CN108353897A - A kind of pesticide microcapsule suspending agent and preparation method thereof - Google Patents
A kind of pesticide microcapsule suspending agent and preparation method thereof Download PDFInfo
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- CN108353897A CN108353897A CN201810258971.4A CN201810258971A CN108353897A CN 108353897 A CN108353897 A CN 108353897A CN 201810258971 A CN201810258971 A CN 201810258971A CN 108353897 A CN108353897 A CN 108353897A
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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
- 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
-
- 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
- A01N37/18—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 the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof
- A01N37/26—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 the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof containing the group; Thio analogues thereof
-
- 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
- A01N53/00—Biocides, pest repellants or attractants, or plant growth regulators containing cyclopropane carboxylic acids or derivatives thereof
-
- 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
- A01N57/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
- A01N57/10—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds
- A01N57/16—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds containing heterocyclic radicals
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- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Zoology (AREA)
- Agronomy & Crop Science (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Dentistry (AREA)
- Wood Science & Technology (AREA)
- Environmental Sciences (AREA)
- Toxicology (AREA)
- Dispersion Chemistry (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing Of Micro-Capsules (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a kind of pesticide microcapsule suspending agent and preparation method thereof, the pesticide microcapsule suspending agent grain size is 0.1 20 microns, and for cyst material using polyurethane or polyureas etc., capsule-core can be pyrethroids class, organic phosphates or phenyl amines pesticide.The present invention, which is polymerize by microreactor with liquid/liquid interface, is made pesticide microcapsule suspending agent, simple for process, microcapsule diameter obtained is controllable and is evenly distributed, and simplifies pesticide microcapsule suspending agent preparation process, production enlarge-effect is reduced, there is important value in terms of pesticide microencapsulation.
Description
Technical field
The present invention relates to chemical technology field, more particularly to a kind of pesticide microcapsule suspending agent and its preparation side
Method.
Background technology
Pesticide is that agricultural volume increase and increasing peasant income are made that huge contribution, but conventional pesticide dosage form for example missible oil, pulvis,
Wettable powder, finish etc. increasingly show the drawbacks such as high poison, high residue, Environmental compatibility difference.In recent years, since people's environmental protection is anticipated
The continuous enhancing known, using high molecular material as cyst wall or cyst membrane, by chemistry, physics or physico-chemical process, by pesticide activity
Substance wraps up, and forms a kind of pesticide microcapsule suspending agent of semipermeability cyst membrane and is gradually approved by people.With Traditional Agricultural
Medicine phases ratio, pesticide microcapsule suspending agent can reduce toxicity, poisoning and the environmental pollution of pesticide, have efficiency time length, to environment
, stable effective ingredients good and be not easy by rain drop erosion the advantages that low with human toxicity.
Although pesticide microcapsule suspending agent achieves certain achievement in research with application aspect, there are still much ask
Topic, mainly processing technology are complicated, and production cost is higher, and technical difficulty is big, and there are certain investment risks.Publication No.
The patent of CN101305725B discloses a kind of chlopyrifos and pymtrozine composite microcapsule suspending agent and preparation method thereof, using original
Position polymerization, i.e., by the pre-polymerization in mild alkaline conditions of the monomers such as formaldehyde and urea or melamine, being adjusted to acid condition makes pre-polymerization
Object molecule is constantly crosslinked, and deposits to form insoluble resin softgel shell in core surfaces, and this method reaction condition is complicated, technological parameter
There is minor change that will influence the size of microcapsules, wall thickness etc., the final performance for influencing drug effect, and the volatility such as formaldehyde used
Raw material also improve the danger of actual production operation.The patent of Publication No. CN103734162B discloses a kind of pyrazoles ether
Bacterium ester micro-capsule suspension makes oil-soluble monomer and water-soluble monomer in oil using interfacial polymerization by adding chain extender
Water termination occurs polycondensation reaction and generates the softgel shell with certain degree of hardness, wraps up active matter, and this method technique is relatively easy,
But the reaction time is longer, and unreacted monomer and certain side reactions can destroy the activity of capsule-core or influence the stability of cyst wall.
Therefore, how a kind of stable and easily controllable method for preparing pesticide microcapsule suspending agent is provided, and is made
The pesticide microcapsule suspending agent of preparation has good stability, permeability, is those skilled in the art's urgent problem to be solved.
