CN1611115A - Lamda-cyhalothrin micro emulsion and its production method - Google Patents
Lamda-cyhalothrin micro emulsion and its production method Download PDFInfo
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- CN1611115A CN1611115A CN 200310101645 CN200310101645A CN1611115A CN 1611115 A CN1611115 A CN 1611115A CN 200310101645 CN200310101645 CN 200310101645 CN 200310101645 A CN200310101645 A CN 200310101645A CN 1611115 A CN1611115 A CN 1611115A
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- gamma cyhalothrin
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Abstract
The present invention provides a method for producing high-effective cyfluthrin microemulsion by utilizing compounding technique. Said invention is aimed at maximally raising pesticide effect of high-effective cyfluthrin microemulsion and reducing use of organic solvent so as to reduce the contamination of pesticide to environment and raise the utilization rate and safety of product. Said invented microemulsion is prepared by using high-effective cyfluthrin, cosolvent, emulsifier and water.
Description
Technical field the invention belongs to the pesticide producing field, is specially a kind of gamma cyhalothrin micro emulsion formulation agent and production method thereof.
Background technology 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 causes people's attention for a long time, and 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.
(english common name Lambda-cyhalothrin, chemical name is gamma cyhalothrin: 3-(2-chloro-3,3,3-fluoro-1-acrylic)-2,2-dimethyl ethylene-acetic acid cyano group (3-Phenoxyphenyl) methyl esters, chemical molecular formula: C
23H
19ClF
3NO
3, other title: Cyhalothrin, cyhalothrin) and be a kind of insecticide of pyrethroid, former medicine is white or beige solid.This insecticide insecticidal spectrum is wide, drug effect is rapid, can be used for preventing and treating insects such as cotton bollworm, cotten aphid, diamond-back moth, cabbage caterpillar, apple leaf miner.Its insecticidal effect is remarkable, and residual life is short, have efficient, tag and characteristics such as stomach toxicity.Wherein action of contace poison is rapid, and the power of knocking down is strong, and is efficient especially to lepidopterous larvae, is a kind of excellent insecticide.
Gamma cyhalothrin is to foretell inside door company by Britain to be developed in 1985, is that first uses the pyrethroid on agricultural in the world, and it also is one of insecticide of Zeneca sales volume maximum.This medical instrument has dosage low, and the leaf-feeding insect in the wide range is had characteristics such as efficient.It also uses in public health with the Icon trade name, or first prevents and treats the insecticide of malaria and other tropical diseases by World Health Organization's evaluation permission.
The gamma cyhalothrin formulation of domestic production is based on missible oil and wetting powder, do not find the report of the relevant gamma cyhalothrin microemulsion in home and abroad as yet, we utilize easily by plant absorbing, functional group is many, physiologically active is big, complexing power is strong, can be directly water-soluble and the characteristics such as adhesive attraction of colloidality, through composite formation, thereby realization improves the drug effect purpose of product.
The object of the invention is to provide a kind of gamma cyhalothrin 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 invention reside in provides a kind of gamma cyhalothrin microemulsion and production method thereof, farthest reduces the use of organic solvent, and synergistic effect is remarkable, thereby reduces 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.Particular content is as follows:
The gamma cyhalothrin microemulsion is made up of the former medicine of gamma cyhalothrin, cosolvent, emulsifier and water, and wherein the percentage by weight of various components is:
Gamma cyhalothrin 1~10%
Cosolvent 1~20%
Emulsifier 5~20%
Water 30~70%
Cosolvent described in the above-mentioned gamma cyhalothrin microemulsion is any one or the two or more combination in dimethyl formamide, ethanol, isopropyl alcohol, n-butanol, n-amyl alcohol, acetone, cyclohexanone, aromatic hydrocarbons and those skilled in the art cosolvent of generally acknowledging.
Emulsifier described in the above-mentioned gamma cyhalothrin microemulsion is a farming breast 500
#, 600
#, 700
#, NP-10,1601
#, 2000
#, PF-690, BY-130, tween-120,11
#Or have any one or two or more combinations in the material of similar features.
Above-mentioned gamma cyhalothrin microemulsion is characterized in that containing stabilizing agent, and purpose is physics and the chemical stability that increases microemulsion, and wherein the percentage by weight of various components is:
Gamma cyhalothrin 1~10%
Cosolvent 1~20%
Emulsifier 5~20%
Stabilizing agent 5~10%
Water 30~80%
The above-mentioned described stabilizing agent of gamma cyhalothrin microemulsion is ethylene glycol, polyethylene glycol, urea, glycerine and well known to a person skilled in the art any one of stabilizing agent.
The production method of specific implementation method gamma cyhalothrin microemulsion, it is characterized in that the former medicine of gamma cyhalothrin is dissolved in the cosolvent, drop 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 gamma cyhalothrin.
