CN106561641A - Micro-capsule suspending-suspending agent containing pyraclostrobin and fluopyram and preparation method of micro-capsule suspending-suspending agent - Google Patents

Micro-capsule suspending-suspending agent containing pyraclostrobin and fluopyram and preparation method of micro-capsule suspending-suspending agent Download PDF

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CN106561641A
CN106561641A CN201610989950.0A CN201610989950A CN106561641A CN 106561641 A CN106561641 A CN 106561641A CN 201610989950 A CN201610989950 A CN 201610989950A CN 106561641 A CN106561641 A CN 106561641A
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weight
fluopyram
pyraclostrobin
agent
solution
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高敬雨
徐妍
东琴
潘静
刘润峰
陈秋明
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BEIJING MINDLEADER AGROSCIENCE Co Ltd
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BEIJING MINDLEADER AGROSCIENCE Co Ltd
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/02Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
    • A01N25/04Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/34Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
    • A01N43/40Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N47/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/08Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
    • A01N47/10Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
    • A01N47/24Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof containing the groups, or; Thio analogues thereof

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Dentistry (AREA)
  • Plant Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Agronomy & Crop Science (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Toxicology (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention discloses a preparation method of a micro-capsule suspending-suspending agent containing pyraclostrobin and fluopyram. The preparation method includes the following steps that (1), a first solution is uniformly mixed with a second solution, and a first material is obtained; (2), a buffer solution is added into the first material, the pH value of the mixed solution is adjusted to be 5-7, and a second material is obtained; (3), an acidic pH regulator is added into the second material, the pH value of the mixed solution is adjusted to be 3-4, and a third solution is obtained; (4), the third material is subjected to solidification and condensation treatment, the pH value of a solidification and condensation product is adjusted to be 6.5-7.5, and a fourth material is obtained; (5), the fluopyram suspending agent is added into the fourth material, and a fifth material is obtained. The prepared micro-capsule suspending-suspending agent containing pyraclostrobin and fluopyram has better storage stability and can prevent and treat crop diseases in a slow-release manner in a long term, lower times for spraying of the suspending agent and reduce the dosage.

Description

The microcapsule suspension-suspendinagent agent and its system of a kind of pyraclostrobin-containing and fluopyram Preparation Method
Technical field
It relates to technical field of pesticide, in particular it relates to the microcapsule of a kind of pyraclostrobin-containing and fluopyram Suspension-suspending agent and preparation method thereof.
Background technology
Pyraclostrobin is a kind of new antibacterial, the effect with protection, treatment and blade infiltration conduction.Pyrazoles ether Bacterium ester has raising prevention effect, reduces dosage, reduces cost, delays what Drug resistance was produced with fluopyram compounding use Effect, but traditional pyraclostrobin fluopyram compounding suspending agent, exist and are susceptible to reunite, solidify, in the external world Under the conditions of easy failure shortcoming, cause to be difficult storage, prevention effect poor.
Therefore, need the medicament of a kind of new pyraclostrobin of exploitation and fluopyram badly, can with storage-stable and Extend the lasting period.
The content of the invention
The purpose of the disclosure is to provide the pharmaceutical preparations of a kind of pyraclostrobin and fluopyram, the pharmaceutical preparations storage The stable and lasting period is long.
To achieve these goals, present disclose provides the microcapsule suspension of a kind of pyraclostrobin-containing and fluopyram- The preparation method of suspending agent, the preparation method comprises the steps:(1) the first solution is mixed homogeneously with the second solution, is obtained First material;Wherein, first solution contains amino resins performed polymer aqueous solution, and second solution contains pyraclostrobin Cream, first solution is (1-5) with the weight ratio of second solution:1;(2) buffering is added in the first material Solution, it is 5-7 to adjust mixed solution pH value, obtains second material;(3) acidic ph modifier is added in the second material, It is 3-4 to adjust mixed solution pH value, obtains 3 material;(4) 3 material is carried out solidifying bunching process;Adjust described The pH value of solidification bunching product is 6.5-7.5, obtains 4 materials;(5) fluopyram is added to hang in the 4 materials Floating agent, obtains the 5th material;The 4 materials are 1 with the weight ratio of the fluopyram suspending agent:(0.1-1).
On the other hand, the disclosure additionally provides the pyraclostrobin-containing that prepared by above method and fluopyram Microcapsule suspension-suspendinagent agent.
By above-mentioned technical proposal, the pyraclostrobin fluopyram microcapsule prepared using disclosed method Suspension-suspending agent has preferable bin stability, being capable of slow release long-acting ground preventing and treating corps diseases, reduction times for spraying and use Dose, it is cost-effective, alleviate the pollution to environment.
Other feature and advantage of the disclosure will be described in detail in subsequent specific embodiment part.
Specific embodiment
Hereinafter specific embodiment of this disclosure is described in detail.It should be appreciated that described herein concrete Embodiment is merely to illustrate and explains the disclosure, is not limited to the disclosure.
Disclosure first aspect:A kind of system of the microcapsule suspension-suspendinagent agent of pyraclostrobin-containing and fluopyram is provided Preparation Method, the preparation method may include steps of:(1) the first solution is mixed homogeneously with the second solution, obtains the first thing Material;Wherein, first solution contains amino resins performed polymer aqueous solution, and second solution contains pyraclostrobin missible oil, First solution is (1-5) with the weight ratio of second solution:1;(2) buffer solution is added in the first material, It is 5-7 to adjust mixed solution pH value, obtains second material;(3) acidic ph modifier is added in the second material, adjusts mixed Conjunction solution ph is 3-4, obtains 3 material;(4) 3 material is carried out solidifying bunching process;Adjust the solidification poly- The pH value of contracting product is 6.5-7.5, obtains 4 materials;(5) fluopyram suspending agent is added in the 4 materials, is obtained To the 5th material;The 4 materials are 1 with the weight ratio of the fluopyram suspending agent:(0.1-1).
In the disclosure, pyraclostrobin (pyraclostrobin) chemical name is:N- [2- [[1- (4- chlorphenyls) pyrroles Azoles -3- bases] oxygen methyl] phenyl]-N- methoxy carbamate methyl ester;Molecular formula:C19H18ClN3O4, relative molecular weight 387.8, No. CAS:175013-18-0, structural formula is as follows:
Fluopyram (fluopyram), molecular formula C16H11ClF6N2O3, relative molecular weight 396.7, No. CAS: 658066-35-4, structural formula is as follows:
The pyraclostrobin fluopyram microcapsule suspension-suspendinagent agent prepared using disclosed method have compared with Good bin stability, can prevent and treat corps diseases slow release long-acting, reduce times for spraying and dosage, cost-effective, subtract The light pollution to environment.
According to the disclosure in a first aspect, the preparation method of amino resins performed polymer aqueous solution described in step (1) can be with From the conventional use of various methods of those skilled in the art, the disclosure has no particular limits to this;It is described under preferable case Amino resins performed polymer aqueous solution can be obtained by formaldehyde, containing amino-compound and water prepolymerization, the formaldehyde, the change containing amino Compound can be 1 with the weight ratio of water:(0.2-12.5):(2-7);The compound containing amino can include carbamide, trimerization At least one in cyanamide and benzoguanamine;The prepolymerized condition includes:PH value can be 8-10, and temperature can be 60-80 DEG C, the response time can be 0.5-3 hours.
