CN110250170A - A kind of preparation method and application of Metalaxyl-M pyraclostrobin microcapsule suspending agent - Google Patents
A kind of preparation method and application of Metalaxyl-M pyraclostrobin microcapsule suspending agent Download PDFInfo
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- CN110250170A CN110250170A CN201910591357.4A CN201910591357A CN110250170A CN 110250170 A CN110250170 A CN 110250170A CN 201910591357 A CN201910591357 A CN 201910591357A CN 110250170 A CN110250170 A CN 110250170A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N47/00—Biocides, 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
- A01N47/08—Biocides, 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
- A01N47/10—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
- A01N47/24—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof containing the groups, or; Thio analogues thereof
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01C—PLANTING; SOWING; FERTILISING
- A01C1/00—Apparatus, or methods of use thereof, for testing or treating seed, roots, or the like, prior to sowing or planting
- A01C1/06—Coating or dressing seed
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01C—PLANTING; SOWING; FERTILISING
- A01C1/00—Apparatus, or methods of use thereof, for testing or treating seed, roots, or the like, prior to sowing or planting
- A01C1/08—Immunising seed
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N25/00—Biocides, 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
- A01N25/02—Biocides, 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
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N25/00—Biocides, 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
- A01N25/26—Biocides, 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 in coated particulate form
- A01N25/28—Microcapsules or nanocapsules
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/44—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids
- A01N37/46—N-acyl derivatives
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Abstract
The present invention relates to pesticide fields, disclose a kind of preparation method of Metalaxyl-M pyraclostrobin microcapsule suspending agent, comprising: a, are uniformly mixed urea-formaldehyde resin performed polymer aqueous solution and the dispersible oil-suspending agent of pyraclostrobin Metalaxyl-M, obtain first material；B, the pH value for adjusting the first material is 5.5-6.5, obtains second material；C, it is 3-5 that its pH value is adjusted after stirring the second material 30-60 minutes, obtains third material；D, third material carries out polycondensation, after then the pH value of the material after polycondensation is adjusted to neutrality with one of dispersing agent, thickener, film forming agent, mill base and antifreezing agent or a variety of be uniformly mixed；The usage amount of organic solvent can be effectively reduced in preparation method of the invention, the safety to seed sprouting is improved, reduces environmental pollution, and significantly improve the storage stability of the microcapsule suspending agent containing Metalaxyl-M and pyraclostrobin and the control efficiency to disease, extend the lasting period, increases crop yield.
Description
Technical field
The present invention relates to technical field of pesticide, and in particular, to a kind of Metalaxyl-M pyraclostrobin microcapsule suspending agent
Preparation method and application.
Background technique
Metalaxyl-M is vapour Ba-Jia Ji (Ciba-Geigy) company, Switzerland exploitation in 1977 using phenyl ring as the amide of parent
Class fungicide, its feature are with protection, treatment, a kind of higher fungicide of systemic activity of systemic activity, its effect machine
Manage it is similar to other same type fungicide, can influence pathogen respiratory electron transport chain albumen composition II (succinic acid take off
Hydrogen enzyme), to reach bacteriostasis.Each stage that pest and disease damage germ can occur in plant plays curative effect, treats ovum
Bacterium pest and disease damage excellent.Have to a variety of pest and disease damages caused by egg bacteria and the samping off as caused by phytophthora, seed rot disease etc.
Prevention and preventive and therapeutic effect well.
But Metalaxyl-M is easy to degrade in the soil, so Metalaxyl-M can all produce when applying as seed treatment
Give birth to the rapidly losing and rotten of effective component.Therefore, it needs to study according to market applicable cases a kind of environmentally friendly, safe and efficient steady
Fixed Metalaxyl-M seed treatment.
Pyraclostrobin is the methoxy acrylic bactericide of BASF AG's exploitation, and the mechanism of action is mitochondria
Respiration inhibitor permeates conduction with protection, treatment, blade that is, by preventing electronics transfer in cytochromes synthesize,
And there is wide sterilization spectrum, activity height, low toxin.
But its easily hydrolyzed and photodissociation, so can all generate the effective elements of the medicine when many pyraclostrobin dosage form applications
It is lost and rotten.In addition, pyraclostrobin is to fish high poison, so causing water body using Shi Douhui from the closer place in water source
Biological death.Therefore, need to study a kind of environmental protection according to market applicable cases, safety, efficient pyraclostrobin dosage form.
The microcapsule formulation of two-spot compounding is since there are two kinds of effective components at present, and prepares microcapsules system with conventional method
Agent, two kinds of effective components need different types of a large amount of organic solvents to be dissolved, not only to seed sprouting there are risk, and meeting
Pollute environment.
Summary of the invention
In order to overcome drawbacks described above, the present invention provides a kind of Metalaxyl-M pyraclostrobin microcapsule suspending agent and its preparation
Method, the pyraclostrobin Metalaxyl-M microcapsule suspending agent stable storing being prepared by this method and can effectively prevent big
Field crops seedling stage disease.And the method that the present invention uses is added without organic solvent during the preparation process, and safety in utilization is good, green
Methyl oleate, mineral oil, the vegetable oil etc. that colour circle is protected, improve the safety to seed, and reduce the pollution to environment.
To achieve the goals above, the present invention provides a kind of preparation side of Metalaxyl-M pyraclostrobin microcapsule suspending agent
Method, the preparation method include the following steps:
(1) the first solution and second liquid are uniformly mixed, obtain first material；Wherein, first solution contains urine
Element-formaldehyde resin performed polymer aqueous solution；The second liquid, which contains pyraclostrobin Metalaxyl-M, can be dispersed oil-suspending agent；Institute
The weight ratio for stating the first solution and the second liquid is (1-5): 1；
(2) first material is uniformly mixed with buffer solution, to adjust pH value as 5.5-6.5, obtains second material；
(3) it is uniformly mixed after stirring the second material 30-60 minutes with acidic pH adjustor, is to adjust pH value
3-5 obtains third material；
(4) the third material is subjected to polycondensation, obtains polycondensation product, and by the polycondensation product
PH value be adjusted to 6.5-7.5；
(5) by the polycondensation product and dispersing agent, thickener, film forming agent, mill base and antifreezing agent after the adjusting pH value
One of or it is a variety of be uniformly mixed, obtain Metalaxyl-M pyraclostrobin micro-capsule hang seed treatment microcapsule suspending agent.
The present invention also provides a kind of Metalaxyl-M pyraclostrobin microcapsule suspending agent, which is by above
What the method was prepared.
The present invention contains Metalaxyl-M, pyraclostrobin microcapsule suspending agent using new method preparation, not only overcomes raw medicine
Defect, extend the lasting period, and increase traditional dissolution-encystation method preparation two-spot compounding microcapsules stability, have
Effect enhances the storage stability of Metalaxyl-M pyraclostrobin microcapsule suspending agent and the control efficiency to crops seedling stage disease.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The present invention provides a kind of preparation method of Metalaxyl-M pyraclostrobin microcapsule suspending agent, which includes
Following steps:
(1) the first solution and second liquid are uniformly mixed, obtain first material；Wherein, first solution contains urine
Element-formaldehyde resin performed polymer aqueous solution；The second liquid, which contains pyraclostrobin Metalaxyl-M, can be dispersed oil-suspending agent；Institute
The weight ratio for stating the first solution and the second liquid is (1-5): 1；
(2) first material is uniformly mixed with buffer solution, to adjust pH value as 5.5-6.5, obtains second material；
(3) it is uniformly mixed after stirring the second material 30-60 minutes with acidic pH adjustor, is to adjust pH value
3-5 obtains third material；
(4) the third material is subjected to polycondensation, obtains polycondensation product, and by the polycondensation product
PH value be adjusted to 6.5-7.5；
(5) by the polycondensation product and dispersing agent, thickener, film forming agent, mill base and antifreezing agent after the adjusting pH value
One of or it is a variety of be uniformly mixed, obtain Metalaxyl-M pyraclostrobin microcapsule suspending agent.
