CN102640754A - Cyazofamid microcapsule suspending agent and preparation method thereof - Google Patents
Cyazofamid microcapsule suspending agent and preparation method thereof Download PDFInfo
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- CN102640754A CN102640754A CN2012100954576A CN201210095457A CN102640754A CN 102640754 A CN102640754 A CN 102640754A CN 2012100954576 A CN2012100954576 A CN 2012100954576A CN 201210095457 A CN201210095457 A CN 201210095457A CN 102640754 A CN102640754 A CN 102640754A
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Abstract
本发明公开了一种氰霜唑微胶囊悬浮剂及其制备方法，包括如下重量份的组分：氰霜唑1～10份，囊芯溶剂3～20份，壁材5～20份，乳化剂3～10份，分散剂1～5份，水补足100份。本发明还公开了上述氰霜唑微胶囊悬浮剂的制备方法。本发明提供了一种持效期长、低毒、对环境友好、人畜安全，对病害不易产生抗药性的氰霜唑微胶囊剂悬浮剂。该制剂性能稳定，易降解，对农作物病害持效期长，对环境污染很小。与现有技术相比，提供了一种更为环境友好的农药制剂，满足农业无公害防治需要。The invention discloses a microcapsule suspending agent of Cyazofamid and a preparation method thereof. 3-10 parts of agent, 1-5 parts of dispersant, and 100 parts of water. The invention also discloses a preparation method of the above-mentioned cyazofamid microcapsule suspension. The invention provides a microcapsule suspending agent of cyazofamid, which is long-lasting, low in toxicity, friendly to the environment, safe for humans and animals, and not easy to produce drug resistance to diseases. The preparation has stable performance, is easy to degrade, has a long lasting effect on crop diseases, and has little environmental pollution. Compared with the prior art, a more environment-friendly pesticide preparation is provided, which meets the needs of agricultural pollution-free prevention and control.
Description
Technical field
The present invention relates to a kind of disinfectant use in agriculture and preparation method thereof, a kind of specifically cyanogen frost azoles micro-capsule suspension and preparation method thereof.
Background technology
Chemical control is the important means of human control agricultural damage by disease and insect; Chemical pesticide plays important effect to the increasing both production and income that guarantees agricultural; Yet the use of agricultural chemicals when ensureing that grain security is produced, has also brought a series of environment and social concerns such as residual, pollution.Only be because chemical pesticide itself, and be to a great extent because the formulations of pesticide are processed and application process is unreasonable causes.It is reported that the availability of conventional type agricultural chemicals has only 20%～30%, and percent of loss by all means is up to 50%～60%, this not only is a kind of waste economically, and has caused large-scale environmental pollution.Therefore, develop safety, high-efficiency environment friendly, prolongation lasting period, alleviate poisoning, reduce the novel form preparation residual, that increase the range of application of agricultural chemicals of agricultural chemicals in environment and become one of developing direction of the following formulations of pesticide.
Cyanogen frost azoles claims that again the match seat goes out.Molecular formula: C
13H
13ClN
4O
2S.Chemical name: 4-chloro-2-cyanic acid-N, N-dimethyl-5-p-methylphenyl imidazoles-1-sulfonamide.
Cyanogen frost azoles mechanism of action is the supply that the electronics transmission of mitochondrial cytochrome b c1 complex in the blocking-up Oomycete germ body comes interfering energy, and its binding site is the Q1 center of enzyme, does not have cross tolerance with other bactericide.It possibly be owing to the sensitivity difference of target enzyme to medicament causes that its height to pathogen is selected activity.Plasmodiophora brassica bacteria to Oomycete fungi such as downy mildew, false downy mildew, phytophthora, pythium spp and Plasmodiophoromycetes has very high biologically active.
But the duration of the cyanogen that uses at present frost azoles control germ is shorter relatively, causes the frequent medication of peasant and improves constantly dosing, and many areas have all caused drug-fast generation, and the lasting period that for this reason prolongs this medicament becomes the problem that needs to be resolved hurrily.In addition, the formulation that cyanogen frost azoles uses at present is main with missible oil still, owing to use a large amount of organic solvents, not only consumes a large amount of petrochemical industry resources, and environment has also been caused very big pressure.After cyanogen frost azoles processed micro-capsule suspension, not only can improve its stability, prolong the lasting period, reduce application times and amount of application, can also alleviate its harmful effect environment and agricultural product, thereby the safety of raising medication.