Invention content
In view of this, the present invention provides a kind of pesticide microcapsule suspending agent, including following components in percentage by weight：
Active ingredient 1%-50%, cyst material 2%-10%, dispersant 1%-10%, antifoaming agent 0%-2%, synergist
0.2%-4% and preservative 0%-5%, surplus are water.
The advantageous effect of above-mentioned technical proposal is：Provide one kind can processability it is stable and have the function of uniform slow release
Pesticide microcapsule suspension agent prescription.
Preferably, the active ingredient is cypermethrin, fenvalerate, Fenpropathrin, gamma cyhalothrin, bromine cyanogen chrysanthemum
Any one or a few in ester, Biphenthrin, chlopyrifos, phoxim, pirimiphos-methyl, alachlor, Acetochlor, pretilachlor is mixed
Close object.
Preferably, the cyst material is polyurethane or one kind in polyureas or mixture.
Further, the cyst material is obtained by reaction monomers A and reaction monomers B polycondensation reactions, wherein reacting
Monomer A includes methyl diphenylene diisocyanate, toluene di-isocyanate(TDI), isophorone diisocyanate, dicyclohexyl methyl hydride
Diisocyanate or hexamethylene diisocyanate are one such or a variety of；Reaction monomers B includes ethylenediamine, hexamethylene diamine, two
Ethylene triamine, triethylene tetramine, ethylene glycol, propylene glycol or polyethylene glycol are one such or a variety of；Reaction monomers A and reaction are single
The weight ratio of body B is 1:0.1-0.5.
Preferably, the dispersant is lignosulfonates, APES formaldehyde condensation product, polymeric carboxylic
Any one or a few mixture in salt, the naphthalene sulfonate of modification, alkyl phenol polyoxyethylene ether, EO/PO block polyethers.
Preferably, the antifoaming agent is organic silicon defoamer and/or polyether antifoam agent；The synergist is organosilicon, pine
Any one or a few mixture in aliphatic radical vegetable oil, palm kernel fatty acid methyl esters；The preservative is benzoic acid, benzene first
Any one or a few mixture in acid sodium-salt, sorbic acid, sorbic acid sylvite, sulphite.
The advantageous effect of above-mentioned technical proposal is：In specific produce and use, can according to actual demand to pesticide variety and
Cyst material is chosen, and can be selected auxiliary agent according to the pesticide variety and cyst material type of selection and actual demand
It takes so that react the more abundant of progress, the pesticide microcapsule suspending agent of preparation has best performance.
It is another object of the present invention to provide a kind of preparation method of pesticide microcapsule suspending agent, this method equipment volumes
It is small, it is simple for process, by adjusting the technological parameter of micro-reaction device, Multiple Pesticides microcapsule suspending agent product, and grain size can be obtained
Uniform, controllable, then a variety of safeties are good, and stability is high by the preferred of active constituent content and auxiliary agent type, capable of preparing,
Pesticide microcapsule suspending agent with sustained release performance, specifically includes following steps：
1) by active ingredient and reaction monomers A mixed dissolutions, prepared composition dephasing；
2) dispersant, antifoaming agent and reaction monomers B are added to the water, are stirred evenly, be prepared into continuous phase；
3) rate of injecting for injecting pump in microreactor channel and microreactor channel is adjusted, is then pumped while being pushed away with injecting
The continuous phase of the dispersed phase and the middle preparation of the step 2) of noting the middle preparation of the step 1), which enters in microreactor channel, to be carried out instead
It answers；
Preferably, 40-60 DEG C of microreactor channel interior reaction temperature, reaction time 1-60min in the step 3).
The advantageous effect of above-mentioned technical proposal is：By controlling rational reaction temperature so that reaction has high reaction speed
Rate.
Further, the microreactor used in the step 3) includes heat exchange layers；The heat exchange layers are that electricity adds
Thermosphere, heat radiation band or microwave heating layer.
The advantageous effect of above-mentioned technical proposal is：It can choose whether to be heated according to actual production demand.
Preferably, the microreactor channel is made of metal channel, ceramic system channel or engineering plastics channel.