In the present invention, it is the amides using phenyl ring as parent that Metalaxyl-M (metalaxyl-M), which is also mefenoxam,
Fungicide, its feature are with protection, treatment, the higher fungicide of systemic activity.Chemical name is N- (2,6- dimethylbenzene
Base)-N- (Methoxyacetyl)-D- alanine methyl esters, CAS accession number 70630-17-0, relative molecular weight: 279.33, knot
Shown in structure formula such as formula (1):
Pyraclostrobin is compound N-[2- [1- (4- chlorphenyl) -1H- pyrazole-3-yl oxygen methyl] phenyl] (N- methoxy
Base) methyl carbamate trade name, English name pyraclostrobin, molecular formula C19H18ClN3O4, average molecular matter
Amount 387.8, No. CAS: 175013-18-0, shown in structural formula such as formula (2):
According to the present invention, by the Metalaxyl-M raw medicine, pyraclostrobin raw medicine by be sanded and etc. be prepared into and can divide
Oil-suspending agent is dissipated, first material is prepared into performed polymer, is then uniformly mixed the first material with buffer solution, to adjust
PH value is 5.5-6.5, obtains second material；The second material is uniformly mixed with acidic pH adjustor, to adjust pH value
For 3-5, when obtaining third material, the Metalaxyl-M pyraclostrobin microcapsule suspension developing agent storage being prepared is stablized, and is not easy to send out
Raw reunion and solidification phenomenon solve the defect of conventional method preparation two-spot compounding microcapsules, and have to sprout term disease good
Control efficiency.
Further, it is preferable in step (1), the urea-formaldehyde resin performed polymer aqueous solution by containing urea, formaldehyde and
The material liquid prepolymerization of water obtains；It is preferred that it is 8-10 that the prepolymerized condition, which includes: pH value, temperature is 70-75 DEG C, when reaction
Between be 1-2 hours.
It is further preferred that urea-formaldehyde resin performed polymer aqueous solution can be by the material liquid prepolymerization containing urea, formaldehyde and water
It obtains；Further preferred urea-formaldehyde resin performed polymer aqueous solution can be by urea, the formalin that concentration is 35-45 weight %
Solution and water prepolymerization obtain, and the molar ratio of formaldehyde and urea can be 1:(0.5-1), the volume ratio of water and formalin can
Think 1:(0.5-2).
, according to the invention it is preferred to which urea-formaldehyde resin performed polymer aqueous solution can be 35-45 weight % by urea, concentration
Formalin prepolymerization, then be added water dilute to obtain the urea-formaldehyde resin performed polymer aqueous solution.
Further, in step (1), oil-suspending agent is can be dispersed in the pyraclostrobin Metalaxyl-M, can be ability
The preparation of preparation method well known to field technique personnel, the present invention are not particularly limited it.Under preferable case, the pyrazoles ether bacterium
Oil-suspending agent can be dispersed in ester Metalaxyl-M can be situated between containing pyraclostrobin raw medicine, Metalaxyl-M raw medicine, emulsifier and oiliness
Matter；The emulsifier preferably includes lauryl sodium sulfate, neopelex, styrene-maleic anhydride copolymer, rouge
Fat alcohol polyoxyethylene ether, anhydrous sorbitol polyoxyethylene poly-oxygen propylene aether, sorbitan monostearate polyoxyethylene ether, the moon
At least one of lauryl sulfate, alkyl phenol polyoxyethylene ether, castor oil polyoxyethylene ether and EO-PO block copolymer；Institute
It states oil medium and preferably includes at least one of methyl oleate, ethyl oleate, vegetable oil, mineral oil, paraffin oil；Wherein, excellent
The weight ratio for selecting the pyraclostrobin raw medicine, Metalaxyl-M raw medicine, emulsifier and oil medium is 1:(0.1-10): (1-
10): (1-10).
The Metalaxyl-M pyraclostrobin can be dispersed oil-suspending agent preparation method and preferably include: by Metalaxyl-M original
Medicine, pyraclostrobin raw medicine successively mixed with emulsifier, oil medium, dispersion and sand milling, obtains pyrrole described in step (1)
Oil-suspending agent can be dispersed in azoles kresoxim-methyl Metalaxyl-M.
, according to the invention it is preferred to can be dispersed in oil-suspending agent in the pyraclostrobin Metalaxyl-M, Metalaxyl-M is former
Medicine, pyraclostrobin raw medicine exist with aerosol form.
, according to the invention it is preferred to which the Metalaxyl-M raw medicine, the suspended particulates average grain diameter of pyraclostrobin raw medicine are respectively
It is 1-5 microns.
Further, in order to promote the performance of microcapsule suspending agent, in preferred steps (2), the buffer solution is containing suitable
When the Conjugate Acid-Base Pairs of concentration and proper proportion, two kinds of substances of the conjugate acid and base centering are collectively referred to as buffering pair, such as lemon
For acid-sodium citrate buffering to citric acid and sodium citrate is referred to, the total concentration of citric acid-sodium citrate buffering pair is lemon
The sum of concentration of acid group.The pH value of the buffer solution can be 3-5；The total concentration of buffering pair can be in the buffer solution
1-5 weight %, wherein the buffer solution can be the conventional use of various buffer solutions of those skilled in the art, preferably feelings
Under condition, buffering in the buffer solution is to may include citric acid-sodium citrate, citrate-phosphate disodium hydrogen and acetic acid-second
At least one of sour sodium.
Further, in order to improve clad ratio, the uniformity and the softgel shell compactness of micro-capsule, in step (3), the acidity
PH adjusting agent can be the conventional use of various substances that can reduce pH value of those skilled in the art, described under preferable case
The concentration of acidic ph modifier can be 1-10 weight %；The solute of the acidic ph modifier may include hydrogen chloride, sulfuric acid,
At least one of acetic acid, ammonium chloride and phosphoric acid.
Further, in order to further improve the particle diameter distribution and storage of Metalaxyl-M pyraclostrobin microcapsule suspending agent
Deposit stability, in step (5), the dispersing agent includes neopelex, sodium methylene bis-naphthalene sulfonate, 1- methyl naphthalene sulphur
Sour sodium formaldehyde condensation product, benzyl naphthalene sulfonic acid-formaldehyde condensation product, sodium lignin sulfonate, desugar sodium lignin sulfonate, desugar condensation wood
Quality sodium sulfonate, Succinate sodium sulfonate, pull open powder, nonylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether, polycarboxylate,
At least one of naphthalene sulfonate, EO-PO block copolymer and pull open powder.
A preferred embodiment of the invention, the polycondensation product and dispersing agent, film forming agent, mill base weight
Amount is than being 1:(0.01-0.05).
According to the present invention, the thickener and antifreezing agent can be the conventional use of reagent of those skilled in the art, preferably
In the case of, the thickener include aluminum magnesium silicate, xanthan gum, polyethylene glycol, polyvinyl alcohol, carboxymethyl cellulose, bentonite and
One of white carbon black is a variety of.
According to the present invention preferably, the antifreezing agent include one of ethylene glycol, 1,2-PD, glycerine and urea or
It is a variety of.
A preferred embodiment of the invention, by it is described adjusting pH value after polycondensation product and dispersing agent,
Thickener and antifreezing agent are uniformly mixed, it is preferable that the weight ratio of the polycondensation product, dispersing agent, thickener and antifreezing agent can
Think 1:(0.01-0.05): (0.001-0.005): (0.05-0.1).