According to the disclosure in a first aspect, the preparation method of pyraclostrobin missible oil described in step (1) can from this The conventional use of various methods of art personnel, the disclosure has no particular limits to this;Under preferable case, the pyrazoles ether Bacterium emulsifiable concentrate can contain pyraclostrobin, organic solvent and emulsifying agent;The organic solvent can include petroleum ether, acetic acid second At least one in ester, methyl oleate, dimethylbenzene and solvent naphtha, the emulsifying agent can include sodium lignin sulfonate, dodecane Base sodium sulfate, dodecylbenzene sodium sulfonate, styrene-maleic anhydride copolymer, fatty alcohol-polyoxyethylene ether, anhydrous sorbitol gather Oxygen ethylene polyethenoxy ether, sorbitan monostearate polyoxyethylene ether, sodium laurylsulfate, polyvinyl alcohol, polycarboxylic acids At least one in salt and naphthalene sulfonate;In order to further lift the pollution of the feature of environmental protection, reduction of composition pesticide to environment, institute The weight ratio for stating pyraclostrobin, organic solvent and emulsifying agent can be 1:(0.1-5):(0.01-0.2).
According to the disclosure in a first aspect, the clad ratio of microcapsule, uniform can be improved using the method for adjusted stepwise pH value Degree and softgel shell compactness, so as to further improve the storage of the microcapsule suspension-suspendinagent agent of pyraclostrobin-containing and fluopyram Deposit stability and prevention effect:Add buffer solution to adjust pH value in the first material in step (2) and obtain second for 5-7 Material, right containing buffering in the buffer solution, the buffering is to adopting those skilled in the art conventional use of various Material, under preferable case, the buffering is to including citric acid-sodium citrate, citrate-phosphate disodium hydrogen and acetic acid-second At least one in sour sodium, the concentration of the buffer solution can be 1-5 weight %, and pH value is 3-5.5;To institute in step (3) State addition acidic ph modifier regulation pH value in the second solution and obtain 3 material for 3-4, the acidic ph modifier can be adopted With the conventional use of various materials for reducing pH value of those skilled in the art, under preferable case, the acidic ph modifier can be with Including at least one in hydrochloric acid, sulphuric acid, phosphoric acid, acetic acid and ammonium chloride, the concentration of the acidic ph modifier can be 1-10 Weight %;The pH value that the solidification bunching product is adjusted in step (4) is 6.5-7.5, and the method for adjusting pH value can be ability The conventional use of various methods of field technique personnel, the disclosure has no particular limits to this.
Can include in a first aspect, solidifying the condition of bunching process described in step (4) according to the disclosure:40 DEG C- 2-7 hour is processed under the conditions of 70 DEG C.
According to the disclosure in a first aspect, in order to avoid suspending agent occur aggregation, precipitation, hardened phenomenon, preferable case Under can also be containing at least one in dispersant, thickening agent, antifreezing agent in the 4 materials;The solidification bunching product, The dispersant, the thickening agent, the weight ratio of the antifreezing agent are 1:(0.01-0.2):(0.001-0.002):(0.02- 0.15)。
According to the disclosure in a first aspect, the preparation method of fluopyram suspending agent can be adopted described in step (5) The conventional use of various methods of those skilled in the art, the disclosure has no particular limits to this.Under preferable case, the fluorine pyrrole Bacterium amide contains 1-5 μm of fluopyram, water and adjuvant, the weight ratio of the fluopyram, water and the adjuvant For 1:(2-4):(0.5-1);Preferably, the adjuvant is included in dispersant, thickening agent, defoamer, antifreezing agent and preservative At least one;The fluopyram, the dispersant, the thickening agent, the defoamer, the antifreezing agent and described anti- The weight ratio of rotten agent can be 1:(0.1-0.5):(0.01-0.02):(0.01-0.02):(0.1-0.5):(0.005-0.01).
Dispersant, thickening agent, defoamer, antifreezing agent and preservative described in above technical scheme can adopt this area skill The conventional use of various materials of art personnel, the disclosure has no particular limits to this.Under preferable case, the dispersant can be wrapped Include dodecylbenzene sodium sulfonate, sodium methylene bis-naphthalene sulfonate, 1- methyl naphthalene sulfonate formaldehyde condensates, the contracting of benzyl naphthalenesulfonateformaldehyde formaldehyde Compound, sodium lignin sulfonate, desaccharide sodium lignin sulfonate, desaccharide are condensed sodium lignin sulfonate, Succinate sodium sulfonate, pull open At least one in powder, NPE and fatty alcohol-polyoxyethylene ether;The thickening agent can include Magnesiumaluminumsilicate, At least one in xanthan gum, Polyethylene Glycol, polyvinyl alcohol, carboxymethyl cellulose, bentonite and white carbon;The defoamer can With including at least one in polyether antifoam agent and organic silicon defoamer;The antifreezing agent can include ethylene glycol, 1,2- the third two At least one in alcohol, glycerol and carbamide;The preservative can include sodium benzoate, benzoic acid, sorbic acid and sorbic acid At least one in potassium.
According to the disclosure in a first aspect, described in step (1) mix condition can include:60-80 DEG C, mixing speed For 1500-3000 rev/min;The condition mixed described in step (2) can include:40-70 DEG C, mixing speed is 1000- 1200 revs/min;The condition mixed described in step (3) can include:40-70 DEG C, mixing speed is 1200-1500 DEG C.
The second aspect of the disclosure, there is provided pyraclostrobin-containing and fluorine pyrrole that as described above method is prepared The microcapsule suspension-suspendinagent agent of bacterium amide.
The disclosure is further described by the following examples, is not limited to the disclosure.
In embodiment and comparative example, pyraclostrobin is purchased from Huifeng Agricultural Chemistry Co., Ltd., Jiangsu;Fluopyram is purchased From Bayer Bitterfeld GmbH crop science company;Tripolycyanamide is purchased from Beijing Chemical Plant;Carbamide is purchased from Beijing Chemical Plant;Benzoguanamine Purchased from Beijing Chemical Plant;Formaldehyde is purchased from Beijing Chemical Plant;Sorbitan monostearate polyoxyethylene ether is changed very much purchased from Nanjing Chemical Co., Ltd.;Sodium lauryl sulphate is purchased from Beijing Science and Technology Ltd. of Zhong Chuan HTC;Sodium lignin sulfonate is purchased from Beijing Science and Technology Ltd. of Zhong Chuan HTC;Dodecylbenzene sodium sulfonate is purchased from Beijing Science and Technology Ltd. of Zhong Chuan HTC;Polyvinyl alcohol is purchased From Zhengzhou Ao Cai industrial chemicals company limited;Fatty alcohol-polyoxyethylene ether is purchased from Xingtai blue star auxiliary reagent factory;Magnesiumaluminumsilicate is purchased from lake Nan Pengtai new high-tech materials company limited;Bentonite is purchased from Anji County, Zhejiang Province Gekko Swinhonis organobentonite company limited;Organic silicon defoamer Purchased from Shanghai Mitugao New Material Group;Ethylene glycol, glycerol and 1,2- Propylene Glycol are purchased from Beijing Chemical Plant;Xanthan gum is purchased from mountain Dong Zhong pavilions limited company;Sodium benzoate is purchased from the magnificent Zhi Bo Science and Technology Ltd.s in Beijing;200# solvent naphthas are purchased from Jiangsu China Human relations Chemical Co., Ltd.;150# solvent naphthas are purchased from Hualun Chemical Co., Ltd., Jiangsu;Petroleum ether is limited purchased from western Gansu Province chemical industry share Company;Ethyl acetate is purchased from Xilong Chemical Co., Ltd.