The pesticide micro capsule suspending agent is meant and utilizes natural or synthetic macromolecular material to form the nucleocapsid structure small container, agricultural chemicals coated wherein, and be suspended in the formulations of pesticide in the water.It comprises softgel shell and capsule-core two parts, and capsule-core is the active ingredient and the solvent of agricultural chemicals, and softgel shell is the macromolecular material of film forming.This formulation is divided into continuous phase and discontinuous phase, and continuous phase is water and auxiliary agent, the agricultural chemicals tiny capsules that discontinuous phase is coated.This formulation has slow releasing function, the longevity of residure is long, stability is high, toxicity is low, preventive effect is high; With water is dispersion medium; Reduce the usage amount of organic solvent,, more help the sustainable development of agricultural for practicing thrift fossil energy, protecting the Agro-ecology balance significant.
The preparation method of pesticide micro capsule has spray-on process, hypobaric drying method, list (answering) coacervation, situ aggregation method, interfacial polymerization etc., wherein situ aggregation method because easy to operate, production cost is low, uses at present comparatively extensive.
Situ aggregation method is that former medicine, solvent, emulsifier and water are mixed the back with homogenizer shearing becoming O/w emulsion; Then water-soluble monomer is joined in the water and milk agricultural chemicals; Through adding catalyzer; Make the water-soluble monomer polymerization reaction take place be deposited in the agricultural chemicals surface and coat film forming, finally obtain the process of microcapsules.
Reported with the Lauxite to be the wall material through document retrieval " agricultural chemicals " the 49th the 6th phase of volume of June in 2010, adopted situ aggregation method to prepare the trefanocide micro-capsule suspension.Chinese patent CN1663379 discloses a kind of method for preparing pesticide avermectin microcapsule; Chinese patent CN101396018 discloses urea-formaldehyde resin microcapsule agent of a kind of weed killer herbicide sethoxydim and preparation method thereof; Chinese patent CN101803599A discloses a kind of method for preparing biological pesticide spinosad microcapsule preparation; Above pesticide micro capsule preparation method prepares urea resin prepolymer with urea and formaldehyde according to the certain molar ratio example earlier under the alkali condition; Then core materials is mixed with into emulsion with urea resin prepolymer, obtains through heat cure.
Summary of the invention
The purpose of this invention is to provide a kind of cyanogen frost azoles microcapsule formulations suspending agent, can greatly reduce the environmental pollution of agricultural chemicals, increase operation rate, prolong the lasting period, delay pesticide resistance,, serve agricultural production for pesticide industry provides a kind of novel form and new product.
Another object of the present invention provides a kind of preparation method of above-mentioned cyanogen frost azoles micro-capsule suspension.
The present invention realizes through following technical scheme: a kind of cyanogen frost azoles micro-capsule suspension comprises the component of following weight portion: 1～10 part of cyanogen frost azoles, and 3～20 parts of capsule-core solvents, 5～20 parts of wall materials, 3～10 parts of emulsifier, 1～5 part of dispersant, water are supplied 100 parts.
Wherein said capsule-core solvent is one or more among xylol, cyclohexanone, ethyl acetate, N-Methyl pyrrolidone, diethyl phthalate, dibutyl phthalate, Solvesso100, Solvesso150, the Solvesso200.
Described cyst material is the urea resin prepolymer aqueous solution, is to be mixed with weight ratio 1:1～1:2.5 by urea and formaldehyde, obtains through polycondensation reaction.
Described emulsifier is one or more in APES, styryl phenol polyethenoxy ether, alkaryl phenol polyethenoxy ether phosphate, castor oil polyoxyethylene ether, alkylbenzenesulfonate, alkylphenol-polyethenoxy phosphate, maleic acid di-sec-octyl sodium sulfonate, polyol fatty acid ester and the ethylene oxide adduct thereof.
Described dispersant is one or more in SOPA-270, dispersant NNO, sodium lignin sulfonate, the dispersant 2700.
Described pH regulator agent is sodium hydroxide or watery hydrochloric acid.
A kind of preparation method of cyanogen frost azoles micro-capsule suspension.
(1) urea is dissolved in the formaldehyde, the weight ratio that urea and formaldehyde mix is 1:1～1:2.5, and using sodium hydroxide to regulate the pH value is 7～8; Under 60～80 ℃ of conditions of temperature, stirring at low speed, insulation reaction 0.5～4 hour; Generate the transparent Lauxite of thickness; The deionized water that adding equates with urea and formaldehyde gross weight, stirring at low speed obtains the transparent urea resin prepolymer aqueous solution.
(2) at normal temperatures cyanogen frost azoles is dissolved in the capsule-core solvent fully, under stirring condition, adds emulsifier and 20 parts of water, became stable O/W emulsion in 10～20 minutes with 2000 rev/mins of rotating speed cutting;
(3) rotating speed of reduce shearing adds urea resin prepolymer earlier under stirring condition, drip watery hydrochloric acid then and regulate pH value to 3.0, is warming up to 40～60 ℃, react an amount of dispersant of adding after the completion of 1 hour curing cyst wall, and water complements to 100 parts.
