CN106259422A - A kind of auxiliary agent for micro-capsule suspension and preparation method thereof - Google Patents
A kind of auxiliary agent for micro-capsule suspension and preparation method thereof Download PDFInfo
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- CN106259422A CN106259422A CN201610646693.0A CN201610646693A CN106259422A CN 106259422 A CN106259422 A CN 106259422A CN 201610646693 A CN201610646693 A CN 201610646693A CN 106259422 A CN106259422 A CN 106259422A
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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
- 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
-
- 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
-
- 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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2603—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen
- C08G65/2606—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups
- C08G65/2609—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups containing aliphatic hydroxyl groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2636—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing sulfur
Abstract
The invention discloses a kind of auxiliary agent for micro-capsule suspension and preparation method thereof, the structural formula of the auxiliary agent of described micro-capsule suspension is formula A or Formula B, the structural formula that the invention discloses the auxiliary agent for micro-capsule suspension is formula A its preparation method, the structural formula that the invention discloses the auxiliary agent for micro-capsule suspension is Formula B its preparation method, the invention also discloses some application of the micro-capsule suspension auxiliary agent prepared.The auxiliary agent of described micro-capsule suspension can not only prepare particle diameter little and be evenly distributed, encystation form is good, envelop rate is high microcapsule, and can effectively solve the problem of the layering of micro-capsule suspension, precipitation, can be applicable in the micro-capsule suspension of in-situ polymerization and interfacial polymerization.
Description
Technical field
The present invention relates to pesticide field, be specifically related to a kind of auxiliary agent for micro-capsule suspension and preparation method thereof.
Background technology
Microcapsule technology, is that fine particle or drop are used naturally occurring or synthetic macromolecule wall material cladding, and formation has many
Plant the technology of the microencapsulation of performance, it provide the physical barriers between a core and other components.Pesticide micro capsule system
Agent, it is simply that utilize microcapsule technology to pass through chemical method, Physical or physical-chemical process, solid or the former medicine of liquid etc. are coated on tool
There is the sightless tiny capsules of naked eyes formed in semi permeability cyst material.Compared with conventional pesticide dosage form, microcapsule formulation is (micro-
Capsule suspension, microcapsule granule) there is the prolongation lasting period, improve pesticide efficacy, avoid the decomposition of pesticide to run off, subtract
Light toxicity and the feature such as poisoning, reduction environmental pollution.Within 1976, Pennwalt company interfacial polymerization prepares parathion-methyl
The patent of microcapsule goes through, and has started the beginning of pesticide micro capsule application.Hereafter all it is being devoted to pesticide micro capsule both at home and abroad
The exploitation of preparation and development, micro-capsule suspension is that in current pesticides new formulation, technology content is higher, have the one of a DEVELOPMENT PROSPECT very much
Planting novel form, Ye Shi China " 15 " pesticide industrial policy clearly encourages one of novel form of development.
Using water as disperse medium, it is to avoid the pressure that organic solvent and dust bring to environment, but low pole is the most non-
Polar solid pesticide is dispersed in highly polar water with 1-5 μm mean diameter to be needed to overcome the highest surface energy, constitutes heat
Mechanics and Mechanical instability system, during storage, the inherent physical stability of multiphase system is poor, easily causes the layering of product, sinks
Form sediment, affect the outward appearance of microcapsule product, thus affect the popularization and application of microcapsule.
Summary of the invention
For solving problems of the prior art, it is an object of the invention to provide a kind of for micro-capsule suspension
Auxiliary agent and preparation method thereof, the technical solution used in the present invention is:
The structural formula of the auxiliary agent of described micro-capsule suspension is formula A or Formula B, and described formula A is:
Described Formula B is:
Wherein R be H, one in humic acids, phosphate ester ammonium salt；M is H or SO3Na；EO is oxirane, and PO is expoxy propane；
X, y, z, w are the integer of 2-15；M is the integer of 16-30；N is the integer of 8-16；A is the integer of 5-20, and b is the whole of 10-30
Number, a/b=1-2.
Invention further provides the preparation method of the auxiliary agent formula A of micro-capsule suspension, described preparation method bag
Containing following steps:
(1) synthesis of allyl alcohol polyether: initiator 1-propenol-3 is added reactor, is simultaneously introduced catalyst potassium hydroxide (temperature
It is more difficult to react time low, and potassium hydroxide can be added some points more, and during temperature height, reaction is easier to, and potassium hydroxide can lack a little), open stirring,
It is warming up to 80～120 DEG C, and by evacuation or molecular sieve adsorbing and dewatering mode, goes moisture removal to be less than to the weight ratio of moisture
0.3%, then heat to 150～170 DEG C, add oxirane, be incubated ripening 25-40min at 135～165 DEG C after adding, so
Rear addition expoxy propane, its ethylene oxide, expoxy propane are 16～30:8～16 relative to the mol ratio of initiator 1-propenol-3:
1, it is incubated ripening 30-45min at 135～165 DEG C after having reacted, adds phosphorus acid for adjusting pH value after cooling to 80-95 DEG C to 6-
7, obtain allyl alcohol polyether.
(2) synthesis of esterified object of maleic anhydride: in dry reactor, is separately added into salicylic acid and maleic anhydride, drips
Entering catalyst concentrated sulphuric acid post-heating, temperature controls at 80-90 DEG C and is stirred continuously, and maintains reaction 0.5-1h, checks free bigcatkin willow
After acid is qualified, it is cooled to room temperature, is slowly added into water under agitation, ice bath stands cooling, when having mass crystallization to separate out,
Sucking filtration, obtain esterified object of maleic anhydride after drying;Described salicylic acid, maleic anhydride, concentrated sulphuric acid mol ratio are 1:1-3:0.1-
0.2, water and every other raw material weight are than for 3-6:1.