Embodiment 1
It is 8 in pH value by the mixing of tripolycyanamide, formaldehyde and water, temperature obtains melamine to react 1.5h under the conditions of 70 DEG C Amine-for-aldehyde resin prepolymer aqueous solution, wherein, the weight ratio of formaldehyde, tripolycyanamide and water is 1:2.1:2.8.
By pyraclostrobin, 200# solvent naphthas and sorbitan monostearate polyoxyethylene ether mix homogeneously, obtain Pyraclostrobin missible oil, wherein, the pyraclostrobin, 200# solvent naphthas and sorbitan monostearate polyoxyethylene ether Weight ratio be 1:2.5:0.05.
By weight it is 4 by melamine formaldehyde resin performed polymer aqueous solution and pyraclostrobin missible oil:1 with 2000 turns/ The mixing speed mix homogeneously of minute, obtains first material;Then at ambient temperature, by pH value be 4.5, buffering to it is total dense Acetic acid-the sodium acetate buffer solution for 2 weight % is spent, was evenly added in the first material, with 1000 in 1 hour Rev/min mixing speed mix homogeneously, obtain the second material that pH value is adjusted to 6.2;At ambient temperature, it is by concentration The hydrochloric acid of 5 weight % was evenly added in the second material in 1.5 hours, mixed with 1200 revs/min of mixing speed Close uniform, obtain the 3 material that pH value is adjusted to 3.2;Under conditions of 60 DEG C, the 3 material is processed 2 hours, Obtain solidifying bunching product, the triethanolamine for adding 5 weight % adjusts the pH value of the solidification bunching product to 7, adds wood Quality sodium sulfonate, Magnesiumaluminumsilicate and ethylene glycol mix homogeneously, obtain 4 materials, i.e. pyraclostrobin microcapsule suspending agent, wherein, The solidification bunching product is 1 with the weight ratio of sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol:0.01:0.005:0.05.
By fluopyram (content is 95%), the sodium lauryl sulphate of 2 weight %, 6 weight % of 26.3 weight % Sodium lignin sulfonate, the organic silicon defoamer of 0.2 weight %, the ethylene glycol of 5 weight %, the xanthan gum of 0.3 weight %, 0.2 The sodium benzoate of weight % is sufficiently mixed, disperses with the water of 60 weight %, and sand mill is passed through after being uniformly dispersed carries out sand milling, sand milling To suspension of the mean diameter less than 5 microns, fluopyram suspending agent is obtained.
Finally, pyraclostrobin microcapsule suspending agent is mixed with fluopyram suspending agent, adds sodium lignin sulfonate And water, stir, obtain the 5th material, i.e. pyraclostrobin fluopyram microcapsule suspension-suspendinagent agent.Wherein, pyrazoles Kresoxim-methyl microcapsule suspending agent is 1 with the weight ratio of fluopyram suspending agent, sodium lignin sulfonate:0.3:0.05.
Embodiment 2
It is 8 in pH value by the mixing of tripolycyanamide, formaldehyde and water, temperature obtains melamine to react 1.5h under the conditions of 70 DEG C Amine-for-aldehyde resin prepolymer aqueous solution, wherein, the weight ratio of formaldehyde, tripolycyanamide and water is 1:4.2:3.5.
By pyraclostrobin, 150# solvent naphthas and sodium lignin sulfonate mix homogeneously, pyraclostrobin missible oil is obtained, its In, the weight ratio of the pyraclostrobin, 150# solvent naphthas and sodium lignin sulfonate is 1:0.5:0.1.
By weight it is 2 by melamine formaldehyde resin performed polymer aqueous solution and pyraclostrobin missible oil:1 with 1500 turns/ The mixing speed mix homogeneously of minute, obtains first material;Then at ambient temperature, by pH value be 3, buffering to total concentration For the acetic acid-sodium acetate buffer solution of 2 weight %, be evenly added in 1 hour in the first material, with 1100 turns/ The mixing speed mix homogeneously of minute, obtains the second material that pH value is adjusted to 6;At ambient temperature, it is 6 weights by concentration The hydrochloric acid of amount % was evenly added in the second material in 1 hour, equal with 1300 revs/min of mixing speed mixing It is even, obtain the 3 material that pH value is adjusted to 3;Under conditions of 50 DEG C, the 3 material is processed 4 hours, consolidate Change bunching product, and add the triethanolamine of 5 weight % the pH value of the solidification bunching product to be adjusted to 7, add dodecane Base benzene sulfonic acid sodium salt, xanthan gum and glycerol, mix homogeneously obtains 4 materials, i.e. pyraclostrobin microcapsule suspending agent, wherein, The solidification bunching product is 1 with the weight ratio of dodecylbenzene sodium sulfonate, xanthan gum and glycerol:0.05:0.01:0.1.
By fluopyram (content is 95%), the sodium lauryl sulphate of 2 weight %, 6 weight % of 26.3 weight % Sodium lignin sulfonate, the organic silicon defoamer of 0.2 weight %, the ethylene glycol of 5 weight %, the xanthan gum of 0.3 weight %, 0.2 The sodium benzoate of weight % is sufficiently mixed, disperses with the water of 60 weight %, and sand mill is passed through after being uniformly dispersed carries out sand milling, sand milling To suspension of the mean diameter less than 5 microns, fluopyram suspending agent is obtained.
Finally, pyraclostrobin microcapsule suspending agent is mixed with fluopyram suspending agent, adds sodium lignin sulfonate And water, stir, obtain the 5th material, i.e. pyraclostrobin fluopyram microcapsule suspension-suspendinagent agent.Wherein, pyrazoles Kresoxim-methyl microcapsule suspending agent is 1 with the weight ratio of fluopyram suspending agent, sodium lignin sulfonate:0.5:0.1.
Embodiment 3
It is 8 in pH value by the mixing of tripolycyanamide, formaldehyde and water, temperature obtains melamine to react 1.5h under the conditions of 70 DEG C Amine-for-aldehyde resin prepolymer aqueous solution, wherein, the weight ratio of formaldehyde, tripolycyanamide and water is 1:6.3:5.
By pyraclostrobin, 200# solvent naphthas and sorbitan monostearate polyoxyethylene ether mix homogeneously, obtain Pyraclostrobin missible oil, wherein, the pyraclostrobin, 200# solvent naphthas and sorbitan monostearate polyoxyethylene ether Weight ratio be 1:3:0.15.
