CN101530077B - Mixed micro-emulsion of azoxystrobin and difenoconazole and preparation method thereof - Google Patents
Mixed micro-emulsion of azoxystrobin and difenoconazole and preparation method thereof Download PDFInfo
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- CN101530077B CN101530077B CN200810101925XA CN200810101925A CN101530077B CN 101530077 B CN101530077 B CN 101530077B CN 200810101925X A CN200810101925X A CN 200810101925XA CN 200810101925 A CN200810101925 A CN 200810101925A CN 101530077 B CN101530077 B CN 101530077B
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Abstract
The invention discloses a mixed micro-emulsion of azoxystrobin and difenoconazole, and a preparation method thereof. The micro-emulsion comprises the components by weight percentages as follows: 3 to 20 percent of azoxystrobin, 1 to 10 percent of difenoconazole, 3 to 25 percent of emulsifier, 3 to 15 percent of penetrating agent, 3 to 30 percent of latent solvent and the balance of de-ionized water. The preparation method includes the following steps of: firstly, stirring and mixing the azoxystrobin, the difenoconazole, the emulsifier, the penetrating agent and the latent solvent uniformly in a high-speed shear, then adding de-ionized water, stirring and mixing the mixture uniformly, standing for 5 to 15 hours, heating to 45 to 50 DEG C and stirring fully, thus obtaining the product. By making use of the synergized action of the azoxystrobin and the difenoconazole, the micro-emulsion overcomes the drug resistance of plant pathogens, improves the application effect of reagents, increases the reagent ranges and remedies the defects of single dosage. The invention is simple in preparation process, lower in production cost and suitable for large-area popularization and application.
Description
Technical field
The present invention relates to a kind of mixed pesticide technology, relate to a kind of Fluoxastrobin and the Difenoconazole microemulsion and preparation method thereof that is mixed specifically.
Technical background
Fluoxastrobin
English name: AMISTAR, CAS number: 131860-33-8.
The benzeneacetate of chemical name: methyl (α E)-2-[[6-(2-cyanophenoxy)-4-pyrimidinyl] oxy]-α-(methoxymethylene).
Molecular formula: C22H17N3O5.
Molecular weight is 403.4.
This product is first commercial methoxy acrylic bactericide that Syngenta Co.,Ltd succeeds in developing; Efficiently, wide spectrum, nearly all fungi steel (Ascomycetes, Basidiomycetes, Oomycete and Fungi Imperfecti) disease such as powdery mildew, rust, glume blight, net blotch, downy mildew, rice blast etc. are all had good activity.Can be used for cauline leaf spraying, seed treatment, also can carry out soil treatment, be mainly used in cereal, paddy rice, peanut, grape, potato, fruit tree, vegetables, coffee, lawn etc.Using dosage is 25-400g/hm2, and commodity are called Abound, Amistar, Heritage, Quadris, Admire.
Former medicine is a brown solid, M.P.114-116 ℃.Pure article are white crystalline solid, M.P.116 ℃.Relative density 1.34, vapour pressure 1.1 * 10-7mPa (20 ℃).Solvability 6mg/L in the water (20 ℃) is slightly soluble in hexane, n-octyl alcohol, is dissolved in methyl alcohol, toluene, acetone, is soluble in ethyl acetate, acetonitrile, carrene.The photodissociation half life period was 2 weeks in the aqueous solution, to hydrolysis-stable.
This product is the maximum strobilurin series bactericidal agent of global sales; Sales volume in 2006 has surpassed 500,000,000 dollars, patent phase to 2010 year, domestic existing minority manufacturer production and sale at present; Price is at 100～1,300,000 yuan/ton, and product specification has content greater than 93% and greater than 95% two kind.Big raw materials for production cost the best of this product can be accomplished between 30～350,000 yuan/ton.
The production difficulty of this product mainly contains the following aspects:
1, the cost of equipment of this product is higher, produce per year 50 tons of products only cost of equipment just need about 2,000,000 yuan.18 of the agitated reactors (basic configuration) that comprise 2000-3000, wherein also requiring has autoclave, and supporting facility will have high-vacuum pump group, destilling tower etc.
2, this product intermediate (benzo glycol) can cause serious allergicly, about irritated duration two weeks, and does not have what specific drug.
