CN1530012A - Bromohydropyrethrin emulsion and production thereof - Google Patents
Bromohydropyrethrin emulsion and production thereof Download PDFInfo
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- CN1530012A CN1530012A CNA031193471A CN03119347A CN1530012A CN 1530012 A CN1530012 A CN 1530012A CN A031193471 A CNA031193471 A CN A031193471A CN 03119347 A CN03119347 A CN 03119347A CN 1530012 A CN1530012 A CN 1530012A
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- decis
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Abstract
A deltamethrin microemulsion is disclosed. Its preparing process features that the water instead of organic solvent and proper surfactant and assistant are used for decreasing its environmental pollution and a superfine emulsifying process is used for higher physical and chemical stability, dispersity and effect.
Description
Technical field
The invention belongs to the pesticide producing field, be specially decis micro-emulsion form and production method thereof.
Background technology
Decis has another name called FMC-45498, decis, dextrorotation along bromine nitrile phenothrin, triumphant security times spy, and English name is Decamethrin, K-othrin, Decis, Deltamethrin.Chemical formula: C
22H
19Br
2NO
3, molecular weight: 505.24, pure product are white crystal, tasteless.Decis was invented in 1980, belong to third generation pyrethroid insecticides, be put into state key new product planning in 2000, this product has desinsection wide spectrum, efficient, moderate toxicity, low-residual, hold imitate long, insecticidal action is fast, insecticidal activity is high, have extremely strong stomach toxicity and action of contace poison, tool to refuse the effect of keeping away.Can be widely used in various pests and sanitary insect pest on the crops such as control cotton, fruit tree, vegetables, tobacco, tealeaves.The whole world only has France, India and China to produce.The manufacturer of China has: Yangnong Chemical Co., Ltd., Jiangsu, big chemical industry Co., Ltd, Nanjing Sen Li auxiliary reagent factory, the Nanjing red sun group company etc. of reaching in Changzhou Tianjin.
Botanical pesticide aspect, natural chrysanthemum ester (pyrethrin) are one of successful examples of bionical transformation.The appearance of photostability permethrin makes the chrysanthemum ester come into field control, and is sign with the decis, makes insecticide enter the super-high-efficient epoch.The situation of residue of pesticide in the agricultural product more and more causes people's attention.Agricultural product are used any agricultural chemicals, become the focus that people pay close attention to day by day, and to this, agricultural sector investigates through prudent, and formal recommendation goes out the pesticide species that non-polluted farm product is used.These recommend pesticide species, mostly have characteristics such as efficient, low-residual, not only can kill the damage by disease and insect on the crops, and can reach the residue criterion of green agriculture, can relievedly use.Wherein, synthetic pesticide chrysanthemum ester class just comprises decis.
Along with the continuous propelling and the China joined WTO that realize the agricultural modernization process, use chemical pesticide to become the important means of guaranteeing agricultural foison.Agricultural chemicals can be retrieved the crop yield loss of 15%-30%, the more important thing is, to some disease pest and weeds, chemical control is still effectively preventing method so far.But chemical pesticide owing to reach irrational use for a long time, in a large number, has also caused the pollution to environment in its huge effect of performance.Some agricultural chemicals and solvent thereof can be trapped in for a long time it is constantly polluted atmosphere, water and soil earth.Because pollutant can pass through food chain, human beings'health and vegeto-animal growth are worked the mischief, therefore in science, reasonably utilize low-toxin farm chemicals in, also must development environmental type pesticidal preparations.Thereby under the prerequisite of guaranteeing the agricultural produce good harvest, can also keep good Agro-ecology balance.
China's pesticide original medicine output, preparation output occupy the second in the world, but the not enough world of agricultural chemicals annual sales amount agricultural chemicals total sales volume 8%.One of reason is the of poor quality of agricultural chemicals, is difficult to participate in intense market competition.On the formulation structure, states such as China missible oil ratio American and Britain, method are much higher, and they are much lower for the ratio of novel form, with external having a long way to go.
China's decis formulation is based on wetting powder, missible oil at present.The production of missible oil and use need a large amount of organic solvents, cause the waste of industrial chemicals.In addition, the use of solvent and emulsifier makes the cost up of pesticidal preparations, and missible oil is made troubles to transportation, packing, easily produces agricultural chemicals volatilization, seepage phenomenon, influences the quality and the drug effect of product.Addressing these problems, is the trend of development with the formulation Water-borne modification.
