CN1220432C - Aqueous carbosulfan emulsion and preparing method thereof - Google Patents
Aqueous carbosulfan emulsion and preparing method thereof Download PDFInfo
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- CN1220432C CN1220432C CN 03122177 CN03122177A CN1220432C CN 1220432 C CN1220432 C CN 1220432C CN 03122177 CN03122177 CN 03122177 CN 03122177 A CN03122177 A CN 03122177A CN 1220432 C CN1220432 C CN 1220432C
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- aqueous emulsion
- acid ester
- phosphoric acid
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Abstract
The present invention relates to aqueous emulsion whose effective ingredient is carbosulfan and a preparation method thereof. The aqueous emulsion contains the following ingredients by weight percentage: 1 to 40% of carbosulfan, 0.1 to 10% of at least one phosphoric acid ester type anion surface active agent as an emulsifying agent, 0.1 to 10% of at least one polyacrylic acid derivative as a dispersing agent, 1 to 15% of at least one epoxide as a stabilizing agent and balance of water.
Description
Technical field
The present invention relates to carbosulfan aqueous emulsion and preparation method thereof.
Background technology
Pesticide emulsion in water is to be matrix with water, utilizes physicochemical liquid-in-liquid dispersions system theoretical and that method is prepared is efficient, storing safety, low pollution novel form.This formulation oil phase drop dispersible granule footpath uses no or little organic solvent less than 3 microns, cost and missible oil quite or lower slightly, active ingredient dispersity height, good drug efficacy.The general water content of aqueous emulsion has not only been saved a large amount of organic solvents more than 50%, and has alleviated the pressure to environment greatly, and is significant for protection Agro-ecology balance, more helps the sustainable development of agricultural.
Carbosulfan (carbosulfan) is a kind of known wide spectrum, the carbamate insecticide of low toxicity, can prevent eliminating aphis, various pests such as mite, wireworm, beet flea beetle, colorado potato beetle, fruit tree leaf roller, oriental fruit moth and scale insect.The preparation of this pesticide product with use can referring to, for example, external new varieties of pesticides handbook, 11-14 page or leaf, Sha Jiajun, Chemical Industry Press, 1998.
The carbosulfan formulation has wetting powder, missible oil etc.For example, US 4,281, and 014A discloses various stabilized preparations for example missible oil, wetting powder, the granula etc. that contain carbosulfan, and wherein disclose and adopted the stabilizing agent of epoxides as carbosulfan, but wherein unexposed carbosulfan aqueous emulsion.In addition, JP-A-3167105, AU 2 621 684A also disclose and have adopted the stabilizing agent of epoxides as carbamate insecticide.
The water-base emulsion of carbamate insecticide is also disclosed in the prior art, for example, CN1 139 371A, CN 1 087 466A, CN 85 05954A, JP-A-61024506.But specifically do not mention or hint the aqueous emulsion of carbosulfan.
The present inventor finds by further investigation, adopt the emulsification-dispersion-stabilising system of phosphoric acid ester anion surfactant-polyacrylic acid-epoxides, can make the carbosulfan aqueous emulsion of physicochemical property excellence, this aqueous emulsion has that resolution ratio is low, emulsion property is stable and the excellent reliable advantage of drug effect, so finished the present invention.
Summary of the invention
The purpose of this invention is to provide a kind of carbosulfan aqueous emulsion with good stability.
Another object of the present invention provides the preparation method of described preparation.
Aqueous emulsion of the present invention comprises
1) 1-40% carbosulfan by weight;
2) at least a phosphoric acid ester anion surfactant of 0.1-10% by weight as emulsifier;
3) at least a polyacrylic acid derivative of 0.1-10% by weight as dispersant;
4) by weight 1-15% at least a as stabilizing agent epoxides and
5) water surplus.
Preferably, aqueous emulsion of the present invention comprises
1) 5-25% carbosulfan by weight;
2) at least a phosphoric acid ester anion surfactant of 1-10% by weight as emulsifier;
3) at least a polyacrylic acid derivative of 1-10% by weight as dispersant;
4) by weight 2-15% at least a as stabilizing agent epoxides and
5) water surplus.
In preferred embodiments, also contain the cosolvent of 0.1-5% by weight in the preparation of the present invention.
Aqueous emulsion is a kind of eco-friendly pesticidal preparations.As a kind of pesticidal preparations, aqueous emulsion should have good heat storage stability, freeze-thaw stability and water dilution stability.Because of containing a large amount of water in the said preparation, the ammonia carbamates agricultural chemicals (for example carbosulfan) that generally speaking is easy to hydrolysis is difficult to be processed into chemically stable aqueous emulsion.Therefore, selecting specific processing aids for example emulsifier, co-emulsifier and auxiliary agent thereof etc., is the key that makes the aqueous emulsion of qualified carbamate chemicals for agriculture (for example carbosulfan).