(3) in a kettle., by different to esterified object of maleic anhydride, toluene solvant and catalyst peroxidating formyl or azo two
Butyronitrile is thrown to reactor, when being heated with stirring to temperature 60-80 DEG C, is simultaneously added dropwise allyl alcohol polyether, acrylic acid, styrene, first
The solution of benzene mixing, described acrylic acid: styrene: esterified object of maleic anhydride: allyl alcohol polyether mol ratio=1:1:1-2:1-2,
Solvent toluene and every other raw material weight are than for 3:1;Control time for adding, at 1-2 hour, is warming up to 70-85 after dropping
DEG C insulation 1.5-4h, makes reaction carry out completely, removes toluene solvant, and regulating pH value with sodium hydroxide is about 7 to obtain formula A's
Product.
Invention further provides the preparation method of the auxiliary agent Formula B of micro-capsule suspension, described preparation method bag
Containing following steps:
(1) concentrated sulphuric acid is added in reactor, then be slowly added into salicylamide, after being heated with stirring to 60-70 DEG C, be continuously heating to
110 DEG C of insulation reaction 3-4 hour, filtration is drained, and obtains sulfosalisylic crude amide, is added by crude product in reactor, adds and steams
Distilled water, is heated with stirring to 70-80 DEG C, filters after it all dissolves, and filtrate is cooled to less than 25 DEG C, centrifugal, rejection filter, dried
Obtain sulfosalisylic amide highly finished product, be 6-7 by highly finished product sodium hydroxide regulation pH value, filter, i.e. obtain sodium sulfonate after drying
Salicylamide；Described salicylamide and the mass ratio of concentrated sulphuric acid are 1:3-4, distilled water and the matter of sulfosalisylic crude amide
Amount ratio is 3-4:1.
(2) sodium sulfonate salicylamide or salicylamide step (1) prepared mixes with potassium hydroxide, stirs, and rises
Temperature carries out evacuation process after 60-80 DEG C, is again warming up to 80-120 DEG C, adds oxirane, described oxirane and 6-
The mol ratio of heptyne alcohol is (10-15): 1, after insulation 30min, adds expoxy propane, and described expoxy propane rubs with 6-heptyne alcohol
Your ratio is (15-20): 1, is incubated 30min, cooling, and then regulation pH value is 6-7, prepares sodium sulfonate salicylamide polyethers or bigcatkin willow
Amide polyethers；
(3) humic acid and p-methyl benzenesulfonic acid are added in the sodium sulfonate salicylamide polyethers that step (2) prepares, described humic acid with
The mol ratio of sodium sulfonate salicylamide polyethers is 1:(3-6), it is passed through nitrogen, regulation temperature is 120-135 DEG C, reacts 60-
90min, prepares product--the sodium sulfonate salicylamide polyether ester compound of Formula B；Or by sodium sulfonate salicyloyl prepared for step (2)
Amine polyethers adds reactor, and under high-speed stirred, room temperature (charging process temperature is less than 40 DEG C) is slowly added to five oxidations two in batches
Phosphorus, sodium sulfonate salicylamide polyethers and phosphorus pentoxide mol ratio are 2.6-3.2:1, and feed time is 1-2h, afterwards, more slowly
It is warmed up to 70-80 DEG C, insulation successive reaction 4-5h, after adding 4-5% water hydrolysis 2h, cool to 50-60 DEG C, use ethanolamine
Neutralization pH value, to 6-7, obtains the product of Formula B--sodium sulfonate salicylamide polyether phosphate ammonium salt.
Having the beneficial effects that of the auxiliary agent of the micro-capsule suspension of the present invention:
(1) formula A is the high molecular polymer of pectinate texture, and molecular skeleton is made up of main chain and many side chains, and main chain introduces benzene
Ring, is coated with closely former medicine granule, plays good anchorage effect, difficult drop-off；Side chain introduce fatty alcohol ether,
Grain surface forms huge three-dimensional adsorption structure, produces sterically hindered effect；
(2) formula A is polyelectrolyte, and there is dissociable hydrophobic and hydrophilic group its linear carbon chain both sides, can be at profit
Align on interface, and adsorb on the surface of capsule-core material so that it is surface, with certain electric charge, forms stronger bearing
Electric field, produces enrichment to material with positive charge in solution, makes what they oriented to gather to oil droplet surface, and absorption is at capsule
Around core, the beneficially formation of microcapsule.
(3) Formula B introduces humic acids is larger molecular organics so that the polymer in system is enriched to condensed phase state
Core surfaces, forms smooth liquid film, obtains smooth microcapsule after solidification.
The auxiliary agent of micro-capsule suspension of the present invention can not only prepare particle diameter little and be evenly distributed, encystation form
The microcapsule good, envelop rate is high, and can effectively solve the problem of the layering of micro-capsule suspension, precipitation, can be applicable to
In the micro-capsule suspension of in-situ polymerization and interfacial polymerization.
Detailed description of the invention
Further illustrate the present invention by the following examples, but be not limited to the scope of the present invention.
Embodiment one
The preparation method of the auxiliary agent formula A of micro-capsule suspension, described preparation method comprises the steps of
1, initiator 1mol 1-propenol-3 is added reactor, be simultaneously introduced 1.2g potassium hydroxide catalyst, open stirring, be warming up to
100-120 DEG C, being slowly dividedly in some parts 30mol oxirane, after adding, 140 ± 5 DEG C of insulation ripening 25min, are then dividedly in some parts
8mol expoxy propane, 140 ± 5 DEG C of insulation ripening 45min after having reacted, with phosphoric acid regulating ph value to 6-7 after being cooled to 85 DEG C,
Obtain allyl alcohol polyether.
2, in dry reactor, it is separately added into 1mol salicylic acid and 2mol maleic anhydride, instills catalyst 0.2mol
Concentrated sulphuric acid post-heating, temperature controls at 80-90 DEG C and is stirred continuously, and maintains reaction 0.5-1h, after checking that free salicylic acid is qualified,
Being cooled to room temperature, be slowly added into water under agitation, water is 5:1 with the weight ratio of every other raw material, stands on ice bath
Cooling, when having mass crystallization to separate out, sucking filtration, obtains esterified object of maleic anhydride after drying.