By weight it is 3 by melamine formaldehyde resin performed polymer aqueous solution and pyraclostrobin missible oil:1 with 2500 turns/ The mixing speed mix homogeneously of minute, obtains first material;Then at ambient temperature, by pH value be 3.8, buffering to it is total dense Acetic acid-the sodium acetate buffer solution for 0.55 weight % is spent, was evenly added in 1.5 hours in the first material, with 1200 revs/min of mixing speed mix homogeneously, obtains the second material that pH value is adjusted to 5.5;At ambient temperature, will be dense Spend the hydrochloric acid for 5 weight % to be evenly added in 1 hour in the second material, with 1400 revs/min of mixing speed Mix homogeneously, obtains the 3 material that pH value is adjusted to 3.5;Under conditions of 45 DEG C, the 3 material is processed into 6 little When, obtain solidifying bunching product, and add the triethanolamine of 5 weight % the pH value of the solidification bunching product to be adjusted to 7, plus Enter sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol mix homogeneously, obtain 4 materials, i.e. pyraclostrobin microcapsule suspending agent, Wherein, the solidification bunching product and the weight ratio of sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol are 1:0.1:0.015: 0.15。
By fluopyram (content is 95%), the sodium lauryl sulphate of 2 weight %, 6 weight % of 26.3 weight % Sodium lignin sulfonate, the organic silicon defoamer of 0.2 weight %, the ethylene glycol of 5 weight %, the xanthan gum of 0.3 weight %, 0.2 The sodium benzoate of weight % is sufficiently mixed, disperses with the water of 60 weight %, and sand mill is passed through after being uniformly dispersed carries out sand milling, sand milling To suspension of the mean diameter less than 5 microns, fluopyram suspending agent is obtained.
Finally, pyraclostrobin microcapsule suspending agent is mixed with fluopyram suspending agent, adds sodium lignin sulfonate And water, stir, obtain the 5th material, i.e. pyraclostrobin fluopyram microcapsule suspension-suspendinagent agent.Wherein, pyrazoles Kresoxim-methyl microcapsule suspending agent is 1 with the weight ratio of fluopyram suspending agent, sodium lignin sulfonate:0.8:1.
Embodiment 4
It is 8 in pH value by the mixing of tripolycyanamide, formaldehyde and water, temperature obtains melamine to react 1.5h under the conditions of 70 DEG C Amine-for-aldehyde resin prepolymer aqueous solution, wherein, the weight ratio of formaldehyde, tripolycyanamide and water is 1:8.4:7.
By pyraclostrobin, petroleum ether and sodium lauryl sulphate mix homogeneously, pyraclostrobin missible oil is obtained, wherein, The weight ratio of the pyraclostrobin, petroleum ether and sodium lauryl sulphate is 1:5:0.2.
By weight it is 5 by melamine formaldehyde resin performed polymer aqueous solution and pyraclostrobin missible oil:1 with 3000 turns/ The mixing speed mix homogeneously of minute, obtains first material;Then at ambient temperature, by pH value be 4.5, buffering to it is total dense Acetic acid-the sodium acetate buffer solution for 2 weight % is spent, was evenly added in the first material, with 1200 in 1 hour Rev/min mixing speed mix homogeneously, obtain the second material that pH value is adjusted to 6.5;At ambient temperature, it is by concentration The hydrochloric acid of 5 weight % was evenly added in the second material in 1.5 hours, mixed with 1500 revs/min of mixing speed Close uniform, obtain the 3 material that pH value is adjusted to 3.7;Under conditions of 60 DEG C, the 3 material is processed 2 hours, Obtain solidifying bunching product, and add the triethanolamine of 5 weight % the pH value of the solidification bunching product to be adjusted to 7, add Fatty alcohol-polyoxyethylene ether, bentonite and 1,2-PD mix homogeneously, obtain pyraclostrobin microcapsule suspending agent, wherein, institute It is 1 that solidification bunching product is stated with the weight ratio of fatty alcohol-polyoxyethylene ether, bentonite and 1,2- Propylene Glycol:0.2:0.02:0.15.
By fluopyram (content is 95%), the sodium lauryl sulphate of 2 weight %, 6 weight % of 26.3 weight % Sodium lignin sulfonate, the organic silicon defoamer of 0.2 weight %, the ethylene glycol of 5 weight %, the xanthan gum of 0.3 weight %, 0.2 The sodium benzoate of weight % is sufficiently mixed, disperses with the water of 60 weight %, and sand mill is passed through after being uniformly dispersed carries out sand milling, sand milling To suspension of the mean diameter less than 5 microns, fluopyram suspending agent is obtained.
Finally, pyraclostrobin microcapsule suspending agent is mixed with fluopyram suspending agent, adds sodium lignin sulfonate And water, stir, obtain the 5th material, i.e. pyraclostrobin fluopyram microcapsule suspension-suspendinagent agent.Wherein, pyrazoles Kresoxim-methyl microcapsule suspending agent is 1 with the weight ratio of fluopyram suspending agent, sodium lignin sulfonate:1:2.
Embodiment 5
It is 8 in pH value by the mixing of tripolycyanamide, formaldehyde and water, temperature obtains melamine to react 1.5h under the conditions of 70 DEG C Amine-for-aldehyde resin prepolymer aqueous solution, wherein, the weight ratio of formaldehyde, tripolycyanamide and water is 1:0.42:2.
By pyraclostrobin, 200# solvent naphthas and sorbitan monostearate polyoxyethylene ether mix homogeneously, obtain Pyraclostrobin missible oil, wherein, the pyraclostrobin, 200# solvent naphthas and sorbitan monostearate polyoxyethylene ether Weight ratio be 1:0.1:0.01.
By weight it is 1 by melamine formaldehyde resin performed polymer aqueous solution and pyraclostrobin missible oil:1 with 2000 turns/ The mixing speed mix homogeneously of minute, obtains first material;Then at ambient temperature, by pH value be 4.5, buffering to it is total dense The citrate-phosphate disodium hydrogen buffer solution for 2 weight % is spent, was evenly added in 1 hour in the first material, with 1100 revs/min of mixing speed mix homogeneously, obtains the second material that pH value is adjusted to 7;At ambient temperature, by concentration Hydrochloric acid for 5 weight % was evenly added in the second material in 1.5 hours, with 1300 revs/min of mixing speed Mix homogeneously, obtains the 3 material that pH value is adjusted to 4;Under conditions of 60 DEG C, the 3 material is processed 2 hours, Obtain solidifying bunching product, and add the triethanolamine of 5 weight % the pH value of the solidification bunching product to be adjusted to 7, add Sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol mix homogeneously, obtain 4 materials, i.e. pyraclostrobin microcapsule suspending agent, its In, the solidification bunching product is 1 with the weight ratio of sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol:0.02:0.001: 0.02。
By fluopyram (content is 95%), the sodium lauryl sulphate of 2 weight %, 6 weight % of 26.3 weight % Sodium lignin sulfonate, the organic silicon defoamer of 0.2 weight %, the ethylene glycol of 5 weight %, the xanthan gum of 0.3 weight %, 0.2 The sodium benzoate of weight % is sufficiently mixed, disperses with the water of 60 weight %, and sand mill is passed through after being uniformly dispersed carries out sand milling, sand milling To suspension of the mean diameter less than 5 microns, fluopyram suspending agent is obtained.
Finally, pyraclostrobin microcapsule suspending agent is mixed with fluopyram suspending agent, adds sodium lignin sulfonate And water, stir, obtain the 5th material, i.e. pyraclostrobin fluopyram microcapsule suspension-suspendinagent agent.Wherein, pyrazoles Kresoxim-methyl microcapsule suspending agent is 1 with the weight ratio of fluopyram suspending agent, sodium lignin sulfonate:0.2:0.5.
Embodiment 6
It is 8 in pH value by the mixing of tripolycyanamide, formaldehyde and water, temperature obtains melamine to react 1.5h under the conditions of 70 DEG C Amine-for-aldehyde resin prepolymer aqueous solution, wherein, the weight ratio of formaldehyde, tripolycyanamide and water is 1:0.84:2.5.