The present inventor finds by further investigation, adopts the emulsification-dispersion-stabilising system of phosphoric acid ester anion surfactant-polyacrylic acid-epoxides, can make the carbosulfan aqueous emulsion of physicochemical property excellence.Not only resolution ratio is low for this aqueous emulsion, emulsion property stable, and drug effect is excellent reliable.The successful preparation of carbosulfan aqueous emulsion, the safety that can improve production, storing effectively and use, and its use can significantly reduce the pollution to environment, and therefore, said preparation has positive society and Significance for Environment.
In the present invention, the surfactant that is fit to is selected from the phosphoric acid ester anion surfactant with well emulsify performance, for example phosphoric acid ester anion surfactant, for example aliphatic acid polyethenoxy ether phosphoric acid ester such as linoleic acid polyoxyethylene ether phosphate, linolenic acid polyoxyethylene ether phosphate, castor oil acid polyoxyethylene ether phosphate etc.; The alkyl polyoxyethylene ether phosphoric acid ester is C for example
8-C
24-alkyl or alkyl phenyl polyoxyethylene ether phosphate for example can be, iso-octyl alcohol polyoxyethylene ether phosphate, ethoxylated dodecyl alcohol phosphate, polyoxyethylene octadecanol phosphate etc.; Alkylphenol polyoxyethylene phosphate, hexyl, octyl group, decyl mixed alcohol polyoxyethylene ether phosphate etc.; Alkylphenol polyoxyethylene phosphoric acid ester such as C
8-C
18-alkylphenol-polyethenoxy mono phosphoric acid ester (two) ester can be for example OPEO phosphate, polyoxyethylene nonylphenol ether phosphate, binonylphenol polyoxyethylene ether phosphate, dodecylphenol polyoxyethylene ether phosphate, tetradecylphenol polyoxyethylene ether phosphate and cetyl phenol polyethenoxy ether phosphate; Benzene alkylphenol polyoxyethylene phosphoric acid ester such as phenethyl phenol polyethenoxy ether phosphate and slaine or amine salt.Preferably surfactant can be wherein a kind of, also can be its mixture.The EO value of the phosphoric acid ester anion surfactant that is fit to is generally 2-20 according to the difference of the type of selected phosphate, is preferably 4-16.
The dispersant that is fit to is selected from polyacrylic acid derivative, for example polyacrylic acid, Sodium Polyacrylate, maleic anhydride/acrylic copolymer, acrylic acid/hydroxypropyl acrylate copolymer.Preferably polyacrylic acid and Sodium Polyacrylate.Dispersant can be wherein a kind of, also can be its mixture.Molecular weight (MW) size of the polyacrylic acid derivative that is fit to is preferably 3000-7000 in the scope of 1000-10000.
The stabilizing agent that is fit to is selected from epoxides, for example epoxychloropropane, epoxidized soybean oil, epoxy linseed oil, epoxidation castor oil.Stabilizing agent can be wherein a kind of, also can be its mixture.Preferably epoxychloropropane, epoxidized soybean oil and epoxy linseed oil particularly preferably are epoxychloropropane and epoxidized soybean oil.
For the present invention, the content of oxirane for example is generally 3-10% by weight in the adoptable epoxide stabilizer, is preferably 5-8% by weight.
In preparation of the present invention, the content of cosolvent is 0.1-5%.
The cosolvent that is fit to is selected from arene for example dimethylbenzene, toluene, trimethylbenzene etc.
The present invention can also contain other auxiliary element such as antifreezing agent, suspending agent, sterilization defoamer etc.
The antifreezing agent that is fit to is selected from for example C of lower aliphatic alcohols
2-C
6Alcohols, for example ethanol, propyl alcohol, isopropyl alcohol, ethylene glycol, the tert-butyl alcohol and propane diols, preferred propane diols and ethylene glycol are as antifreezing agent.
The suspending agent that is fit to can be the suspension aids that various routines are used for liquid preparation, for example alkylnaphthalene sulfonate, lignosulphonates, polyoxyethylene polyoxypropylene block copolymer etc.
The defoamer that is fit to is a silicone defoaming agent, for example: methyl polysiloxane.
The bactericide that is fit to is formaldehyde and isothiazolinone disinfecting agent.
This aqueous emulsion preparation can prepare in a known manner, for example adopts phase conversion method, soluble oils method, second emulsifying method, referring to, formulations of pesticide process technology (second edition), 406-407 page or leaf, Liu Bulin, Chemical Industry Press, in October, 1998.But preferably prepare according to the method among this paper embodiment.