3, by 2mol step 1 product esterified object of maleic anhydride, part toluene, 6.25 grams of catalyst benzoyl peroxides
(BPO) first throw to reactor, when being heated with stirring to temperature 80 DEG C, be simultaneously added dropwise 2mol step 1 product allyl alcohol polyether, 1mol
Acrylic acid and 1mol styrene and part toluene mixture liquid, solvent toluene and every other raw material weight ratio for 3:1, controls dropping
Time, at 1-2 hour, is warming up to 75 DEG C of insulation about 3h, makes reaction carry out completely after dropping, reaction uses hydrogen-oxygen after terminating
Changing sodium regulation pH value is about 7, i.e. obtains the product of formula A--polycarboxylate-01.
The preparation method of the auxiliary agent Formula B of micro-capsule suspension, described preparation method comprises the steps of
1, being added in reactor by concentrated sulphuric acid, then be slowly added into salicylamide, the mass ratio of salicylamide and concentrated sulphuric acid is 1:3,
After being heated with stirring to 60-70 DEG C, being continuously heating to 110 DEG C of insulation reaction 3-4 hour, filtration is drained, and obtains crude product, is added by crude product
Entering in reactor, add distilled water, the mass ratio of distilled water and sulfosalisylic crude amide is 3:1, is heated with stirring to 70-80
DEG C, to filter after it all dissolves, filtrate is cooled to less than 25 DEG C, centrifugal, rejection filter, i.e. obtains highly finished product, by highly finished product after drying
It is 6-7 with sodium hydroxide regulation pH value, filters, i.e. obtain sodium sulfonate salicylamide after drying；
2,1mol step 1 product sodium sulfonate salicylamide is added reactor, be simultaneously introduced the potassium hydroxide that weight ratio is 3 ‰ and make
For catalyst, stirring, it is warming up to 60-80 DEG C of evacuation, to remove moisture removal, then heats to 80-100 DEG C, be slowly dividedly in some parts
10mol oxirane, is incubated ripening 30min, is then dividedly in some parts 20mol expoxy propane, is incubated ripe after having reacted after adding
Change 30min, regulate pH value 6-7 after cooling, prepare sodium sulfonate salicylamide polyethers；
3, step 2 product sodium sulfonate salicylamide polyethers being added reactor, under high-speed stirred, (charging process temperature does not surpasses room temperature
Cross 40 DEG C) it is slowly added to phosphorus pentoxide in batches, sodium sulfonate salicylamide polyethers and phosphorus pentoxide mol ratio are 3:1, charging
Time is 1.5-2h, afterwards, is more slowly warmed up to 80 DEG C, insulation successive reaction 4h, after adding 4% water hydrolysis 2h, cools to
50-60 DEG C, with in ethanolamine and pH value to 6-7, obtain the product of Formula B--polyethers-01.
Embodiment 2
The preparation method of the auxiliary agent formula A of micro-capsule suspension, described preparation method comprises the steps of
1, initiator 1mol 1-propenol-3 is added reactor, be simultaneously introduced 1.2g potassium hydroxide catalyst, open stirring, be warming up to
100-120 DEG C, being slowly dividedly in some parts 18mol oxirane, after adding, 140 ± 5 DEG C of insulation ripening 25min, are then dividedly in some parts
18mol expoxy propane, 140 ± 5 DEG C of insulation ripening 45min after having reacted, with phosphoric acid regulating ph value to 6-after being cooled to 85 DEG C
7, obtain allyl alcohol polyether.
2, in dry reactor, it is separately added into 1mol salicylic acid and 2mol maleic anhydride, instills catalyst 0.2mol
Concentrated sulphuric acid post-heating, temperature controls at 80-90 DEG C and is stirred continuously, and maintains reaction 0.5-1h, after checking that free salicylic acid is qualified,
Being cooled to room temperature, be slowly added into water under agitation, water is 5:1 with the weight ratio of every other raw material, stands on ice bath
Cooling, when having mass crystallization to separate out, sucking filtration, obtains esterified object of maleic anhydride after drying.
3, by 2mol step 1 product esterified object of maleic anhydride, part toluene, 6.25 grams of catalyst benzoyl peroxides
(BPO) first throw to reactor, when being heated with stirring to temperature 80 DEG C, be simultaneously added dropwise 2mol step 1 product allyl alcohol polyether, 1mol
Acrylic acid and 1mol styrene and part toluene mixture liquid, solvent toluene and every other raw material weight ratio for 3:1, controls dropping
Time, at 1-2 hour, is warming up to 75 DEG C of insulation about 3h, makes reaction carry out completely after dropping, reaction uses hydrogen-oxygen after terminating
Changing sodium regulation pH value is about 7, i.e. obtains the product of formula A--polycarboxylate-02
The preparation method of the auxiliary agent Formula B of micro-capsule suspension, described preparation method comprises the steps of
1, being added in reactor by concentrated sulphuric acid, then be slowly added into salicylamide, the mass ratio of salicylamide and concentrated sulphuric acid is 1:3,
After being heated with stirring to 60-70 DEG C, being continuously heating to 110 DEG C of insulation reaction 3-4 hour, filtration is drained, and obtains crude product, is added by crude product
Entering in reactor, add distilled water, the mass ratio of distilled water and sulfosalisylic crude amide is 3:1, is heated with stirring to 70-80
DEG C, to filter after it all dissolves, filtrate is cooled to less than 25 DEG C, centrifugal, rejection filter, i.e. obtains highly finished product, by highly finished product after drying
It is 6-7 with sodium hydroxide regulation pH value, filters, i.e. obtain sodium sulfonate salicylamide after drying；
2,1mol step 1 product sodium sulfonate salicylamide is added reactor, be simultaneously introduced the potassium hydroxide that weight ratio is 3 ‰ and make
For catalyst, stirring, it is warming up to 60-80 DEG C of evacuation, to remove moisture removal, then heats to 80-100 DEG C, be slowly dividedly in some parts
10mol oxirane, is incubated ripening 30min, is then dividedly in some parts 20mol expoxy propane, is incubated ripe after having reacted after adding
Change 30min, regulate pH value 6-7 after cooling, prepare sodium sulfonate salicylamide polyethers；
3, by the step 2 product sodium sulfonate salicylamide polyethers that obtains and humic acids during 6:1 is dosed to reactor in molar ratio,
Weight ratio be the p-methyl benzenesulfonic acid of 3 ‰ as catalyst in the case of, by solvent toluene circumfluence method, be passed through nitrogen and protect
Protecting, esterification temperature controls at 120-135 DEG C, and preferred temperature is 125-130 DEG C, i.e. obtains the product of Formula B--polyethers-02；
Described solvent toluene circumfluence method is: use sleeve, and described sleeve pipe is outer equipped with condensed water, and described sleeve pipe is built with the first evaporated
Benzene, by the method for condensed water condensing reflux toluene.
