CN1703957A - Cis form cypermethrin micellar emulsion and its production method - Google Patents
Cis form cypermethrin micellar emulsion and its production method Download PDFInfo
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- CN1703957A CN1703957A CN 200410046020 CN200410046020A CN1703957A CN 1703957 A CN1703957 A CN 1703957A CN 200410046020 CN200410046020 CN 200410046020 CN 200410046020 A CN200410046020 A CN 200410046020A CN 1703957 A CN1703957 A CN 1703957A
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- cypermethrin
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Abstract
The invention provides a cis-form cypermethrin micellar emulsion and its production method, wherein the constituents include (by weight percentage) alphamethrin 1-10%, auxiliary solvent 1-20%, emulsifying agent 5-20%, stabilizing agent 0-10%, water 40-70%.
Description
Technical field
The invention belongs to the pesticide producing field, be specially a kind of alpha-cypermethrin micro emulsion formulation agent and production method thereof.
Background technology
For a long time, along with being extensive use of of chemical pesticide, to the pollution that how to reduce environment with to people and animals' murder by poisoning, more and more cause people's attention, reducing toxicity, improving drug effect is that agricultural chemicals development institute becomes.At present, China is relatively backward aspect formulations of pesticide development and exploitation, is example with missible oil and wetting powder, and its consumption accounts for 70～80% of total amount of formulation; And formulation is more single, and the ratio of former medicine and preparation is 1: 6, then about 1: 30 of developed country, and both fall far short.Obviously, this can not adapt to current agricultural production development far away, and especially the agricultural product structural adjustment can influence the marketing and the service life of Pesticidal products to a great extent to the variation of agricultural chemicals demand.Because the formulations of pesticide are single, operation technique also lags behind level of developed countries.By the transformation of formulation,, also remedied the deficiency of former medicine development ability simultaneously to adapt to the requirement of sustainable development.
The comparatively convenient liquid formulation generally that reaches in the use of pesticidal preparations.For a long time, the use of chemical pesticide, using maximum is cream preparation.In processing missible oil process, need to produce and use a large amount of organic solvents, as benzene,toluene,xylene or the like, the use of a large amount of organic solvents not only causes the waste of industrial chemicals, and since the combustibility of solvent on transportation, storage and container selection, also be restricted.Simultaneously, brought very big murder by poisoning for environment and human health, economic development and environment for human survival that will crisis country.Developed country limits or forbids using in a large number the pesticide new variety registration of toxic organic solvent preparations such as benzene,toluene,xylene from sustainable development target.Therefore, develop novel liquid formulation, become the trend of the times of agricultural chemicals development to reduce or to get rid of these virulent organic solvents.Wherein, Water-borne modification is exactly one of dominant direction of formulations of pesticide development.And, the novel form of agricultural chemicals also can increase new feature to agricultural chemicals, more can give full play to the action characteristic of former medicine self, overcome and remedy the deficiency of the original formulation of agricultural chemicals, toxicity and excitant to people and animals are all lower, and can alleviate the poisoning to crop, improve physico chemistry and biological property, enlarge range of application, prolong the service life of medicament etc.
Microemulsion (Microemulsion), international code name: the ME of formulation is made up of water, water-insoluble and water-soluble substance, and former medicine is with the microparticulate preparation wherein of 0.01～0.1 μ.It is a stable homogeneous phase solubility system on the thermodynamics, and outward appearance is transparence, and microcosmic is to be the limiting condition that aqueous emulsion fully disperses for the big micellar dispersion that expands.Its physics, chemical stability are good, and is strong to plant and insect tissue cell permeability, the absorption ratio height, and preventive effect is good, simultaneously, has production, storing and safe in utilization, and environmental pollution is little, helps the improvement of ecotope.
Alpha-cypermethrin [english common name Alpha-cypermethrin, chemical name is: (1R)-and cis-2,2-dimethyl-3-(2, the 2-dichloroethylene) cyclopropane-carboxylic acid-(S)-a-cyano group-3-phenoxy group benzyl ester/(1S)-cis-2,2-dimethyl-3-(2, the 2-dichloroethylene) cyclopropane-carboxylic acid---(R)-a-cyano group-3-phenoxy group benzyl ester (mixture), chemical molecular formula: C
22H
19C
12NO
3, CAS registration number 86753-92-6, outward appearance: white is to cream-colored crystalline solid, other title: efficiently going out hundred can (Fastac), efficiently pacifies green treasured (Bestox), struggle (Fendona)].It is made up of the efficient isomer of cypermethrin, its activity is about cypermethrin 1-3 doubly, so the unit are consumption still less, and effect is stronger, its scope of application, controlling object, handling characteristics, the mechanism of action are identical with cypermethrin, are a kind of excellent insecticide.