Present composition application dosage, the difference according to factors such as different crops, time of application, weather conditions is generally 50-1500g a.i./ha, is preferably 100-750g a.i./ha.The general foliage applying that adopts, for example foliar spray is handled.Also can do other and handle as seed dressing, filling root etc., in this case, can adjust application dosage as required.For example when soil treatment control soil insect, application dosage is in the scope of 100-3000g a.i./ha.
Embodiment
The present invention describes with the following example, but does not limit the present invention.
Example of formulations 1:5% carbosulfan aqueous emulsion
Carbosulfan 5%
Dimethylbenzene 2%
Ethylene glycol 5%
OPEO phosphate 5%
Polyacrylic acid (MW5000) 2%
Epoxidized soybean oil 5%
Water to 100%
In the load weighted water of preliminary election, add the processing aids that measures, fully stir, make system form a kind of uniform dispersion emulsion system, under high-speed stirred, in system, slowly add with the carbosulfan that is dissolved in dimethylbenzene, finish, continue fully to stir, can be made into aqueous emulsion.Can be diluted to the white milk shape emulsion of any concentration to water.
Adopt the step identical, prepare following example of formulations with example of formulations.
Example of formulations 2:5% carbosulfan aqueous emulsion
Carbosulfan 5%
Dimethylbenzene 3%
Isopropyl alcohol 5%
Ethoxylated dodecyl alcohol phosphate 5%
Sodium Polyacrylate (MW3000) 2%
Epoxychloropropane 3%
Silicon defoaming agent 1%
Water to 100%
Example of formulations 3:10% carbosulfan aqueous emulsion
Carbosulfan 10%
Toluene 3%
Propane diols 5%
Dodecylphenol polyoxyethylene ether phosphate 5%
Maleic anhydride/acrylic copolymer (MW3000) 2%
Epoxidized soybean oil 5%
Water to 100%
Example of formulations 4:5% carbosulfan aqueous emulsion
Carbosulfan 5%
Dimethylbenzene 2%
Ethylene glycol 5%
Polyoxyethylene nonylphenol ether phosphate 5%
Maleic anhydride/acrylic copolymer (MW3000) 2%
Epoxidized soybean oil 5%
Water to 100%
Example of formulations 5:10% carbosulfan aqueous emulsion
Carbosulfan 10%
Toluene 5%
The tert-butyl alcohol 2%
Phenethyl phenol polyethenoxy ether phosphoric acid ester sodium 5%
Sodium Polyacrylate (MW6000) 2%
Epoxy linseed oil 3%
Silicon defoaming agent 1%
Water to 100%
Example of formulations 6:20% carbosulfan aqueous emulsion
Carbosulfan 20%
Dimethylbenzene 5%
Linolenic acid polyoxyethylene ether phosphate 5%
Sodium Polyacrylate (MW7000) 2%
Epoxidized soybean oil 3%
Silicon defoaming agent 1%
Water to 100%
Comparative formulations embodiment 1:20% carbosulfan missible oil
Carbosulfan 20%
Ethanol 10%
0P-21 10％
2201 10％
The newborn 500# 2% of farming
The dimethylbenzene surplus
The physicochemical property of carbosulfan aqueous emulsion of the present invention is:
Outward appearance: white stable emulsion;
Low-temperature stability: following 2 weeks layering, crystallization do not occur at 0 ℃;
Heat storage stability: storage lamination do not occur at 2 weeks under 54 ℃
Stability of emulsion: with the water-reducible emulsion-stabilizing of any ratio;
Ageing stability: can stablize under the normal temperature and store more than 2 years.
Below be the heat storage data of three samples of 20% carbosulfan aqueous emulsion of embodiment 6:
| Test event | The sample explanation | No. 1 sample | No. 2 samples | No. 3 samples |
| Effective content (%) | Before the heat storage | 20.10 | 20.09 | 20.11 |
| After the heat storage | 20.05 | 20.03 | 20.05 | |
| Degradation rate (%) | 0.25 | 0.30 | 0.30 | |
| PH value | Before the heat storage | 8.0 | 8.0 | 8.1 |
| After the heat storage | 7.9 | 7.8 | 7.9 | |
| Emulsion stability | Before the heat storage | Qualified | Qualified | Qualified |
| After the heat storage | Qualified | Qualified | Qualified | |
| Conclusion | Qualified | Qualified | Qualified |
Illustrate: hot storage condition is 54 ℃, stores test result after 14 days
As can be known from the table data: 20% carbosulfan aqueous emulsion has good product bin stability, and its performance meets the requirement that pesticide emulsion in water is stored index (the general requirement is＜5%) fully.
