CN115152749A - Aqueous suspension and preparation method thereof - Google Patents
Aqueous suspension and preparation method thereof Download PDFInfo
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- CN115152749A CN115152749A CN202210620911.9A CN202210620911A CN115152749A CN 115152749 A CN115152749 A CN 115152749A CN 202210620911 A CN202210620911 A CN 202210620911A CN 115152749 A CN115152749 A CN 115152749A
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- aqueous suspension
- solution
- heating
- synergist
- agent
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- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000007900 aqueous suspension Substances 0.000 title claims description 41
- 239000000375 suspending agent Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 33
- 238000003756 stirring Methods 0.000 claims description 32
- 239000000243 solution Substances 0.000 claims description 23
- 239000002270 dispersing agent Substances 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 21
- 239000000080 wetting agent Substances 0.000 claims description 21
- 239000002562 thickening agent Substances 0.000 claims description 20
- 230000001804 emulsifying effect Effects 0.000 claims description 19
- 239000013543 active substance Substances 0.000 claims description 18
- 239000000839 emulsion Substances 0.000 claims description 18
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 16
- 239000003755 preservative agent Substances 0.000 claims description 12
- 230000002335 preservative effect Effects 0.000 claims description 12
- 238000010008 shearing Methods 0.000 claims description 12
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 9
- 239000005760 Difenoconazole Substances 0.000 claims description 8
- 239000005857 Trifloxystrobin Substances 0.000 claims description 8
- -1 acetylene glycol Chemical compound 0.000 claims description 8
- BQYJATMQXGBDHF-UHFFFAOYSA-N difenoconazole Chemical compound O1C(C)COC1(C=1C(=CC(OC=2C=CC(Cl)=CC=2)=CC=1)Cl)CN1N=CN=C1 BQYJATMQXGBDHF-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- ONCZDRURRATYFI-TVJDWZFNSA-N trifloxystrobin Chemical compound CO\N=C(\C(=O)OC)C1=CC=CC=C1CO\N=C(/C)C1=CC=CC(C(F)(F)F)=C1 ONCZDRURRATYFI-TVJDWZFNSA-N 0.000 claims description 8
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- 229910019142 PO4 Inorganic materials 0.000 claims description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 6
- 229920001400 block copolymer Polymers 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 6
- 239000010452 phosphate Substances 0.000 claims description 6
- 230000002528 anti-freeze Effects 0.000 claims description 5
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 4
- 229920000570 polyether Polymers 0.000 claims description 4
- 108010010803 Gelatin Proteins 0.000 claims description 3
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 3
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 3
- 239000008273 gelatin Substances 0.000 claims description 3
- 229920000159 gelatin Polymers 0.000 claims description 3
- 235000019322 gelatine Nutrition 0.000 claims description 3
- 235000011852 gelatine desserts Nutrition 0.000 claims description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
- 229920005646 polycarboxylate Polymers 0.000 claims description 3
- 239000000230 xanthan gum Substances 0.000 claims description 3
- 235000010493 xanthan gum Nutrition 0.000 claims description 3
- 229920001285 xanthan gum Polymers 0.000 claims description 3
- 229940082509 xanthan gum Drugs 0.000 claims description 3
- FBKRJCSYOMDOKB-UHFFFAOYSA-N 2,3,4-triphenylphenol Chemical compound C=1C=CC=CC=1C1=C(C=2C=CC=CC=2)C(O)=CC=C1C1=CC=CC=C1 FBKRJCSYOMDOKB-UHFFFAOYSA-N 0.000 claims description 2
- FJKROLUGYXJWQN-UHFFFAOYSA-M 4-hydroxybenzoate Chemical compound OC1=CC=C(C([O-])=O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-M 0.000 claims description 2
- 239000005711 Benzoic acid Substances 0.000 claims description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 235000010489 acacia gum Nutrition 0.000 claims description 2
- 239000001785 acacia senegal l. willd gum Substances 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 235000010233 benzoic acid Nutrition 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- BEFDCLMNVWHSGT-UHFFFAOYSA-N ethenylcyclopentane Chemical compound C=CC1CCCC1 BEFDCLMNVWHSGT-UHFFFAOYSA-N 0.000 claims description 2
- 150000002191 fatty alcohols Chemical class 0.000 claims description 2
- UZRCGISJYYLJMA-UHFFFAOYSA-N phenol;styrene Chemical compound OC1=CC=CC=C1.C=CC1=CC=CC=C1 UZRCGISJYYLJMA-UHFFFAOYSA-N 0.000 claims description 2
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 235000010199 sorbic acid Nutrition 0.000 claims description 2
- 239000004334 sorbic acid Substances 0.000 claims description 2
- 229940075582 sorbic acid Drugs 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 239000000575 pesticide Substances 0.000 abstract description 7