(4) discharging: add sodium hydrate aqueous solution and regulate pH value to 7.0.
In the cyst wall solidify reaction process, whenever at a distance from sampling in 15 minutes 1 time, use the capsule process of each stage of reaction of microscopic examination, use the pH value of pH meter monitoring reaction course.
Advantage of the present invention and good effect are following.
1, cyanogen frost azoles micro-capsule suspension provided by the invention, flash-point is high, does not burn and does not explode, and produces storage and safe in utilization.
2, cyanogen frost azoles micro-capsule suspension provided by the invention, farm chemical ingredients slowly discharges after the dispenser, can a dispenser protect one season of effect, practices thrift medicament, saves man-hour.
3, cyanogen frost azoles micro-capsule suspension provided by the invention, contact toxicity and peculiar smell reduce greatly, make the operator avoid harm.
4, cyanogen frost azoles micro-capsule suspension provided by the invention, consumption of organic solvent reduces more than 30%, has significantly reduced the pollution of harmful aromatic hydrocarbons to environment, helps environmental protection.
5, cyanogen frost azoles micro-capsule suspension provided by the invention, product cost is low, stable performance, good drug efficacy, the lasting period is long, and low toxicity is environmentally friendly, to the person poultry safety, can satisfy agriculture non-environmental pollution control needs.
6, cyanogen frost azoles micro-capsule suspension of the present invention, small investment of production equipment, the preparation method operates easily.
Embodiment
Essence is for a better understanding of the present invention explained technology contents of the present invention with embodiment below, but content of the present invention is not limited thereto.
Embodiment 1:2% cyanogen frost azoles micro-capsule suspension.
The urea resin prepolymer water solution preparation method: urea is dissolved in the formaldehyde, and the weight ratio that urea and formaldehyde mix is 1:1～1:2.5, and using sodium hydroxide to regulate the pH value is 8; Under 80 ℃ of conditions of temperature, stirring at low speed, insulation reaction 2 hours; Generate the transparent Lauxite of thickness; The deionized water that adding equates with urea and formaldehyde gross weight, stirring at low speed obtains the transparent urea resin prepolymer aqueous solution;
At normal temperatures 2% cyanogen frost azoles is dissolved in 5% xylol fully, under stirring condition, adds 5% emulsifier castor oil polyoxyethylene ether and 20% water, became stable O/W emulsion in 10～20 minutes with 2000 rev/mins of rotating speed cutting;
The rotating speed that reduction is sheared adds urea resin prepolymer earlier under stirring condition, drip watery hydrochloric acid then and regulate pH value to 3.0, is warming up to 60 ℃, reacts to add 1% dispersant NNO after 1 hour curing cyst wall is accomplished, and water complements to 100%;
Add sodium hydrate aqueous solution and regulate pH value to 7.0, promptly make 2% cyanogen frost azoles micro-capsule suspension.
Light microscope is observed down, and obtaining average grain diameter is the 2% cyanogen frost azoles micro-capsule suspension of 2.5～10.5um.
Embodiment 2:8% cyanogen frost azoles micro-capsule suspension.
The urea resin prepolymer water solution preparation method: urea is dissolved in the formaldehyde, and the weight ratio that urea and formaldehyde mix is 1:1～1:2.5, and using sodium hydroxide to regulate the pH value is 8; Under 70 ℃ of conditions of temperature, stirring at low speed, insulation reaction 3 hours; Generate the transparent Lauxite of thickness; The deionized water that adding equates with urea and formaldehyde gross weight, stirring at low speed obtains the transparent urea resin prepolymer aqueous solution;
At normal temperatures 8% cyanogen frost azoles is dissolved in 15% xylol fully, under stirring condition, adds 7% emulsifier styryl phenol polyethenoxy ether and 20% water, became stable O/W emulsion in 10～20 minutes with 2000 rev/mins of rotating speed cutting;
The rotating speed that reduction is sheared adds urea resin prepolymer earlier under stirring condition, drip watery hydrochloric acid then and regulate pH value to 3.0, is warming up to 60 ℃, reacts to add 3% dispersant sodium lignin sulfonate after 1.5 hours curing cyst walls are accomplished, and water complements to 100%;
Add sodium hydrate aqueous solution and regulate pH value to 7.0, promptly make 8% cyanogen frost azoles micro-capsule suspension.
Light microscope is observed down, and obtaining average grain diameter is the 8% cyanogen frost azoles micro-capsule suspension of 2.5～10.5um.