The production method of above-mentioned gamma cyhalothrin microemulsion, it is characterized in that the former medicine of gamma cyhalothrin is dissolved in the cosolvent, drop 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 gamma cyhalothrin.
Embodiment one: 25 kilograms of gamma cyhalothrins are dissolved in 20 kilograms of dimethylbenzene, drop into 10 kilograms of farming breasts 500 again
#With 40 kilogram 700
#, stir, drop into then and be equipped with in 905 kilograms of dispersion medium water, give homogenizer and be mixed to transparent strongly.Promptly get 1000 kilogram of 2.5% gamma cyhalothrin microemulsion.
Embodiment two: with the 2.5% gamma cyhalothrin microemulsion that the embodiment of the invention one is prepared the Toxicity Determination of diamond-back moth is tested, see EXPERIMENTAL EXAMPLE one.
Embodiment three: the aphid on the 2.5% gamma cyhalothrin microemulsion control vegetables of preparing with the embodiment of the invention one, prevent and treat method and the results are shown in EXPERIMENTAL EXAMPLE two.
Embodiment four: the particle size distribution range of the 2.5% gamma cyhalothrin microemulsion of preparing with the embodiment of the invention one, see EXPERIMENTAL EXAMPLE three.
Embodiment five: the test of the performance of the 2.5% gamma cyhalothrin microemulsion of preparing with the embodiment of the invention one, see EXPERIMENTAL EXAMPLE four.
Embodiment six: the 2.5% gamma cyhalothrin microemulsion of producing with the embodiment of the invention one 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.
EXPERIMENTAL EXAMPLE one: the present invention's 2.5% gamma cyhalothrin microemulsion is to the Toxicity Determination experiment of diamond-back moth
Experimental pharmacy:
2.5% efficient cyhalothrin emulsifiable concentrate Syngenta Co.,Ltd production commercially available prod
2.5% gamma cyhalothrin microemulsion example of formulations one of the present invention
Adopt the test of pesticide effectiveness of 2.5% gamma cyhalothrin microemulsion of the embodiment of the invention one, 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:
2.5% gamma cyhalothrin 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 |
EXPERIMENTAL EXAMPLE two: the anti-field control effectiveness test that eliminates aphis of the present invention's 2.5% gamma cyhalothrin microemulsion.
Experimental pharmacy:
2.5% efficient cyhalothrin emulsifiable concentrate Jiangsu hormone study institute production commercially available prod
2.5% gamma cyhalothrin aqueous emulsion Switzerland Syngenta Co.,Ltd production commercially available prod
2.5% gamma cyhalothrin microemulsion example of formulations one of the present invention
The above-mentioned microemulsion product that adopts the embodiment of the invention one 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, to handle respectively back 1 day, 7 days investigation aphid larva quantity is calculated as follows control efficiency:
Ta: insect population quantity after the treatment region dispenser
Tb: insect population quantity before the treatment region dispenser
Ca: insect population quantity after the treatment region dispenser
Cb: insect population quantity before the treatment region dispenser
The anti-field control effectiveness test result that eliminates aphis of 2.5% gamma cyhalothrin 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 |
Aqueous emulsion 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.
EXPERIMENTAL EXAMPLE three: the particle size distribution range of the present invention's 2.5% gamma cyhalothrin microemulsion
The above-mentioned microemulsion product that adopts the embodiment of the invention one 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 | ????20~80 |
EXPERIMENTAL EXAMPLE four: the test of the performance of the present invention's 2.5% gamma cyhalothrin microemulsion
The above-mentioned microemulsion product that adopts the embodiment of the invention one to prepare, quality meets following technical indicator after tested:
Index name | Index |
Gamma cyhalothrin content (%m/m) (20 ℃) | ????≥2.5 |
The pH value | ????5.0-7.0 |
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 |
Claims (10)
1, a kind of gamma cyhalothrin microemulsion is characterized in that being made up of the former medicine of gamma cyhalothrin, cosolvent, emulsifier and water, and wherein the percentage by weight of various components is:
Gamma cyhalothrin 1~10%
Cosolvent 1~20%
Emulsifier 5~20%
Water 30~70%
2, gamma cyhalothrin microemulsion according to claim 1 is characterized in that described cosolvent is meant dimethyl formamide, ethanol, isopropyl alcohol, n-butanol, n-amyl alcohol, acetone, cyclohexanone, aromatic hydrocarbons or has any one or two or more combinations in the material of similar features.
3, gamma cyhalothrin microemulsion according to claim 1 is characterized in that described emulsifier is meant 500
#, 600
#, 700
#, NP-10,1601
#, 2000
#, PF-690, BY-130, tween-120,11
#Or has in the material of similar features one or more a combination.
4, gamma cyhalothrin microemulsion according to claim 1 is characterized in that described stabilizing agent is any one among ethylene glycol, polyethylene glycol, urea, glycerine or the material with similar features.