- 230000000052 comparative effect Effects 0.000 description 18
- 239000003814 drug Substances 0.000 description 17
- 239000002245 particle Substances 0.000 description 16
- 229940079593 drug Drugs 0.000 description 12
- 238000005338 heat storage Methods 0.000 description 12
- 238000005303 weighing Methods 0.000 description 11
- 238000012360 testing method Methods 0.000 description 10
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 238000001914 filtration Methods 0.000 description 7
- 238000009472 formulation Methods 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 238000003860 storage Methods 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000005457 optimization Methods 0.000 description 4
- 235000013339 cereals Nutrition 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000002518 antifoaming agent Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- BOLQUPOXTWHXIX-UHFFFAOYSA-N OC1=CC=CC=C1.C=1C=CC=CC=1C=C(C=1C=CC=CC=1)C1=CC=CC=C1 Chemical compound OC1=CC=CC=C1.C=1C=CC=CC=1C=C(C=1C=CC=CC=1)C1=CC=CC=C1 BOLQUPOXTWHXIX-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 150000002009 diols Chemical class 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/44—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids
- A01N37/50—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids the nitrogen atom being doubly bound to the carbon skeleton
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
- A01N43/647—Triazoles; Hydrogenated triazoles
- A01N43/653—1,2,4-Triazoles; Hydrogenated 1,2,4-triazoles
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P3/00—Fungicides
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Plant Pathology (AREA)
- Environmental Sciences (AREA)
- Zoology (AREA)
- Engineering & Computer Science (AREA)
- Pest Control & Pesticides (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Dentistry (AREA)
- Agronomy & Crop Science (AREA)
- Chemical & Material Sciences (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Mycology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Toxicology (AREA)
- Microbiology (AREA)
Abstract
The invention relates to the technical field of pesticide preparations, in particular to an aqueous suspending agent and a preparation method thereof.
Description
Technical Field
The invention relates to the technical field of pesticide preparations, in particular to an aqueous suspending agent and a preparation method thereof.
Background
The aqueous suspending agent or suspending agent refers to a preparation which can uniformly disperse solid raw medicines which are insoluble or slightly soluble in water under the action of a surfactant. The suspending agent mainly comprises pesticide raw materials, a wetting agent, a dispersing agent, a thickening agent, an antifreezing agent, a defoaming agent, water and the like.
The traditional pesticide suspending agent processing technology mainly adopts multiple mixing and multi-stage sand grinding, and relates to equipment such as a homogenizing mixer and a horizontal sand mill. The processing process is generally that the raw medicine, water, wetting agent, dispersing agent, defoaming agent and the like are mixed uniformly in a homogenizing mixer and are ground in multiple stages until the grain diameter is less than 5 mu m; adding thickener, antifreeze, antiseptic, etc., homogenizing, mixing, and filtering to obtain the final product. Sanding machines are the key equipment for suspending agent processing, and sanding typically includes primary sanding, secondary sanding, and fine grinding. However, the product obtained by the process has larger grain size and uneven grain size distribution, which leads to poor heat storage stability of the product, especially when different kinds of ingredients are compounded. Although different components are compounded, the control effect can be improved, the sterilization range is enlarged, the dosage of the effective components is reduced, the medication cost is saved, and the environmental pollution is reduced, so that the composition is an important means for comprehensively controlling rice diseases. However, when a low-melting-point raw drug such as difenoconazole and trifloxystrobin is compounded, the melting point of the mixed components is reduced, the viscosity of the raw drug is increased, creaming or equipment blockage due to shear softening is easier to occur in the preparation process of the suspending agent compared with a single low-melting-point raw drug, the loss amount of the drug is large in the process of preparing the aqueous suspending agent by adopting the prior art, creaming is easy to occur in the hot storage period or a large amount of water is separated out, and the hot storage stability is poor.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defects of large medicament loss and poor heat storage stability of the aqueous suspension prepared by the prior art, thereby providing the aqueous suspension and the preparation method thereof.