The alpha-cypermethrin formulation of domestic production has missible oil, wetting powder and suspending agent abroad based on missible oil.Do not find the report of the relevant alpha-cypermethrin microemulsion in home and abroad as yet, we utilize this formulation is the characteristics of matrix with water, have also simultaneously that effective rate of utilization height, product stability are good, production, storing and safe in utilization, environmental pollution is little, helps the advantages such as improvement of ecotope.Through composite formation, thereby realization improves the performance of product.
The object of the invention is to provide a kind of alpha-cypermethrin microemulsion and production method thereof, makes the effective ingredient particle ultra tiny, crop and target insect adhesive force are improved, and penetration power enhancing, particularly antagonism insect, insecticidal effect obviously improves.Farthest reduce the pollution of agricultural chemicals to environment, and the physical and chemical stability that improves medicament, the service life of prolongation medicament.
It is solvent that the technology of the present invention advance is with water, and O/W is formed thermodynamic stable system, its appearance transparent, and effective ingredient is distributed between 10～70nm.Show following characteristics: Environmental compatibility is good, activity is high, safety is good, market capacity is big.
Summary of the invention
The purpose of this invention is to provide a kind of alpha-cypermethrin microemulsion and production method thereof, particular content is as follows:
Alpha-cypermethrin microemulsion of the present invention is made up of the former medicine of alpha-cypermethrin, cosolvent, emulsifier, stabilizing agent and water, and wherein the percentage by weight of various components is:
Alpha-cypermethrin 1～10%
Cosolvent 1～20%
Emulsifier 5～20%
Stabilizing agent 0～10%
Water 40～70%
Wherein the stabilizing agent amount of being preferably 1～10%.
Among the present invention, cosolvent is meant alcohols (as ethanol, isopropyl alcohol, n-butanol, n-amyl alcohol, hexanol etc.), ketone (as acetone, cyclohexanone etc.), amide-type (as dimethyl formamide etc.), naphthenic (as cyclohexane etc.), aromatic hydrocarbons (as benzene,toluene,xylene, Fluhyzon etc.), also can be to well known to a person skilled in the art other cosolvent.Cosolvent can be any one or two or more combination wherein.Preferred cosolvent is selected from ethanol, isopropyl alcohol, n-butanol, n-amyl alcohol, acetone, cyclohexanone, dimethyl formamide, cyclohexane, benzene, toluene and dimethylbenzene.
Among the present invention, emulsifier is meant non-ionic surface active agent and/or anion surfactant.The non-ionic surface active agent that can adopt is for example castor oil ethylene oxide adduct, phenethyl phenol polyethenoxy ether, phenethyl phenol polyethenoxy polyethenoxy ether, phenethyl phenol polyethenoxy ether phosphate, alkylphenol polyoxyethylene formaldehyde condensation products, benzylbiphenyl phenol polyethenoxy ether, alkylphenol polyoxyethylene, xenol APEO etc.The anion surfactant that can adopt be for example alkylbenzenesulfonate (as C
10-C
14-alkyl benzene calcium sulfonate, magnesium, sodium salt), C
8-C
20-alkylsurfuric acid sodium salt (as lauryl sodium sulfate salt), styrene polyoxyethylene ether ammonium sulfate salt etc.Preferably, the compound of non-ionic surface active agent and anion surfactant.When the present invention specifically implements, preferably adopt commercially available various emulsifier types, for example, emulsifier can be selected from No. 500, farming breast, agricultural emulsifier NO series (as the newborn 601-606 of farming number), Nongru-700 series is (as peaceful newborn No. 36, No. 37, peaceful breast, Nongru-700-1,700-2, the newborn SPF of farming), NP-10, No. 1600 series of farming breast are (as farming breast 1601,1602, peaceful breast 33, No. 34), No. 2000, farming breast, No. 11, farming breast, No. 12, farming breast, PF-690, BY series is (as peaceful newborn 110,120,130,140, the EL emulsifier), tween series is (as Tween-40, Tween-60, Tween-80), Sorpol series (Sorpol KS, Sorpol KD, Sorpol-2676, Sorpol-2678S etc.) or have any one or two or more combinations in the emulsifier of similar features.