Further, in order to guarantee Metalaxyl-M pyraclostrobin microcapsule suspending agent as in seed treatment warning and
Sustained release, filming performance, in step (5), by after the adjusting pH value polycondensation product and dispersing agent, thickener, film forming agent,
Mill base and antifreezing agent are uniformly mixed, and the film forming agent and mill base can be the conventional use of reagent of those skilled in the art.
Under preferable case, the film forming agent may include Arabic gum, animal glue, methylcellulose, ethyl cellulose, hydroxyl
Sodium carboxymethylcellulose pyce, polyvinyl alcohol, polyethylene glycol, polyacrylamide, Sodium Polyacrylate, equal polyvinyl acetate, polysaccharide are high
At least one of molecular compound and cellulose derivative.
Under preferable case, the mill base includes red or blue water-soluble mill base.
The weight ratio of the polycondensation product, film forming agent and mill base can be 1:(0.01-0.1): (0.05-0.2).
Further, in order to promote the performance of Metalaxyl-M pyraclostrobin microcapsule suspending agent, in preferred steps (1),
Mixed condition includes: that mixing speed can be 500-1000 revs/min；In preferred steps (2), mixed condition be can wrap
It includes: under the conditions of 25-35 DEG C, buffer solution being at the uniform velocity added in 0.5-1 hours, mixing speed is 200-300 revs/min；It is preferred that
In ground step (3), mixed condition may include: that acid ph value is at the uniform velocity added in 1-2 hours and adjusts under the conditions of 25-35 DEG C
Agent, mixing speed are 300-500 revs/min.
Wherein, it is at the uniform velocity added and refers to during addition, the additional amount in the unit time is essentially identical.
In accordance with the present invention it is preferred that it is 40-65 DEG C that the polycondensation condition, which includes solidification temperature, curing time 2-6
Hour, curing mode can be mechanical stirring；Pass through triethylamine solution, triethanolamine solution, hydroxide after the completion of polycondensation
The pH value of product after the polycondensation is adjusted to 6.5-7.5 by least one of sodium solution, potassium hydroxide solution pH adjusting agent.
The present invention also provides a kind of Metalaxyl-M pyraclostrobin microcapsule suspending agents, wherein the suspending agent is basis
What preparation method of the present invention obtained.
The present invention provides application of the Metalaxyl-M pyraclostrobin microcapsule suspending agent in seed treatment.
According to the present invention, Metalaxyl-M pyraclostrobin seed treatment microcapsule suspending agent provided by the invention is not only stored
The phenomenon that stablizing, being not susceptible to reunion and solidify, and the sick, damping-off to sprout term disease such as Achlya spp, Causal Organism of Maize Basal Stalk,
Wheat sharp eyespot etc. has good control efficiency.
The present invention is described further by the following examples.It should be understood that embodiment described herein
It is merely to illustrate and explain the present invention, is not intended to restrict the invention.
Embodiment 1
Urea is uniformly mixed with the formalin that concentration is 37 weight %, is 9 in pH value, under the conditions of temperature is 72 DEG C
React 1.5h；Water dilution is added, obtains urea-formaldehyde resin performed polymer aqueous solution, wherein the molar ratio of formaldehyde and urea is 1:
0.5, the volume ratio of water and formalin is 1:1.
By Metalaxyl-M raw medicine, pyraclostrobin raw medicine, methyl oleate and sorbitan monooleate polyoxyethylene ether
(Tween80) successively through mixing, dispersion and sand milling, obtaining Metalaxyl-M pyraclostrobin can be dispersed oil-suspending agent, wherein institute
State Metalaxyl-M raw medicine, pyraclostrobin raw medicine, the weight of methyl oleate and sorbitan monostearate polyoxyethylene ether
Than for 1:1:6:2.
Oil-suspending agent can be dispersed in gained urea-formaldehyde resin performed polymer aqueous solution and Metalaxyl-M pyraclostrobin to exist
It is uniformly mixed under 800 revs/min of mixing speed, first material is obtained, wherein the urea-formaldehyde resin performed polymer aqueous solution
The weight ratio that oil-suspending agent can be dispersed with Metalaxyl-M pyraclostrobin is 3:1；It at room temperature, is 4 by pH value, buffering
Pair total concentration be 3 weight % citric acid-sodium citrate buffer, above-mentioned first object is evenly added in 1 hour
It in material, is uniformly mixed with 250 revs/min of mixing speed, to adjust pH value as 6.0, obtains second material；In room temperature condition
Under, the hydrochloric acid that concentration is 5 weight % is evenly added in above-mentioned second material in 1.5 hours, with 400 revs/min
Mixing speed is uniformly mixed, and to adjust pH value as 4.0, obtains third material；Under conditions of 55 DEG C, by the third material into
Row polycondensation 2.5 hours, obtain polycondensation product；And triethanolamine is added by the pH value tune of the polycondensation product
It saves to 7.0；Polycarboxylate Atlox-4913, aluminum magnesium silicate, ethylene glycol, sodium cellulose glycolate, red mill base mixing is added
It is even, obtain 4 materials, i.e. pyraclostrobin Metalaxyl-M microcapsule suspending agent；Wherein, the polycondensation product and poly- carboxylic
Hydrochlorate, aluminum magnesium silicate, ethylene glycol, sodium cellulose glycolate, red mill base weight ratio be 1:0.02:0.003:0.05:0.05:
0.1。
Embodiment 2
Urea is uniformly mixed with the formalin that concentration is 37 weight %, is 10 in pH value, temperature is 75 DEG C of conditions
Lower reaction 2h；Water dilution is added, obtains urea-formaldehyde resin performed polymer aqueous solution, wherein the molar ratio of formaldehyde and urea is 1:
0.5, the volume ratio of water and formalin is 1:1.
By Metalaxyl-M raw medicine, pyraclostrobin raw medicine, mineral oil and castor oil polyoxyethylene ether BY-125 successively through mixed
Splitting or integrating is dissipated and is sanded, and obtaining Metalaxyl-M pyraclostrobin can be dispersed oil-suspending agent, wherein the Metalaxyl-M raw medicine, pyrrole
The weight ratio of azoles kresoxim-methyl raw medicine, mineral oil and styrene-maleic anhydride copolymer is 1:10:10:10.
Oil-suspending agent can be dispersed in gained urea-formaldehyde resin performed polymer aqueous solution and Metalaxyl-M pyraclostrobin to exist
It is uniformly mixed under 1000 revs/min of mixing speed, first material is obtained, wherein the urea-formaldehyde resin performed polymer is water-soluble
The weight ratio that oil-suspending agent can be dispersed in liquid and Metalaxyl-M pyraclostrobin is 5:1；It at room temperature, is 5 by pH value, slow
The total concentration of punching pair is acetic acid-sodium acetate buffer solution of 5 weight %, and above-mentioned first material is evenly added in 1 hour
In, it is uniformly mixed with 300 revs/min of mixing speed, to adjust pH value as 6.5, obtains second material；At room temperature,
The hydrochloric acid that concentration is 10 weight % is evenly added in above-mentioned second material in 2 hours, with 500 revs/min of stirring
Speed is uniformly mixed, and to adjust pH value as 3.0, obtains third material；Under conditions of 60 DEG C, the third material is consolidated
Change polycondensation 3 hours, obtains polycondensation product；And sodium hydroxide is added to be adjusted to the pH value of the polycondensation product
7.5；Sodium lignin sulfonate, xanthan gum, glycerine, PVAC polyvinylalcohol -1799, red mill base is added to be uniformly mixed, obtains the 4th
Material, i.e. pyraclostrobin Metalaxyl-M microcapsule suspending agent；Wherein, the polycondensation product and sodium lignin sulfonate, Huang
Virgin rubber, glycerine, polyvinyl alcohol, red mill base weight ratio be 1:0.05:0.005:0.1:0.1:0.2.