Therefore, the invention provides a preparation method of the aqueous suspending agent, which comprises the following steps:
s1, a step: dissolving a wetting agent and an emulsifying dispersant by water to obtain a solution;
and S2, a step: mixing the solution with active substances, and heating to obtain emulsion;
and S3, a step: and shearing and stirring the emulsion while heating, then cooling, and mixing the mixed solution with a thickening agent to prepare the aqueous suspension.
Further, in the step S2, heating is performed under stirring, preferably, at a rotation speed of 200 to 1000rpm and a temperature of 70 to 80 ℃.
Wherein the heating time may be 10min or more (e.g., 15-30 min).
Further, in the step S3, the speed of shearing and stirring is 4000-8000rpm, the heating temperature is 70-80 ℃, and the time is at least 20min (for example, 15-50 min).
Further, in the step S3, the mixed solution is cooled to below 30 ℃ and then is mixed with the thickening agent at the rotating speed of 200-1000 rpm.
Further, the wetting agent is at least one selected from acetylene glycol polyoxyethylene ether, fatty alcohol polyoxyethylene ether and styrene phenol polyoxyethylene ether, and is preferably acetylene glycol polyoxyethylene ether.
Further, the emulsifying dispersant is at least one selected from polyoxyethylene polyoxypropylene ether block copolymer, polyoxyethylene polyoxypropylene ether block copolymer phosphate, triphenyl phenol polyoxyethylene ether phosphate, alkyl polyoxyethylene polyoxybutylene block copolymer phosphate and polycarboxylate; and/or, the thickening agent is selected from at least one of xanthan gum, arabic gum, gelatin and polyvinyl alcohol.
Further, the water suspending agent comprises 10-60% of pharmaceutical active substances, 1-5.5% of wetting agents, 1-20% of emulsifying and dispersing agents, 0.05-0.5% of thickening agents and 30-60% of water by taking the total mass of the water suspending agent as 100%.
Further, the pharmaceutical active substance is selected from at least one of difenoconazole and trifloxystrobin; preferably, the pharmaceutically active substance comprises difenoconazole and trifloxystrobin in a mass ratio of 5:1-1:5.
Further, the aqueous suspension also comprises 0-10% of synergist (such as 5-10% of synergist), 2-6% of antifreezing solution and/or 0.1-2% of preservative, wherein the total mass of the aqueous suspension is 100%.
Further, in the step S3, when the mixed solution is mixed with the thickener, an antifreeze and/or a synergist and/or a preservative are also mixed; and/or, the solution in the step S1 also contains a synergist.
Further, the antifreezing solution is at least one of urea, propylene glycol and glycerol; and/or, the preservative is selected from at least one of benzoic acid, sorbic acid, cason and p-hydroxybenzoate; and/or the synergist is selected from at least one of isomeric alcohol ether and organosilicon polyether.
Wherein the isomeric alcohol ether can adopt isomeric alcohol ether with the carbon atom number of 10-13.
The technical scheme of the invention has the following advantages:
1. according to the aqueous suspending agent provided by the invention, the wetting agent and the emulsifying dispersant are dissolved by adopting water, the obtained solution is mixed with the medicinal active substance and then heated to prepare the emulsion, then the emulsion is sheared and stirred, and is mixed with the thickening agent after being cooled, so that the medicament loss of the prepared aqueous suspending agent is greatly improved, the particle size of the aqueous suspending agent is small and uniformly distributed, the thermal storage stability is obviously improved, sanding is not needed, the particle size change before and after thermal storage is small, and the phenomena of creaming and a large amount of water precipitation can not occur.