In the later stage eighties, the beginning of the nineties, China's formulations of pesticide had large development, and microemulsion and aqueous emulsion just progressively replace missible oil.And microemulsion is a kind of novel liquid formulation of developing in recent years, belong to a kind of of aqueous emulsion, it is medium with water, acts on water-fast effective active component by dispersion, emulsification etc., by homogenizing process it is dispersed in the water, forms thermodynamic stable system.Disperse phase is after homogenizing, and liquid-drop diameter is less than 100nm, so appearance transparent, physics, chemical stability are good, and is strong to plant and insect tissue cell permeability, the absorption ratio height, and preventive effect is good.Microemulsion replaces a large amount of organic solvents with water, reduces the waste and the pollution of solvent, reduces preparation toxicity, and the dispersity height has advantages such as not firing not quick-fried, storing and transporting security, is the most preferred dosage form that replaces missible oil, meets the developing direction of the formulations of pesticide in the world.
China's microemulsion kind in the market seldom, and is under test mostly.This mainly is because at present the microemulsion quality stability of preparation is poor, and complicated process of preparation, production cost height can't realize that factor such as industrialization causes.We are by screening and research to multiple solvent, emulsifier, preparation technology, the consumption of water reaches about 80%, replaced in the missible oil formulation a large amount of practical organic solvents, reduced the pollution of agricultural chemicals environment, through ultra micro refinement processing system each the microemulsion of steady quality, good drug efficacy.And preparation technology is simple, realizes industrialization easily.
The object of the invention is to provide a kind of decis 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
We are by screening and research to multiple solvent, emulsifier, preparation technology, replace a large amount of organic solvents with water, reduced the pollution of agricultural chemicals to environment, use suitable surfactant, auxiliary agent, decis microemulsion by ultra micro refinement processing and preparing, its physics, chemical stability are good, emulsifying dispersivity is strong, it is the environmental-pollution insecticide of a kind of efficient, wide spectrum, low toxicity, its drug effect is higher than domestic other similar preparation, safety is good and environmentally safe, preparation technology is simple, realizes industrialization easily.
The decis microemulsion is made up of decis, cosolvent, emulsifier and water, and wherein the percentage by weight of various components is:
Decis 1～10%
Cosolvent 1～20%
Emulsifier 5～20%
Water 30～80%
Cosolvent described in the above-mentioned decis microemulsion is any one or the two or more combination in dimethyl formamide, ethanol, isopropyl alcohol, n-butanol, n-amyl alcohol, acetone, cyclohexanone and those skilled in the art cosolvent of generally acknowledging.
Emulsifier described in the above-mentioned decis microemulsion is a farming breast 500
#, 600
#, 700
#, NP-10, PNP-10, EL-40,1601
#, 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 decis microemulsion is characterized in that containing synergist, and purpose is in order to improve control efficiency, and wherein the percentage by weight of each component is:
Decis 1～10%
Cosolvent 1～20%
Emulsifier 5～20%
Synergist 5～10%
Water 30～80%
The described synergist of above-mentioned decis microemulsion is that piperonyl butoxide, Octachlorodipropyl Ether, azone and those skilled in the art generally acknowledge any one of synergist.
Above-mentioned decis 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:
Decis 1～10%
Cosolvent 1～20%
Emulsifier 5～20%
Synergist 5～10%
Stabilizing agent 5～10%
Water 30～70%
The above-mentioned described stabilizing agent of decis microemulsion is ethylene glycol, polyethylene glycol, urea, glycerine and well known to a person skilled in the art any one of stabilizing agent.
Specific implementation method
The production method of decis microemulsion, it is characterized in that the former powder of decis 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 decis microemulsion.
The production method of above-mentioned decis microemulsion, it is characterized in that the former powder of decis is dissolved in the cosolvent, drop into emulsifier, drop into synergist and stabilizing agent again, stir, put into then and mix strongly in the homogenizer that dispersion medium water is housed and homogenize, promptly get the decis microemulsion.
Embodiment one: 25 kilograms of decises are dissolved in 100 kilograms of dimethylbenzene, drop into 40 kilograms of farming breasts 500 again
#With 30 kilogram 790
#, stir, drop into then and be equipped with in 805 kilograms of dispersion medium water, give homogenizer and be mixed to transparent strongly.Promptly get 1000 kilogram of 2.5% decis microemulsion.
Embodiment two: the 2.5% decis microemulsion of producing with the embodiment of the invention one becomes 5 concentration with reagent agent by the geometric ratio gradient dilution, adopt the cotton bollworm on the PetterShi spray tower standard measure spraying control cotton, verify its toxicity of tagging, prevent and treat method and the results are shown in EXPERIMENTAL EXAMPLE one.
Embodiment three: the 3000 times of cotton bollworms that prevent and treat down on the cotton of 2.5% decis microemulsion dilution with the embodiment of the invention one is produced, carry out field control effectiveness test with experimental technique two, and prevent and treat method and the results are shown in EXPERIMENTAL EXAMPLE two.
