CN108200913A - A kind of emamectin benzoate microcapsule suspending agent and preparation method thereof - Google Patents

A kind of emamectin benzoate microcapsule suspending agent and preparation method thereof Download PDF

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Publication number
CN108200913A
CN108200913A CN201611188341.1A CN201611188341A CN108200913A CN 108200913 A CN108200913 A CN 108200913A CN 201611188341 A CN201611188341 A CN 201611188341A CN 108200913 A CN108200913 A CN 108200913A
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Prior art keywords
temperature
isocyanates
preparation
water
oil
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CN201611188341.1A
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Chinese (zh)
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不公告发明人
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Qingdao Xiangzhi Electronic Technology Co Ltd
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Qingdao Xiangzhi Electronic Technology Co Ltd
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Priority to CN201611188341.1A priority Critical patent/CN108200913A/en
Publication of CN108200913A publication Critical patent/CN108200913A/en
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Classifications

    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/02Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
    • A01N25/04Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • A01N25/06Aerosols
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/26Biocides, 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
    • A01N25/28Microcapsules or nanocapsules
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/90Biocides, 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

Abstract

A kind of emamectin benzoate microcapsule suspending agent and preparation method thereof is related to a kind of agricultural chemical insecticide and preparation method thereof.By the way that the mixture of cresylene isocyanates and Cyclohexyl isocyanate and amine are reacted to obtain microencapsulation product, photodegradation rate of the effective ingredient emamectin-benzoate during storage and use can be reduced, improve stability of the effective ingredient in microcapsule suspending agent, it further improves utilization rate of active components, the drug resistance growth rate for slowing down pest, improve to pest controling effect, have concurrently quick-acting and long-acting.

