CN102599165A - Azoxystrobin microcapsule suspending agent and preparation method thereof - Google Patents

Azoxystrobin microcapsule suspending agent and preparation method thereof Download PDF

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Publication number
CN102599165A
CN102599165A CN2012100394485A CN201210039448A CN102599165A CN 102599165 A CN102599165 A CN 102599165A CN 2012100394485 A CN2012100394485 A CN 2012100394485A CN 201210039448 A CN201210039448 A CN 201210039448A CN 102599165 A CN102599165 A CN 102599165A
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China
Prior art keywords
fluoxastrobin
urea
capsule
azoxystrobin
preparation
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CN2012100394485A
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Chinese (zh)
Inventor
曹希敏
孟宪秋
王龙江
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Guangdong Zhongxun Agri Science Corp
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Guangdong Zhongxun Agri Science Corp
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Priority to CN2012100394485A priority Critical patent/CN102599165A/en
Publication of CN102599165A publication Critical patent/CN102599165A/en
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Abstract

The invention discloses an Azoxystrobin microcapsule suspending agent and a preparation method of the Azoxystrobin microcapsule suspending agent. The Azoxystrobin microcapsule suspending agent is composed of the following components in percentage by weight: 1-10% of Azoxystrobin, 3-20% of capsule core solvent, 5-20% of capsule wall material, 1-10% of emulsifying agent, 1-5% of dispersant, 0.5-7% of antifreezing agent, 0.1-10% of pH regulator and the balance of deionized water. The invention also discloses a preparation method of the Azoxystrobin microcapsule suspending agent. According to the invention, Azoxystrobin is prepared into a new dosage form, the defects of oil emulsion, wettable powder, suspending agent and other dosage forms are overcome, the use cost of the farmer is reduced, the environmental pollution, the pesticide toxicity and the product cost are also reduced, and the safety and effect of the pesticide are improved.