Embodiment four: the 2.5% decis microemulsion of producing with the embodiment of the invention one dilutes 3000 times, the 3500 times poisoning of observing down various vegetables, the result shows that this medicine to spinach, wild cabbage, leaf mustard, cabbage mustard, logical dish, cowpea, cucumber, tomato, capsicum, leek, green onion etc. poisoning does not take place all, and is safe in utilization on these crops.
EXPERIMENTAL EXAMPLE one: the test of pesticide effectiveness of the present invention's 2.5% decis microemulsion
Adopt the test of pesticide effectiveness of 2.5% decis microemulsion of the embodiment of the invention one, reagent agent is become 5 concentration by the geometric ratio gradient dilution, other establishes the clear water contrast.To for examination worm picking in culture dish, adopt the spraying of PetterShi spray tower standard measure, every ware 1mL.With blotting paper inhale remove unnecessary soup after, every cephalont singly is placed in the foster scolite that fills artificial feeding, adds a cover tampon.At 25 ± 1 ℃, under the artificial supplementation illumination 14 hours every days, dead, the borer population of living of investigation in 48 hours.Dead criterion is to touch polypide, and complete motionless person is dead.The every repetition repeated 3 times for 20 of examination worms.Obtain toxicity regression line and LC with method of least squares
50Value, 95% confidence limit and correlation coefficient r value.
The toxicity test result such as the table 1 of decis microemulsion, deltamethrin milk oil, decis wetting powder:
Table 1 toxicity test result
| Reagent agent toxicity regression formula r value LC 5095% confidence limit (y=) is (ppm) (ppm) |
| Decis microemulsion 3.8432+1.0491x 0.9889 20.9 9.8-17.9 deltamethrin milk oil 3.3320+1.3300x 0.9993 29.9 22.1-40.5 decis wettable 2.4480+1.1500x 0.9900 74.9 28.9-47.4 pulvis |
Experimental pharmacy:
2.5% bromine cyanogen decis microemulsion Beijing Penta Nanotech. Co., Ltd
2.5% deltamethrin milk oil Liaoning Province Dalian Kai Fei Chemical Co., Ltd
EXPERIMENTAL EXAMPLE two: the control cotton bollworm field control effectiveness test of the present invention's 2.5% decis microemulsion.
Adopt the control cotton bollworm field control effectiveness test of 2.5% decis microemulsion of the embodiment of the invention one, as the field control effectiveness test of control cotton bollworm, triplicate of every processing, the repetition in every sub-district is adopted district's group arrangement at random, sub-district area 50M
2, adopt knapsack sprayer to carry out conventional spray, to handle respectively back 1 day, 7 days investigation cotton bollworm larvae quantity is calculated as follows control efficiency:
Control efficiency (%)=(1-Ta * Cb/Tb * Ca) * 100
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
2.5% decis microemulsion control cotton bollworm field control effectiveness test result:
| Handle | Extension rate | Mark district preventive effect (%) | |
| ????1d | ????7d | ||
| 2.5% decis microemulsion | ????3000 | ????99 | ????84.2 |
| 2.5% deltamethrin milk oil | ????3000 | ????98.2 | ????83.7 |
Experimental pharmacy:
2.5% bromine cyanogen decis microemulsion Beijing Penta Nanotech. Co., Ltd
2.5% deltamethrin milk oil Liaoning Province Dalian Kai Fei Chemical Co., Ltd
EXPERIMENTAL EXAMPLE three: the particle size distribution range of the present invention's 2.5% decis microemulsion
Adopt the particle size distribution range of 2.5% decis microemulsion of the embodiment of the invention one, this experiment adopts transmission electron microscope (TEM) and laser light scattering particle size analyzer that the present invention is carried out grain size analysis, and analysis result is as follows:
| Method name | Particle mean size (nm) |
| Transmission electron microscope | ????30 |
| The laser light scattering Particle Size Analyzer | ????10～70 |
EXPERIMENTAL EXAMPLE four: the test of the stability of the present invention's 2.5% decis microemulsion
The test of the stability of 2.5% decis microemulsion of the employing embodiment of the invention one by to the hot and cold storage of 2.5% decis microemulsion and the analysis of resolution ratio, is verified stability of the present invention.Cold storage is adopted-10 ℃ of storages 7 days, and 54 ± 2 ℃ of storages 14 days are adopted in the heat storage.Its result is as follows:
| Test name | Experimental index | Experimental result |
| One, cold storage | ||
| Frost resistance | Do not have and freeze | Do not have and freeze |
| Whether there are crystallization or precipitation to separate out | Do not have | Do not have |
| Emulsibility | Qualified | Qualified |
| Two, heat storage | ||
| Whether there are crystallization or precipitation to separate out | Do not have | Do not have |
| Emulsibility | Qualified | Qualified |
| The effective ingredient resolution ratio | ????≤3％ | ????2.0 |
Claims (10)
1, a kind of decis microemulsion is characterized in that being made up of decis, cosolvent, emulsifier and water, and wherein the percentage by weight of various components is:
Decis 1 ~ 10%
Cosolvent 1 ~ 20%
Emulsifier 5 ~ 20%
Water 30 ~ 80%
2, decis 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 or has any one or two or more combinations in the material of similar features.
