CN109526969A - A kind of high-content capillary aqueous emulsion and preparation method thereof - Google Patents
A kind of high-content capillary aqueous emulsion and preparation method thereof Download PDFInfo
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- CN109526969A CN109526969A CN201811387903.4A CN201811387903A CN109526969A CN 109526969 A CN109526969 A CN 109526969A CN 201811387903 A CN201811387903 A CN 201811387903A CN 109526969 A CN109526969 A CN 109526969A
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- 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
- A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
- A01N43/36—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom five-membered rings
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- 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
- 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
- A01N25/22—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 ingredients stabilising the active ingredients
-
- 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
- A01N25/30—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 characterised by the surfactants
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- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Dentistry (AREA)
- Wood Science & Technology (AREA)
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- Dispersion Chemistry (AREA)
- Chemical & Material Sciences (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The present invention provides a kind of high-content capillary aqueous emulsion and preparation method thereof, is related to technical field of pesticide.The high-content capillary aqueous emulsion, be grouped as according to mass percentage by following group: capillary 10%-25%, solvent 10-25%, emulsifier 8-10%, antifreezing agent 3-7%, stabilizer 3-8%, deionized water supply quality to 100%.The present invention also provides the preparation methods of the high-content capillary aqueous emulsion, include the following steps: to mix capillary, solvent, emulsifier and stabilizer by formula rate, stir evenly, antifreezing agent and deionized water are added in a shear condition, emulsification, obtains high-content capillary aqueous emulsion.Aqueous emulsion of the present invention, it overcomes the defect that existing capillary aqueous emulsion too high levels are watered rear easily crystallization, and preparation method is simple and efficient.
Description
Technical field
The present invention relates to technical field of pesticide, and in particular to a kind of high-content worm nitrile nitrile aqueous emulsion and preparation method thereof.
Background technique
Aqueous emulsion is one or more kinds of pesticide active ingredients, and the stable cream of high dispersive is formed in water system decentralized medium
Shape liquid system, the development of aqueous emulsion starts from later period the 1970s, until the nineties is rapidly developed.Aqueous emulsion and cream
Oil, wettable powder are compared with dosage forms such as water dispersible granules, and with good penetrability, adhesiveness is strong, advantages of environment protection, greatly
Improve the bioactivity of medicament.
Capillary English name: Chlorfenapyr, No. CAS: 122453-73-0, molecular formula: C15H11BrClF3N2O,
Molecular weight: 407.61.Capillary belongs to a kind of pyroles Insecticidal and acaricidal agent of structure novel, to brill moth, piercing and sucking and chewing type evil
Worm and mite class have excellent preventive effect.It is broad spectrum insecticide, acaricide that the medicament, which has the feature that,；Have stomach toxicity concurrently and work of tagging
With；With other insecticide no interactions resistances；There is medium residual activity on crop；It absorbs in nutrient solution through root system selective
Systemic activity；Medium to mammal Oral toxicity, percutaneous toxicity is lower；Effective formulation rate is low (100g effective component/hm2).
The significant desinsection of capillary, acaricidal activity and unique chemical structure are widely paid attention to and are paid close attention to by people.
Aqueous emulsion is a kind of environmental-friendly dosage form, be the direction that country advocates energetically, and capillary aqueous emulsion contains at present
Measure it is lower, be no more than 10%, reason is that high-concentration aqueous emulsion is watered rear easy crystallization.
Summary of the invention
The object of the present invention is to provide a kind of high-content capillary aqueous emulsions, it overcomes existing capillary water and milk agent content
The excessively high defect for being watered rear easily crystallization.
A kind of high-content capillary aqueous emulsion is grouped as according to mass percentage by following group: capillary 10%-
25%, solvent 10-25%, emulsifier 8-10%, antifreezing agent 3-7%, stabilizer 3-8%, deionized water supply quality extremely
100%.
In the present invention, the solvent is one or more of cyclohexanone, dimethylbenzene, vegetable oil.
In the present invention, the emulsifier is the mixture of nonionic surfactant A and B；
The structural formula of the nonionic surfactant A is as follows:
Wherein m=3-18 and m are integer；
The structural formula of the nonionic surfactant B is as follows:
Wherein a=3-10, b=
5-12 and a, b are integer.