Embodiment 3
The preparation method of the auxiliary agent Formula B of micro-capsule suspension, described preparation method comprises the steps of
1, being added in reactor by concentrated sulphuric acid, then be slowly added into salicylamide, the mass ratio of salicylamide and concentrated sulphuric acid is 1:3,
After being heated with stirring to 60-70 DEG C, being continuously heating to 110 DEG C of insulation reaction 3-4 hour, filtration is drained, and obtains crude product, is added by crude product
Entering in reactor, add distilled water, the mass ratio of distilled water and sulfosalisylic crude amide is 3:1, is heated with stirring to 70-80
DEG C, to filter after it all dissolves, filtrate is cooled to less than 25 DEG C, centrifugal, rejection filter, i.e. obtains highly finished product, by highly finished product after drying
It is 6-7 with sodium hydroxide regulation pH value, filters, i.e. obtain sodium sulfonate salicylamide after drying；
2,1mol step 1 product sodium sulfonate salicylamide is added reactor, be simultaneously introduced the potassium hydroxide that weight ratio is 3 ‰ and make
For catalyst, stirring, it is warming up to 60-80 DEG C of evacuation, to remove moisture removal, then heats to 80-100 DEG C, be slowly dividedly in some parts
15mol oxirane, is incubated ripening 30min, is then dividedly in some parts 15mol expoxy propane, is incubated ripe after having reacted after adding
Change 30min, regulate pH value 6-7 after cooling, prepare sodium sulfonate salicylamide polyethers；
3, by the step 2 product sodium sulfonate salicylamide polyethers that obtains and humic acids during 3:1 is dosed to reactor in molar ratio,
Weight ratio be the p-methyl benzenesulfonic acid of 3 ‰ as catalyst in the case of, by solvent toluene circumfluence method, be passed through nitrogen and protect
Protecting, esterification temperature controls at 120-135 DEG C, and preferred temperature is 125-130 DEG C, i.e. obtains the product of Formula B--polyethers-03；
Described solvent toluene circumfluence method is: use sleeve, and described sleeve pipe is outer equipped with condensed water, and described sleeve pipe is built with the first evaporated
Benzene, by the method for condensed water condensing reflux toluene.--i.e. obtaining the product of Formula B--polyethers-03
The application of the micro-capsule suspension auxiliary agent that embodiment one, embodiment two, embodiment three are prepared:
1, the preparation of 30% chlorpyrifos microcapsule suspension agent it is applied to
Equipped with thermometer, agitating device there-necked flask in add carbamide and formaldehyde, mol ratio is 1: 2.0, adds 2 after dissolving
Times formaldehyde and the deionized water of weight of urea, with sodium hydroxide regulation pH value to 8, be warming up to 70 DEG C, and it is little that stirring at low speed reacts 1
Time, i.e. obtain Lauxite prepolymer aqueous solution.
Under room temperature, the 30.92g 97% former medicine of chlopyrifos is dissolved in 10.0g dimethylbenzene, is stirring evenly and then adding on 20g
State Lauxite prepolymer aqueous solution, and add the product of 2g formula A--polycarboxylate-01,1500 revs/min of stirrings are formed stable
O/W emulsion；Reduce rotating speed to 800 revs/min, in batches in 60 minutes add dilute hydrochloric acid regulation system pH to 2.0, polycondensation reaction
1.5 hour；Thereafter it is warming up to 45 DEG C of solidification cyst walls and after 1.5 hours, adds sodium hydroxide regulation pH to 6-7, add 5g Formula B
Product--polyethers-01, adds 2% xanthan gum solution 5g and 3 grams of ethylene glycol, with water, system gross weight is reached 100g, stir
Mix and uniformly i.e. obtain 30% micro-capsule water suspending agent for killing tick.
Table 1 30% chlorpyrifos microcapsule suspension agent index
| Chlopyrifos mass percent | 30% |
| Outward appearance | White liquid |
| PH value | 5-7 |
| Mean diameter, D50 | Less than 5 μm |
| Envelop rate | More than 90% |
| Suspensibility (200 times) stability | More than 90% |
| Low-temperature stability | Qualified |
| Heat storage stability (54 ± 2 DEG C, 14d) resolution ratio | Less than 2% |
| Often store stability (2 years) | Qualified |
2, the preparation of 2.5% gamma cyhalothrin micro-capsule suspension it is applied to
Equipped with thermometer, agitating device there-necked flask in add carbamide and formaldehyde, mol ratio is 1: 1.75, adds after dissolving
2 times of formaldehyde and the deionized water of weight of urea, with sodium hydroxide regulation pH value to 8, be warming up to 70 DEG C, stirring at low speed reaction 1
Hour, i.e. obtain Lauxite prepolymer aqueous solution.
Under room temperature, the 2.6g 97% former medicine of gamma cyhalothrin is dissolved in 4.0g dimethylbenzene, is stirring evenly and then adding into
5g above-mentioned Lauxite prepolymer aqueous solution, and add the product of 2g formula A--polycarboxylate-02,1500 revs/min of stirrings are formed
Stable O/W emulsion；Reduce rotating speed to 800 revs/min, in batches in 60 minutes add dilute hydrochloric acid regulation system pH to 2.0, polycondensation
React 1.5 hours；Thereafter it is warming up to 45 DEG C of solidification cyst walls and after 1.5 hours, adds sodium hydroxide regulation pH to 6-7, add 4g formula
The product of B--polyethers-02, adds 2% xanthan gum solution 10g and 3 grams of ethylene glycol, system gross weight is reached with water
100g, stirs and i.e. obtains 2.5% gamma cyhalothrin microcapsules SC.