3, decis microemulsion according to claim 1 is characterized in that described emulsifier is meant 500
#, 600
#, 700
#, NP-10, PNP-10, EL-40,1601
#, 2000
#, PF-690, BY-130, tween-120,11
#Or has in the material of similar features one or more a combination.
4, decis microemulsion according to claim 1 is characterized in that being made up of decis, cosolvent, synergist, emulsifier and water, and wherein the percentage by weight of various components is:
Decis 1 ~ 10%
Cosolvent 1 ~ 20%
Emulsifier 5 ~ 20%
Synergist 5 ~ 10%
Water 30 ~ 80%
5, decis microemulsion according to claim 4 is characterized in that being made up of decis, cosolvent, synergist, stabilizing agent, emulsifier and water, and wherein the percentage by weight of various components is:
Decis 1 ~ 10%
Cosolvent 1 ~ 20%
Emulsifier 5 ~ 20%
Synergist 5 ~ 10%
Stabilizing agent 5 ~ 10%
Water 30 ~ 70%
6,, it is characterized in that described synergist is any one among piperonyl butoxide, Octachlorodipropyl Ether, azone or the material with similar features according to claim 4 or 5 described decis microemulsions.
7, decis 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.
8, the production method of decis microemulsion according to claim 1, it is characterized in that the former powder of decis 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 decis microemulsion.
9, the production method of decis microemulsion according to claim 8, it is characterized in that the former powder of decis is dissolved in the cosolvent, drop into emulsifier, drop into synergist and 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 decis.
10, according to Claim 8 or the production method of 9 described decis microemulsions, it is characterized in that the present invention can be used for producing the binary or the ternary built microemulsion of decis and other insecticide, bactericide, plant growth regulator.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031193471A CN1530012A (en) | 2003-03-17 | 2003-03-17 | Bromohydropyrethrin emulsion and production thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031193471A CN1530012A (en) | 2003-03-17 | 2003-03-17 | Bromohydropyrethrin emulsion and production thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1530012A true CN1530012A (en) | 2004-09-22 |
Family
ID=34285072
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA031193471A Pending CN1530012A (en) | 2003-03-17 | 2003-03-17 | Bromohydropyrethrin emulsion and production thereof |
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| Country | Link |
|---|---|
| CN (1) | CN1530012A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105557742A (en) * | 2016-03-04 | 2016-05-11 | 扬州大学 | Sanitary pesticide nano emulsion and preparation method thereof |
| CN105994388A (en) * | 2016-06-20 | 2016-10-12 | 河南中天恒信生物化学科技有限公司 | Environment-friendly tobacco pesticide and preparation method thereof |
| CN107136057A (en) * | 2017-06-30 | 2017-09-08 | 扬州大学 | A kind of highly effective and safe pyrethrin nanometer aqueous emulsion and preparation method thereof |
| CN111053805A (en) * | 2019-12-27 | 2020-04-24 | 内蒙古农业大学 | External emulsion for camel vaginal myiasis and preparation method thereof |
| CN111567551A (en) * | 2020-06-10 | 2020-08-25 | 济南中科绿色生物工程有限公司 | Insecticidal composition and insecticide thereof |
-
2003
- 2003-03-17 CN CNA031193471A patent/CN1530012A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105557742A (en) * | 2016-03-04 | 2016-05-11 | 扬州大学 | Sanitary pesticide nano emulsion and preparation method thereof |
| CN105994388A (en) * | 2016-06-20 | 2016-10-12 | 河南中天恒信生物化学科技有限公司 | Environment-friendly tobacco pesticide and preparation method thereof |
| CN107136057A (en) * | 2017-06-30 | 2017-09-08 | 扬州大学 | A kind of highly effective and safe pyrethrin nanometer aqueous emulsion and preparation method thereof |
| CN111053805A (en) * | 2019-12-27 | 2020-04-24 | 内蒙古农业大学 | External emulsion for camel vaginal myiasis and preparation method thereof |
| CN111567551A (en) * | 2020-06-10 | 2020-08-25 | 济南中科绿色生物工程有限公司 | Insecticidal composition and insecticide thereof |
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