Description

A kind of emamectin benzoate microcapsule suspending agent and preparation method thereof
Technical field
The present invention relates to a kind of agricultural chemical insecticide and preparation method thereof more particularly to a kind of emamectin benzoate benzoic acid Salt microcapsule suspension formulation and preparation method thereof.
Background technology
Emamectin-benzoate (emamectin benzoate) is repairing for farm antibiotics AVERMECTIN B1 Product is adornd, there is advantages, the insecticidal activity such as ultra high efficiency, low toxicity (preparation is closely nontoxic), noresidue, nuisanceless to be carried compared with avermectin for it The high 1-3 order of magnitude, existing stomach poison function simultaneous action of contace poison again, larva and other many pests and mite to lepidopterous insects The activity of class is high, it has therefore proved that also there is good effect under low-down dosage (0.084-2g/ha), it is main in production at present It to be compounded with other active ingredients and the dosage forms such as missible oil, microemulsion, aqueous emulsion, water dispersible granules is made.
In recent years, because it increases, the stability of active ingredient, the longevity of residure was long, reduces contact toxicity, different for the microencapsulation of pesticide Taste mitigates, reduces the advantage of hazardous solvent dosage and reduction to the pollution of environment etc., by the wide of field of pesticide preparation General concern.Since photodissociation easily occurs for emamectin-benzoate, especially water and certain solvents can its significantly accelerated photodissociation, Its drug effect is greatly reduced, microencapsulation dosage form, which is made, can weaken its photodissociation characteristic, have centainly excellent compared with other dosage forms Gesture.
Invention content
The object of the present invention is to provide a kind of emamectin benzoate microcapsule suspending agents and preparation method thereof, will The mixture of cresylene isocyanates and Cyclohexyl isocyanate reacts to obtain microencapsulation product with amine, it is possible to reduce effectively Photodegradation rate of the composition emamectin-benzoate during storage and use improves effective ingredient in microcapsule suspension Stability in agent further improves utilization rate of active components, slows down resistance development.
Following technical scheme may be used to realize in the purpose of the present invention:
A kind of emamectin benzoate microcapsule suspending agent, it is characterised in that:The oil phase of said preparation is using following The substance of weight content is raw material:
Emamectin-benzoate 0.1-20%;
The mixture 1-12% of cresylene isocyanates and Cyclohexyl isocyanate, preferably 2-10%;
Aliphatic hydrocarbon 10-90%, preferably 30-70%;
Oil-soluble polymerization dispersant 1-15%, preferably 3-10%;
Amine 0.1-5%, preferably 0.5-2%;
The water phase of said preparation is substantially made of water, and the weight content of water is 15-50%, in addition it can include polyethylene The weight content of the mixture of alcohol and gum arabic, polyvinyl alcohol and gum arabic is respectively 0.1-3%, preferably 0.1- 1%th, 0.01-8%, preferably 0.05-5%;
Said preparation may also include the auxiliary agent of following weight content:
Emulsifier 1-8%, preferably 2-5%;
Dispersant 1-8%, preferably 2-5%;
Preservative 0.05-0.5%, preferably 0.1-0.3%;
Thickener 0.01-0.2%, preferably 0.05-0.15%.
The weight ratio of the mixture of the cresylene isocyanates and hexamethylene isocyanates is:Cresylene isocyanic acid Ester:Cyclohexyl isocyanate is 1:0.3-2, preferably 1:0.5-1.5.
Emulsifier is can be free of in the auxiliary agent.
The aliphatic hydrocarbon includes one or both of paraffin oil, mineral oil mixture.
The oil-soluble polymerization dispersant includes alkyl vinyl pyrrolidinone copolymer class such as AgrimerAL10LC (production of ISP companies), phosphoric acid ester such as Hordaphos215 (production of Clariant companies), polymerization hydroxy stearate acids are for example One or both of Atlox LP (production of Uniqema companies) mixtures.
It is mixed that the amine includes one or both of ethylidene -1,2- diamines, diethylenetriamines, trien Close object.
The emulsifier include non-ionic block copolymer such as Atlox4912 (production of Uniqema companies), Ethylan NS-500LQ (Akzo Nobel N.V.'s production), one kind in Pluronic PE (BASF AG's production) or Two kinds of mixtures.
The dispersant includes phenolformaldehyde condensate class such as Baykanol SL (Bayer AG's production), polycarboxylic acids (BASF AG gives birth to by salt such as Tersperse2700 (production of Huntsman companies), naphthalenesulfonate such as Tamol NN Production), one or both of styrylphenol ethoxyquin species such as Soprophor 4D 384 (Rhodia's production) Mixture.
The preservative includes one or both of Preventol D2, Preventol D7 (Bayer AG's production) Mixture.
The thickener includes one kind in xanthans class such as Kelcan S, Manugel XG (production of ISP companies) Or two kinds of mixtures.