Embodiment 3
Urea is uniformly mixed with the formalin that concentration is 37 weight %, is 9 in pH value, under the conditions of temperature is 72 DEG C
React 1.5h；Water dilution is added, obtains urea-formaldehyde resin performed polymer aqueous solution, wherein the molar ratio of formaldehyde and urea is 1:
0.5, the volume ratio of water and formalin is 1:1.
By Metalaxyl-M raw medicine, pyraclostrobin raw medicine, methyl oleate and neopelex successively through mixed splitting or integrating
It dissipates and is sanded, obtaining Metalaxyl-M pyraclostrobin can be dispersed oil-suspending agent, wherein the Metalaxyl-M raw medicine, pyrazoles ether
The weight ratio of bacterium ester raw medicine, methyl oleate and sorbitan monostearate polyoxyethylene ether is 1:1:6:2.
Oil-suspending agent can be dispersed in gained urea-formaldehyde resin performed polymer aqueous solution and Metalaxyl-M pyraclostrobin to exist
It is uniformly mixed under 800 revs/min of mixing speed, first material is obtained, wherein the urea-formaldehyde resin performed polymer aqueous solution
The weight ratio that oil-suspending agent can be dispersed with Metalaxyl-M pyraclostrobin is 3:1；It at room temperature, is 4 by pH value, buffering
Pair total concentration be 3 weight % citric acid-sodium citrate buffer, above-mentioned first object is evenly added in 1 hour
It in material, is uniformly mixed with 250 revs/min of mixing speed, to adjust pH value as 6.0, obtains second material；In room temperature condition
Under, the hydrochloric acid that concentration is 5 weight % is evenly added in above-mentioned second material in 1.5 hours, with 400 revs/min
Mixing speed is uniformly mixed, and to adjust pH value as 4.0, obtains third material；Under conditions of 55 DEG C, by the third material into
Row polycondensation 2.5 hours, obtain polycondensation product；And triethanolamine is added by the pH value tune of the polycondensation product
It saves to 7.0；Polycarboxylate SD-816, aluminum magnesium silicate, ethylene glycol, sodium cellulose glycolate, red mill base is added to be uniformly mixed, obtains
To 4 materials, i.e. pyraclostrobin Metalaxyl-M microcapsule suspending agent；Wherein, the polycondensation product and polycarboxylate,
Aluminum magnesium silicate, ethylene glycol, sodium cellulose glycolate, red mill base weight ratio be 1:0.02:0.003:0.05:0.05:0.1.
Embodiment 4
Urea is uniformly mixed with the formalin that concentration is 37 weight %, is 7.5 in pH value, temperature is 77 DEG C of conditions
Lower reaction 2.5h；Water dilution is added, obtains urea-formaldehyde resin performed polymer aqueous solution, wherein the molar ratio of formaldehyde and urea is
The volume ratio of 1:1, water and formalin is 1:2.
Metalaxyl-M raw medicine, pyraclostrobin raw medicine, methyl oleate and castor oil polyoxyethylene ether BY-110 are successively passed through
Mixing, dispersion and sand milling, obtaining Metalaxyl-M pyraclostrobin can be dispersed oil-suspending agent, wherein the Metalaxyl-M raw medicine,
The weight ratio of pyraclostrobin raw medicine, methyl oleate and castor oil polyoxyethylene ether is 1:1:10:5.
Oil-suspending agent can be dispersed in gained urea-formaldehyde resin performed polymer aqueous solution and Metalaxyl-M pyraclostrobin to exist
It is uniformly mixed under 500 revs/min of mixing speed, first material is obtained, wherein the urea-formaldehyde resin performed polymer aqueous solution
The weight ratio that oil-suspending agent can be dispersed with Metalaxyl-M pyraclostrobin is 5:1；It at room temperature, is 4 by pH value, buffering
Pair total concentration be 3 weight % acetic acid-sodium acetate buffer solution, be evenly added in above-mentioned first material in 1 hour,
It is uniformly mixed with 200 revs/min of mixing speed, to adjust pH value as 6.2, obtains second material；It at room temperature, will be dense
Degree is that the acetic acid of 5 weight % is evenly added in above-mentioned second material in 1.5 hours, with 500 revs/min of mixing speed
It is uniformly mixed, to adjust pH value as 3.0, obtains third material；Under conditions of 60 DEG C, the third material is subjected to solidification contracting
Poly- 3 hours, obtain polycondensation product；And potassium hydroxide is added, the pH value of the polycondensation product is adjusted to 7；It is added
Sodium methylene bis-naphthalene sulfonate, aluminum magnesium silicate, ethylene glycol, Arabic gum, red mill base are uniformly mixed, and obtain 4 materials, i.e. pyrrole
Azoles kresoxim-methyl Metalaxyl-M microcapsule suspending agent；Wherein, the polycondensation product and sodium methylene bis-naphthalene sulfonate, alumina silicate
Magnesium, ethylene glycol, Arabic gum, red mill base weight ratio be 1:0.02:0.001:0.05:0.01:0.15.
Embodiment 5
Urea is uniformly mixed with the formalin that concentration is 37 weight %, is 10 in pH value, temperature is 70 DEG C of conditions
Lower reaction 1h；Water dilution is added, obtains urea-formaldehyde resin performed polymer aqueous solution, wherein the molar ratio of formaldehyde and urea is 1:
0.2, the volume ratio of water and formalin is 1:2.
By Metalaxyl-M raw medicine, pyraclostrobin raw medicine, methyl oleate and sorbitan monostearate polyoxyethylene
For ether successively through mixing, dispersion and sand milling, obtaining Metalaxyl-M pyraclostrobin can be dispersed oil-suspending agent, wherein the essence first
White spirit raw medicine, pyraclostrobin raw medicine, the weight ratio of methyl oleate and sldium lauryl sulfate are 1:12:15:0.5.
Oil-suspending agent can be dispersed in gained urea-formaldehyde resin performed polymer aqueous solution and Metalaxyl-M pyraclostrobin to exist
It is uniformly mixed under 1000 revs/min of mixing speed, first material is obtained, wherein the urea-formaldehyde resin performed polymer is water-soluble
The weight ratio that oil-suspending agent can be dispersed in liquid and Metalaxyl-M pyraclostrobin is 2:1；It at room temperature, is 3 by pH value, slow
The total concentration of punching pair is the citric acid-sodium citrate buffer of 2 weight %, and above-mentioned first is evenly added in 1 hour
It in material, is uniformly mixed with 200 revs/min of mixing speed, to adjust pH value as 5.8, obtains second material；In room temperature condition
Under, the acetic acid that concentration is 5 weight % is evenly added in above-mentioned second material in 2 hours, with 400 revs/min stir
It mixes speed to be uniformly mixed, to adjust pH value as 3.0, obtains third material；Under conditions of 50 DEG C, the third material is carried out
Polycondensation 3 hours, obtain polycondensation product；And potassium hydroxide is added to be adjusted to the pH value of the polycondensation product
7；Pull open powder, bentonite, ethylene glycol, Sodium Polyacrylate, red mill base is added to be uniformly mixed, obtains 4 materials, i.e. pyrazoles ether
Bacterium ester Metalaxyl-M microcapsule suspending agent；Wherein, the polycondensation product and pull open powder, bentonite, ethylene glycol, polyacrylic acid
Sodium, red mill base weight ratio be 1:0.04:0.004:0.05:0.01:0.15.