Pyraclostrobin, ethyl acetate and polyvinyl alcohol is uniform, pyraclostrobin missible oil is obtained, wherein, it is described The weight ratio of pyraclostrobin, ethyl acetate and polyvinyl alcohol is 1:1.5:0.02.
By weight it is 4 by melamine formaldehyde resin performed polymer aqueous solution and pyraclostrobin missible oil:1 with 2000 turns/ The mixing speed mix homogeneously of minute, obtains first material;Then at ambient temperature, by pH value be 4.5, buffering to it is total dense Acetic acid-the sodium acetate buffer solution for 2 weight % is spent, was evenly added in the first material, with 1000 in 0.5 hour Rev/min mixing speed mix homogeneously, obtain the second material that pH value is adjusted to 6.2;At ambient temperature, it is by concentration The hydrochloric acid of 5 weight % was evenly added in the second material in 1.5 hours, mixed with 1200 revs/min of mixing speed Close uniform, obtain the 3 material that pH value is adjusted to 3.2;Under conditions of 60 DEG C, the 3 material is processed 2 hours, Obtain solidifying bunching product, and add the triethanolamine of 5 weight % the pH value of the solidification bunching product to be adjusted to 7, add Sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol mix homogeneously, obtain 4 materials, i.e. pyraclostrobin microcapsule suspending agent, its In, the solidification bunching product is 1 with the weight ratio of sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol:0.15:0.002: 0.04。
By fluopyram (content is 95%), the sodium lauryl sulphate of 2 weight %, 6 weight % of 26.3 weight % Sodium lignin sulfonate, the organic silicon defoamer of 0.2 weight %, the ethylene glycol of 5 weight %, the xanthan gum of 0.3 weight %, 0.2 The sodium benzoate of weight % is sufficiently mixed, disperses with the water of 60 weight %, and sand mill is passed through after being uniformly dispersed carries out sand milling, sand milling To suspension of the mean diameter less than 5 microns, fluopyram suspending agent is obtained.
Finally, pyraclostrobin microcapsule suspending agent is mixed with fluopyram suspending agent, adds sodium lignin sulfonate And water, stir, obtain the 5th material, i.e. pyraclostrobin fluopyram microcapsule suspension-suspendinagent agent.Wherein, pyrazoles Kresoxim-methyl microcapsule suspending agent is 1 with the weight ratio of fluopyram suspending agent, sodium lignin sulfonate:0.1:0.01.
Embodiment 7
It is 8 in pH value by the mixing of carbamide, formaldehyde and water, temperature obtains urea-formaldehyde to react 1.5h under the conditions of 70 DEG C Resin prepolymer aqueous solution, wherein, the weight ratio of formaldehyde, carbamide and water is 1:4:2.8.
By pyraclostrobin, 200# solvent naphthas and sorbitan monostearate polyoxyethylene ether mix homogeneously, obtain Pyraclostrobin missible oil, wherein, the pyraclostrobin, 200# solvent naphthas and sorbitan monostearate polyoxyethylene ether Weight ratio be 1:2.5:0.05.
By weight it is 4 by urea-formaldehyde resin performed polymer aqueous solution and pyraclostrobin missible oil:1 with 2000 revs/min Mixing speed mix homogeneously, obtain first material;Then at ambient temperature, by pH value be 4.5, buffering to total concentration be Acetic acid-the sodium acetate buffer solution of 2 weight %, was evenly added in the first material in 1.5 hours, with 1000 turns/ The mixing speed mix homogeneously of minute, obtains the second material that pH value is adjusted to 6.2;At ambient temperature, it is 5 weights by concentration The hydrochloric acid of amount % was evenly added in the second material in 1.5 hours, equal with 1200 revs/min of mixing speed mixing It is even, obtain the 3 material that pH value is adjusted to 3.2;Under conditions of 60 DEG C, the 3 material is processed 2 hours, obtained Solidification bunching product, and add the triethanolamine of 5 weight % the pH value of the solidification bunching product to be adjusted to 7, add wooden Plain sodium sulfonate, Magnesiumaluminumsilicate and ethylene glycol mix homogeneously, obtain 4 materials, i.e. pyraclostrobin microcapsule suspending agent, wherein, institute It is 1 that solidification bunching product is stated with the weight ratio of sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol:0.01:0.005:0.05.
By fluopyram (content is 95%), the sodium lauryl sulphate of 2 weight %, 6 weight % of 26.3 weight % Sodium lignin sulfonate, the organic silicon defoamer of 0.2 weight %, the ethylene glycol of 5 weight %, the xanthan gum of 0.3 weight %, 0.2 The sodium benzoate of weight % is sufficiently mixed, disperses with the water of 60 weight %, and sand mill is passed through after being uniformly dispersed carries out sand milling, sand milling To suspension of the mean diameter less than 5 microns, fluopyram suspending agent is obtained.
Finally, pyraclostrobin microcapsule suspending agent is mixed with fluopyram suspending agent, adds sodium lignin sulfonate And water, stir, obtain the 5th material, i.e. pyraclostrobin fluopyram microcapsule suspension-suspendinagent agent.Wherein, pyrazoles Kresoxim-methyl microcapsule suspending agent is 1 with the weight ratio of fluopyram suspending agent, sodium lignin sulfonate:0.3:0.05.
Embodiment 8
It is 8 in pH value by the mixing of carbamide, formaldehyde and water, temperature obtains urea-formaldehyde to react 1.5h under the conditions of 70 DEG C Resin prepolymer aqueous solution, wherein, the weight ratio of formaldehyde, carbamide and water is 1:2:2.8.
By pyraclostrobin, 200# solvent naphthas and sorbitan monostearate polyoxyethylene ether mix homogeneously, obtain Pyraclostrobin missible oil, wherein, the pyraclostrobin, 200# solvent naphthas and sorbitan monostearate polyoxyethylene ether Weight ratio be 1:2:0.06.
By weight it is 3 by urea-formaldehyde resin performed polymer aqueous solution and pyraclostrobin missible oil:1 with 2000 revs/min Mixing speed mix homogeneously, obtain first material;Then at ambient temperature, by pH value be 3.6, buffering to total concentration be The citric acid-sodium citrate buffer of 4 weight %, was evenly added in the first material, with 1000 in 1 hour Rev/min mixing speed mix homogeneously, obtain the second material that pH value is adjusted to 6.2;At ambient temperature, it is by concentration The phosphoric acid of 4 weight % was evenly added in the second material in 1.5 hours, mixed with 1200 revs/min of mixing speed Close uniform, obtain the 3 material that pH value is adjusted to 3.2;Under conditions of 60 DEG C, the 3 material is processed 2 hours, Obtain solidifying bunching product, and add the triethanolamine of 5 weight % the pH value of the solidification bunching product to be adjusted to 6.5, plus Enter sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol mix homogeneously, obtain 4 materials, i.e. pyraclostrobin microcapsule suspending agent, Wherein, the solidification bunching product and the weight ratio of sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol are 1:0.02:0.004: 0.04。
By fluopyram (content is 95%), the sodium lauryl sulphate of 2 weight %, 6 weight % of 26.3 weight % Sodium lignin sulfonate, the organic silicon defoamer of 0.2 weight %, the ethylene glycol of 5 weight %, the xanthan gum of 0.3 weight %, 0.2 The sodium benzoate of weight % is sufficiently mixed, disperses with the water of 60 weight %, and sand mill is passed through after being uniformly dispersed carries out sand milling, sand milling To suspension of the mean diameter less than 5 microns, fluopyram suspending agent is obtained.