The preparation method of above-mentioned emamectin benzoate microcapsule suspending agent, which is characterized in that this method includes Following processing step:
(1) oil phase is prepared
At ambient temperature, emamectin-benzoate, aliphatic hydrocarbon, oil-soluble polymerization dispersant are ground Afterwards, cresylene isocyanates and hexamethylene isocyanates are added in while stirring, oil phase is made, reaction temperature increases at this time, Raised temperature need to be controlled at 20-50 DEG C;
(2) water phase is prepared
Polyvinyl alcohol and gum arabic are added to the water, water phase is made, heating makes polyvinyl alcohol and gum arabic faster Dissolving, this process should control temperature the ice water after 30-100 DEG C, dissolving to cool down;
(3) microcapsule suspending agent is prepared
By being stirred for dispersion machine, oil phase is dispersed in water phase, speed of agitator is 20000 revs/min, should during dispersion Temperature is controlled at 10-40 DEG C;Treat that temperature is down to 15 DEG C hereinafter, addition amine aqueous solution, is then stirred while heating, reaching will Stop heating, and keep the temperature and continue stirring 20 hours after seeking temperature, this process heating and temperature control is at 40-80 DEG C;It is cooled to room Under the conditions of temperature, the auxiliary agents such as preservative, dispersant, emulsifier, thickener are added in, temperature can increase after adding in auxiliary agent, should incite somebody to action at this time Temperature is controlled at 10-50 DEG C, obtains emamectin benzoate microcapsule suspending agent.
In the step (2), temperature is preferably controlled in 30-90 DEG C when preparing water phase.
In the step (3), dispersion temperature is preferably controlled in 10-30 DEG C;Heating temperature is preferably controlled in 50-70 DEG C;Add Temperature is preferably controlled in 10-40 DEG C when entering auxiliary agent.
The present invention can directly be watered dilution spraying and use.
The emamectin benzoate microcapsule suspending agent of the present invention compared with prior art, generates following beneficial to effect Fruit:(1) stability of effective ingredient emamectin-benzoate is improved, the utilization rate of effective ingredient is improved, slows down evil The drug resistance growth rate of worm;(2) it significantly improves to pest controling effect, has quick-acting and long-acting, (3) alternative high poison agriculture concurrently Medicine, and field dosage is greatly reduced, effectively reduce environmental pollution and pesticide residue.
Specific embodiment
With reference to embodiment, the present invention is further described.
Embodiment 1
(1) oil phase is prepared:At ambient temperature, by 1.8g emamectin-benzoates, 20gAt loxLP and After the grinding of 100g mineral oils, 5g cresylenes isocyanates and 3g Cyclohexyl isocyanates are added in while stirring, at this time Reaction temperature increases, and raised temperature is controlled at 30 DEG C;
(2) water phase is prepared:70 DEG C are heated to, 1g polyvinyl alcohol and 6g gum arabics are dissolved in 130g deionized waters In, ice water cools down after dissolving;
(3) microcapsule suspending agent is prepared:Oil phase is mixed with water after conjunction and is divided with dispersion machine with 20000 revs/min of rotating speed Dissipate, during dispersion temperature control treat that temperature is down to 15 DEG C hereinafter, adding in the mixing of 2.8g diethylenetriamines and 2.8g water at 30 DEG C Object is heated to 50 DEG C while stirring, and keeps the temperature and is stirred 20 hours at 50 DEG C, is cooled under room temperature, adds in 0.3g Preventol D2,0.3g Preventol D7,6g Tersperse 2700,6g Pluronic PE, 8g 2%Kelcan S solution, at this time temperature raising, temperature is controlled at 40 DEG C, finally obtaining emamectin-benzoate content is 0.6%th, average grain diameter is 11.8 microns of microcapsule suspending agent.
Embodiment 2
(1) oil phase is prepared:At ambient temperature, by 30g emamectin-benzoates, 200g AtloxLP and 1000g mineral oils add in 16g cresylenes isocyanates and 12g Cyclohexyl isocyanates while stirring after grinding, this When reaction temperature increase, by raised temperature control at 40 DEG C;
(2) water phase is prepared:70 DEG C are heated to, 12g polyvinyl alcohol and 3g gum arabics are dissolved in 350g deionized waters In, ice water cools down after dissolving;
(3) microcapsule suspending agent is prepared:Oil phase is mixed with water after conjunction and is divided with dispersion machine with 20000 revs/min of rotating speed Dissipate, during dispersion temperature control treat that temperature is down to 20 DEG C hereinafter, add in 20g50% diethylenetriamines solution at 40 DEG C, stir on one side It mixes and is heated to 55 DEG C on one side, maintain the temperature at 55 DEG C and stir 20 hours, be cooled under room temperature, add in 0.8gPreventol D2,0.8g Preventol D7,30g Baykanol SL, 44g2%Kelcan S solution, it is warm at this time Degree raising, temperature is controlled at 30 DEG C, finally obtains that emamectin-benzoate content is 1%, average grain diameter is 11.4 microns of microcapsule suspending agent.