Embodiment 6
Urea is uniformly mixed with the formalin that concentration is 37 weight %, is 9 in pH value, under the conditions of temperature is 70 DEG C
React 1h；Water dilution is added, obtains urea-formaldehyde resin performed polymer aqueous solution, wherein the molar ratio of formaldehyde and urea is 1:1,
The volume ratio of water and formalin is 1:1.
Successively by Metalaxyl-M raw medicine, pyraclostrobin raw medicine, methyl oleate and EO-PO block copolymer AtloxG5000
Through mixing, dispersion and sand milling, obtaining Metalaxyl-M pyraclostrobin can be dispersed oil-suspending agent, wherein the Metalaxyl-M is former
Medicine, pyraclostrobin raw medicine, the weight ratio of methyl oleate and EO-PO block copolymer are 1:1:10:5.
Oil-suspending agent can be dispersed in gained urea-formaldehyde resin performed polymer aqueous solution and Metalaxyl-M pyraclostrobin to exist
It is uniformly mixed under 500 revs/min of mixing speed, first material is obtained, wherein the urea-formaldehyde resin performed polymer aqueous solution
The weight ratio that oil-suspending agent can be dispersed with Metalaxyl-M pyraclostrobin is 1:1；It at room temperature, is 2 by pH value, buffering
Pair total concentration be 5.5 weight % citric acid-sodium citrate buffer, above-mentioned first is evenly added in 1 hour
It in material, is uniformly mixed with 200 revs/min of mixing speed, to adjust pH value as 5.5, obtains second material；In room temperature condition
Under, the phosphoric acid solution that concentration is 1 weight % is evenly added in above-mentioned second material in 2 hours, with 400 revs/min
Mixing speed be uniformly mixed, with adjust pH value be 4.0, obtain third material；Under conditions of 50 DEG C, by the third material
It carries out polycondensation 3 hours, obtains polycondensation product；And potassium hydroxide is added by the pH value tune of the polycondensation product
It saves to 7；Pull open powder, xanthan gum, ethylene glycol, Sodium Polyacrylate, red mill base is added to be uniformly mixed, obtains 4 materials, i.e. pyrrole
Azoles kresoxim-methyl Metalaxyl-M microcapsule suspending agent；Wherein, the polycondensation product and pull open powder, xanthan gum, ethylene glycol, poly- third
Olefin(e) acid sodium, red mill base weight ratio be 1:0.04:0.002:0.05:0.01:0.15.
Embodiment 7
Urea is uniformly mixed with the formalin that concentration is 37 weight %, is 9 in pH value, under the conditions of temperature is 70 DEG C
React 1h；Water dilution is added, obtains urea-formaldehyde resin performed polymer aqueous solution, wherein the molar ratio of formaldehyde and urea is 1:
0.5, the volume ratio of water and formalin is 1:1.
Metalaxyl-M raw medicine, pyraclostrobin raw medicine, soybean oil and EO-PO block copolymer D800 are successively mixed,
Dispersion and sand milling, obtaining Metalaxyl-M pyraclostrobin can be dispersed oil-suspending agent, wherein the Metalaxyl-M raw medicine, pyrazoles
The weight ratio of kresoxim-methyl raw medicine, vegetable oil and EO-PO block copolymer is 1:0.1:10:5.
Oil-suspending agent can be dispersed in gained urea-formaldehyde resin performed polymer aqueous solution and Metalaxyl-M pyraclostrobin to exist
It is uniformly mixed under 500 revs/min of mixing speed, first material is obtained, wherein the urea-formaldehyde resin performed polymer aqueous solution
The weight ratio that oil-suspending agent can be dispersed with Metalaxyl-M pyraclostrobin is 1:1；It at room temperature, is 4 by pH value, buffering
Pair total concentration be 4 weight % citric acid-sodium citrate buffer, above-mentioned first object is evenly added in 1 hour
It in material, is uniformly mixed with 200 revs/min of mixing speed, to adjust pH value as 5.5, obtains second material；In room temperature condition
Under, by concentration be 0.5 weight % phosphoric acid solution be evenly added in above-mentioned second material in 0.5 hour, with 200 turns/
The mixing speed of minute is uniformly mixed, and to adjust pH value as 4.0, obtains third material；Under conditions of 50 DEG C, by the third
Material carries out polycondensation 3 hours, obtains polycondensation product；And triethanolamine is added by the pH of the polycondensation product
Value is adjusted to 6.5；Naphthalene sulfonate Morwet-D425, bentonite, ethylene glycol, Sodium Polyacrylate, red mill base mixing is added
It is even, obtain 4 materials, i.e. pyraclostrobin Metalaxyl-M microcapsule suspending agent；Wherein, the polycondensation product and naphthalene sulphur
Hydrochlorate, xanthan gum, ethylene glycol, Sodium Polyacrylate, red mill base weight ratio be 1:0.03:0.002:0.05:0.01:0.15.
Embodiment 8
Urea is uniformly mixed with the formalin that concentration is 37 weight %, is 9 in pH value, under the conditions of temperature is 70 DEG C
React 1h；Water dilution is added, obtains urea-formaldehyde resin performed polymer aqueous solution, wherein the molar ratio of formaldehyde and urea is 1:
0.5, the volume ratio of water and formalin is 1:2.
By Metalaxyl-M raw medicine, pyraclostrobin raw medicine, paraffin oil and sldium lauryl sulfate successively through mixing, dispersion and sand
Mill, obtaining Metalaxyl-M pyraclostrobin can be dispersed oil-suspending agent, wherein the Metalaxyl-M raw medicine, pyraclostrobin are former
The weight ratio of medicine, paraffin oil and sldium lauryl sulfate is 1:5:5:5.
Oil-suspending agent can be dispersed in gained urea-formaldehyde resin performed polymer aqueous solution and Metalaxyl-M pyraclostrobin to exist
It is uniformly mixed under 600 revs/min of mixing speed, obtains first material, wherein the urea-formaldehyde resin performed polymer is water-soluble
The weight ratio that oil-suspending agent can be dispersed in liquid and Metalaxyl-M pyraclostrobin is 1:1；It at room temperature, is 3 by pH value, slow
The total concentration of punching pair is the citric acid-sodium citrate buffer of 2 weight %, and above-mentioned first is evenly added in 1 hour
It in material, is uniformly mixed with 200 revs/min of mixing speed, to adjust pH value as 5.5, obtains second material；In room temperature condition
Under, the hydrochloric acid that concentration is 4 weight % is evenly added in above-mentioned second material in 1 hour, with 200 revs/min stir
It mixes speed to be uniformly mixed, to adjust pH value as 3.0, obtains third material；Under conditions of 40 DEG C, the third material is carried out
Polycondensation 4 hours, obtain polycondensation product；And triethanolamine is added to be adjusted to the pH value of the polycondensation product
6.5；Naphthalene sulfonate Morwet-D425, bentonite, urea, Sodium Polyacrylate, red mill base is added to be uniformly mixed, obtains the 4th
Material, i.e. pyraclostrobin Metalaxyl-M microcapsule suspending agent；Wherein, the polycondensation product and naphthalene sulfonate, xanthan gum,
Urea, Sodium Polyacrylate, red mill base weight ratio be 1:0.03:0.002:0.1:0.01:0.15.
Embodiment 9
Urea is uniformly mixed with the formalin that concentration is 37 weight %, is 9 in pH value, under the conditions of temperature is 70 DEG C
React 1.5h；Water dilution is added, obtains urea-formaldehyde resin performed polymer aqueous solution, wherein the molar ratio of formaldehyde and urea is 1:
0.5, the volume ratio of water and formalin is 1:2.