The cyanogen frost azoles micro-capsule suspension that the present invention prepares is compared with granule without having improved stability with existing wetting powder; Also prolonged the lasting period; Reduced application times and amount of application, also alleviated its harmful effect, thereby improved the safety of medication environment and agricultural product.
Claims (2)
1. cyanogen frost azoles micro-capsule suspension is characterized in that: the component that comprises following weight portion: 1～10 part of cyanogen frost azoles, and 3～20 parts of capsule-core solvents, 5～20 parts of wall materials, 3～10 parts of emulsifier, 1～5 part of dispersant, water are supplied 100 parts;
Wherein said capsule-core solvent is one or more among xylol, cyclohexanone, ethyl acetate, N-Methyl pyrrolidone, diethyl phthalate, dibutyl phthalate, Solvesso100, Solvesso150, the Solvesso200;
Described cyst material is the urea resin prepolymer aqueous solution, is to be mixed with weight ratio 1:1～1:2.5 by urea and formaldehyde, obtains through polycondensation reaction;
Described emulsifier is one or more in APES, styryl phenol polyethenoxy ether, alkaryl phenol polyethenoxy ether phosphate, castor oil polyoxyethylene ether, alkylbenzenesulfonate, alkylphenol-polyethenoxy phosphate, maleic acid di-sec-octyl sodium sulfonate, polyol fatty acid ester and the ethylene oxide adduct thereof;
Described dispersant is one or more in SOPA-270, dispersant NNO, sodium lignin sulfonate, the dispersant 2700;
Described pH regulator agent is sodium hydroxide or watery hydrochloric acid.
2. the preparation method of cyanogen frost azoles micro-capsule suspension is characterized in that:
(1) urea is dissolved in the formaldehyde, the weight ratio that urea and formaldehyde mix is 1:1～1:2.5, and using sodium hydroxide to regulate the pH value is 7～8; Under 60～80 ℃ of conditions of temperature, stirring at low speed, insulation reaction 0.5～4 hour; Generate the transparent Lauxite of thickness; The deionized water that adding equates with urea and formaldehyde gross weight, stirring at low speed obtains the transparent urea resin prepolymer aqueous solution;
(2) at normal temperatures cyanogen frost azoles is dissolved in the capsule-core solvent fully, under stirring condition, adds emulsifier and 20 parts of water, became stable O/W emulsion in 10～20 minutes with 2000 rev/mins of rotating speed cutting;
(3) rotating speed of reduce shearing adds urea resin prepolymer earlier under stirring condition, drip watery hydrochloric acid then and regulate pH value to 3.0, is warming up to 40～60 ℃, react an amount of dispersant of adding after the completion of 1 hour curing cyst wall, and water complements to 100 parts;
(4) discharging: add sodium hydrate aqueous solution and regulate pH value to 7.0;
In the cyst wall solidify reaction process, whenever at a distance from sampling in 15 minutes 1 time, use the capsule process of each stage of reaction of microscopic examination, use the pH value of pH meter monitoring reaction course.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107318849A (en) * | 2017-08-02 | 2017-11-07 | 天津市农药研究所 | A kind of preparation and its application of 26% Fluoxastrobin cyazofamid micro-capsule suspension |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101578987A (en) * | 2009-06-26 | 2009-11-18 | 陕西标正作物科学有限公司 | Cyazofamid aqueous emulsion and preparation method thereof |
| WO2010013250A2 (en) * | 2008-07-31 | 2010-02-04 | Sol-Gel Technologies Ltd. | Microcapsules comprising active ingredients and a metal oxide shell, a method for their preparation and uses thereof |
| CN101132851B (en) * | 2005-03-01 | 2010-11-24 | 巴斯福股份公司 | Fast-release microcapsule products |
| CN102123589A (en) * | 2008-08-19 | 2011-07-13 | 石原产业株式会社 | Method for controlling degradation of agricultural chemical active ingredient |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101132851B (en) * | 2005-03-01 | 2010-11-24 | 巴斯福股份公司 | Fast-release microcapsule products |
| WO2010013250A2 (en) * | 2008-07-31 | 2010-02-04 | Sol-Gel Technologies Ltd. | Microcapsules comprising active ingredients and a metal oxide shell, a method for their preparation and uses thereof |
| CN102123589A (en) * | 2008-08-19 | 2011-07-13 | 石原产业株式会社 | Method for controlling degradation of agricultural chemical active ingredient |
| CN101578987A (en) * | 2009-06-26 | 2009-11-18 | 陕西标正作物科学有限公司 | Cyazofamid aqueous emulsion and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107318849A (en) * | 2017-08-02 | 2017-11-07 | 天津市农药研究所 | A kind of preparation and its application of 26% Fluoxastrobin cyazofamid micro-capsule suspension |
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