Can also contain stabilizing agent in case of necessity in the microemulsion of the present invention, be used to increase the physics and the chemical stability of microemulsion.Accord with stabilizing agent of the present invention and be for example 2-expoxy propane, butyl glycidyl ether, polyethylene glycol diglycidyl ether or sorbierite, isopropyl alcohol, n-butanol, ethylene glycol, polyethylene glycol, urea, propane diols, glycerine, turpentine oil and well known to a person skilled in the art in the stabilizing agent any one.Preferably ethylene glycol, polyethylene glycol, glycerine, turpentine oil and urea, this class stabilizing agent has the dual function of stabilizing agent and antifreezing agent.Its consumption is 1-10%.
The water that adopts among the present invention can be running water, deionized water etc., preferably deionized water such as distilled water.
The present invention also comprises the preparation method of microemulsion of the present invention, these method process following steps,
A. the former medicine of alpha-cypermethrin is dissolved in the cosolvent;
B. add emulsifier, water adds stabilizing agent in case of necessity;
C. mix.
Below be one of adoptable method:
The former medicine of alpha-cypermethrin is dissolved in the cosolvent, drops into emulsifier, stir, put into then and mix strongly in the homogenizer that dispersion medium water is housed and homogenize, promptly get the agent of littleization of alpha-cypermethrin.
Also can adopt following method:
The former medicine of alpha-cypermethrin is dissolved in the cosolvent, drops into emulsifier, drop into stabilizing agent again, stir, put into then and mix strongly in the homogenizer that dispersion medium water is housed and homogenize, promptly get the agent of littleization of alpha-cypermethrin.
Littleization of alpha-cypermethrin of the present invention agent farthest reduces the use of organic solvent, and has synergistic effect, thereby improves the effective availability of former medicine, can reduce the pollution of agricultural chemicals to environment, improves safety in utilization; Simultaneously, the present invention has improved the medicament storage-stable, and to adhesiveness and the permeability of plant, to insect preventive effect height, the lasting period is long, and is for optimization formula of the present invention, all the more so.
Embodiment
Further specify the present invention by the following examples, but not as limitation of the present invention.
Embodiment 1: 50 kilograms of alpha-cypermethrins are dissolved in 60 kilograms of dimethylbenzene, drop into 40 kilograms of farming breasts 500 again
#, 40 kilogram 690
#With 40 kilogram 790
#, stir, drop into then and be equipped with in 770 kilograms of dispersion medium water, give homogenizer and be mixed to transparent strongly.Promptly get 1000 kilogram of 4.5% alpha-cypermethrin microemulsion.
Its middle peasant's breast 500
#, 690
#, 790
#Be alkyl benzene calcium sulfonate, phenol derivatives ethoxylate, first the contract code name of nonyl phenol ethoxylate material, buy from chemical plant, Lvshun, Dalian
Embodiment 2: with the 4.5% alpha-cypermethrin microemulsion that the embodiment of the invention 1 is prepared the Toxicity Determination of diamond-back moth is tested.
Experimental pharmacy:
4.5% alpha-cypermethrin missible oil Tianjin dragon lantern chemical industry Co., Ltd production commercially available prod
4.5% alpha-cypermethrin microemulsion example of formulations 1 of the present invention
Adopt the test of pesticide effectiveness of 4.5% alpha-cypermethrin microemulsion of the embodiment of the invention 1, the blade medicine embrane method is adopted in this test, the fresh cabbage blade of not used agricultural chemicals (oneself cultivation) is dipped in 10s in the insecticide solution of series concentration respectively, taking-up is dried in the shade and is placed in the 9cm plastic culture dish, every ware inserts 10 of diamond-back moth third-instar larvaes, and each concentration is established three repetitions.Check statistics behind the 24h, calculate LC
50Experimental result:
4.5% alpha-cypermethrin microemulsion Toxicity Determination result
| The medicament title | The regression equation slope | ??LC 50??(mg/L) | 95% confidence limit (mg/L) | Variance analysis |
| Missible oil | ??1.116±0.258 | ??7.267 | ??3.549-12.033 | ??A |
| Microemulsion | ??1.492±0.323 | ??6.96 | ??3.814-10.930 | ??A |
Embodiment 3: the aphid on the 4.5% alpha-cypermethrin microemulsion control vegetables of preparing with the embodiment of the invention 1, prevent and treat method and the result is as follows.