2. The aqueous suspension agent provided by the invention can further improve the particle size uniformity of the aqueous suspension agent by limiting the formation condition of emulsion, namely heating under the conditions that the rotating speed is 200-1000rpm and the temperature is 70-80 ℃ or limiting the speed of shearing and stirring to be 4000-8000rpm for at least 20min, so that the thermal storage stability is further improved.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
Acetylenic diol polyoxyethylene ethers are available from the company Ikeka chemical company and may be used in the WA series, for example WA420 to WA485; the isomeric alcohol ethers are provided by the optimization chemical company and have the trade mark SP103 and the like. Polyoxyethylene polyoxypropylene block polyethers and their phosphate esters are available from the optimization chemical company as model numbers 703D, 703DP, 1050P, 1601 and 1602, etc. Polycarboxylates are provided by optimization chemical company, and may be 401, 404, 408, etc. Xanthan gum is available from Wuhanwangrong technologies, inc. The cason is purchased from Shandong Wantai chemical Co., ltd. Silicone polyether was purchased from mezzo, model SAG672. Triphenylethylene phenol polyoxyethylene ether, 601-604 series, provided by the chemical company of optimization; gelatin is purchased from bioscience, inc., yinghe, anhui; the purity of the trifloxystrobin and the difenoconazole are both 97 percent.
Example 1
This example provides an aqueous suspension concentrate having a total weight of 1 ton and consisting of:
the preparation method comprises the following steps:
(1) Weighing a wetting agent, an emulsifying dispersant and a synergist according to a prescription, adding the wetting agent, the emulsifying dispersant and the synergist into 250kg of deionized water, and stirring and dissolving at 800rpm to obtain a solution;
(2) Weighing the medicinal active substances according to the prescription, adding into the solution in the step (1), heating at 75 deg.C for 30min under stirring at 800rpm to obtain emulsion;
(3) Shearing and stirring the emulsion at 75 ℃ and 6000rpm for 35min, and testing the particle size of the emulsion by using a laser particle size distribution instrument, wherein the average particle size is less than or equal to 5 mu m; stopping heating, continuing to reduce the temperature under the condition of shearing and stirring at 6000rpm, reducing the stirring speed to 500r/min when the temperature of the mixed solution reaches 30 ℃, adding an antifreezing solution, a thickening agent and a preservative, adding deionized water until the total weight is 1 ton, uniformly stirring at 500rpm, and filtering to obtain the aqueous suspension.
Example 2
This example provides an aqueous suspension formulation having a total weight of 1 ton, and the formulation is as follows:
the preparation method comprises the following steps:
(1) Weighing a wetting agent, an emulsifying dispersant and a synergist according to a formula, adding the wetting agent, the emulsifying dispersant and the synergist into 250kg of deionized water, and stirring and dissolving at 800rpm to obtain a solution;
(2) Weighing the medicinal active substances according to the prescription, adding the medicinal active substances into the solution obtained in the step (1), and heating at 800rpm for 25min at 75 ℃ to obtain emulsion;
(3) Shearing and stirring the emulsion at the temperature of 80 ℃ and the rotating speed of 4000rpm for 45min, and testing the particle size of the emulsion by using a laser particle size distribution instrument, wherein the average particle size is less than or equal to 5 mu m; stopping heating, continuing to reduce the temperature under the condition of shearing and stirring at 6000rpm, reducing the stirring speed to 500r/min when the temperature of the mixed solution reaches 20 ℃, adding an antifreezing solution, a thickening agent and a preservative, adding deionized water until the total weight is 1 ton, uniformly stirring at 500rpm, and filtering to obtain the aqueous suspension.
Example 3
This example provides an aqueous suspension formulation having a total weight of 1 ton, and the formulation is as follows:
the preparation method comprises the following steps:
(1) Weighing a wetting agent, an emulsifying dispersant and a synergist according to a formula, adding the wetting agent, the emulsifying dispersant and the synergist into 250kg of deionized water, and stirring and dissolving at 500rpm to obtain a solution;
(2) Weighing the medicinal active substances according to the prescription, adding into the solution in the step (1), heating at 800rpm for 20min at 78 deg.C to obtain emulsion;
(3) Shearing and stirring the emulsion for 20min at the temperature of 80 ℃ and the rotating speed of 5000rpm, and testing the particle size of the emulsion by using a laser particle size distribution instrument, wherein the average particle size is less than or equal to 5 mu m; stopping heating, continuing to reduce the temperature under the condition of shearing and stirring at 5000rpm, reducing the stirring speed to 300r/min when the temperature of the mixed solution reaches 30 ℃, adding an antifreezing solution, a thickening agent and a preservative, adding water until the total weight is 1 ton, uniformly stirring at 300rpm, and filtering to obtain the aqueous suspension.