Description

Fluoxastrobin micro-capsule suspension and preparation method thereof
Technical field
The present invention relates to a kind of disinfectant use in agriculture and preparation method thereof, a kind of specifically Fluoxastrobin 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.The pesticide micro capsule suspending agent is to utilize capsule-core that microencapsulation technology will contain former medicine to be encapsulated in the suspending agent of the fine particle that forms in the special cyst material, and the capsule diameter of agricultural chemicals microcapsule suspending agent is generally 1~20 μ m.The agricultural chemicals microcapsule suspending agent is compared following advantage with conventional dosage forms: prolonged the lasting period of agricultural chemicals, the stability that has improved active component, active substance be wrapped in improved in the cyst wall safety, effectively reduce former medicine composition to the stimulus to the sense organ of human body, reduce poisoning, help the composite, friendly more of agricultural chemicals environment to crop.
Fluoxastrobin is the cruel series bactericidal agent of methoxy acrylic acid; Efficiently, wide spectrum, nearly all mycota (Ascomycotina, Basidiomycotina, Mastigomycotina and Deuteromycotina) disease such as powdery mildew, rust, glume blight, net blotch, downy mildew, rice blast etc. are all had good activity.Have protection, treat, root out, infiltration, systemic activity, be mainly used in cereal paddy rice, peanut, grape, potato, fruit tree, vegetables, coffee, lawn etc.
At present; Mostly the Fluoxastrobin formulation of producing and using is suspending agent and missible oil, also has the azoxystrobin water emulsion prescription open, but existing azoxystrobin water emulsion still need use a certain amount of aromatic hydrocarbons organic solvent; And do not add suitable builder; And control efficiency is relatively poor, and is short when drug effect continues, and the Fluoxastrobin application concentration is big, the control cost is high.The Fluoxastrobin micro-capsule suspension can prolong the lasting period, overcomes pest resistance to insecticide, little to environmental pressure, economize on resources, help the sustainable development of agricultural and the protection of environment.
Summary of the invention
The purpose of this invention is to provide a kind of Fluoxastrobin micro-capsule suspension and preparation method thereof, solve the blank of present Fluoxastrobin microcapsule formulations suspending agent,, serve agricultural production for pesticide industry provides a kind of novel form and new product.
The present invention realizes through following technical scheme: a kind of Fluoxastrobin micro-capsule suspension; Form by following components in weight percentage: Fluoxastrobin 1%~10%, capsule-core solvent 3%~20%, cyst material 5%~20%, emulsifier 1%~10%; Dispersant 1%~5%; Antifreezing agent 0.5%~7%, pH regulator agent 0.1%~10%, surplus is a deionized water.
Wherein said capsule-core solvent is one or more in dimethyl formamide, ethanol, isopropyl alcohol, n-butanol, hexane, n-octyl alcohol, n-amyl alcohol, acetone, cyclohexanone, xylol, ethyl acetate, N-Methyl pyrrolidone, diethyl phthalate, acetonitrile, carrene, the dibutyl phthalate.
Described cyst material is the urea resin prepolymer aqueous solution, is to be mixed with weight ratio 1:1.5~1:2.5 by urea and formaldehyde, obtains through polycondensation reaction.
Described emulsifier is one or more in agricultural newborn 33#, 34#, 500#, 600#, 700#, NP-10, PNP-10, EL-40,1601#, 2000#, PF-690, BY-130, the tween-120.
Described dispersant is one or more in SOPA-270, dispersant NNO, sodium lignin sulfonate, the dispersant 2700.
Described antifreezing agent is one or more in ethylene glycol, propane diols, glycerine, the diethylene glycol.
Described pH regulator agent is sodium hydroxide or acetate.
The present invention is a kind of Fluoxastrobin micro-capsule suspension that adopts the situ aggregation method preparation, and its preparation method is following:
(1) urea is dissolved in the formaldehyde, the weight ratio that urea and formaldehyde mix is 1:1.5~1:2.5, and it is 8~9 that the NaOH solution of use 10% is regulated the pH value; With extremely clarification of magnetic stirrer, under 60~80 ℃ of conditions of temperature, stirring at low speed; Insulation reaction 1~1.5 hour generates 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) preparation of Fluoxastrobin mixture solution: will the normal temperature state be powdery or block Fluoxastrobin be dissolved in solvent (the solvent usage amount so that the Fluoxastrobin dissolving or disperse till) in; The emulsifier of adding 1%~10% carries out fully emulsified; Under 30 ℃ temperature, after 1000~1500 rev/mins of rotating speeds stirrings it is fully disperseed.