Experimental pharmacy:
4.5% alpha-cypermethrin missible oil Tianjin dragon lantern chemical industry Co., Ltd production commercially available prod
4.5% alpha-cypermethrin missible oil Germany BASF AG production commercially available prod
4.5% alpha-cypermethrin microemulsion example of formulations 1 of the present invention
The above-mentioned microemulsion product that adopts the embodiment of the invention 1 to prepare, this EXPERIMENTAL EXAMPLE are the field efficacy experiments at aphid.Triplicate of every processing, the repetition in every sub-district is adopted district's group arrangement at random, sub-district area 20M
2, adopt knapsack sprayer to carry out conventional spray, handled respectively back 1 day, 7 days investigation aphid larva quantity, the result is as follows:
The anti-field control effectiveness test result that eliminates aphis of 4.5% alpha-cypermethrin microemulsion
| Handle | Worm radix (head) | One day | Three days | Seven days | ||||||
| Borer population (head) alive | The rate that goes down (%) | Proofread and correct preventive effect (%) | Borer population (head) alive | The rate that goes down (%) | Proofread and correct preventive effect (%) | Borer population (head) alive | The rate that goes down (%) | Proofread and correct preventive effect (%) | ||
| Missible oil 30ml/ mu | ??1117 | ??316 | ??71.71 | ??76.84a ??A | ??207 | ??81.47 | ??87.40a ??A | ??198 | ??82.27 | ??90.18ab ??A |
| Microemulsion 20ml/ mu | ??1152 | ??372 | ??67.71 | ??73.57a ??A | ??225 | ??80.47 | ??86.73a ??A | ??260 | ??77.43 | ??87.50ab ??A |
| Microemulsion 30ml/ mu | ??798 | ??142 | ??82.21 | ??85.44a ??A | ??87 | ??89.10 | ??92.59a ??A | ??85 | ??89.35 | ??94.10a ??A |
| Missible oil 30ml/ mu | ??687 | ??171 | ??75.11 | ??79.63a ??A | ??110 | ??83.99 | ??89.12a ??A | ??124 | ??81.95 | ??90.00ab ??A |
| ??CK | ??1222 | ??1493 | ??-22.18 | ??- | ??1798 | ??-47.14 | ??- | ??2206 | ??-80.52 | |
Poisoning does not take place in for examination concentration.
Embodiment 4: the particle size distribution range of the 4.5% alpha-cypermethrin microemulsion of preparing with the embodiment of the invention 1, the result is as follows.
The above-mentioned microemulsion product that adopts the embodiment of the invention 1 to prepare, particle size distribution range are measured and are adopted transmission electron microscope (TEM) and laser particle size analysis method, and the present invention is carried out grain size analysis, and analysis result is as follows:
| Method name | Granularity (nm) |
| Transmission electron microscope | ??50 |
| Laser particle size analysis | ??20～70 |
Embodiment 5: the test of the performance of the 4.5% alpha-cypermethrin microemulsion of preparing with the embodiment of the invention 1.
The above-mentioned microemulsion product that adopts the embodiment of the invention 1 to prepare, quality meets following technical indicator after tested:
| Index name | Index |
| Alpha-cypermethrin content (%m/m) (20 ℃) | ??≥4.5 |
| The pH value | ??6.0-7.0 |
| Stability of emulsion (diluting 200 times) | Qualified |
| Low-temperature stability (0 ± 2 ℃) | Qualified |
| Heat storage stability (54 ± 2 ℃) | Qualified |
| Transparency temperature scope (0-50 ℃) | Qualified |
Annotate: low-temperature stability and heat storage stability test, carried out once at least in per 3 months
Embodiment 6: the 4.5% alpha-cypermethrin microemulsion of producing with the embodiment of the invention 1 dilutes 2000 times, the 3000 times poisoning of observing down various vegetables and other field crops, the result shows that this medicine to spinach, wild cabbage, leaf mustard, cabbage mustard, logical dish, cowpea, cucumber, tomato, capsicum, leek, green onion, beet, fruit tree, cotton etc. poisoning does not take place all, and is safe in utilization on these crops.