In the present invention, the antifreezing agent is selected from one or more of ethylene glycol, propylene glycol, glycerine, urea.
In the present invention, the stabilizer is the mixture of beta-cyclodextrin and hydroxy ethylene diphosphonic acid.
The present invention also provides the preparation method of the high-content capillary aqueous emulsion, include the following steps: capillary, molten
Agent, emulsifier and stabilizer are mixed by formula rate, are stirred evenly, and antifreezing agent and deionization are added in a shear condition
Water, emulsification, obtains high-content capillary aqueous emulsion.
Capillary aqueous emulsion of the present invention is easy to use, and when use is diluted with water, and can use as needed a variety of insecticide-applying way:
1, spraying using ultra-low volume technology after being diluted with water 1-10 times；2, spraying using low dosage after being diluted with water 10-100 times；3,
Using conventional spraying after being diluted with water 500-1000 times.
The invention has the following advantages: capillary concentration has reached 10- in (1) capillary aqueous emulsion of the present invention
25%, physicochemical properties stablize, be not easily decomposed it is rotten, and be watered dilution after will not crystallize, solve existing capillary water and milk
Agent concentration is watered the industry problems of easy crystallization after being higher than 10%；In addition after heat is stored up (54 DEG C) 14 days, is refrigerated 14 days (- 4 DEG C) still
Stablize.After control aqueous emulsion 1,4,7 without stabilizer in aqueous emulsion of the present invention and emulsifier is watered 100 times of dilutions, 20 minutes
Interior crystallization, and heat storage (54 DEG C) after 14 days condensate oil, stability it is poor.Without containing beta cyclodextrin or when hydroxy ethylene diphosphonic acid,
Its stability with to compare aqueous emulsion 1,4,7 similar.(2) capillary aqueous emulsion of the present invention significantly improves capillary to sensitive crop
Safety, cost performance be much higher than existing capillary preparation.(3) high-content capillary aqueous emulsion of the present invention increases capillary pair
The absorption and permeance property of target plant, improve the effective rate of utilization of drug.
Specific embodiment
Beta-cyclodextrin used in the embodiment of the present invention, No. CAS is 7585-39-9.
Embodiment one
Aqueous emulsion 1 is 10% capillary aqueous emulsion, is grouped as according to mass percentage by following group: capillary 10%,
Cyclohexanone (solvent) 8%, dimethylbenzene (solvent) 5%, nonionic surfactant A1 (emulsifier) 4%, non-ionic surface active
Agent B1 (emulsifier) 4%, ethylene glycol (antifreezing agent) 5%, beta-cyclodextrin (stabilizer) 2%, hydroxy ethylene diphosphonic acid (are stablized
Agent) 1%, deionized water supplies quality to 100%.
Wherein the structural formula of nonionic surfactant A1 is as follows:
The structural formula of nonionic surfactant B1 is as follows:
Capillary raw medicine, solvent, emulsifier and stabilizer are mixed by formula rate first, stirred evenly, is cut in height
Antifreezing agent and deionized water is added in (5000 revs/min of cutter revolving speed) under tangent condition, under high shear conditions (cutter revolving speed
5000 revs/min) emulsification 50min, obtain aqueous emulsion 1.
Aqueous emulsion 1 is compareed according to mass percentage, is grouped as by following group: capillary 10%, cyclohexanone (solvent)
8%, dimethylbenzene (solvent) 5%, pesticide emulsifier 600 # (commercial product) 4%, farm chemical emulgent L62# (commercial product) 4%,
Ethylene glycol (antifreezing agent) 5%, deionized water supplies quality to 100%.
Control aqueous emulsion 2: it is grouped as according to mass percentage by following group: capillary 10%, cyclohexanone (solvent)
8%, dimethylbenzene (solvent) 5%, nonionic surfactant A1 (emulsifier) 4%, nonionic surfactant B1 (emulsifier)
4%, ethylene glycol (antifreezing agent) 5%, beta cyclodextrin (stabilizer) 2%, deionized water supplies 100%.