3, this product intermediate (4, the 6-dichloro pyrimidine) highly volatile at normal temperatures, its drying course requires high Difenoconazole (Difenoconazole) to equipment, and pure article are the colourless crystallization body, and industrial goods are pale yellow powder.100.3 ℃ of relative density 1.19 (23 ℃) fusing points, vapour pressure 8.4mPa (20 ℃).Solvability (20 ℃): water 26.6mg/L.Be soluble in most organic solvent, 20 ℃ of g/kg) hexane 1.3, methyl alcohol 101, xylol 30.Stability≤300 ℃ is stable, and mobility is little in soil, slowly degraded.
Difenoconazole belongs to triazole bactericidal agent, has interior absorption, is sterol demethylation inhibitor, and fungicidal spectrum is wide.Foliar treatment or seed treatment can improve output and the guaranteed quality of crop, for capsule Gammaproteobacteria, Basidiomycetes with comprise that imperfect fungus that Alternaria Ascochyta, the mould genus of tail spore, Colletotrichum, ball seat Pseudomonas, Phoma, Ramularia, Septoria, black star spore belong to, Erysiphaceae, Uredinales and some are planted and pass pathogen lasting protection and therapeutic activity are arranged.To the disease of grape, peanut, a kind of fruit, such as apple, pear, etc., potato, wheat and various vegetables, consumption is 30-125g (a.i.)/ha.Be used for 75-125g, (a.i.)/ha has tall and erect the effect to cercospora leaf spot of sugar beet; 125-250g (a.i.)/ha used once in the wheat growth phase, can effectively prevent and treat glume blight, leaf blight, rust and by concentrating the microbial mildew of causing a disease; With 125g (a.i.)/ha, prevent and treat target, leaf spot of peanut, net blotch, prevent and treat apple scab, powdery mildew with 2.5-5.0g (a.i.)/ha; Prevent and treat grape powdery mildew with 30-50g (a.i.)/Ha.
In recent years, developed countries such as Great Britain and America are to an organic solvent restriction increasingly stringent in the pesticidal preparations, and organic solvents such as xylol, toluene are disabled to be the solvent of agricultural chemicals.This is a kind of challenge to cream preparation.And wetting powder and pulvis can bring dust pollution, thereby impel agricultural chemicals to develop along efficient (super-high-efficient), low toxicity, safety, biorational and the good direction of Environmental compatibility.People are when strengthening the novel pesticide research and development; Pay attention to research and development more to the formulations of pesticide; It wherein is the direction that the pesticides new formulation of matrix has become world's formulations of pesticide research and development with water; And as a kind of novel water-based pesticide formulation, a kind of so just environment friendly agricultural preparation of microemulsion.
Summary of the invention
The object of the present invention is to provide a kind of Fluoxastrobin and the Difenoconazole microemulsion and preparation method thereof that is mixed.
Another object of the present invention is that with antibacterial substance Fluoxastrobin and Difenoconazole be former medicine; A kind of high-efficiency low-toxicity, low cost, environmentally friendly, nuisanceless bactericide that phytopathogen is difficult to develop immunity to drugs are provided, promptly can be used for the Fluoxastrobin of control of plant disease such as crops, fruits and vegetables and the microemulsion that Difenoconazole is mixed.
The object of the invention is realized through following technical scheme:
A kind of Fluoxastrobin and the Difenoconazole microemulsion that is mixed with percentage by weight, comprises following component: Fluoxastrobin 3-20%, and Difenoconazole 1-10%, emulsifier 3-25%, bleeding agent 3-15%, cosolvent 3-30%, deionized water supplies 100%.
Described emulsifier is selected from one or more in calcium dodecyl benzene sulfonate, sodium alkyl benzene sulfonate, alkyl benzene sulphonate barium salt and the dodecyl sodium naphthalene sulfonate of anionic.Perhaps one or more in the calcium dodecyl benzene sulfonate of anionic, sodium alkyl benzene sulfonate, alkyl benzene sulphonate barium salt and the dodecyl sodium naphthalene sulfonate.
Described bleeding agent is selected from one or more in sulfosuccinate di-sec-octyl sodium salt, kerosene, diesel oil and the azone.
Described cosolvent is selected from one or more in isoamyl alcohol, cyclohexanone, ethyl acetate and the n-butanol.The present invention realizes through following steps:
Earlier Fluoxastrobin, Difenoconazole, emulsifier, bleeding agent and cosolvent are mixed in high-speed shearing machine by prescription; Add deionized water again; Mix, left standstill 5-15 hour, be heated to 45-50 ℃; After fully stirring, promptly can be made into Fluoxastrobin and the Difenoconazole microemulsion that is mixed.