The advantageous effect of above-mentioned technical proposal is：When carrying out micro-capsule preparation reaction, pesticide material and auxiliary agent raw material are prevented
Microreactor channel is caused to corrode, ensures the degree of purity and advantageous effect of product pesticide, while ensureing the use of microreactor
Service life.
Another object of the present invention is to provide a kind of applications for the method preparing pesticide microcapsule suspending agent, are applied to pesticide
The material inlet end of multiple microreactors is specially sequentially connected in series, the outlet end of product by the continuous production of microcapsule suspending agent
It is sequentially connected in series, forms micro- reaction system of serialization, lab scale craft indifference is directly amplified, by the quantity for increasing microchannel
To realize life can be directly amplified by increasing the characteristic size of microchannel, therefore any change need not be made
Production has very high application value.
In summary technical solution, the beneficial effects of the invention are as follows：
(1) present invention prepares pesticide microcapsule suspending agent by microreactor serialization, and simple for process, microcapsule diameter is controllable,
And particle diameter distribution is uniform；
(2) the microreactor volume-diminished that the present invention uses, only the 1/100 of traditional batch reaction kettle or even 1/1000；
(3) the serialization microreactor system that the present invention uses, mass-and heat-transfer is efficient, can better controlling reaction temperature
With the shortening residence time, change the severity of chemical reaction, effectively avoid the generation of side reaction, keeps chemical reaction rate close
Its kinetic limitations；
(4) the continuous preparation method reaction process that the present invention uses is safer, different from traditional batch reaction kettle, micro- anti-
It is continuous flow reaction to answer device, therefore the chemical quantity stopped in the reactor is always seldom, and essential safety may be implemented, and
Microreactor is closed, can be endangered to avoid caused by Toxic material；
(5) the microreactor mixing efficiency used in the continuous preparation method that the present invention uses is high, micro- logical by designing
Road, convection current weight is folded to be strengthened mixing or is mixed using injection stream collision, can be lacked with even without emulsifier, you can formed
Emulsion；
(6) the microreactor mixing efficiency used in the continuous preparation method that the present invention uses is high, micro- logical by designing
Road, convection current weight is folded to be strengthened mixing or is mixed using injection stream collision, and emulsifier can not be had to, you can emulsion is formed,
Effectively reduce manufacturing cost.
Specific implementation mode
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
The every other embodiment that art personnel are obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment 1
20% Biphenthrin microcapsules is prepared according to the following steps
1) preparation of dispersed phase：By 20% Biphenthrin, 4% methyl diphenylene diisocyanate and 5% detergent alkylate
Sulfoacid calcium is uniformly mixed；
2) preparation of continuous phase：4% lignosulfonates, 1% ethylenediamine, 5% organic silicon defoamer and 40% water stir
It mixes uniformly；
3) molding of microcapsules：Above-mentioned dispersed phase and continuous phase are respectively charged into stirred tank, dispersed phase and continuous phase are matched
Identical to inject pump, dispersed phase stirred tank is injected with the speed of 100mL/min, and continuous phase stirred tank is with the speed of 200ul/min
It injects, dispersed phase and continuous phase solution form micro-capsule in microreactor channel, and Microcapsules Size is between 1-2 microns；
4) solidification of micro-capsule：Microreactor channel temperature is controlled at 40 DEG C, is controlled discharging speed, is kept microcapsules micro- in waveform
1h is reacted in channel of reactor, is formed and is stablized microcapsule structure；
5) preparation of microcapsule suspending agent：1% preservative, 2% synergist is added, water is supplied 100%, stirred evenly.
In order to optimize said program, according to the demand of production and application, cypermethrin, penta chrysanthemum of cyanogen also can be selected in pesticide active ingredient
Ester, Fenpropathrin, gamma cyhalothrin, decis, chlopyrifos, phoxim, pirimiphos-methyl, alachlor, Acetochlor, third
One or more of careless amine mixture；
In order to optimize above-mentioned technical proposal, methyl diphenylene diisocyanate can also be changed to toluene di-isocyanate(TDI), different Buddhist
That ketone diisocyanate, dicyclohexyl methyl hydride diisocyanate or hexamethylene diisocyanate are one such or a variety of；Second
Diamines can also be changed to hexamethylene diamine, diethylenetriamine, triethylene tetramine, ethylene glycol, propylene glycol or polyethylene glycol it is one such or
It is a variety of；
In order to optimize said program, dispersant is also chosen as the poly- polyoxyethylene ether formaldehyde condensation products of alkyl phenol, macromolecule carboxylic
One or more of hydrochlorate, the naphthalene sulfonate of modification, alkyl phenol polyoxyethylene ether, EO/PO block polyethers mixture；
In order to optimize said program, antifoaming agent is also chosen as polyether antifoam agent.