(3) preparation of Fluoxastrobin microcapsules: the urea resin prepolymer aqueous solution joined at 1000~1500 rev/mins of rotating speeds stir in the above-mentioned Fluoxastrobin mixture solution down, stir 15 minutes stable emulsions of formation, reduce stir speed (S.S.) to 500 rev/min again; Add an amount of acetate slowly, its pH value is transferred to 5, temperature rises to 60~80 ℃; Isothermal reaction is cyst wall curing completion after 2 hours; It is 7 that the NaOH solution of use 10% is regulated the pH value with product, adds an amount of dispersant, antifreezing agent, complements to 100% with deionized water; Sheared 15 minutes with 6000 rev/mins then, promptly obtain the Fluoxastrobin micro-capsule suspension.
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.
The present invention compared with prior art, it is few to have an equipment investment, technology is easy to control, stable reaction is suitable for suitability for industrialized production, and has advantages such as sustained release performance.Fluoxastrobin micro-capsule suspension of the present invention has not only solved Fluoxastrobin combines to influence drug effect with soil problem; Reduce consumption through slowly-releasing simultaneously, prolong the drug effect term of validity, consolidate control efficiency; Be difficult for making agricultural chemicals by atmosphere; Sunlight and rainwater destroy and run off, and effectively control reduces the influence to ecotope to phreatic pollution.
Embodiment
Essence is for a better understanding of the present invention explained technology contents of the present invention below in conjunction with specific embodiment, but content of the present invention is not limited thereto.
According to the present invention a kind of preparation method of Fluoxastrobin micro-capsule suspension is provided, can processes the Fluoxastrobin percentage by weight and be 1%~10% micro-capsule suspension.
Embodiment 1:5% Fluoxastrobin micro-capsule suspension.
Urea is dissolved in the formaldehyde, and the weight ratio that urea and formaldehyde mix is 1:2, and it is 8.5 that the NaOH solution of use 10% is regulated the pH value; With extremely clarification of magnetic stirrer, under 70 ℃ of conditions of temperature, stirring at low speed; Insulation reaction 1 hour generates 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, 5% Fluoxastrobin is dissolved in 15% xylol, adds 2% agricultural newborn 600# and carry out fully emulsifiedly, under 30 ℃ temperature, after stirring with 1000 rev/mins of rotating speeds it is fully disperseed.
An amount of urea resin prepolymer aqueous solution joined at 1000 rev/mins of rotating speeds stir in the above-mentioned Fluoxastrobin mixture solution down, stir 15 minutes stable emulsions of formation, reduce stir speed (S.S.) to 500 rev/min again; To wherein adding 0.5% an amount of acetate slowly, its pH value is transferred to 5, temperature rises to 60 ℃; Isothermal reaction is cyst wall curing completion after 2 hours; It is 7 that the NaOH solution of use 10% is regulated the pH value with product, adds dispersant 2% SOPA-270, antifreezing agent 3% ethylene glycol, complements to 100% with deionized water; Sheared 15 minutes with 6000 rev/mins then, promptly obtain 5% Fluoxastrobin micro-capsule suspension.
Embodiment 2:8% Fluoxastrobin micro-capsule suspension.
Urea is dissolved in the formaldehyde, and the weight ratio that urea and formaldehyde mix is 1:2.5, and it is 8.5 that the NaOH solution of use 10% is regulated the pH value; With extremely clarification of magnetic stirrer, under 70 ℃ of conditions of temperature, stirring at low speed; Insulation reaction 1.5 hours generates 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% Fluoxastrobin is dissolved in 15% dimethyl formamide, adds 7% Nongru-700 # and carry out fully emulsifiedly, under 30 ℃ temperature, after stirring with 1500 rev/mins of rotating speeds it is fully disperseed.
An amount of urea resin prepolymer aqueous solution joined at 1500 rev/mins of rotating speeds stir in the above-mentioned Fluoxastrobin mixture solution down, stir 15 minutes stable emulsions of formation, reduce stir speed (S.S.) to 500 rev/min again; To wherein adding 0.5% an amount of acetate slowly, its pH value is transferred to 5, temperature rises to 80 ℃; Isothermal reaction is cyst wall curing completion after 2 hours; It is 7 that the NaOH solution of use 10% is regulated the pH value with product, adds 3% dispersant NNO, antifreezing agent 3% glycerine, complements to 100% with deionized water; Sheared 15 minutes with 6000 rev/mins then, promptly obtain 8% Fluoxastrobin micro-capsule suspension.
Fluoxastrobin micro-capsule suspension properties of product of the present invention are stable, are easy to produce store, and are environmentally friendly, safe in utilization.Through evidence, good preventive effect all arranged to powdery mildew of cucumber, cucumber downy mildew, rice blast, wheat glume blight etc. are multiple; Safety is good, and crops are not had poisoning, is a kind of nuisanceless disinfectant use in agriculture that is worthy of popularization.