The microemulsion that is mixed of the present invention is the microemulsion that contains fungicide active ingredient Fluoxastrobin, Difenoconazole.With respect to prior art, the present invention has following advantage:
1, the present invention is a kind of new high-efficiency fungicide preparation, and plant powdery mildew is had significant drug effect.
2, fungicide preparation of the present invention holds environment, people and other beneficial organism safety, be difficult for producing poisoning, and germ is difficult for it is produced resistance.Each composition in the mixture is being can work in coordination with in process to play a role, and has remedied self deficiency of single agent agricultural chemicals, and has reduced the field pesticides amount of application, has reduced the production cost.
3, fungicide preparation flash-point of the present invention high, do not fire not quick-friedly, produce and safe in utilization, bin stability is good, can deposit more than 2 years.
4, fungicide preparation preparing process of the present invention is simple, is medium with water, and product cost is lower, is suitable for large scale application.
Specific embodiments
In order to understand the present invention better, below in conjunction with embodiment the present invention is described further, but the scope that the present invention requires to protect is not limited to the scope that embodiment representes.
Embodiment 1:
Take by weighing Fluoxastrobin 3.0kg, Difenoconazole 3.0kg; After mixing in high-speed shearing machine with polyoxyethylene glycol 2.0kg, sulfosuccinate di-sec-octyl sodium salt 3.0kg, isoamyl alcohol 4.0kg then, add deionized water 85.0kg at last again, mix; Left standstill 5 hours; Be heated to 45 ℃, after fully stirring, promptly can be made into microemulsion.
Embodiment 2:
Take by weighing Fluoxastrobin 4.0kg, Difenoconazole 5.0kg; After mixing in high-speed shearing machine with benzylphenol APEO 4.0kg, diesel oil 3.0kg, cyclohexanone 4.0kg, isoamyl alcohol 4.0kg then, add deionized water 76kg at last again, mix; Left standstill 6 hours; Be heated to 45 ℃, after fully stirring, promptly can be made into microemulsion.
Embodiment 3:
Take by weighing Fluoxastrobin 6.0kg, Difenoconazole 5.0kg; After mixing in high-speed shearing machine with polyoxyethylene glycol 4.0kg, phenethyl phenol polyethenoxy ether 6.0kg, NPE 3.0kg, azone 4.0kg, isoamyl alcohol 4.0kg, ethyl acetate 3.0kg, n-butanol 4.0kg then, add deionized water 61kg at last again, mix; Left standstill 6 hours; Be heated to 50 ℃, after fully stirring, promptly can be made into microemulsion.
Embodiment 4:
Take by weighing Fluoxastrobin 12.0kg, Difenoconazole 8.0kg; After mixing in high-speed shearing machine with polyoxyethylene glycol 6.0kg, phenethyl phenol polyethenoxy ether 5.0kg, NPE 5.0kg, sulfosuccinate di-sec-octyl sodium salt 4.0k g, cyclohexanone 8.0kg, ethyl acetate 4.0kg then, add deionized water 48kg at last again, mix; Left standstill 5 hours; Be heated to 50 ℃, after fully stirring, promptly can be made into microemulsion.
Claims (6)
1. Fluoxastrobin and the Difenoconazole microemulsion that is mixed is characterized in that by weight percentage, comprises following component: Fluoxastrobin 3-20%; Difenoconazole 1-10%, emulsifier 3-25%, bleeding agent 3-15%; Cosolvent 3-30%, deionized water supplies 100%.
2. Fluoxastrobin according to claim 1 and the Difenoconazole microemulsion that is mixed is characterized in that described emulsifier is selected from one or more in the polyoxyethylene glycol of nonionic, phenethyl phenol polyethenoxy ether, NPE and the benzylphenol APEO.
3. Fluoxastrobin according to claim 1 and the Difenoconazole microemulsion that is mixed is characterized in that described emulsifier is selected from one or more in the calcium dodecyl benzene sulfonate of anionic, sodium alkyl benzene sulfonate, alkyl benzene sulphonate barium salt and the dodecyl sodium naphthalene sulfonate.