Finally, pyraclostrobin microcapsule suspending agent is mixed with fluopyram suspending agent, adds sodium lignin sulfonate And water, stir, obtain the 5th material, i.e. pyraclostrobin fluopyram microcapsule suspension-suspendinagent agent.Wherein, pyrazoles Kresoxim-methyl microcapsule suspending agent is 1 with the weight ratio of fluopyram suspending agent, sodium lignin sulfonate:0.2:0.03.
Embodiment 9
It is 8 in pH value by the mixing of benzoguanamine, formaldehyde and water, temperature obtains benzene to react 1.5h under the conditions of 70 DEG C Substituted melamine-formaldehyde resin performed polymer aqueous solution, wherein, the weight ratio of formaldehyde, benzoguanamine and water is 1:3.2: 2.8。
By pyraclostrobin, 200# solvent naphthas and sorbitan monostearate polyoxyethylene ether mix homogeneously, obtain Pyraclostrobin missible oil, wherein, the pyraclostrobin, 200# solvent naphthas and sorbitan monostearate polyoxyethylene ether Weight ratio be 1:2:0.06.
By weight it is 4 by benzoguanamine-formaldehyde resin performed polymer aqueous solution and pyraclostrobin missible oil:1 with 2000 revs/min of mixing speed mix homogeneously, obtains first material;Then at ambient temperature, it is that 4, buffering is right by pH value Total concentration be 4 weight % citric acid-sodium citrate buffer, the first material was evenly added in 1 hour In, with 1000 revs/min of mixing speed mix homogeneously, obtain the second material that pH value is adjusted to 6.2;In room temperature condition Under, the sulphuric acid that concentration is 5 weight % was evenly added in the second material in 1.5 hours, with 1200 revs/min Mixing speed mix homogeneously, obtains the 3 material that pH value is adjusted to 3.2;Under conditions of 60 DEG C, by the 3 material Process 2 hours, obtain solidifying bunching product, and add the triethanolamine of 5 weight % to adjust the pH value of the solidification bunching product Save to 7.5, add sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol mix homogeneously, obtain 4 materials, i.e. pyraclostrobin micro- Capsule suspending agent, wherein, the solidification bunching product is 1 with the weight ratio of sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol: 0.03:0.005:0.05.
By fluopyram (content is 95%), the sodium lauryl sulphate of 2 weight %, 6 weight % of 26.3 weight % Sodium lignin sulfonate, the organic silicon defoamer of 0.2 weight %, the ethylene glycol of 5 weight %, the xanthan gum of 0.3 weight %, 0.2 The sodium benzoate of weight % is sufficiently mixed, disperses with the water of 60 weight %, and sand mill is passed through after being uniformly dispersed carries out sand milling, sand milling To suspension of the mean diameter less than 5 microns, fluopyram suspending agent is obtained.
Finally, pyraclostrobin microcapsule suspending agent is mixed with fluopyram suspending agent, adds sodium lignin sulfonate And water, stir, obtain the 5th material, i.e. pyraclostrobin fluopyram microcapsule suspension-suspendinagent agent.Wherein, pyrazoles Kresoxim-methyl microcapsule suspending agent is 1 with the weight ratio of fluopyram suspending agent, sodium lignin sulfonate:0.15:0.04.
Comparative example 1
It is after obtaining first material, to adjust pH value without acetic acid-sodium acetate buffer solution, directly with the difference of embodiment 1 Connect and adopt concentration the pH value of material is adjusted to into 3.2 for the hydrochloric acid of 5 weight %.
Comparative example 2
It is 3.2 without the salt acid for adjusting pH value for adding 5 weight % after obtaining second material to be with the difference of embodiment 1 The step of, directly second material is carried out to solidify bunching process.
Comparative example 3
It is to obtain solidifying after bunching product with the difference of embodiment 1, does not adjust pH for 7.
Comparative example 4
It is after obtaining first material, to be adjusted using the acetic acid-sodium acetate buffer solution of 2 weight % with the difference of embodiment 1 Section mixed solution pH value obtains second material for 4.
Comparative example 5
It is after obtaining first material, to be adjusted using the acetic acid-sodium acetate buffer solution of 2 weight % with the difference of embodiment 1 The pH value of section mixed solution obtains second material for 8.
Comparative example 6
It is after obtaining second material, using the hydrochloric acid of 5 weight % the pH of mixed solution to be adjusted with the difference of embodiment 1 It is worth and obtains 3 material for 2.
Comparative example 7
It is after obtaining second material, using the hydrochloric acid of 5 weight % the pH of mixed solution to be adjusted with the difference of embodiment 1 It is worth and obtains 3 material for 5.
Comparative example 8
It is to obtain solidifying after bunching product with the difference of embodiment 1, using the triethanolamine of 5 weight % mixing is adjusted The pH value of solution is 6, adds sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol mix homogeneously, obtains 4 materials.
Comparative example 9
It is to obtain solidifying after bunching product with the difference of embodiment 1, using the triethanolamine of 5 weight % mixing is adjusted The pH value of solution is 8, adds sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol mix homogeneously, obtains 4 materials.
Comparative example 10
By pyraclostrobin, 200# solvent naphthas and sorbitan monostearate polyoxyethylene ether mix homogeneously, obtain Pyraclostrobin missible oil, wherein, the pyraclostrobin, 200# solvent naphthas and sorbitan monostearate polyoxyethylene ether Weight ratio be 1:2.5:0.05.Method same as Example 1 prepares fluazinam suspending agent, by pyraclostrobin missible oil and fluorine pyridine Amine suspending agent is 1 by weight:0.3 mixing, obtains the micro- suspension emulsion of pyraclostrobin fluopyram.
Comparative example 11
By pyraclostrobin, 200# solvent naphthas and sorbitan monostearate polyoxyethylene ether mix homogeneously, obtain Pyraclostrobin oil phase, water is slowly dropped in pyraclostrobin oil phase, is stirred in Deca, and adds ethylene glycol and xanthan Glue, obtains the pyraclostrobin aqueous emulsion of 25 weight %.Wherein, the pyraclostrobin, 200# solvent naphthas, anhydrous sorbitol list The weight ratio of stearate polyoxyethylene ether, water, ethylene glycol and xanthan gum is 1:2.5:0.05:1.2:0.005:0.001.
Comparative example 12
By fluopyram (content is 95%), the sodium lauryl sulphate of 2 weight %, 6 weight % of 26.3 weight % Sodium lignin sulfonate, the organic silicon defoamer of 0.2 weight %, the ethylene glycol of 5 weight %, the xanthan gum of 0.3 weight %, 0.2 The sodium benzoate of weight % is sufficiently mixed, disperses with the water of 60 weight %, and sand mill is passed through after being uniformly dispersed carries out sand milling, sand milling To suspension of the mean diameter less than 5 microns, fluopyram suspending agent is obtained.
Testing example 1
This testing example is used for the pyraclostrobin fluorine pyrrole bacterium acyl obtained in testing example 1-9 and comparative example 1-9 The heat storage stability of the micro- suspension emulsion of pyraclostrobin fluopyram obtained in amine microcapsule suspension-suspendinagent agent and comparative example 10 And low-temperature stability.