Table 2 2.5% gamma cyhalothrin micro-capsule suspension index
| Gamma cyhalothrin mass percent | 2.5% |
| Outward appearance | White liquid |
| PH value | 5-7 |
| Mean diameter, D50 | Less than 5 μm |
| Envelop rate | More than 90% |
| Suspensibility (200 times) stability | More than 90% |
| Low-temperature stability | Qualified |
| Heat storage stability (54 ± 2 DEG C, 14d) resolution ratio | Less than 2% |
| Often store stability (2 years) | Qualified |
3, the preparation of 2% avermectin microcapsule suspending agent it is applied to
The 95% former medicine of avilamycin of 2.1g is dissolved in 6g Ketohexamethylene and 5g dimethylbenzene, is subsequently adding the toluene diisocyanate of 2g
Acid esters TDI, 0.5g stabilizer BHT stirs (oil phase)；Product by the formula A of 3.0g--polycarboxylate-02 adds 61.2g
Deionized water in stir evenly (aqueous phase)；The oil phase configured to entering aqueous phase and opening high speed homogenizing, form stable O/W breast
Liquid, records D50 less than 5 μm；Open stirring (maintaining 600 turns/min), then the emulsion that homogenizing is good is warming up to 50 DEG C, delays simultaneously
The slow hexamethylene diamine adding 0.1g, maintains stable cyst material solidification temperature 6 hours, the rear product adding 5.0g Formula B--and poly-
Ether-03, ethylene glycol 5.0g, 2% xanthan gum solution 10g, 0.1g triethanolamine adjust pH value to about 7, i.e. prepare the A Wei of 2%
Rhzomorph microcapsule suspending agent.
Table 3 2% avermectin microcapsule suspending agent index
| Avilamycin mass percent | 2% |
| Outward appearance | White liquid |
| PH value | 5-7 |
| Mean diameter, D50 | Less than 5 μm |
| Envelop rate | More than 90% |
| Suspensibility (200 times) stability | More than 90% |
| Low-temperature stability | Qualified |
| Heat storage stability (54 ± 2 DEG C, 14d) resolution ratio | Less than 2% |
| Often store stability (2 years) | Qualified |
Claims (8)
1. the auxiliary agent for micro-capsule suspension, it is characterised in that, the structural formula of the auxiliary agent of described micro-capsule suspension
For formula A or Formula B,
Described formula A is:
;
Described Formula B is:
;
Wherein R be H, one in humic acids, phosphate ester ammonium salt；M is H or SO3Na；EO is oxirane, and PO is expoxy propane；
X, y, z, w are the integer of 2-15；M is the integer of 16-30；N is the integer of 8-16；A is the integer of 5-20, and b is the whole of 10-30
Number, a/b=1-2.
The auxiliary agent of micro-capsule suspension the most according to claim 1, it is characterised in that, described micro-capsule suspension
The structural formula of auxiliary agent is that the preparation method of formula A comprises the steps of
(1) synthesis of allyl alcohol polyether: initiator 1-propenol-3 is added reactor, is simultaneously introduced catalyst potassium hydroxide, opens and stir
Mix, be warming up to 80～120 DEG C, and by evacuation or molecular sieve adsorbing and dewatering mode, go moisture removal little to the weight ratio of moisture
In 0.3%, then heat to 150～170 DEG C, add oxirane, after adding, be incubated ripening 25-40min at 135～165 DEG C,
Be subsequently adding expoxy propane, its ethylene oxide, expoxy propane relative to the mol ratio of initiator 1-propenol-3 be 16～30:8～
16:1, is incubated ripening 30-45min at 135～165 DEG C after having reacted, and adds phosphorus acid for adjusting pH value extremely after cooling to 80-95 DEG C
6-7, obtains allyl alcohol polyether;
(2) synthesis of esterified object of maleic anhydride: in dry reactor, is separately added into salicylic acid and maleic anhydride, and instillation is urged
Agent concentrated sulphuric acid post-heating, temperature controls at 80-90 DEG C and is stirred continuously, and maintains reaction 0.5-1h, checks that free salicylic acid closes
After lattice, it is cooled to room temperature, is slowly added into water under agitation, ice bath stands cooling, when having mass crystallization to separate out, takes out
Filter, obtain esterified object of maleic anhydride after drying;Described salicylic acid, maleic anhydride, concentrated sulphuric acid mol ratio are 1:1-3:0.1-
0.2, water and every other raw material weight are than for 3-6:1;
(3) in a kettle., by esterified object of maleic anhydride, toluene solvant and catalyst peroxidating formyl or azodiisobutyronitrile
Throw in reactor, when being heated with stirring to temperature 60-80 DEG C, be simultaneously added dropwise allyl alcohol polyether, acrylic acid, styrene, toluene mix
The solution closed, described acrylic acid: styrene: esterified object of maleic anhydride: allyl alcohol polyether mol ratio=1:1:1-2:1-2, solvent
Toluene and every other raw material weight are than for 3:1;Control time for adding, at 1-2 hour, is warming up to 70-85 DEG C of guarantor after dropping
Temperature 1.5-4h, makes reaction carry out completely, removes toluene solvant, is about 7 products obtaining formula A with sodium hydroxide regulation pH value
Product;
The structural formula of the auxiliary agent of described micro-capsule suspension is the preparation method of Formula B, comprises the steps of
(1) concentrated sulphuric acid is added in reactor, then be slowly added into salicylamide, after being heated with stirring to 60-70 DEG C, be continuously heating to
110 DEG C of insulation reaction 3-4 hour, filtration is drained, and obtains sulfosalisylic crude amide, is added by crude product in reactor, adds and steams
Distilled water, is heated with stirring to 70-80 DEG C, filters after it all dissolves, and filtrate is cooled to less than 25 DEG C, centrifugal, rejection filter, dried
Obtain sulfosalisylic amide highly finished product, be 6-7 by highly finished product sodium hydroxide regulation pH value, filter, i.e. obtain sodium sulfonate after drying
Salicylamide；Described salicylamide and the mass ratio of concentrated sulphuric acid are 1:3-4, distilled water and the quality of sulfosalisylic crude amide
Ratio is 3-4:1;
(2) sodium sulfonate salicylamide or salicylamide step (1) prepared mixes with potassium hydroxide, stirs, is warming up to
Carry out evacuation process after 60-80 DEG C, be again warming up to 80-120 DEG C, add oxirane, described oxirane and 6-heptyne
The mol ratio of alcohol is 10-15:1, after insulation 30min, adds expoxy propane, and described expoxy propane with the mol ratio of 6-heptyne alcohol is
15-20:1, is incubated 30min, cooling, and then regulation pH value is 6-7, prepares sodium sulfonate salicylamide polyethers or salicylamide gathers
Ether；
(3) humic acid and p-methyl benzenesulfonic acid are added in the sodium sulfonate salicylamide polyethers that step (2) prepares, described humic acid with
The mol ratio of sodium sulfonate salicylamide polyethers is 1:3-6, is passed through nitrogen, and regulation temperature is 120-135 DEG C, reacts 60-90min,
Prepare product--the sodium sulfonate salicylamide polyether ester compound of Formula B；Or by sodium sulfonate salicylamide polyethers prepared for step (2)
Adding reactor, under high-speed stirred, room temperature (charging process temperature is less than 40 DEG C) is slowly added to phosphorus pentoxide, sulfonic acid in batches
Sodium salicylamide polyethers and phosphorus pentoxide mol ratio are 2.6-3.2:1, and feed time is 1-2h, afterwards, is more slowly warmed up to
70-80 DEG C, insulation successive reaction 4-5h, after adding 4-5% water hydrolysis 2h, cool to 50-60 DEG C, with in ethanolamine and pH
Value, to 6-7, obtains the product of Formula B--sodium sulfonate salicylamide polyether phosphate ammonium salt.