Claims (2)

1. a kind of emamectin benzoate microcapsule suspending agent, it is characterised in that:The oil phase of said preparation is using following heavy The substance for measuring content is raw material:
Emamectin-benzoate 0.1-20%;
The mixture 1-12% of cresylene isocyanates and hexamethylene isocyanates, cresylene isocyanates: hexamethylene isocyanic acid The weight ratio of ester is 1: 0.3-2;
Aliphatic hydrocarbon 10-90%;
Oil-soluble polymerization dispersant 1-15%;
Amine 0.1-5%;
The aliphatic hydrocarbon includes one or both of paraffin oil, mineral oil mixture;
The oil-soluble polymerization dispersant includes alkyl vinyl pyrrolidinone copolymer class, phosphoric acid ester, polymerization hydroxy stearate One or both of acids mixture;
The amine includes the mixing of one or both of ethylidene -1,2- diamines, diethylenetriamines, trien Object;
The water phase of said preparation is made of water, and the weight content of water is 15-50%, also comprises polyvinyl alcohol and gum arabic The weight content of mixture, polyvinyl alcohol and gum arabic is respectively 0.1-3%, 0.01-8%;
Said preparation includes the auxiliary agent of following weight content:
Emulsifier 1-8%;
Dispersant 1-8%;
Preservative 0.05-0.5%;
Thickener 0.01-0.2%;
Said preparation is made of the method comprising the following steps that:
(1) oil phase is prepared
At ambient temperature, after emamectin-benzoate, aliphatic hydrocarbon, oil-soluble polymerization dispersant being ground, Cresylene isocyanates and hexamethylene isocyanates are added in while stirring, oil phase is made, at this time reaction temperature increase, need by Raised temperature control is at 20-50 DEG C;
(2) water phase is prepared
Polyvinyl alcohol and gum arabic are added to the water, water phase is made, heating makes polyvinyl alcohol and gum arabic faster molten Solution, this process should control temperature the ice water after 30-100 DEG C, dissolving to cool down;
(3) microcapsule suspending agent is prepared
By being stirred for dispersion machine, oil phase is dispersed in water phase, speed of agitator is 20000 revs/min, should will be warm during dispersion Degree control is at 10-40 DEG C;Treat that temperature is down to 15 DEG C hereinafter, addition amine aqueous solution, then stirs while heating, reach requirement temperature Stop heating after degree, and keep the temperature and continue stirring 20 hours, this process heating and temperature control is at 40-80 DEG C;It is cooled to room temperature item Under part, preservative, dispersant, emulsifier, thickening agent aid are added in, temperature can increase after adding in auxiliary agent, at this time should be by temperature control System obtains emamectin benzoate microcapsule suspending agent at 10-50 DEG C.
2. a kind of emamectin benzoate microcapsule suspending agent according to claim 1, it is characterised in that:The system The oil phase of agent uses the substance of following weight content as raw material:
Emamectin-benzoate 0.1-20%;
The mixture 2-10% of cresylene isocyanates and hexamethylene isocyanates, cresylene isocyanates: hexamethylene isocyanic acid Ester is 1: 0.5-1.5;
Aliphatic hydrocarbon 30-70%;
Oil-soluble polymerization dispersant 3-10%;
Amine 0.5-2%;
The water phase of said preparation is made of water, and the weight content of water is 15-50%, also comprises polyvinyl alcohol and gum arabic The weight content of mixture, polyvinyl alcohol and gum arabic is respectively 0.1-1%, 0.05-5%;Said preparation includes following heavy Measure the auxiliary agent of content:
Emulsifier 2-5%;
Dispersant 2-5%;
Preservative 0.1-0.3%;
Thickener 0.05-0.15%.
CN201611188341.1A 2016-12-20 2016-12-20 A kind of emamectin benzoate microcapsule suspending agent and preparation method thereof Pending CN108200913A (en)

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Application Number Priority Date Filing Date Title
CN201611188341.1A CN108200913A (en) 2016-12-20 2016-12-20 A kind of emamectin benzoate microcapsule suspending agent and preparation method thereof

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114868743A (en) * 2022-06-22 2022-08-09 山东潍坊润丰化工股份有限公司 Pesticide microcapsule suspending agent and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114868743A (en) * 2022-06-22 2022-08-09 山东潍坊润丰化工股份有限公司 Pesticide microcapsule suspending agent and preparation method thereof

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