By Metalaxyl-M raw medicine, pyraclostrobin raw medicine, methyl oleate and sorbitan monostearate polyoxyethylene
For ether successively through mixing, dispersion and sand milling, obtaining Metalaxyl-M pyraclostrobin can be dispersed oil-suspending agent, wherein the essence first
White spirit raw medicine, pyraclostrobin raw medicine, the weight ratio of methyl oleate and sorbitan monostearate polyoxyethylene ether are 1:
1:5:4。
Oil-suspending agent can be dispersed in gained urea-formaldehyde resin performed polymer aqueous solution and Metalaxyl-M pyraclostrobin to exist
It is uniformly mixed under 1000 revs/min of mixing speeds, first material is obtained, wherein the urea-formaldehyde resin performed polymer aqueous solution
The weight ratio that oil-suspending agent can be dispersed with Metalaxyl-M pyraclostrobin is 4:1；It at room temperature, is 4 by pH value, buffering
Pair total concentration be 2 weight % acetic acid-sodium acetate buffer solution, be evenly added in above-mentioned first material in 1 hour,
It is uniformly mixed with 200 revs/min of mixing speed, to adjust pH value as 6.2, obtains second material；It at room temperature, will be dense
Degree is that the hydrochloric acid of 5 weight % is evenly added in above-mentioned second material in 1.5 hours, with 500 revs/min of mixing speed
It is uniformly mixed, to adjust pH value as 4.0, obtains third material；Under conditions of 60 DEG C, the third material is subjected to solidification contracting
Poly- 2 hours, obtain polycondensation product；And the triethanolamine of 5 weight % is added by the pH value tune of the polycondensation product
It saves to 7；Polycarboxylate Atlox 4913, aluminum magnesium silicate, ethylene glycol, equal vinylacetate, red mill base is added to be uniformly mixed, obtains
To 4 materials, i.e. pyraclostrobin Metalaxyl-M microcapsule suspending agent；Wherein, the polycondensation product and polycarboxylate,
Aluminum magnesium silicate, ethylene glycol, equal vinylacetate, red mill base weight ratio be 1:0.005:0.006:0.15:0.15:0.25.
Embodiment 10
Urea is uniformly mixed with the formalin that concentration is 37 weight %, is 9 in pH value, under the conditions of temperature is 70 DEG C
React 1.5h；Water dilution is added, obtains urea-formaldehyde resin performed polymer aqueous solution, wherein the molar ratio of formaldehyde and urea is 1:
0.5, the volume ratio of water and formalin is 1:2.
By Metalaxyl-M raw medicine, pyraclostrobin raw medicine, methyl oleate and sorbitan monostearate polyoxyethylene
For ether successively through mixing, dispersion and sand milling, obtaining Metalaxyl-M pyraclostrobin can be dispersed oil-suspending agent, wherein the essence first
White spirit raw medicine, pyraclostrobin raw medicine, the weight ratio of methyl oleate and sorbitan monostearate polyoxyethylene ether are 1:
1:5:4。
Oil-suspending agent can be dispersed in gained urea-formaldehyde resin performed polymer aqueous solution and Metalaxyl-M pyraclostrobin to exist
Under 400 revs/min of mixing speeds be uniformly mixed, obtain first material, wherein the urea-formaldehyde resin performed polymer aqueous solution and
The weight ratio that oil-suspending agent can be dispersed in Metalaxyl-M pyraclostrobin is 4:1；It at room temperature, is 3 by pH value, buffering pair
Total concentration be 3 weight % acetic acid-sodium acetate buffer solution, be evenly added in above-mentioned first material in 2 hours, with
100 revs/min of mixing speed is uniformly mixed, and to adjust pH value as 6.2, obtains second material；At room temperature, by concentration
Hydrochloric acid for 5 weight % is evenly added in above-mentioned second material in 2.5 hours, mixed with 600 revs/min of mixing speed
It closes uniformly, to adjust pH value as 4.0, obtains third material；Under conditions of 60 DEG C, the third material is subjected to polycondensation
2 hours, obtain polycondensation product；And the triethanolamine that 5 weight % are added adjusts the pH value of the polycondensation product
To 7；Polycarboxylate, aluminum magnesium silicate, ethylene glycol, sodium carboxymethylcellulose, red mill base is added to be uniformly mixed, obtains the 4th object
Material, i.e. seed treatment pyraclostrobin Metalaxyl-M microcapsule suspending agent；Wherein, the polycondensation product and polycarboxylate,
Aluminum magnesium silicate, ethylene glycol, sodium carboxymethylcellulose, red mill base weight ratio be 1:0.02:0.02:0.1:0.05:0.15.
Comparative example 1
The difference from embodiment 1 is that adjusting pH without citric acid-sodium citrate buffer after obtaining first material
Value directlys adopt the hydrochloric acid that concentration is 5 weight % and the pH value of material is adjusted to 4.0.
Comparative example 2
The difference from embodiment 1 is that after obtaining first material, using pH value for the total concentration of 4, buffering pair is 2 weights
After material pH value is adjusted to 6 by the citric acid-sodium citrate buffer of amount %, without the step of adjusting pH value for the second time.
Comparative example 3
The difference from embodiment 1 is that third material without heating stirring solidification process, directly with dispersing agent, increase
Thick dose, antifreezing agent, film forming agent, mill base mixing, obtain Metalaxyl-M pyraclostrobin micro-capsule and hang microcapsule suspending agent.
The common situ aggregation method of comparative example 4 prepares Metalaxyl-M pyraclostrobin seed treatment microcapsule suspending agent.
Method according to the embodiment 1 prepares melamine formaldehyde resin performed polymer aqueous solution.
By gained melamine formaldehyde resin performed polymer aqueous solution and Metalaxyl-M pyraclostrobin missible oil 800 turns/
It is uniformly mixed under minute stirring rate, obtains first material.Wherein the melamine formaldehyde resin performed polymer aqueous solution and essence
The weight ratio of metalaxyl pyraclostrobin missible oil is 4:1；The Metalaxyl-M pyraclostrobin missible oil is by Metalaxyl-M original
Medicine, pyraclostrobin raw medicine, dimethylbenzene and triphenyl vinyl phenol polyoxyethylene ether composition, the Metalaxyl-M raw medicine, pyrazoles
The weight ratio of kresoxim-methyl raw medicine, dimethylbenzene and triphenyl vinyl phenol polyoxyethylene ether is 1:1:10:1.
At room temperature, the citric acid-sodium citrate that pH value is 4, the total concentration of buffering pair is 3 weight % is buffered molten
Liquid is evenly added in above-mentioned first material in 1 hour, is uniformly mixed with 250 revs/min of mixing speed, to adjust
PH value is 6.0, obtains second material；At room temperature, the hydrochloric acid that concentration is 5 weight % is evenly added in 1.5 hours
Enter into above-mentioned second material, be uniformly mixed with 400 revs/min of mixing speed, to adjust pH value as 4.0, obtains third object
Material；Under conditions of 55 DEG C, the third material is carried out polycondensation 2.5 hours, polycondensation product is obtained；And it is added
The pH value of the polycondensation product is adjusted to 7.0 by triethanolamine；Polycarboxylate, aluminum magnesium silicate, ethylene glycol, methylol is added
Sodium cellulosate, red mill base are uniformly mixed, and obtain 4 materials, i.e. pyraclostrobin Metalaxyl-M microcapsule suspending agent；Wherein,
The polycondensation product and polycarboxylate, aluminum magnesium silicate, ethylene glycol, sodium cellulose glycolate, red mill base weight ratio be
1:0.02:0.003:0.05:0.05:0.1。
5 interfacial polymerization of comparative example prepares Metalaxyl-M pyraclostrobin microcapsule suspending agent
Metalaxyl-M raw medicine, pyraclostrobin raw medicine, dimethylbenzene, toluene di-isocyanate(TDI) are uniformly mixed, oily phase is obtained,
The metalaxyl raw medicine, pyraclostrobin raw medicine, dimethylbenzene, toluene di-isocyanate(TDI) weight ratio be 1:1:2:0.05；By water
It is uniformly mixed with calcium dodecyl benzene sulfonate, obtains water phase, the weight ratio of the water and calcium dodecyl benzene sulfonate is 1:0.05.