Heat storage stability is tested:The pyraclostrobin fluopyram obtained in embodiment 1-9 and comparative example 1-9 is micro- The micro- suspension emulsion of pyraclostrobin fluopyram obtained in capsule suspension-suspending agent and comparative example 10 is fitted in container, sealing In being positioned over the constant temperature oven of (54 ± 2) DEG C afterwards, take out after standing 14 days, according to GB/T14825-2006 standards, determine and suspend Rate, the results are shown in Table 1.
Low-temperature stability is determined:The pyraclostrobin fluopyram obtained in embodiment 1-9 and comparative example 1-9 is micro- The micro- suspension emulsion of pyraclostrobin fluopyram obtained in capsule suspension-suspending agent and comparative example 10 is fitted in container, sealing After be placed in (0 ± 2) DEG C refrigerator, keep 1h, at interval of 15min stir once, each 15s, observation outward appearance have unchanged, (0 ± 2) DEG C continues to place 7 days, then takes out and is placed under room temperature condition after standing recovery, according to GB/T14825-2006 standards, Suspensibility is determined, 1 is the results are shown in Table.
Table 1
As it can be seen from table 1 the pyrazoles ether bacterium that the preparation method in the preparation method and comparative example of present invention offer is obtained Ester fluopyram microcapsule suspension-suspendinagent agent is compared with more preferable thermal storage stability and low tempertaure storage stability,.
Testing example 2
This testing example is used to determine the preventing and treating of embodiment 1-9, comparative example 1-12 Pesticides medicament to citrus anthracnose Effect.A certain amount of distilled water is added before test, is stirred, the active component adjusted respectively in each embodiment, comparative example is dense Spend for 10 weight %.
Test site:Chenzhou, Hunan Province Hua Tang towns, experimental plot is Citrus planting base for many years, and experimental plot physical features is flat, fertility It is medium, earth in quality.Each treatment region Citrus after dispenser routinely production management.
Concrete steps include, are 30kg/ mus according to formulation rate, by embodiment 1-9, comparative example using knapsack sprayer Medicinal liquid after the adjustment concentration of 1-12 is sprayed respectively to the Citrus plant of each growing area, and blank control group is clear using equivalent Water is sprayed to the Citrus plant in growing area.
After dispenser 10 days, 20 days, 30 days and 50 days investigation anthrax prevention effect, concrete test method according to《Pesticide Field control effectiveness test criterion》Carry out.Using random 5 points samplings, each processes cell and investigates 25 plants of Citrus, investigation each treatment region Anthrax prevention effect on each treatment region Citrus, by formula (1) disease index is calculated, and formula (2) calculates prevention effect, as a result such as table 2 It is shown.
Table 2
Testing example 3
This testing example is used to determine the pyraclostrobin fluopyram obtained in embodiment 1-9, comparative example 1-9 The micro- suspension emulsion of pyraclostrobin fluopyram, the pyrazoles of comparative example 11 obtained in microcapsule suspension-suspendinagent agent, comparative example 10 The fluopyram suspending agent Pesticides medicament of kresoxim-methyl aqueous emulsion and comparative example 12 is carried out to the prevention effect of citrus anthracnose Test.A certain amount of distilled water is added before test, stir, adjust will obtain in embodiment 1-9, comparative example 1-9 respectively The pyraclostrobin fluopyram obtained in pyraclostrobin fluopyram microcapsule suspension-suspendinagent agent, comparative example 10 Active component in the fluopyram suspending agent of micro- suspension emulsion, the pyraclostrobin aqueous emulsion of comparative example 11 and comparative example 12 is dense Spend for 10 weight %.
Test site:Hunan Province Jiangyong County.The plot physical features is flat, and fertility is preferable.Each treatment region Citrus after dispenser are pressed Conventional production management.
Concrete steps include, are 30kg/ mus according to spouting liquid, by embodiment 1-9, comparative example using knapsack sprayer The pyraclostrobin obtained in the pyraclostrobin fluopyram microcapsule suspension-suspendinagent agent, the comparative example 10 that obtain in 1-9 The fluopyram suspending agent Chinese medicine of the micro- suspension emulsion of fluopyram, the pyraclostrobin aqueous emulsion of comparative example 11 and comparative example 12 Liquid is uniformly sprayed respectively on the Citrus plant of each growing area, and blank control group is using equivalent clear water to the Citrus in growing area Plant is sprayed, and during dispenser, with plastic sheeting neighbor cell is blocked, and prevents medicament from interfering.
The anthrax prevention effect on 10 days, 20 days, 30 days and 50 days investigation Citrus after the dispenser, concrete test method according to 《Pesticide field efficacy medicine test criterion》Carry out.Using random 5 points samplings, each processes cell and investigates 25 plants of Citrus chachiensiss Hort. each treatment region Fructus Citri tangerinae, investigates anthrax prevention effect on each treatment region Citrus, according to formula (3) calculating disease index, according to formula (4) prevention effect, Concrete outcome is shown in Table 3:
Table 3
From table 2 and table 3 as can be seen that the preparation method that the disclosure is provided passes through adjusted stepwise pH value, specifically stirring The pyraclostrobin fluopyram microcapsule suspension-suspension prepared under the reaction conditions such as rotating speed, emulsifying dispersant, solvent Agent, prevents and treats the effect of corps diseases in which can obtain slow release long-acting.And pyraclostrobin fluorine pyrrole bacterium acyl prepared by this method Amine microcapsule suspension-suspendinagent agent effect is much better than pyraclostrobin aqueous emulsion single dose, fluopyram suspending agent single dose.This public affairs Other agent of the pyraclostrobin fluopyram microcapsule suspension-suspendinagent agent opened relative to pyraclostrobin fluopyram Type, with the lasting period it is long the characteristics of, it is possible to decrease times for spraying and dosage, it is cost-effective, wherein the organic solvent for containing is few, can To reduce the pollution to environment.
The preferred implementation of the disclosure described in detail above, but, the disclosure is not limited in the embodiment Detail, in the range of the technology design of the disclosure, various simple variants can be carried out with technical scheme of this disclosure, this A little simple variants belong to the protection domain of the disclosure.
It is further to note that each particular technique feature described in the specific embodiment, in not lance In the case of shield, can be combined by any suitable means.In order to avoid unnecessary repetition, the disclosure to it is various can The compound mode of energy is no longer separately illustrated.
Additionally, combination in any can also be carried out between a variety of embodiments of the disclosure, as long as it is without prejudice to this Disclosed thought, it should equally be considered as disclosure disclosure of that.

Claims (10)

1. a kind of preparation method of the microcapsule suspension-suspendinagent agent of pyraclostrobin-containing and fluopyram, it is characterised in that the system Preparation Method comprises the steps:
(1) the first solution is mixed homogeneously with the second solution, obtains first material;Wherein, first solution contains amino tree Fat performed polymer aqueous solution, second solution contains pyraclostrobin missible oil, the weight of first solution and second solution Amount is than being (1-5):1;
(2) buffer solution is added in the first material, it is 5-7 to adjust mixed solution pH value, obtains second material;
(3) acidic ph modifier is added in the second material, it is 3-4 to adjust mixed solution pH value, obtains 3 material;
(4) 3 material is carried out solidifying bunching process, obtains solidifying bunching product;Adjust the solidification bunching product PH value is 6.5-7.5, obtains 4 materials;
(5) fluopyram suspending agent is added in the 4 materials, the 5th material is obtained;The 4 materials and the fluorine The weight ratio of pyrrole bacterium amide suspending agents is 1:(0.1-1).