Comparative example 1
This comparative example provides an aqueous suspension, the same formulation as in example 1, except for the difference in the preparation method, and the aqueous suspension of this comparative example was prepared as follows:
(1) Weighing the medicinal active substance, the wetting agent, the emulsifying dispersant and the synergist according to the prescription, adding the medicinal active substance, the wetting agent, the emulsifying dispersant and the synergist into 250kg of deionized water, stirring and dissolving at 800rpm, and performing multistage wet sanding to ensure that the average particle size of suspended particles is less than or equal to 5 microns; discharging;
(2) And (2) adding an antifreezing solution, a thickening agent and a preservative into the feed liquid obtained in the step (1), adding water until the total weight is 1 ton, uniformly stirring at 500rpm, and filtering to obtain the water suspension agent.
Comparative example 2
This comparative example provides an aqueous suspension, the same formulation as in example 1, except for the preparation method, and the preparation method of the aqueous suspension of this comparative example is as follows:
(1) Weighing the medicinal active substance according to the prescription, heating at 75 deg.C for 15min to obtain molten medicine;
(2) Weighing a wetting agent, an emulsifying dispersant and a synergist according to a formula, adding the wetting agent, the emulsifying dispersant and the synergist into 250kg of deionized water, stirring and dissolving at 800rpm, heating to 75 ℃, increasing the stirring speed to 6000rpm, adding a molten drug, shearing and stirring at the temperature of 75 ℃ and the rotation speed of 6000rpm for 30min, stopping heating, reducing the temperature to 30 ℃, adding an antifreezing solution, a thickening agent and a preservative, adding water until the total weight is 1 ton, uniformly stirring at 500rpm, and filtering to obtain the water suspension.
Comparative example 3
This comparative example provides an aqueous suspension, the same formulation as in example 1, except for the difference in the preparation method, and the aqueous suspension of this comparative example was prepared as follows:
(1) Weighing a wetting agent, an emulsifying dispersant, a thickening agent and a synergist according to a formula, adding the wetting agent, the emulsifying dispersant, the thickening agent and the synergist into 250kg of deionized water, stirring at 800rpm, and uniformly dispersing to obtain a mixed solution;
(2) Weighing the medicinal active substances according to the prescription, adding the medicinal active substances into the solution in the step (1), heating at the temperature of 75 ℃ at 800rpm for 30min to obtain emulsion, shearing and stirring the emulsion at the temperature of 75 ℃ and the rotation speed of 6000rpm for 30min, then cooling to 30 ℃, adding the antifreeze and the preservative, adding water to the total weight of 1 ton, uniformly stirring at 500rpm, and filtering to obtain the water suspension.
Experimental example 1 effective content of the drug
The aqueous suspensions prepared in examples 1-3 and comparative example 2 were tested for the amount of active drug in the suspension, as shown in Table 1. Loss rate = (theoretical content-measured content)/theoretical value × 100%, where theoretical content = drug addition/total amount of aqueous suspension agent × 97%.
TABLE 1 viscosity and content results
Compared with the water suspending agent prepared in the comparative example 2, the content of difenoconazole and the loss rate of trifloxystrobin content obtained in each example of the invention are obviously reduced.
Experimental example 2 viscosity and Heat storage stability
The aqueous suspensions obtained in examples 1 to 3 and comparative examples 1 and 3 were tested for viscosity, and the aqueous suspensions obtained in the above examples and comparative examples were left at 54 ℃ for 14 days, and the state was observed, and the water evolution rate after the left standing was calculated, the water evolution rate = height of upper water/total height.
TABLE 2 results of viscosity and water extraction
| viscosity/(Unit: mPas) | Water separation rate | |
| Example 1 | 650 | 1％ |
| Example 2 | 610 | 3％ |
| Example 3 | 680 | 2％ |
| Comparative example 1 | 1280 | —— |
| Comparative example 3 | 530 | 13％ |
Among them, the aqueous suspension obtained in comparative example 1 gradually caked and creamed during hot storage and could not be used. The aqueous suspension prepared in comparative example 3 has severe water segregation, while the aqueous suspension prepared in examples 1 to 3 of the present invention has stable state, no caking and creaming phenomenon and low water segregation rate, and the heat storage stability is significantly improved compared with comparative examples 1 and 3.
Experimental example 3 effective content and particle size before and after Heat storage and graduation thereof
Each of the examples in experimental example 3 was tested for the mass fraction of active drug in the aqueous suspension before standing at 54 ℃ (before heat storage) and after 14 days (after heat storage), and for the D90 and PDI values of the aqueous suspension before and after heat storage.