Control aqueous emulsion 3: it is grouped as according to mass percentage by following group: capillary 10%, cyclohexanone (solvent)
8%, dimethylbenzene (solvent) 5%, nonionic surfactant A1 (emulsifier) 4%, nonionic surfactant B1 emulsifier
4%, ethylene glycol (antifreezing agent) 5%, hydroxy ethylene diphosphonic acid (stabilizer) 1%, deionized water supplies 100%.
Compare aqueous emulsion 1-3's the preparation method is as follows: first by capillary raw medicine, solvent, emulsifier, stabilizer press recipe ratio
Example is mixed, and is stirred evenly, and antifreezing agent and deionization is added in (5000 revs/min of cutter revolving speed) under high shear conditions
Water, (5000 revs/min of cutter revolving speed) emulsifies 50min under high shear conditions, obtains control aqueous emulsion.
Embodiment two
Aqueous emulsion 2 is 15% capillary aqueous emulsion, is grouped as according to mass percentage by following group: capillary 15%,
Cyclohexanone (solvent) 10%, dimethylbenzene (solvent) 8%, nonionic surfactant A2 (emulsifier) 5%, non-ionic surface active
Agent B2 (emulsifier) 5%, ethylene glycol (antifreezing agent) 5%, beta-cyclodextrin (stabilizer) 3%, hydroxy ethylene diphosphonic acid (are stablized
Agent) 2%, deionized water supplies quality to 100%.
The structural formula of nonionic surfactant A2 is as follows:
The structural formula of nonionic surfactant B2 is as follows:
The aqueous emulsion 1 during the preparation method is the same as that of Example 1 of aqueous emulsion 2.
Aqueous emulsion 4 is compareed according to mass percentage, is grouped as by following group: capillary 15%, cyclohexanone (solvent)
10%, dimethylbenzene (solvent) 8%, pesticide emulsifier 600 # (emulsifier) 5%, farm chemical emulgent L62# (emulsifier) 5%, second two
Alcohol (antifreezing agent) 5%, deionized water supplies quality to 100%.
Control aqueous emulsion 5 is grouped as according to mass percentage by following group: capillary 15%, cyclohexanone (solvent)
10%, dimethylbenzene (solvent) 8%, nonionic surfactant A2 (emulsifier) 5%, nonionic surfactant B2 (emulsifier)
5%, ethylene glycol (antifreezing agent) 5%, beta-cyclodextrin (stabilizer) 3%, deionized water supplies 100%.
Control aqueous emulsion 6 is grouped as according to mass percentage by following group: capillary 15%, cyclohexanone (solvent)
10%, dimethylbenzene (solvent) 8%, nonionic surfactant A2 (emulsifier) 5%, nonionic surfactant B2 (emulsifier)
5%, ethylene glycol (antifreezing agent) 5%, hydroxy ethylene diphosphonic acid (stabilizer) 2%, deionized water supplies 100%.
Control aqueous emulsion 4-6 compares aqueous emulsion 1-3 during the preparation method is the same as that of Example 1.
Embodiment three
Aqueous emulsion 3 is 20% capillary aqueous emulsion, is grouped as according to mass percentage by following group: capillary 20%,
Cyclohexanone (solvent) 15%, dimethylbenzene (solvent) 8%, nonionic surfactant A3 (emulsifier) 5%, non-ionic surface active
Agent B3 (emulsifier) 5%, ethylene glycol (antifreezing agent) 5%, beta-cyclodextrin (stabilizer) 5%, hydroxy ethylene diphosphonic acid (are stablized
Agent) 3%, deionized water supplies quality to 100%.
The structural formula of nonionic surfactant A3 is as follows:
The structural formula of nonionic surfactant B3 is as follows:
The aqueous emulsion 1 during the preparation method is the same as that of Example 1 of aqueous emulsion 3.
Aqueous emulsion 7 is compareed, is grouped as according to mass percentage by following group: capillary 20%, cyclohexanone 15%, diformazan
Benzene 8%, emulsifier 600 # (commercial product) 5%, emulsifier L62# (commercial product) 5%, ethylene glycol 5%, deionized water is supplied
Quality is to 100%.