The auxiliary agent of micro-capsule suspension the most according to claim 1, it is characterised in that, described micro-capsule suspension
The structural formula of auxiliary agent is that the preparation method of formula A comprises the steps of
(1), initiator 1mol 1-propenol-3 is added reactor, be simultaneously introduced 1.2g potassium hydroxide catalyst, open stirring, be warming up to
100-120 DEG C, being slowly dividedly in some parts 30mol oxirane, after adding, 140 ± 5 DEG C of insulation ripening 25min, are then dividedly in some parts
8mol expoxy propane, 140 ± 5 DEG C of insulation ripening 45min after having reacted, with phosphoric acid regulating ph value to 6-7 after being cooled to 85 DEG C,
Obtain allyl alcohol polyether;
(2), in dry reactor, it is separately added into 1mol salicylic acid and 2mol maleic anhydride, instills catalyst 0.2mol dense
Sulphuric acid post-heating, temperature controls at 80-90 DEG C and is stirred continuously, and maintains reaction 0.5-1h, after checking that free salicylic acid is qualified, cold
But to room temperature, being slowly added into water under agitation, water is 5:1 with the weight ratio of every other raw material, stands cold on ice bath
But, when having mass crystallization to separate out, sucking filtration, esterified object of maleic anhydride is obtained after drying;
(3), by 2mol step 1 product esterified object of maleic anhydride, part toluene, 6.25 grams of catalyst benzoyl peroxides (BPO)
First throw to reactor, when being heated with stirring to temperature 80 DEG C, be simultaneously added dropwise 2mol step 1 product allyl alcohol polyether, 1mol propylene
Acid and 1mol styrene and part toluene mixture liquid, solvent toluene and every other raw material weight ratio for 3:1, controls time for adding
At 1-2 hour, being warming up to 75 DEG C of insulation about 3h, make reaction carry out completely after dropping, reaction uses sodium hydroxide after terminating
Regulation pH value is about 7, i.e. obtains the product of formula A--polycarboxylate-01;
The structural formula of the auxiliary agent of described micro-capsule suspension is the preparation method of Formula B, comprises the steps of
(1), being added in reactor by concentrated sulphuric acid, then be slowly added into salicylamide, the mass ratio of salicylamide and concentrated sulphuric acid is 1:
3, after being heated with stirring to 60-70 DEG C, it is continuously heating to 110 DEG C of insulation reaction 3-4 hour, filtration is drained, and obtains crude product, by crude product
Adding in reactor, add distilled water, the mass ratio of distilled water and sulfosalisylic crude amide is 3:1, is heated with stirring to 70-80
DEG C, to filter after it all dissolves, filtrate is cooled to less than 25 DEG C, centrifugal, rejection filter, i.e. obtains highly finished product, by highly finished product after drying
It is 6-7 with sodium hydroxide regulation pH value, filters, i.e. obtain sodium sulfonate salicylamide after drying；
(2), 1mol step 1 product sodium sulfonate salicylamide is added reactor, be simultaneously introduced the potassium hydroxide that weight ratio is 3 ‰
As catalyst, stirring, it is warming up to 60-80 DEG C of evacuation, to remove moisture removal, then heats to 80-100 DEG C, add the most in batches
Enter 10mol oxirane, be incubated ripening 30min after adding, be then dividedly in some parts 20mol expoxy propane, be incubated after having reacted
Ripening 30min, regulates pH value 6-7, prepares sodium sulfonate salicylamide polyethers after cooling；
(3), step 2 product sodium sulfonate salicylamide polyethers being added reactor, under high-speed stirred, room temperature is slowly added to five in batches
Aoxidizing two phosphorus, sodium sulfonate salicylamide polyethers and phosphorus pentoxide mol ratio are 3:1, and feed time is 1.5-2h, afterwards, then delays
Slowly 80 DEG C it are warmed up to, insulation successive reaction 4h, after adding 4% water hydrolysis 2h, cool to 50-60 DEG C, with in ethanolamine and pH
Value, to 6-7, obtains the product of Formula B--polyethers-01.