Embodiment 2
30% pirimiphos-methyl microcapsule formulations are prepared according to the following steps
1) preparation of dispersed phase：By 30% pirimiphos-methyl, 4% methyl diphenylene diisocyanate and 3% styryl
Phenol polyethenoxy ether is uniformly mixed；
2) preparation of continuous phase：4% alkyl phenol polyoxyethylene ether, 1% ethylenediamine, 0.5% organic silicon defoamer and
20% water stirs evenly；
3) molding of microcapsules：Above-mentioned dispersed phase and continuous phase are respectively charged into stirred tank, dispersed phase and continuous phase are matched
Identical to inject pump, two stirred tanks are injected with the speed of 100ul/min, and dispersed phase and continuous phase solution are logical in microreactor
Microcapsules are formed in road, Microcapsules Size can be between 5-6 microns；
4) solidification of microcapsules：Microreactor channel temperature is controlled at 50 DEG C, is controlled discharging speed, is made microcapsules in waveform
It is reacted 30 minutes in microreactor channel, is formed and stablize microcapsule structure；
5) preparation of microcapsule formulations：1% preservative, 2% synergist is added, water is supplied 100%, stirred evenly.
In order to optimize said program, according to actual production use demand, cypermethrin, cyanogen also can be selected in pesticide active ingredient
Valerate, Fenpropathrin, gamma cyhalothrin, decis, Biphenthrin, chlopyrifos, phoxim, pendimethalin, second grass
One or more of amine mixture；
In order to optimize above-mentioned technical proposal, methyl diphenylene diisocyanate can also be changed to toluene di-isocyanate(TDI), different Buddhist
That ketone diisocyanate, dicyclohexyl methyl hydride diisocyanate or hexamethylene diisocyanate are one such or a variety of；Second
Diamines can also be changed to hexamethylene diamine, diethylenetriamine, triethylene tetramine, ethylene glycol, propylene glycol or polyethylene glycol it is one such or
It is a variety of；
In order to optimize said program, dispersant is also chosen as lignosulfonates, alkyl phenol polyoxyethylene ether formaldehyde condensation
One or more of object, polymeric carboxylic salt, the naphthalene sulfonate of modification, EO/PO block polyethers mixture；
In order to optimize said program, antifoaming agent is also chosen as polyether antifoam agent.
Embodiment 3
50% Acetochlor microcapsule formulations are prepared according to the following steps
1) preparation of dispersed phase：By 50% Acetochlor, 4% methyl diphenylene diisocyanate and 3% fatty alcohol polyoxy second
Alkene ether is uniformly mixed；
2) preparation of continuous phase：The naphthalene sulfonate of 4% modification, 1% ethylenediamine, 1% polyether antifoam agent and 20% water stir
It mixes uniformly；
3) molding of microcapsules：Above-mentioned dispersed phase and continuous phase are respectively charged into stirred tank, dispersed phase and continuous phase are matched
Identical to inject pump, dispersed phase stirred tank is injected with the speed of 200ul/min, and continuous phase stirred tank is with the speed of 130ul/min
It injects, dispersed phase and continuous phase solution form microcapsules in microreactor channel, and Microcapsules Size can be between 3-4 microns；
4) solidification of microcapsules：Microreactor channel temperature is controlled at 60 DEG C, is controlled discharging speed, is made microcapsules in waveform
It is reacted 20 minutes in microreactor channel, is formed and stablize microcapsule structure；
5) preparation of microcapsule formulations：1% preservative, 1% synergist is added, water is supplied 100%, stirred evenly.