Though above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, not departing from the these modifications or improvements basically of spirit of the present invention, all belong to the scope of protection of present invention.
Claims (10)
1. carbosulfan aqueous emulsion, it comprises
1) carbosulfan of 1-40% by weight;
2) at least a phosphoric acid ester anion surfactant of 0.1-10% by weight as emulsifier;
3) at least a polyacrylic acid derivative of 0.1-10% by weight as dispersant;
4) at least a epoxies thing of 1-15% by weight as stabilizing agent.
2. aqueous emulsion according to claim 1, wherein
1) carbosulfan of 5-25% by weight;
2) at least a phosphoric acid ester anion surfactant of 1-10% by weight as emulsifier;
3) at least a polyacrylic acid derivative of 1-10% by weight as dispersant;
4) at least a epoxies thing of 2-15% by weight as stabilizing agent.
3. aqueous emulsion according to claim 1 and 2, wherein, the phosphoric acid ester anion surfactant is selected from aliphatic acid polyethenoxy ether phosphoric acid ester, alkyl or alkyl phenyl polyoxyethylene ether phosphate class, alkylphenol polyoxyethylene phosphoric acid ester and aralkyl phenol polyethenoxy ether phosphoric acid ester.
4. according to the aqueous emulsion of claim 3, wherein, the phosphoric acid ester anion surfactant is selected from C
8-C
24-alkyl or alkyl phenyl polyoxyethylene ether phosphate, C
8-C
18-alkylphenol-polyethenoxy mono phosphoric acid ester/dibasic acid esters, benzene alkylphenol polyoxyethylene phosphoric acid ester.
5. aqueous emulsion according to claim 1 and 2, wherein, the dispersant polyacrylic acid derivative is selected from polyacrylic acid, Sodium Polyacrylate, maleic anhydride/acrylic copolymer, acrylic acid/hydroxypropyl acrylate copolymer, and molecular weight is 1000-10000.
6. aqueous emulsion according to claim 1 and 2, wherein, stabilizing agent is selected from epoxidised soybean oil, epoxidized linseed, epoxidation castor oil and epoxychloropropane.
7. aqueous emulsion according to claim 1 wherein, also contains the cosolvent of 0.1-5%.
8. according to the aqueous emulsion of claim 7, wherein, cosolvent is an arene.
9. according to claim 1 or 7 described aqueous emulsions, wherein, also contain antifreezing agent, suspending agent, bactericide and defoamer.
10. according to the aqueous emulsion of claim 9, wherein, antifreezing agent is C
1-C
4-lower aliphatic alcohols.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03122177 CN1220432C (en) | 2002-12-17 | 2003-04-23 | Aqueous carbosulfan emulsion and preparing method thereof |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN02155698 | 2002-12-17 | ||
| CN02155698.9 | 2002-12-17 | ||
| CN 03122177 CN1220432C (en) | 2002-12-17 | 2003-04-23 | Aqueous carbosulfan emulsion and preparing method thereof |
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| CN1451276A CN1451276A (en) | 2003-10-29 |
| CN1220432C true CN1220432C (en) | 2005-09-28 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 03122177 Expired - Lifetime CN1220432C (en) | 2002-12-17 | 2003-04-23 | Aqueous carbosulfan emulsion and preparing method thereof |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BRPI0500857A (en) * | 2005-03-09 | 2006-11-14 | Fmc Quimica Do Brasil Ltda | Carbosulfan-based pesticide compositions, process for their preparation, process for insect / mite / nematode control as well as use of said compositions |
| CN100464636C (en) * | 2005-09-22 | 2009-03-04 | 湖南化工研究院 | Aqueous emulsion of pesticides Bassa, carbosulfan, phosphor methylpyrimidine, and preparation method |
| CN102258014A (en) * | 2011-05-17 | 2011-11-30 | 广西田园生化股份有限公司 | Quinalphos emulsion in water and preparation method thereof |
| CN102283251B (en) * | 2011-07-04 | 2013-03-13 | 朱晓鸣 | Agricultural sterilization solution |
| CN103300029A (en) * | 2012-03-12 | 2013-09-18 | 刘勤学 | Emamectin benzoate-carbosulfan emulsion in water and application of same in prevention and treatment of Meloidogyne incognita |
| CN106472498B (en) * | 2016-08-31 | 2019-12-03 | 湖南海利化工股份有限公司 | A kind of compound stabilizer and the preparation method and application thereof for carbofuran derivative |
| WO2024032778A1 (en) * | 2022-08-12 | 2024-02-15 | Adama Makhteshim Ltd. | Liquid pesticidal composition |
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