The oil is mutually sheared 5 minutes under 20000 revs/min of rate with water phase, O/W emulsion, the oil are obtained
Mutually and the weight ratio of water phase is 1:1；Ethylenediamine is added into the O/W emulsion, and stirs 1 hour, obtains Metalaxyl-M
Pyraclostrobin microcapsule suspension；Polycarboxylate, silicic acid are added in the Metalaxyl-M pyraclostrobin microcapsule suspension
Magnalium, ethylene glycol, sodium cellulose glycolate, red mill base, obtain pyraclostrobin Metalaxyl-M seed treatment microcapsule suspension
Agent, the Metalaxyl-M pyraclostrobin microcapsule suspension, polycarboxylate, aluminum magnesium silicate, ethylene glycol, hydroxymethyl cellulose
Sodium, red mill base weight ratio be 1:0.02:0.003:0.05:0.05:0.1.
6 Metalaxyl-M pyraclostrobin suspoemulsion of comparative example
Metalaxyl-M raw medicine, pyraclostrobin raw medicine, polycarboxylate, xanthan gum, ethylene glycol and water are uniformly mixed, through sand
Grinding machine is ground to partial size less than 5 μm, obtains Metalaxyl-M pyraclostrobin suspoemulsion, the metalaxyl raw medicine, pyrazoles ether bacterium
Ester raw medicine, polycarboxylate, xanthan gum, ethylene glycol and water weight ratio be 1:1:0.02:0.003:0.05:15.
7 Metalaxyl-M seed treatment microcapsule suspending agent of comparative example
Metalaxyl-M seed treatment microcapsule suspending agent is prepared according to the method for embodiment 1.
8 pyraclostrobin seed treatment microcapsule suspending agent of comparative example
Pyraclostrobin seed treatment microcapsule suspending agent is prepared according to the method for embodiment 1.
Testing example 1
The heat storage stability of sample of this testing example for being prepared in testing example 1-10 and comparative example 1-8
And low-temperature stability.
Heat storage stability test: the sample being prepared in embodiment 1-10 and comparative example 1-8 is fitted into container, is sealed
It is placed in the constant temperature oven of (54 ± 2) DEG C afterwards, takes out observation after standing 14 days, according to GB/T14825-2006 standard, measurement
The suspensibility of sample, the results are shown in Table 1.
Low-temperature stability measurement: the sample being prepared in embodiment 1-10 and comparative example 1-8 is fitted into container, is sealed
Be placed in (0 ± 2) DEG C refrigerator, keep 1h, stir primary, each 15s at interval of 15min, observation appearance have it is unchanged,
(0 ± 2) DEG C continues to place 7 days, then takes out after being placed in and standing restore under room temperature, according to GB/T14825-2006 standard,
The suspensibility for measuring sample, the results are shown in Table 1.
Table 1
In table 1, through embodiment 1-10 it can be seen that the smart first that the method provided by the present invention is prepared compared with comparative example 1-8
White spirit pyraclostrobin seed treatment microcapsule suspending agent has good heat storage stability and low tempertaure storage stability, the present invention
In the method for offer, oil is mutually made into dispersible oil-suspending agent, substep pH value is adjusted to the processing of Metalaxyl-M pyraclostrobin
The storage stability of microcapsule suspending agent has extremely important effect.
Testing example 2
This testing example imitates sample obtained in embodiment 1-10 and comparative example 1-8 to the prevention and treatment of seedling rot on rice
Fruit and influence to paddy growth situation are tested, and testing location is selected in Jiangsu Province Huai'an, the selected experimental plot soil fertilizer of institute
Power is medium, and management is fine, and planted rice varieties are new two excellent 98, and planting type is live streaming, and Dressing before sowing dries laggard
Row presoaking and germinating, 30~50g (a.i.)/100kg seed, medical fluid ratio are 1:50, after planting normal management.
Test is dressed seed respectively after suitable quantity of water is added in the sample that embodiment 1-10 and comparative example 1-8 are obtained, blank pair
According to not dressing seed, each processing is repeated 3 times, and amounts to 54 cells, and every 66.7 ㎡ of cell carries out random alignment to cell.
After planting 10d investigates the occurring degree of emergence rate, after planting 30d investigation seedling growing way, seedling rot, and harvest time surveys real
It produces, calculates average product.
Investigation method:
Investigation seedling growing way: every cell takes at 5 points at random, and every takes 10 plants of rice seedlings measurement plant heights, hundred Miao Xianchong.
Efficacy survey: every cell takes 5 points of investigation at random, and every takes 100 plants, digs seedling depth 30cm, withered with the dirty green of seedling
Extremely, old complaint color is secretly index Investigate incidence, calculates relative control effect.
Harvest time each cell surveys real production, and estimates per mu yield according to area.
It respectively the results are shown in Table 1.
Seedling rot relative control effect (%)=(PT-CK)/CK × 100
In formula: CK --- blank district disease incidence；
PT --- treatment region disease incidence.
Table 2
In the above testing example 2, it is known that the pyraclostrobin Metalaxyl-M that technical solution of the present invention obtains
Seed treatment microcapsule suspending agent is coated processing and can be improved emergence rate, promotes crops seedling stage growth, and can significantly extend pair
The lasting period of crops seedling stage disease was finally reached volume increase still 90% or more to the control efficiency of base rot disease after 30 days
Effect.
Testing example 3
This testing example is to sample obtained in embodiment 1-10 and comparative example 1-8 to banded sclerotial blight, full rot on wheat
Control efficiency and the lasting period tested, testing location is selected in Hebei province Baoding, and the selected experimental plot soil fertility of institute is medium,
Management is fine, and planted wheat breed is wheat 175 in new, Dressing before sowing, 30~50g (a.i.)/100kg seed, medical fluid
Than for 1:50, after planting normal management.
Test is dressed seed respectively after suitable quantity of water is added in the sample that embodiment 1-10 and comparative example 1-8 are obtained, blank pair
According to not dressing seed, each processing is repeated 3 times, and amounts to 54 cells, and every 66.7 ㎡ of cell carries out random alignment to cell.
10d, 30d, 60d investigate banded sclerotial blight, full rot incidence after wheat emergence, and each treatment region uses at random 5 points
Sampling, every cell investigate 30 plants, investigate banded sclerotial blight, full rot disease incidence, calculate relative control effect.
Banded sclerotial blight/full rot relative control effect (%)=(PT-CK)/CK × 100
In formula: CK --- blank district disease incidence；
PT --- treatment region disease incidence；
It respectively the results are shown in Table 3.
Table 3
In the above testing example, according to the result in table 2, table 3 it can be found that through embodiment 1-10 and comparative example 1-8
Compare it can be seen that preparation method provided by the invention makes cream after doing oily phase using dispersible oil-suspending agent, by buffer solution and
Under the specific reaction conditions such as specific combination, adjusted stepwise reaction system, the corresponding emulsifier of selection, the solvent of acidic ph modifier
The Metalaxyl-M pyrazoles ether that the Metalaxyl-M pyraclostrobin microcapsule suspending agent being prepared is prepared relative to other methods
Bacterium ester micro capsule suspending agent, non-encapsulated form, single dose dosage form prevent and treat the effect of sprout term disease in which can obtain slow release long-acting, thus
Times for spraying and dosage are reduced, save the cost reduces the pollution to environment.
