops sand milling after claimed range (actual measurement average grain diameter 4.56 μ m), obtain the suspending agent SC of Difenoconazole.
Second step: the propiconazole of 15g is dissolved in the aliphatic solvent oil of 8g (commercial material), obtains oil phase after stirring; The emulsifier LS of 3.0g (Nantong Lian Nong company polyoxyethylene polyethers product), the 43g difenoconazole suspending agent SC for preparing are joined in the deionization of 20.3g and stir evenly (water); The oil phase configuring, to entering water and opening high speed homogenizing, is formed to stable suspension emulsion SE.
The 3rd step: open in the Difenoconazole propiconazole suspension emulsion SE preparing and stir (maintaining 180 turn/min), then add xanthans (2%) aqueous solution, PVAC polyvinylalcohol 0.5g, the bactericide Sodium Benzoate 0.2g of propane diols 2.0g, 7.0g to stir, (average granula 2.39 μ of final products m) to make 30% Difenoconazole propiconazole suspension emulsion SE.
Embodiment tri-,
The first step: by 30g deionized water and Cresplus 1209 1.0g (the nonionic wetting dispersing agent product of standing grain major company), Atlox 4913 3.0g (polycarboxylate salt dispersant's agent product of standing grain major company), silicone defoaming agent 1g mixing and stirring, then after the difenoconazole technical material that drops into 20g is uniformly dispersed, carry out serialization sand milling by horizontal sand mill, sand milling temperature is controlled at below 40 ℃, granularity reaches and stops sand milling after claimed range (actual measurement average grain diameter 3.8 μ m), obtain the suspending agent SC of Difenoconazole.
Second step: the propiconazole of 20g is dissolved in the EXXSOL D80 of 8g (Exxon Mobil Corporation's aliphatic solvent oil), obtains oil phase after stirring; The emulsifier Atlox 4912 of 4.0g (the block high polymer product of standing grain major company), the 54.5g difenoconazole suspending agent SC for preparing are joined in the deionization of 10g and stir evenly (water); The oil phase configuring, to entering water and opening high speed homogenizing, is formed to stable suspension emulsion SE.
The 3rd step: open in the Difenoconazole propiconazole suspension emulsion SE preparing and stir (maintaining 180 turn/min), then add xanthans (2%) aqueous solution, PVAC polyvinylalcohol 1.0g, the bactericide KF88 0.1g of 3.0g to stir, (average granula 3.05 μ of final products m) to make 40% Difenoconazole propiconazole suspension emulsion SE.
The key technical indexes of the present invention is as following table:
| Sequence number | Active ingredient total content | Outward appearance | Average grain diameter, μ m | Dilution stability | Thermodynamic stability | Freeze and melt examination | Suspensibility, % |
| Embodiment mono- | 20％ | White uniform liquid | 1.43 | Qualified | Qualified | Qualified | 93.5 |
| Embodiment bis- | 30％ | White thick liquid | 2.39 | Qualified | Qualified | Qualified | 95.2 |
| Embodiment tri- | 40％ | White thick liquid | 3.05 | Qualified | Qualified | Qualified | 95.6 |
Claims (7)
1. the preparation method of Difenoconazole propiconazole suspension emulsion, is characterized in that, adopts the component substance that mainly contains following percentage by weight:
Described adjuvant is antifreeze, bactericide and silicone defoaming agent;
Comprise the following steps:
Step 1: add wetting dispersing agent, silicone defoaming agent mixing and stirring in deionized water, then after dropping into difenoconazole technical material and being uniformly dispersed, carry out serialization sand milling by horizontal sand mill, sand milling temperature is controlled at below 40 ℃, granularity stops sand milling after reaching claimed range, obtains the suspending agent of Difenoconazole;
Step 2: propiconazole is dissolved in solvent, obtains oil phase after stirring; The difenoconazole suspending agent that emulsifier, step 1 are prepared joins in dried up and stirs evenly and obtain water; The oil phase configuring poured in water and open high speed homogenizing, forming suspension emulsion;
Step 3: the suspension emulsion that whipping step two obtains, then add antifreeze, thickener, bactericide, stir, make Difenoconazole propiconazole suspension emulsion finished product.
2. the preparation method of Difenoconazole propiconazole suspension emulsion according to claim 1, is characterized in that, it is average grain diameter 1 μ m～5 μ m that the suspending agent granularity described in step 1 reaches requirement.
3. the preparation method of Difenoconazole propiconazole suspension emulsion according to claim 1, it is characterized in that, described wetting dispersing agent is selected two kinds or three kinds of above being used in combination in naphthalenesulfonic acid-formaldehyde condensate, fatty alcohol polyethenoxy ether class, alkylphenol polyoxyethylene class, macromolecule EO-PO block copolymer, lignosulfonates, styrene phenol formaldehyde resin polyoxyethylene ether phosphate salt, styryl phenol polyethenoxy polyethenoxy ether, alkyl naphthalene formaldehyde condensate sulfonates, polymerization of carboxylic acid salt.
4. the preparation method of Difenoconazole propiconazole suspension emulsion according to claim 1, it is characterized in that, described solvent is selected from the one in toluene, dimethylbenzene, aliphatic solvent oil, cyclohexanone, methylated vegetable oil, mineral oil, aromatic solvent naphtha, 1-METHYLPYRROLIDONE, carrene, methyl-sulfoxide, benzinum.
5. the preparation method of Difenoconazole propiconazole suspension emulsion according to claim 1, it is characterized in that, described emulsifier is selected one or more kinds of being used in combination in macromolecule EO-PO block copolymer, Nonyl pheno NP series, fatty alcohol-polyoxyethylene ether AEO series, polyoxyethylene nonylphenol ether phosphate, styrene phenol formaldehyde resin polyoxyethylene ether phosphate salt, this dish SPAN series, soil temperature TWEEN series.
6. the preparation method of Difenoconazole propiconazole suspension emulsion according to claim 1, it is characterized in that, described thickener is selected from the one or more kinds of combinations in xanthans, cellulose ether and derivative thereof, polyethylene glycol, aluminium-magnesium silicate, bentonite, kaolin, diatomite, white carbon, polyvinyl alcohol, gelatin, gum Arabic.
7. the Difenoconazole propiconazole suspension emulsion that the method described in employing claim 1-6 any one is produced, is characterized in that, mainly contains the component of following percentage by weight:
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| CN103518736A (en) * | 2013-09-10 | 2014-01-22 | 江苏长青农化股份有限公司 | Difenoconazole and propiconazole suspension concentrate emulsion |
| CN104186482B (en) * | 2014-07-31 | 2015-12-09 | 天津市华宇农药有限公司 | The preparation method of solvent-free Difenoconazole propiconazole suspension emulsion |
| CN104839170A (en) * | 2015-04-15 | 2015-08-19 | 王盼盼 | Sterilization agent for removing crisp pear calyxes and preventing diseases and insect pests caused by fungi |
| CN115581227B (en) * | 2022-09-20 | 2023-09-26 | 河北威远生物化工有限公司 | Preparation method of pesticide suspoemulsion |
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