In order to optimize said program, according to actual production and use demand, the also optional cypermethrin of pesticide active ingredient,
Fenvalerate, Fenpropathrin, gamma cyhalothrin, decis, Biphenthrin, chlopyrifos, phoxim, pendimethalin, first
One or more of yl pyrimidines phosphorus mixture；
In order to optimize above-mentioned technical proposal, methyl diphenylene diisocyanate can also be changed to toluene di-isocyanate(TDI), different Buddhist
That ketone diisocyanate, dicyclohexyl methyl hydride diisocyanate or hexamethylene diisocyanate are one such or a variety of；Second
Diamines can also be changed to hexamethylene diamine, diethylenetriamine, triethylene tetramine, ethylene glycol, propylene glycol or polyethylene glycol it is one such or
It is a variety of；
In order to optimize said program, dispersant is also chosen as lignosulfonates, alkyl phenol polyoxyethylene ether formaldehyde condensation
One or more of object, alkyl phenol polyoxyethylene ether, polymeric carboxylic salt, EO/PO block polyethers mixture；
In order to optimize said program, antifoaming agent is also chosen as polyether antifoam agent.
Comparative example 1
Conventional batch interfacial polymerization prepares 20% Biphenthrin microcapsule suspending agent
(1) lignin of 20g Biphenthrins, 5g toluene di-isocyanate(TDI)s, 5g calcium dodecyl benzene sulfonates, 4g is weighed respectively
Sulfonate, 2g ethylenediamines, 2g organic silicon defoamers, 5g polycarboxylates, 1g sodium benzoates, 2g synergist, weigh up spare；
(2) dispersed phase is prepared：Above-mentioned load weighted Biphenthrin and hexamethylene diisocyanate are mixed evenly, 50 DEG C
Heating melting；
(3) continuous phase is prepared：By above-mentioned load weighted calcium dodecyl benzene sulfonate, lignosulfonates, organosilicon defoaming
Agent, polycarboxylate and water are mixed evenly, and temperature is 50 DEG C, and continuous phase is prepared；
(4) micro-capsule is prepared：By insulation of equipment at 50 DEG C, by dispersed phase and it is continuous mix after, in 5000rpm down cut breasts
Change 3min (grain size D90Control is at 1~3 micron), obtain oil-in-water emulsion；Above-mentioned title is added portionwise in lower 30 minutes in stirring condition
Measured ethylenediamine then continues to cure 5h under the conditions of 50 DEG C, and making cyst wall, the reaction was complete；
(5) microcapsules is prepared：To the above-mentioned load weighted sodium benzoate of above-mentioned addition, glycerine and aluminium-magnesium silicate, water is used in combination
100g is supplied, is stirred evenly, you can obtains microcapsule suspending agent；
(6) equipment is cleaned：After reaction, the equipment such as reaction kettle and shear agitation are cleaned in time, uses polarity when necessary
Solvent foam washing.
Contrast on effect：
Embodiment 1 is identical with 1 materials of comparative example, and technique is different, to the Biphenthrin microcapsule suspending agent of gained in two into
Row detection, testing result are as follows：
Interpretation of result：As can be seen from the above table, the stability test result compared to 1 embodiment 1 of comparative example is more preferable, especially
It is that effect when carrying out frozen process experiment is more preferable.When main because in technical solution disclosed by the invention, reaction is uniform, secondary anti-
It should lack, encapsulation rate is high, and quality is more stable；Comparative example 1 uses batch reactor technique, resulting product packet stability at later stage real
Some side reactions will continue to change in testing, and influence product stability.It can be seen that the present invention is preferably changed with technique by formula
Kind, Biphenthrin microcapsule suspending agent obtained has excellent survey storage stability, has good practical value.
Each embodiment is described by the way of progressive in this specification, the highlights of each of the examples are with other
The difference of embodiment, just to refer each other for identical similar portion between each embodiment.For device disclosed in embodiment
For, since it is corresponded to the methods disclosed in the examples, so description is fairly simple, related place is said referring to method part
It is bright.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest range caused.
Claims (10)
1. a kind of pesticide microcapsule suspending agent, which is characterized in that including following components in percentage by weight：
Active ingredient 1%-50%, cyst material 2%-10%, dispersant 1%-10%, antifoaming agent 0%-2%, synergist
0.2%-4% and preservative 0%-5%, surplus are water.