4. Fluoxastrobin according to claim 1 and the Difenoconazole microemulsion that is mixed is characterized in that described bleeding agent is selected from one or more in sulfosuccinate di-sec-octyl sodium salt, kerosene, diesel oil and the azone.
5. Fluoxastrobin according to claim 1 and the Difenoconazole microemulsion that is mixed is characterized in that described cosolvent is selected from one or more in isoamyl alcohol, cyclohexanone, ethyl acetate and the n-butanol.
6. any the be mixed preparation method of microemulsion of a described Fluoxastrobin and Difenoconazole of claim 1 to 5; It is characterized in that comprising the steps: earlier Fluoxastrobin, Difenoconazole, emulsifier, bleeding agent and cosolvent being mixed in high-speed shearing machine, add deionized water again, mix by prescription; Left standstill 5-15 hour; Be heated to 45-50 ℃, after fully stirring, promptly can be made into Fluoxastrobin and the Difenoconazole microemulsion that is mixed.
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| CN200810101925XA CN101530077B (en) | 2008-03-14 | 2008-03-14 | Mixed micro-emulsion of azoxystrobin and difenoconazole and preparation method thereof |
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| CN200810101925XA CN101530077B (en) | 2008-03-14 | 2008-03-14 | Mixed micro-emulsion of azoxystrobin and difenoconazole and preparation method thereof |
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| CN101530077B true CN101530077B (en) | 2012-07-25 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101911940A (en) * | 2010-09-08 | 2010-12-15 | 吴元林 | Germicide compounded from azoxystrobin, difenoconazole and cyproconazole and preparation method thereof |
| CN102057912B (en) * | 2010-12-19 | 2013-04-17 | 惠州市银农科技有限公司 | Water suspending agent mixed by difenoconazole and azoxystrobin and preparation method thereof |
| CN102669111B (en) * | 2012-05-24 | 2014-06-04 | 利民化工股份有限公司 | Suspending agent formulated by difenoconazole and azoxystrobin and preparation method thereof |
| AU2013295098B2 (en) * | 2012-07-26 | 2016-06-23 | Syngenta Participations Ag | Fungicidal compositions |
| BR102013027977A2 (en) * | 2013-10-30 | 2015-09-15 | Rotam Agrochem Int Co Ltd | method of increasing yield by treatment with fungicidal compositions |
| CN104521969A (en) * | 2015-01-09 | 2015-04-22 | 姚卫平 | Field barrel-mixing pesticide synergism formula for ustilaginoidea virens and neck blast of rice and spraying method of formula |
| CN105191971A (en) * | 2015-10-16 | 2015-12-30 | 池州市农业技术推广中心 | Synergistic formula, application and pesticide applying method of pesticides in field tank mixing |
| CN109247332A (en) * | 2018-09-15 | 2019-01-22 | 湖南农业大学 | A kind of composition pesticide and its application containing difenoconazole and Fluoxastrobin |
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2008
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Application publication date: 20090916 Assignee: JIXI AGROSINO BIOTECHNOLOGY CO.,LTD. Assignor: BEIJING GREEN AGROSINO Corp. Contract record no.: 2013990000705 Denomination of invention: Mixed micro-emulsion of azoxystrobin and difenoconazole and preparation method thereof Granted publication date: 20120725 License type: Exclusive License Record date: 20131023 |
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Effective date of registration: 20200106 Address after: Xuancheng city Jixi County Hongxing Industrial Park in Anhui province 245300 (Yang Zhen Hong Chuan Cun Hua Yuan) Patentee after: JIXI AGROSINO BIOTECHNOLOGY CO.,LTD. Address before: 100080, Zhongguancun building, No. 27 Zhongguancun street, Beijing, Haidian District, China, 14 floor Patentee before: BEIJING GREEN AGROSINO Corp. |
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Effective date of registration: 20220923 Address after: 1901d, 19th floor, Zhongguancun building, No. 27, Zhongguancun Street, Haidian District, Beijing 100080 Patentee after: BEIJING GREEN AGROSINO CROP TECHNOLOGY CO.,LTD. Patentee after: HEBEI GREEN NONGHUA CROP TECHNOLOGY CO.,LTD. Address before: 245300 Hongxing Industrial Park, Jixi County, Xuancheng City, Anhui Province Patentee before: JIXI AGROSINO BIOTECHNOLOGY CO.,LTD. |