The preferred embodiment of the disclosure is described in detail above, still, during the disclosure is not limited to the above embodiment
Detail a variety of simple variants can be carried out to the technical solution of the disclosure in the range of the technology design of the disclosure, this
A little simple variants belong to the protection scope of the disclosure.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, it can be combined in any appropriate way.In order to avoid unnecessary repetition, the disclosure to it is various can
No further explanation will be given for the combination of energy.
In addition, any combination can also be carried out between a variety of different embodiments of the disclosure, as long as it is without prejudice to originally
Disclosed thought equally should be considered as disclosure disclosure of that.
Claims (10)
1. a kind of preparation method of Metalaxyl-M pyraclostrobin microcapsule suspending agent, which is characterized in that the preparation method includes
Following steps:
(1) the first solution and second liquid are uniformly mixed, obtain first material；Wherein, first solution contains urea-first
Urea formaldehyde performed polymer aqueous solution；The second liquid, which contains pyraclostrobin Metalaxyl-M, can be dispersed oil-suspending agent；Described
The weight ratio of one solution and the second liquid is (1-5): 1；
(2) first material is uniformly mixed with buffer solution, to adjust pH value as 5.5-6.5, obtains second material；
(3) will the second material stir 30-60 minutes after be uniformly mixed with acidic pH adjustor, to adjust pH value as 3-5,
Obtain third material；
(4) the third material is subjected to polycondensation, obtains polycondensation product, and by the pH of the polycondensation product
Value is adjusted to 6.5-7.5；
It (5) will be in the polycondensation product and dispersing agent, thickener, film forming agent, mill base and antifreezing agent after the adjusting pH value
It is one or more to be uniformly mixed, obtain Metalaxyl-M pyraclostrobin microcapsule suspending agent.
2. preparation method according to claim 1, wherein in step (1), the urea-formaldehyde resin performed polymer is water-soluble
Liquid is obtained by the material liquid prepolymerization containing urea, formaldehyde and water；The prepolymerized condition includes: that pH value is 8-10, temperature
It is 70-75 DEG C, the reaction time is 1-2 hours.
3. preparation method according to claim 1 or 2, wherein in step (1), the pyraclostrobin Metalaxyl-M
Dispersible oil-suspending agent contains pyraclostrobin raw medicine, Metalaxyl-M raw medicine, emulsifier and oil medium；
The emulsifier includes lauryl sodium sulfate, neopelex, styrene-maleic anhydride copolymer, fat
Alcohol polyoxyethylene ether, anhydrous sorbitol polyoxyethylene poly-oxygen propylene aether, sorbitan monostearate polyoxyethylene ether, laurel
At least one of alcohol sodium sulphate, alkyl phenol polyoxyethylene ether, castor oil polyoxyethylene ether and EO-PO block copolymer；
The oil medium includes at least one of methyl oleate, ethyl oleate, vegetable oil, mineral oil and paraffin oil；
The pyraclostrobin raw medicine, Metalaxyl-M raw medicine, the weight ratio of emulsifier and oil medium are 1:(0.1-10): (1-
10): (1-10)；
The preparation method that oil-suspending agent can be dispersed in the pyraclostrobin Metalaxyl-M includes: by Metalaxyl-M raw medicine, pyrazoles
Kresoxim-methyl raw medicine successively mixed with emulsifier, oil medium, dispersion and sand milling, obtains pyrazoles ether bacterium described in step (1)
Oil-suspending agent can be dispersed in ester Metalaxyl-M；
The Metalaxyl-M raw medicine, the suspended particulates average grain diameter of pyraclostrobin raw medicine are 1-5 microns.
4. preparation method described in any one of -3 according to claim 1, wherein in step (2), the pH of the buffer solution
Value is 3-5；The total concentration of buffering pair is 1-5 weight % in the buffer solution；Buffering in the buffer solution is to including lemon
At least one of lemon acid-sodium citrate, citrate-phosphate disodium hydrogen and acetic acid-sodium acetate.
5. preparation method described in any one of -4 according to claim 1, wherein in step (3), the acidic ph modifier
Concentration be 1-10 weight %；The solute of the acidic ph modifier includes in hydrogen chloride, sulfuric acid, acetic acid, ammonium chloride and phosphoric acid
At least one.
6. preparation method described in any one of -5 according to claim 1, wherein in step (4), the polycondensation condition
It is 40-65 DEG C including solidification temperature, curing time is 2-6 hours, and curing mode is mechanical stirring；Pass through after the completion of polycondensation
At least one of triethylamine solution, triethanolamine solution, sodium hydroxide solution, potassium hydroxide solution pH adjusting agent is by the solidification
The pH value of product is adjusted to 6.5-7.5 after polycondensation.
7. preparation method described in any one of -6 according to claim 1, wherein in step (5),
The dispersing agent include neopelex, sodium methylene bis-naphthalene sulfonate, 1- methyl naphthalene sulfonate formaldehyde condensate,
Benzyl naphthalene sulfonic acid-formaldehyde condensation product, sodium lignin sulfonate, desugar sodium lignin sulfonate, desugar are condensed sodium lignin sulfonate, fourth two
Acid esters sodium sulfonate, pull open powder, nonylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether, polycarboxylate, naphthalene sulfonate, EO-PO
At least one of block copolymer and pull open powder；
The thickener includes aluminum magnesium silicate, xanthan gum, polyethylene glycol, polyvinyl alcohol, carboxymethyl cellulose, bentonite and hard charcoal
It is one of black or a variety of；
The antifreezing agent includes one of ethylene glycol, 1,2- propylene glycol, glycerine and urea or a variety of；The film forming agent can be with
Including Arabic gum, animal glue, methylcellulose, ethyl cellulose, sodium cellulose glycolate, polyvinyl alcohol, polyethylene glycol, gather
At least one in acrylamide, Sodium Polyacrylate, equal polyvinyl acetate, polysaccharide high-molecular compound and cellulose derivative
Kind；
The mill base includes red or blue water-soluble mill base；
The weight ratio of the polycondensation product and dispersing agent, thickener, antifreezing agent, film forming agent, mill base is 1:(0.01-
0.05): (0.001-0.005): (0.05-0.1): (0.01-0.1): (0.05-0.2).
8. preparation method according to any one of claims 1-7, wherein
In step (1), mixed condition includes: that mixing speed is 500-1000 revs/min；
In step (2), mixed condition includes: that buffer solution, stirring are at the uniform velocity added in 0.5-1 hours under the conditions of 25-35 DEG C
Speed is 200-300 revs/min；
In step (3), mixed condition includes: that acidic pH adjustor is at the uniform velocity added in 1-2 hours under the conditions of 25-35 DEG C,
Mixing speed is 300-500 revs/min.
9. a kind of Metalaxyl-M pyraclostrobin microcapsule suspending agent, wherein the microcapsule suspending agent is according to claim 1 in -8
What preparation method described in any one claim obtained.
10. application of the Metalaxyl-M pyraclostrobin microcapsule suspending agent in seed treatment.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113402321A (en) * | 2021-06-23 | 2021-09-17 | 湖北富邦科技股份有限公司 | Method for preparing calcium-magnesium suspended fertilizer by using nanofiltration seawater to trap carbon dioxide product |
| CN114230395A (en) * | 2021-12-16 | 2022-03-25 | 河北安格诺农化有限公司 | Slow-release pesticide-fertilizer composition and application thereof |
| CN115414865A (en) * | 2022-09-27 | 2022-12-02 | 溢通环保科技（莆田）有限公司 | Anti-settling polymerization inhibitor for diesel oil tail gas treatment fluid and production process thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117441738A (en) * | 2023-12-26 | 2024-01-26 | 山东科赛基农生物工程有限公司 | Seed treatment suspending agent containing metalaxyl-M, pyraclostrobin and fluxapyroxad and application thereof |
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