5, gamma cyhalothrin microemulsion according to claim 1 is characterized in that being made up of the former medicine of gamma cyhalothrin, nano assistant, cosolvent, emulsifier and water, and wherein the percentage by weight of various components is:
Efficient cyhalothrin 1~10%
Cosolvent 1~20%
Emulsifier 5~20%
Stabilizing agent 5~10%
Water 30~60%
6, gamma cyhalothrin microemulsion according to claim 5 is characterized in that described stabilizing agent is any one among ethylene glycol, polyethylene glycol, urea, glycerine or the material with similar features.
7, gamma cyhalothrin microemulsion according to claim 5 is characterized in that described cosolvent is meant dimethyl formamide, ethanol, isopropyl alcohol, n-butanol, n-amyl alcohol, acetone, cyclohexanone, aromatic hydrocarbons or has any one or two or more combinations in the material of similar features.
8, the production method of gamma cyhalothrin microemulsion according to claim 1, it is characterized in that the former medicine of gamma cyhalothrin is dissolved in the cosolvent, drop into emulsifier, stir, put into then and mix strongly in the homogenizer that dispersion medium water is housed and homogenize, promptly get the gamma cyhalothrin microemulsion.
9, the production method of gamma cyhalothrin microemulsion according to claim 5, it is characterized in that the former medicine of gamma cyhalothrin is dissolved in the cosolvent, drop 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 gamma cyhalothrin microemulsion.
10, according to Claim 8 or the production method of 9 described gamma cyhalothrin microemulsions, it is characterized in that the present invention can be used for producing the binary or the ternary built microemulsion of gamma cyhalothrin and other insecticide, bactericide, weed killer herbicide and plant growth regulator.
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103053601A (en) * | 2013-01-06 | 2013-04-24 | 中国检验检疫科学研究院 | Nano-grade hygienic insecticide and preparation method thereof |
CN101632353B (en) * | 2009-08-18 | 2013-06-26 | 青岛星牌作物科学有限公司 | Sodium dodecyl benzene sulfonate aqueous solution and preparation method thereof and application thereof |
CN103563966A (en) * | 2013-11-14 | 2014-02-12 | 河南牧翔动物药业有限公司 | Lambda-cyhalothrin nanoemulsion and preparation method thereof |
CN104542690A (en) * | 2014-12-17 | 2015-04-29 | 天津市华宇农药有限公司 | Lambda-cyhalothrin emulsifiable granule and preparation method and application thereof |
CN105028493A (en) * | 2015-08-06 | 2015-11-11 | 丁德凤 | Pesticide |
CN105284791A (en) * | 2014-10-12 | 2016-02-03 | 安徽迪邦药业有限公司 | Insecticide preparation method |
CN109432077A (en) * | 2018-11-22 | 2019-03-08 | 新疆畜牧科学院兽医研究所(新疆畜牧科学院动物临床医学研究中心) | A kind of long-acting composition of medicine for killing livestock and poultry epizoon that solvent pairs is prepared |
WO2021093268A1 (en) * | 2019-11-12 | 2021-05-20 | 南京华洲药业有限公司 | High-efficiency cyhalothrin nano aqueous solution, preparation method therefor and application thereof |
-
2003
- 2003-10-27 CN CN 200310101645 patent/CN1611115A/en active Pending
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101632353B (en) * | 2009-08-18 | 2013-06-26 | 青岛星牌作物科学有限公司 | Sodium dodecyl benzene sulfonate aqueous solution and preparation method thereof and application thereof |
CN103053601A (en) * | 2013-01-06 | 2013-04-24 | 中国检验检疫科学研究院 | Nano-grade hygienic insecticide and preparation method thereof |
CN103563966A (en) * | 2013-11-14 | 2014-02-12 | 河南牧翔动物药业有限公司 | Lambda-cyhalothrin nanoemulsion and preparation method thereof |
CN105284791A (en) * | 2014-10-12 | 2016-02-03 | 安徽迪邦药业有限公司 | Insecticide preparation method |
CN104542690A (en) * | 2014-12-17 | 2015-04-29 | 天津市华宇农药有限公司 | Lambda-cyhalothrin emulsifiable granule and preparation method and application thereof |
CN105028493A (en) * | 2015-08-06 | 2015-11-11 | 丁德凤 | Pesticide |
CN109432077A (en) * | 2018-11-22 | 2019-03-08 | 新疆畜牧科学院兽医研究所(新疆畜牧科学院动物临床医学研究中心) | A kind of long-acting composition of medicine for killing livestock and poultry epizoon that solvent pairs is prepared |
WO2021093268A1 (en) * | 2019-11-12 | 2021-05-20 | 南京华洲药业有限公司 | High-efficiency cyhalothrin nano aqueous solution, preparation method therefor and application thereof |
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