Claims (2)

1. Fluoxastrobin micro-capsule suspension; It is characterized in that: described Fluoxastrobin micro-capsule suspension is made up of following components in weight percentage: Fluoxastrobin 1%~10%, capsule-core solvent 3%~20%, cyst material 5%~20%, emulsifier 1%~10%; Dispersant 1%~5%; Antifreezing agent 0.5%~7%, pH regulator agent 0.1%~10%, surplus is a deionized water;
Wherein said capsule-core solvent is one or more in dimethyl formamide, ethanol, isopropyl alcohol, n-butanol, hexane, n-octyl alcohol, n-amyl alcohol, acetone, cyclohexanone, xylol, ethyl acetate, N-Methyl pyrrolidone, diethyl phthalate, acetonitrile, carrene, the dibutyl phthalate;
Described cyst material is the urea resin prepolymer aqueous solution, is to be mixed with weight ratio 1:1.5~1:2.5 by urea and formaldehyde, obtains through polycondensation reaction;
Described emulsifier is one or more in agricultural newborn 33#, 34#, 500#, 600#, 700#, NP-10, PNP-10, EL-40,1601#, 2000#, PF-690, BY-130, the tween-120:
Described dispersant is one or more in SOPA-270, dispersant NNO, sodium lignin sulfonate, the dispersant 2700;
Described antifreezing agent is one or more in ethylene glycol, propane diols, glycerine, the diethylene glycol;
Described pH regulator agent is sodium hydroxide or acetate.
2. the preparation method of a Fluoxastrobin micro-capsule suspension is characterized in that:
(1) urea is dissolved in the formaldehyde, the weight ratio that urea and formaldehyde mix is 1:1.5~1:2.5, and it is 8~9 that the NaOH solution of use 10% is regulated the pH value; With extremely clarification of magnetic stirrer, under 60~80 ℃ of conditions of temperature, stirring at low speed; Insulation reaction 1~1.5 hour generates 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) preparation of Fluoxastrobin mixture solution: will be powdery or block Fluoxastrobin is dissolved in the solvent at the normal temperature state; The solvent usage amount is so that till Fluoxastrobin dissolving or the dispersion; The emulsifier of adding 1%~10% carries out fully emulsified; Under 30 ℃ temperature, after 1000~1500 rev/mins of rotating speeds stirrings it is fully disperseed;
(3) preparation of Fluoxastrobin microcapsules: the urea resin prepolymer aqueous solution joined at 1000~1500 rev/mins of rotating speeds stir in the above-mentioned Fluoxastrobin mixture solution down, stir 15 minutes stable emulsions of formation, reduce stir speed (S.S.) to 500 rev/min again; Add an amount of acetate slowly, its pH value is transferred to 5, temperature rises to 60~80 ℃; Isothermal reaction is cyst wall curing completion after 2 hours; It is 7 that the NaOH solution of use 10% is regulated the pH value with product, adds an amount of dispersant, antifreezing agent, complements to 100% with deionized water; Sheared 15 minutes with 6000 rev/mins then, promptly obtain the Fluoxastrobin micro-capsule suspension;
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.
CN2012100394485A 2012-02-21 2012-02-21 Azoxystrobin microcapsule suspending agent and preparation method thereof Pending CN102599165A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103783039A (en) * 2013-12-27 2014-05-14 中国农业科学院植物保护研究所 Azoxystrobin nanocapsule with shell-core structure and preparation method thereof
CN105076145A (en) * 2015-08-20 2015-11-25 广东中迅农科股份有限公司 Microcapsule suspending agent containing azoxystrobin and preparation method thereof
CN106070203A (en) * 2016-06-03 2016-11-09 安徽广信农化股份有限公司 A kind of preparation method of Fluoxastrobin microcapsule
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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JPS5735502A (en) * 1980-04-26 1982-02-26 Bayer Ag Plant treating agent-containing microcapsule suspension, manufacture and use
KR860000446B1 (en) * 1980-12-12 1986-04-26 미쓰이도오 아쓰가가꾸가부시끼 가이샤 Dye stuff-containing microcapsule suspension for recording material
CN1501771A (en) * 2001-04-11 2004-06-02 ������ɽ���� Method of microencapsulating an agricultural active having a high melting point and uses for such materials
CN1709057A (en) * 2005-07-07 2005-12-21 云南大学 Nimbin micro capsule suspension formulation
CN101305725A (en) * 2008-07-17 2008-11-19 浙江省农业科学院 Chlopyrifos and pymtrozine composite microcapsule suspending agent and its preparation method
CN101427687A (en) * 2007-11-08 2009-05-13 联合国南通农药剂型开发中心 High-content chlorpyrifos microcapsule suspension agent and production method
CN101583269A (en) * 2006-11-23 2009-11-18 加特微胶囊股份公司 Novel agrochemical formulations containing microcapsules
CN102349534A (en) * 2011-08-26 2012-02-15 河北北方学院 Imidacloprid and pymetrozine compound microcapsule suspension and preparation method thereof

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5735502A (en) * 1980-04-26 1982-02-26 Bayer Ag Plant treating agent-containing microcapsule suspension, manufacture and use
KR860000446B1 (en) * 1980-12-12 1986-04-26 미쓰이도오 아쓰가가꾸가부시끼 가이샤 Dye stuff-containing microcapsule suspension for recording material
CN1501771A (en) * 2001-04-11 2004-06-02 ������ɽ���� Method of microencapsulating an agricultural active having a high melting point and uses for such materials
CN1709057A (en) * 2005-07-07 2005-12-21 云南大学 Nimbin micro capsule suspension formulation
CN101583269A (en) * 2006-11-23 2009-11-18 加特微胶囊股份公司 Novel agrochemical formulations containing microcapsules
CN101427687A (en) * 2007-11-08 2009-05-13 联合国南通农药剂型开发中心 High-content chlorpyrifos microcapsule suspension agent and production method
CN101305725A (en) * 2008-07-17 2008-11-19 浙江省农业科学院 Chlopyrifos and pymtrozine composite microcapsule suspending agent and its preparation method
CN102349534A (en) * 2011-08-26 2012-02-15 河北北方学院 Imidacloprid and pymetrozine compound microcapsule suspension and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103783039A (en) * 2013-12-27 2014-05-14 中国农业科学院植物保护研究所 Azoxystrobin nanocapsule with shell-core structure and preparation method thereof
CN105076145A (en) * 2015-08-20 2015-11-25 广东中迅农科股份有限公司 Microcapsule suspending agent containing azoxystrobin and preparation method thereof
CN106070203A (en) * 2016-06-03 2016-11-09 安徽广信农化股份有限公司 A kind of preparation method of Fluoxastrobin microcapsule
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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Application publication date: 20120725