The auxiliary agent of micro-capsule suspension the most according to claim 1, it is characterised in that, described micro-capsule suspension
The structural formula of auxiliary agent is that the preparation method of formula A comprises the steps of
(1), initiator 1mol 1-propenol-3 is added reactor, be simultaneously introduced 1.2g potassium hydroxide catalyst, open stirring, be warming up to
100-120 DEG C, being slowly dividedly in some parts 18mol oxirane, after adding, 140 ± 5 DEG C of insulation ripening 25min, are then dividedly in some parts
18mol expoxy propane, 140 ± 5 DEG C of insulation ripening 45min after having reacted, with phosphoric acid regulating ph value to 6-after being cooled to 85 DEG C
7, obtain allyl alcohol polyether;
(2), in dry reactor, it is separately added into 1mol salicylic acid and 2mol maleic anhydride, instills catalyst 0.2mol dense
Sulphuric acid post-heating, temperature controls at 80-90 DEG C and is stirred continuously, and maintains reaction 0.5-1h, after checking that free salicylic acid is qualified, cold
But to room temperature, being slowly added into water under agitation, water is 5:1 with the weight ratio of every other raw material, stands cold on ice bath
But, when having mass crystallization to separate out, sucking filtration, esterified object of maleic anhydride is obtained after drying;
(3), by 2mol step 1 product esterified object of maleic anhydride, part toluene, 6.25 grams of catalyst benzoyl peroxides (BPO)
First throw to reactor, when being heated with stirring to temperature 80 DEG C, be simultaneously added dropwise 2mol step 1 product allyl alcohol polyether, 1mol propylene
Acid and 1mol styrene and part toluene mixture liquid, solvent toluene and every other raw material weight ratio for 3:1, controls time for adding
At 1-2 hour, being warming up to 75 DEG C of insulation about 3h, make reaction carry out completely after dropping, reaction uses sodium hydroxide after terminating
Regulation pH value is about 7, i.e. obtains the product of formula A--polycarboxylate-02;
The structural formula of the auxiliary agent of described micro-capsule suspension is the preparation method of Formula B, comprises the steps of
(1), being added in reactor by concentrated sulphuric acid, then be slowly added into salicylamide, the mass ratio of salicylamide and concentrated sulphuric acid is 1:
3, after being heated with stirring to 60-70 DEG C, it is continuously heating to 110 DEG C of insulation reaction 3-4 hour, filtration is drained, and obtains crude product, by crude product
Adding in reactor, add distilled water, the mass ratio of distilled water and sulfosalisylic crude amide is 3:1, is heated with stirring to 70-80
DEG C, to filter after it all dissolves, filtrate is cooled to less than 25 DEG C, centrifugal, rejection filter, i.e. obtains highly finished product, by highly finished product after drying
It is 6-7 with sodium hydroxide regulation pH value, filters, i.e. obtain sodium sulfonate salicylamide after drying；
(2), 1mol step 1 product sodium sulfonate salicylamide is added reactor, be simultaneously introduced the potassium hydroxide that weight ratio is 3 ‰
As catalyst, stirring, it is warming up to 60-80 DEG C of evacuation, to remove moisture removal, then heats to 80-100 DEG C, add the most in batches
Enter 10mol oxirane, be incubated ripening 30min after adding, be then dividedly in some parts 20mol expoxy propane, be incubated after having reacted
Ripening 30min, regulates pH value 6-7, prepares sodium sulfonate salicylamide polyethers after cooling；
(3), by the step 2 product sodium sulfonate salicylamide polyethers that obtains and humic acids during 6:1 is dosed to reactor in molar ratio,
In the case of the p-methyl benzenesulfonic acid that weight ratio is 3 ‰ is as catalyst, by solvent toluene circumfluence method, it is passed through nitrogen and protects
Protecting, esterification temperature controls at 120-135 DEG C, and preferred temperature is 125-130 DEG C, i.e. obtains the product of Formula B--polyethers-02；
Described solvent toluene circumfluence method is: use sleeve, and described sleeve pipe is outer equipped with condensed water, and described sleeve pipe is built with the first evaporated
Benzene, by the method for condensed water condensing reflux toluene.
The auxiliary agent of micro-capsule suspension the most according to claim 1, it is characterised in that, described micro-capsule suspension
The structural formula of auxiliary agent is the preparation method of Formula B, comprises the steps of
(1), being added in reactor by concentrated sulphuric acid, then be slowly added into salicylamide, the mass ratio of salicylamide and concentrated sulphuric acid is 1:
3, after being heated with stirring to 60-70 DEG C, it is continuously heating to 110 DEG C of insulation reaction 3-4 hour, filtration is drained, and obtains crude product, by crude product
Adding in reactor, add distilled water, the mass ratio of distilled water and sulfosalisylic crude amide is 3:1, is heated with stirring to 70-80
DEG C, to filter after it all dissolves, filtrate is cooled to less than 25 DEG C, centrifugal, rejection filter, i.e. obtains highly finished product, by highly finished product after drying
It is 6-7 with sodium hydroxide regulation pH value, filters, i.e. obtain sodium sulfonate salicylamide after drying；
(2), 1mol step 1 product sodium sulfonate salicylamide is added reactor, be simultaneously introduced the potassium hydroxide that weight ratio is 3 ‰
As catalyst, stirring, it is warming up to 60-80 DEG C of evacuation, to remove moisture removal, then heats to 80-100 DEG C, add the most in batches
Enter 15mol oxirane, be incubated ripening 30min after adding, be then dividedly in some parts 15mol expoxy propane, be incubated after having reacted
Ripening 30min, regulates pH value 6-7, prepares sodium sulfonate salicylamide polyethers after cooling；
(3), by the step 2 product sodium sulfonate salicylamide polyethers that obtains and humic acids during 3:1 is dosed to reactor in molar ratio,
In the case of the p-methyl benzenesulfonic acid that weight ratio is 3 ‰ is as catalyst, by solvent toluene circumfluence method, it is passed through nitrogen and protects
Protecting, esterification temperature controls at 120-135 DEG C, and preferred temperature is 125-130 DEG C, i.e. obtains the product of Formula B--polyethers-03；
Described solvent toluene circumfluence method is: use sleeve, and described sleeve pipe is outer equipped with condensed water, and described sleeve pipe is built with the first evaporated
Benzene, the polyethers-03 that--i.e. obtains the product of Formula B--by the method for condensed water condensing reflux toluene.