Control aqueous emulsion 8 is grouped as according to mass percentage by following group: capillary 20%, cyclohexanone (solvent)
15%, dimethylbenzene (solvent) 8%, nonionic surfactant A3 (emulsifier) 5%, nonionic surfactant B3 (emulsifier)
5%, ethylene glycol (antifreezing agent) 5%, beta-cyclodextrin (stabilizer) 5%, deionized water supplies quality to 100%.
Control aqueous emulsion 9 is grouped as according to mass percentage by following group: capillary 20%, cyclohexanone (solvent)
15%, dimethylbenzene (solvent) 8%, nonionic surfactant A3 (emulsifier) 5%, nonionic surfactant B3 (emulsifier)
5%, ethylene glycol (antifreezing agent) 5%, hydroxy ethylene diphosphonic acid (stabilizer) 3%, deionized water supplies quality to 100%.
The preparation method of aqueous emulsion 7-9 is compareed with control aqueous emulsion 1-3.
Example IV
(1) stability of each aqueous emulsion
Each aqueous emulsion heat into embodiment three of embodiment one is detected to store up 14 days (54 DEG C), refrigerate the stabilization after 14 days (- 4 DEG C)
Property.
Using water, to embodiment one, each aqueous emulsion into embodiment three carries out 100 times of dilutions, sees whether occur after standing
There is the time of crystallization after record dilution in crystallization.
As seen from Table 1, aqueous emulsion 1-3 heat is still stable after storing up 14 days (54 DEG C), refrigerating 14 days (- 4 DEG C).Aqueous emulsion 1-3
After it joined beta cyclodextrin and hydroxy ethylene diphosphonic acid as stabilizer, dilution 100 times after 2 hours without crystallization, make worm
Mite nitrile water-emulsion preparation is more convenient when using.Control aqueous emulsion 1 without containing stabilizer in aqueous emulsion of the present invention and emulsifier, 4,
7 be watered 100 times dilution after, crystallization in 20 minutes, and heat storage (54 DEG C) after 14 days condensate oil, stability it is poor.Without containing beta cyclodextrin
Or when hydroxy ethylene diphosphonic acid, stability with to compare aqueous emulsion 1,4,7 similar.
1 capillary aqueous emulsion stability of table
(2) safety
Capillary aqueous emulsion (embodiment one to embodiment three) is subjected to safety testing on Chinese cabbage respectively, three after medicine
It investigates its safety, calculates capillary aqueous emulsion to the control efficiency of diamondback moth.
The safety of 2 capillary aqueous emulsion of table and to diamondback moth control efficiency
| Aqueous emulsion number | Extension rate | Safety carries out investigation result | To the preventive effect of diamondback moth |
| Aqueous emulsion 1 | 500 times | Grow without exception, blade is good | 92% |
| Aqueous emulsion 2 | 750 times | Grow without exception, blade is good | 95% |
| Aqueous emulsion 3 | 1000 times | Grow without exception, blade is good | 90% |
| Compare aqueous emulsion 1 | 500 times | Lobus cardiacus has obvious burned spot, and old leaf has slight medicine spot | 88% |
| Compare aqueous emulsion 2 | 500 times | Lobus cardiacus has obvious burned spot, and old leaf has slight medicine spot | 89% |
| Compare aqueous emulsion 3 | 500 times | Lobus cardiacus has obvious burned spot, and old leaf has slight medicine spot | 89% |
| Compare aqueous emulsion 4 | 750 times | Lobus cardiacus has obvious burned spot, and old leaf has slight medicine spot | 85% |
| Compare aqueous emulsion 5 | 750 times | Lobus cardiacus has obvious burned spot, and old leaf has slight medicine spot | 86% |
| Compare aqueous emulsion 6 | 750 times | Lobus cardiacus has obvious burned spot, and old leaf has slight medicine spot | 87% |
| Compare aqueous emulsion 7 | 1000 times | Lobus cardiacus has obvious burned spot, and old leaf has slight medicine spot | 87% |
| Compare aqueous emulsion 8 | 1000 times | Lobus cardiacus has obvious burned spot, and old leaf has slight medicine spot | 87% |
| Compare aqueous emulsion 9 | 1000 times | Lobus cardiacus has obvious burned spot, and old leaf has slight medicine spot | 87% |
From table 2 it can be seen that 3 days preventive effects are slightly better than compareing water and milk after medicine using the prevention and treatment diamondback moth of aqueous emulsion 1,2 and 3
Agent 1-9, but control aqueous emulsion 1-9 is significantly better than in the safety to Chinese cabbage.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, although previous embodiment
Invention is explained in detail, it will be apparent, however, to one skilled in the art, that it still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features, all in essence of the invention
Within mind and principle, made any modification, equivalent replacement, improve etc., it should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of high-content capillary aqueous emulsion is grouped as according to mass percentage by following group: capillary 10%-25%,
Solvent 10-25%, emulsifier 8-10%, antifreezing agent 3-7%, stabilizer 3-8%, deionized water supply quality to 100%.