Claims (7)
1, a kind of alpha-cypermethrin microemulsion is characterized in that being made up of the former medicine of alpha-cypermethrin, cosolvent, emulsifier and water, and wherein the percentage by weight of various components is:
Alpha-cypermethrin 1～10%
Cosolvent 1～20%
Emulsifier 5～20%
Water 50～70%.
2, alpha-cypermethrin microemulsion according to claim 1, wherein, it also contains stabilizing agent, and the percentage by weight of each component is as follows
Alpha-cypermethrin 1～10%
Cosolvent 1～20%
Emulsifier 5～20%
Stabilizing agent 1～10%
Water 40～60%.
3, claim 1,2 alpha-cypermethrin microemulsion, wherein cosolvent is selected from ethanol, isopropyl alcohol, n-butanol, n-amyl alcohol, hexanol, acetone, cyclohexanone, dimethyl formamide, cyclohexane, benzene,toluene,xylene, Fluhyzon.
4, claim 1,2 alpha-cypermethrin microemulsion, wherein emulsifier is selected from castor oil ethylene oxide adduct, phenethyl phenol polyethenoxy ether, phenethyl phenol polyethenoxy polyethenoxy ether, phenethyl phenol polyethenoxy ether phosphate, alkylphenol polyoxyethylene formaldehyde condensation products, benzylbiphenyl phenol polyethenoxy ether, alkylphenol polyoxyethylene, xenol APEO, alkylbenzenesulfonate, C
8-C
20-alkylsurfuric acid sodium salt, styrene polyoxyethylene ether ammonium sulfate salt.
5, claim 1,2 alpha-cypermethrin microemulsion, wherein stabilizing agent is selected from 2-expoxy propane, butyl glycidyl ether, polyethylene glycol diglycidyl ether, sorbierite, isopropyl alcohol, n-butanol, ethylene glycol, polyethylene glycol, urea, propane diols, glycerine, turpentine oil.
6, according to the production method of claim 1,2 described alpha-cypermethrin microemulsions, it is characterized in that the former medicine of alpha-cypermethrin is dissolved in the cosolvent, drop into remaining processing auxiliary element, stir, put into then and mix strongly in the homogenizer that dispersion medium water is housed and homogenize, promptly get the agent of littleization of alpha-cypermethrin.
7, the production method of alpha-cypermethrin microemulsion according to claim 6 is characterized in that the present invention can be used for producing the binary or the ternary built microemulsion of alpha-cypermethrin and other insecticide, bactericide, weed killer herbicide and plant growth regulator.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410046020 CN1703957A (en) | 2004-06-01 | 2004-06-01 | Cis form cypermethrin micellar emulsion and its production method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410046020 CN1703957A (en) | 2004-06-01 | 2004-06-01 | Cis form cypermethrin micellar emulsion and its production method |
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|---|---|
| CN1703957A true CN1703957A (en) | 2005-12-07 |
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ID=35575605
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|---|---|---|---|
| CN 200410046020 Pending CN1703957A (en) | 2004-06-01 | 2004-06-01 | Cis form cypermethrin micellar emulsion and its production method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101828547A (en) * | 2010-05-21 | 2010-09-15 | 扬州大学 | Cypermethrin biological pesticide microemulsion |
| CN109984140A (en) * | 2017-12-31 | 2019-07-09 | 海南正业中农高科股份有限公司 | Microemulsion containing S-Ethyl ethylthio sulfonate and hymexazol |
-
2004
- 2004-06-01 CN CN 200410046020 patent/CN1703957A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101828547A (en) * | 2010-05-21 | 2010-09-15 | 扬州大学 | Cypermethrin biological pesticide microemulsion |
| CN109984140A (en) * | 2017-12-31 | 2019-07-09 | 海南正业中农高科股份有限公司 | Microemulsion containing S-Ethyl ethylthio sulfonate and hymexazol |
| CN109984140B (en) * | 2017-12-31 | 2024-01-09 | 海南正业生物科技股份有限公司 | Microemulsion containing ethylicin and hymexazol |
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