TABLE 3 content before and after thermal storage and D90 for the examples
As can be seen from the above table, the content of the two drugs in the aqueous suspension prepared in each example of the present invention changes little before and after heat storage, D90 before and after heat storage is small, PDI is low, particle size distribution is uniform, and the aqueous suspension has good heat storage stability.
Experimental example 4 product Performance index
Taking the water suspending agent prepared in the example 1, testing the mass fractions of trifloxystrobin and difenoconazole in the water suspending agent by adopting a high performance liquid phase method, testing the suspension rate of the medicament by referring to a standard GBT 14825-2006, testing the lasting foamability by referring to a standard GBT 28137-2011, testing the low-temperature stability of the pesticide by referring to a standard GBT 19137-2003, testing the heat storage stability of the pesticide by referring to a standard GBT 19136-2003, testing the pourability by referring to a section 4.9 of the standard compiling specification of a standard HGT 2467.5-2003 pesticide suspending agent product standard, and carrying out a wet sieve test by referring to a GBT 16150-1995 standard.
Table 4 table of performance index of product obtained in example 1
The table shows that the aqueous suspension obtained in example 1 has good properties.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. This need not be, nor should it be exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. A preparation method of an aqueous suspending agent is characterized by comprising the following steps:
s1, a step: dissolving a wetting agent and an emulsifying dispersant by water to obtain a solution;
and S2, a step: mixing the solution with active substances, and heating to obtain emulsion;
and S3, a step: and (3) shearing and stirring the emulsion while heating, then cooling, and mixing the mixed solution with a thickening agent to prepare the aqueous suspension.
2. The production method according to claim 1, wherein in the step S2, heating is performed under stirring; preferably, the heating is carried out at a rotation speed of 200-1000rpm and a temperature of 70-80 ℃.
3. The method according to claim 2, wherein the speed of the shear stirring in the step S3 is 4000 to 8000rpm, the temperature of the heating is 70 to 80 ℃, and the time is at least 20min.
4. The method according to any one of claims 1 to 3, wherein in the step S3, the mixed solution is cooled to a temperature of 30 ℃ or less and then mixed with the thickener at a rotation speed of 200 to 1000 rpm.
5. The production method according to any one of claims 1 to 4, wherein the wetting agent is at least one selected from the group consisting of acetylene glycol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, and styrene phenol polyoxyethylene ether; and/or the emulsifying dispersant is at least one selected from polyoxyethylene polyoxypropylene ether block copolymer, polyoxyethylene polyoxypropylene ether block copolymer phosphate, triphenyl phenol polyoxyethylene ether phosphate, alkyl polyoxyethylene polyoxybutylene block copolymer phosphate and polycarboxylate; and/or, the thickening agent is selected from at least one of xanthan gum, arabic gum, gelatin and polyvinyl alcohol.
6. The method according to any one of claims 1 to 5, wherein the aqueous suspension comprises 10 to 60% of the pharmaceutically active substance, 1 to 5.5% of the wetting agent, 1 to 20% of the emulsifying dispersant, 0.05 to 0.5% of the thickener, and 30 to 60% of water, based on 100% of the total mass of the aqueous suspension.
7. The production method according to any one of claims 1 to 6, wherein the pharmaceutically active substance is selected from at least one of difenoconazole and trifloxystrobin; preferably, the pharmaceutically active substance comprises difenoconazole and trifloxystrobin in a mass ratio of 5:1-1:5.
8. The preparation method according to any one of claims 1 to 7, wherein the aqueous suspension further comprises 0 to 10% of a synergist, 2 to 6% of an antifreeze and/or 0.1 to 2% of a preservative, based on 100% of the total mass of the aqueous suspension.
9. The method according to any one of claims 1 to 8, wherein in the step S3, an antifreezing solution and/or a synergist and/or a preservative are further mixed in the mixture when the thickener is mixed with the mixture; and/or, the solution in the step S1 also contains a synergist.
10. The preparation method according to claim 8 or 9, wherein the antifreeze solution is at least one selected from urea, propylene glycol and glycerol; and/or, the preservative is selected from at least one of benzoic acid, sorbic acid, cason and p-hydroxybenzoate; and/or the synergist is selected from at least one of isomeric alcohol ether and organic silicon polyether.
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