2. high-content capillary aqueous emulsion according to claim 1, it is characterised in that the solvent be cyclohexanone, dimethylbenzene,
One or more of vegetable oil.
3. high-content capillary aqueous emulsion according to claim 1 or claim 2, it is characterised in that the emulsifier is non-ionic surface
The mixture of activating agent A and B；The structural formula of the nonionic surfactant A is as follows:
Wherein m=3-18 and m are integer；
The structural formula of the nonionic surfactant B is as follows:
Wherein a=3-10, b=5-12
And a, b are integer.
4. high-content capillary aqueous emulsion according to claim 3, it is characterised in that the antifreezing agent is selected from ethylene glycol, the third two
One or more of alcohol, glycerine, urea.
5. high-content capillary aqueous emulsion according to claim 4, it is characterised in that the stabilizer is beta-cyclodextrin and hydroxyl
The mixture of base ethylidene diphosphonic acid.
6. the preparation method of high-content capillary aqueous emulsion described in claim 1, it is characterised in that include the following steps: worm mite
Nitrile, solvent, emulsifier and stabilizer are mixed by formula rate, are stirred evenly, and antifreezing agent is added in a shear condition and goes
Ionized water, emulsification, obtains high-content capillary aqueous emulsion.
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Citations (5)
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|---|---|---|---|---|
| US3759861A (en) * | 1969-12-20 | 1973-09-18 | W Shimokawa | Ic or amphoteric surface active agent polymer complex of a carboxy containing polymer and a nonionic cation |
| CN101379963A (en) * | 2008-07-17 | 2009-03-11 | 张少武 | Disinsection aqueous emulsion containing chlorfenapyr |
| CN101406189A (en) * | 2008-10-17 | 2009-04-15 | 广西田园生化股份有限公司 | Aqueous emulsion containing chlorfenapyr and preparation method thereof |
| CN102640752A (en) * | 2012-04-18 | 2012-08-22 | 云南省农业科学院蚕桑蜜蜂研究所 | Acaricide water emulsion composition and preparation method of acaricide water emulsion composition |
| CN105555134A (en) * | 2013-10-03 | 2016-05-04 | 陶氏环球技术有限责任公司 | Microbicidal composition comprising 2-decylthioethylamine |
-
2018
- 2018-11-21 CN CN201811387903.4A patent/CN109526969A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3759861A (en) * | 1969-12-20 | 1973-09-18 | W Shimokawa | Ic or amphoteric surface active agent polymer complex of a carboxy containing polymer and a nonionic cation |
| CN101379963A (en) * | 2008-07-17 | 2009-03-11 | 张少武 | Disinsection aqueous emulsion containing chlorfenapyr |
| CN101406189A (en) * | 2008-10-17 | 2009-04-15 | 广西田园生化股份有限公司 | Aqueous emulsion containing chlorfenapyr and preparation method thereof |
| CN102640752A (en) * | 2012-04-18 | 2012-08-22 | 云南省农业科学院蚕桑蜜蜂研究所 | Acaricide water emulsion composition and preparation method of acaricide water emulsion composition |
| CN105555134A (en) * | 2013-10-03 | 2016-05-04 | 陶氏环球技术有限责任公司 | Microbicidal composition comprising 2-decylthioethylamine |
Non-Patent Citations (3)
| Title |
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| 丁彤等编写: "《中国化工产品大全 下》", 31 October 1994, 化学工业出版社 * |
| 刘步林主编: "《农药剂型加工技术（第二版）》", 31 October 1998, 化学工业出版社 * |
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