2. preparation method according to claim 1, it is characterised in that amino resins performed polymer is water-soluble described in step (1) Liquid is obtained by formaldehyde, containing amino-compound and water prepolymerization, and the weight ratio of the formaldehyde, the compound containing amino and water is 1: (0.2-12.5):(2-7);The compound containing amino includes at least in carbamide, tripolycyanamide and benzoguanamine Kind;The prepolymerized condition includes:PH value is 8-10, and temperature is 60-80 DEG C, and the response time is 0.5-3 hours.
3. preparation method according to claim 1, it is characterised in that pyraclostrobin missible oil contains described in step (1) Pyraclostrobin, organic solvent and emulsifying agent;The organic solvent include petroleum ether, ethyl acetate, methyl oleate, dimethylbenzene and At least one in solvent naphtha, the emulsifying agent includes sodium lignin sulfonate, sodium lauryl sulphate, DBSA Sodium, styrene-maleic anhydride copolymer, fatty alcohol-polyoxyethylene ether, anhydrous sorbitol polyoxyethylene poly-oxygen propylene aether, dehydration mountain In pears alcohol monostearate ester APEO, sodium laurylsulfate, polyvinyl alcohol, polycarboxylate and naphthalene sulfonate at least one Kind;The weight ratio of the pyraclostrobin, organic solvent and emulsifying agent is 1:(0.1-5):(0.01-0.2).
4. preparation method according to claim 1, it is characterised in that containing buffering in buffer solution described in step (2) It is right;The buffering is to including at least one in citric acid-sodium citrate, citrate-phosphate disodium hydrogen and acetic acid-sodium acetate; The concentration of the buffer solution is 1-5 weight %, and pH value is 3-5.5.
5. preparation method according to claim 1, it is characterised in that acidic ph modifier described in step (3) includes salt At least one in acid, sulphuric acid, phosphoric acid, acetic acid and ammonium chloride;The concentration of the acidic ph modifier is 1-10 weight %.
6. preparation method according to claim 1, it is characterised in that solidify the condition that bunching is processed described in step (4) Including:2-7 hour is processed under the conditions of 40 DEG C -70 DEG C.
7. preparation method according to claim 1, it is characterised in that 4 materials described in step (4) are also containing dispersion At least one in agent, thickening agent, antifreezing agent;It is the solidification bunching product, the dispersant, the thickening agent, described antifreeze The weight ratio of agent is 1:(0.01-0.2):(0.001-0.02):(0.02-0.15).
8. preparation method according to claim 1, it is characterised in that fluopyram suspending agent contains described in step (5) There are 1-5 μm of fluopyram, water and adjuvant, the weight ratio of the fluopyram, water and the adjuvant is 1:(2- 4):(0.5-1);Preferably, the adjuvant includes at least in dispersant, thickening agent, defoamer, antifreezing agent and preservative Kind;The weight of the fluopyram, the dispersant, the thickening agent, the defoamer, the antifreezing agent and the preservative Amount is than being 1:(0.1-0.5):(0.01-0.02):(0.01-0.02):(0.1-0.5):(0.005-0.01).
9. preparation method according to claim 1, it is characterised in that the condition mixed described in step (1) includes:60- 80 DEG C, mixing speed is 1500-3000 rev/min;
The condition mixed described in step (2) includes:40-70 DEG C, mixing speed is 1000-1200 rev/min;
The condition mixed described in step (3) includes:40-70 DEG C, mixing speed is 1200-1500 rev/min.
10. the method according to any one in claim 1-9 is prepared pyraclostrobin-containing and fluopyram Microcapsule suspension-suspendinagent agent.
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CN107258777A (en) * 2017-06-21 2017-10-20 北京明德立达农业科技有限公司 A kind of seed treatment microcapsules suspension suspending agent of pyraclostrobin-containing and fluorine azoles bacterium aniline and preparation method thereof
CN107279163A (en) * 2017-07-27 2017-10-24 北京明德立达农业科技有限公司 A kind of microcapsule suspension suspending agent of fluorine-containing ether bacterium acid amides and pyraclostrobin and preparation method thereof
CN107333785A (en) * 2017-06-22 2017-11-10 北京明德立达农业科技有限公司 A kind of microcapsule suspension suspending agent of pyraclostrobin-containing and fluorine azoles ring bacterium amine and preparation method thereof
CN108576017A (en) * 2018-02-08 2018-09-28 河北赛丰生物科技有限公司 A kind of microcapsule suspension-suspendinagent agent and preparation method thereof containing benziothiazolinone and tiger glue adipic acid copper
CN109874793A (en) * 2019-03-18 2019-06-14 允发化工(上海)有限公司 A kind of microcapsule suspension-suspendinagent agent and preparation method thereof of pyraclostrobin-fluazinam
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CN113812413A (en) * 2021-11-02 2021-12-21 中国农业科学院农业环境与可持续发展研究所 Double-loading nano pesticide controlled release agent containing fluopyram and pyraclostrobin and preparation method thereof

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CN107232218A (en) * 2017-05-23 2017-10-10 北京明德立达农业科技有限公司 A kind of microcapsule suspension suspending agent of metsulfovax containing pyrrole and pyraclostrobin and preparation method thereof
CN107258777A (en) * 2017-06-21 2017-10-20 北京明德立达农业科技有限公司 A kind of seed treatment microcapsules suspension suspending agent of pyraclostrobin-containing and fluorine azoles bacterium aniline and preparation method thereof
CN107333785A (en) * 2017-06-22 2017-11-10 北京明德立达农业科技有限公司 A kind of microcapsule suspension suspending agent of pyraclostrobin-containing and fluorine azoles ring bacterium amine and preparation method thereof
CN107279163A (en) * 2017-07-27 2017-10-24 北京明德立达农业科技有限公司 A kind of microcapsule suspension suspending agent of fluorine-containing ether bacterium acid amides and pyraclostrobin and preparation method thereof
CN108576017A (en) * 2018-02-08 2018-09-28 河北赛丰生物科技有限公司 A kind of microcapsule suspension-suspendinagent agent and preparation method thereof containing benziothiazolinone and tiger glue adipic acid copper
WO2020103646A1 (en) * 2018-11-19 2020-05-28 上海明德立达生物科技有限公司 Method for preparing micro-capsule suspension-suspension agent containing lambda-cyhalothrin and lufenuron and micro-capsule suspension-suspension agent thereof
WO2020108197A1 (en) * 2018-11-29 2020-06-04 上海明德立达生物科技有限公司 Microcapsule suspension-suspending agent containing atrazine and s-metolachlor and preparation method therefor
CN109874793A (en) * 2019-03-18 2019-06-14 允发化工(上海)有限公司 A kind of microcapsule suspension-suspendinagent agent and preparation method thereof of pyraclostrobin-fluazinam
CN113812413A (en) * 2021-11-02 2021-12-21 中国农业科学院农业环境与可持续发展研究所 Double-loading nano pesticide controlled release agent containing fluopyram and pyraclostrobin and preparation method thereof

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Application publication date: 20170419