6. according to the application of the auxiliary agent of the micro-capsule suspension described in Claims 2 or 3 or 4 or 5, it is characterised in that, described
The preparation being applied to 30% chlorpyrifos microcapsule suspension agent of the micro-capsule suspension auxiliary agent prepared, comprises the steps:
A). equipped with thermometer, agitating device there-necked flask in add carbamide and formaldehyde, mol ratio is 1: 2.0, adds after dissolving
Entering 2 times of formaldehyde and the deionized water of weight of urea, with sodium hydroxide regulation pH value to 8, be warming up to 70 DEG C, stirring at low speed is reacted
1 hour, i.e. obtain Lauxite prepolymer aqueous solution;
B). under room temperature, the 30.92g 97% former medicine of chlopyrifos is dissolved in 10.0g dimethylbenzene, is stirring evenly and then adding into 20g above-mentioned
Lauxite prepolymer aqueous solution, and add the product of 2g formula A--polycarboxylate-01,1500 revs/min of stirrings are formed stable
O/W emulsion；Reduce rotating speed to 800 revs/min, in batches in 60 minutes add dilute hydrochloric acid regulation system pH to 2.0, polycondensation reaction
1.5 hour；Thereafter it is warming up to 45 DEG C of solidification cyst walls and after 1.5 hours, adds sodium hydroxide regulation pH to 6-7, add 5g Formula B
Product--polyethers-01, adds 2% xanthan gum solution 5g and 3 grams of ethylene glycol, with water, system gross weight is reached 100g, stir
Mix and uniformly i.e. obtain 30% micro-capsule water suspending agent for killing tick.
7. according to the application of the auxiliary agent of the micro-capsule suspension described in Claims 2 or 3 or 4 or 5, it is characterised in that, described
The preparation being applied to 2.5% gamma cyhalothrin micro-capsule suspension of the micro-capsule suspension auxiliary agent prepared, including as follows
Step:
A). equipped with thermometer, agitating device there-necked flask in add carbamide and formaldehyde, mol ratio is 1: 1.75, after dissolving
Adding 2 times of formaldehyde and the deionized water of weight of urea, with sodium hydroxide regulation pH value to 8, be warming up to 70 DEG C, stirring at low speed is anti-
Answer 1 hour, i.e. obtain Lauxite prepolymer aqueous solution;
B). under room temperature, the 2.6g 97% former medicine of gamma cyhalothrin is dissolved in 4.0g dimethylbenzene, is stirring evenly and then adding into 5g
Above-mentioned Lauxite prepolymer aqueous solution, and add the product of 2g formula A--polycarboxylate-02,1500 revs/min of stirrings are formed steady
Fixed O/W emulsion；Reduction rotating speed is to 800 revs/min, and in 60 minutes, addition dilute hydrochloric acid regulation system pH is to 2.0 in batches, and polycondensation is anti-
Answer 1.5 hours；Thereafter it is warming up to 45 DEG C of solidification cyst walls and after 1.5 hours, adds sodium hydroxide regulation pH to 6-7, add 4g Formula B
Product--polyethers-02, add 2% xanthan gum solution 10g and 3 grams of ethylene glycol, with water, system gross weight reached 100g,
Stir and i.e. obtain 2.5% gamma cyhalothrin microcapsules SC.
8. according to the application of the auxiliary agent of the micro-capsule suspension described in Claims 2 or 3 or 4 or 5, it is characterised in that, described
The preparation being applied to 2% avermectin microcapsule suspending agent of the micro-capsule suspension auxiliary agent prepared, comprises the steps:
The 95% former medicine of avilamycin of 2.1g is dissolved in 6g Ketohexamethylene and 5g dimethylbenzene, is subsequently adding the toluene diisocyanate of 2g
Acid esters TDI, 0.5g stabilizer BHT stirs-oil phase；Product by the formula A of 3.0g--polycarboxylate-02 adds 61.2g
Deionized water in stir evenly-aqueous phase；The oil phase configured to entering aqueous phase and opening high speed homogenizing, form stable O/W emulsion,
Record D50 less than 5 μm；Open stirring, maintain 600 turns/min, then the emulsion that homogenizing is good is warming up to 50 DEG C, slowly add simultaneously
Enter the hexamethylene diamine of 0.1g, maintain stable cyst material solidification temperature 6 hours, the rear product adding 5.0g Formula B--polyethers-
03, ethylene glycol 5.0g, 2% xanthan gum solution 10g, 0.1g triethanolamine adjust pH value to about 7, i.e. prepare the Avermectin of 2%
Element microcapsule suspending agent.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110934143A (en) * | 2019-12-24 | 2020-03-31 | 六夫丁作物保护有限公司 | Sterilization composition containing difenoconazole and fluopicolide |
| CN115104603A (en) * | 2022-07-15 | 2022-09-27 | 威尔（福建）生物有限公司 | Oil suspending agent additive and preparation method thereof |
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| US20100075844A1 (en) * | 2006-12-18 | 2010-03-25 | Frank Loeker | Water-absorbing polymer structures produced using polymer dispersions |
| CN103819630A (en) * | 2014-03-05 | 2014-05-28 | 威尔（福建）生物有限公司 | Polyether modified organic silicon defoamer, and preparation method and application thereof |
| CN103977750A (en) * | 2014-03-13 | 2014-08-13 | 中国农科院植保所廊坊农药中试厂 | Preparation technology for pesticide microcapsule |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100075844A1 (en) * | 2006-12-18 | 2010-03-25 | Frank Loeker | Water-absorbing polymer structures produced using polymer dispersions |
| CN103819630A (en) * | 2014-03-05 | 2014-05-28 | 威尔（福建）生物有限公司 | Polyether modified organic silicon defoamer, and preparation method and application thereof |
| CN103977750A (en) * | 2014-03-13 | 2014-08-13 | 中国农科院植保所廊坊农药中试厂 | Preparation technology for pesticide microcapsule |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110934143A (en) * | 2019-12-24 | 2020-03-31 | 六夫丁作物保护有限公司 | Sterilization composition containing difenoconazole and fluopicolide |
| CN115104603A (en) * | 2022-07-15 | 2022-09-27 | 威尔（福建）生物有限公司 | Oil suspending agent additive and preparation method thereof |
| CN115104603B (en) * | 2022-07-15 | 2024-03-26 | 威尔（福建）生物有限公司 | Oil suspending agent auxiliary agent and preparation method thereof |
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