2. a kind of pesticide microcapsule suspending agent according to claim 1, which is characterized in that the active ingredient is chlorine cyanogen chrysanthemum
Ester, fenvalerate, Fenpropathrin, gamma cyhalothrin, decis, Biphenthrin, chlopyrifos, phoxim, methylpyrimidine
Any one or a few mixture in phosphorus, alachlor, Acetochlor, pretilachlor.
3. a kind of pesticide microcapsule suspending agent according to claim 1, which is characterized in that the cyst material polyurethane is poly-
One kind in urea or mixture.
4. a kind of pesticide microcapsule suspending agent according to claim 3, which is characterized in that the cyst material is to pass through reaction
Monomer A and reaction monomers B polycondensation reactions obtain, and wherein reaction monomers A includes methyl diphenylene diisocyanate, toluene diisocyanate
Acid esters, isophorone diisocyanate, dicyclohexyl methyl hydride diisocyanate or hexamethylene diisocyanate are one such
Or it is a variety of；Reaction monomers B includes ethylenediamine, hexamethylene diamine, diethylenetriamine, triethylene tetramine, ethylene glycol, propylene glycol or poly- second two
Alcohol is one such or a variety of；The weight ratio of reaction monomers A and reaction monomers B are 1:0.1-0.5.
5. a kind of pesticide microcapsule suspending agent according to claim 1, which is characterized in that the dispersant is lignin sulfonic acid
Salt, APES formaldehyde condensation product, polymeric carboxylic salt, the naphthalene sulfonate of modification, alkyl phenol polyoxyethylene ether,
Any one or a few mixture in EO/PO block polyethers.
6. according to a kind of preparation method of any pesticide microcapsule suspending agents of claim 1-6, which is characterized in that including with
Lower step：
1) by active ingredient and reaction monomers A mixed dissolutions, prepared composition dephasing；
2) dispersant, antifoaming agent and reaction monomers B are added to the water, are stirred evenly, be prepared into continuous phase；
3) rate of injecting that pump is injected in microreactor channel and microreactor channel is adjusted, then with injecting pump while injecting institute
The continuous phase of the dispersed phase and the middle preparation of the step 2) of stating the middle preparation of step 1), which enters in microreactor channel react, to be obtained
Obtain pesticide microcapsule suspending agent.
7. a kind of preparation method of pesticide microcapsule suspending agent according to claim 7, which is characterized in that in the step 3)
40-60 DEG C of microreactor channel interior reaction temperature, reaction time 1-60min.
8. a kind of preparation method of pesticide microcapsule suspending agent according to claim 7, which is characterized in that in the step 3)
The microreactor used includes heat exchange layers；The heat exchange layers are electric heating layer, heat radiation band or microwave heating layer.
9. a kind of preparation method of pesticide microcapsule suspending agent according to claim 7, which is characterized in that the microreactor
Channel is made of metal channel, ceramic system channel or engineering plastics channel.
10. a kind of application of the preparation method of pesticide microcapsule suspending agent according to claim 7, which is characterized in that application
In the continuous production of pesticide microcapsule suspending agent, specially the material inlet end of multiple microreactors is sequentially connected in series, product
Outlet end is sequentially connected in series, and forms micro- reaction system of serialization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810258971.4A CN108353897B (en) | 2018-03-27 | 2018-03-27 | Pesticide microcapsule suspending agent and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810258971.4A CN108353897B (en) | 2018-03-27 | 2018-03-27 | Pesticide microcapsule suspending agent and preparation method thereof |
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| CN109452272A (en) * | 2018-12-21 | 2019-03-12 | 江苏艾津农化有限责任公司 | A kind of avermectin microcapsule agent and preparation method thereof |
| CN109699642A (en) * | 2018-12-21 | 2019-05-03 | 江苏精禾界面科技有限公司 | A kind of pesticide micro-capsule and preparation method thereof can easily be accommodated rate of release |
| CN109717187A (en) * | 2018-12-21 | 2019-05-07 | 江苏艾津农化有限责任公司 | A kind of chloroacetanilide herbicides microcapsule suspending agent and preparation method thereof |
| CN109757475A (en) * | 2019-03-01 | 2019-05-17 | 杨卫东 | A kind of microcapsule formulation and preparation method thereof coating solid pesticide raw medicine |
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| CN108353897B (en) | 2021-03-16 |
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