CN107864955A - 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
CN107864955A
CN107864955A CN201610852358.6A CN201610852358A CN107864955A CN 107864955 A CN107864955 A CN 107864955A CN 201610852358 A CN201610852358 A CN 201610852358A CN 107864955 A CN107864955 A CN 107864955A
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China
Prior art keywords
isocyanates
preparation
oil
emamectin
temperature
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CN201610852358.6A
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Chinese (zh)
Inventor
李辉
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Qingdao Jiuzhou Thousand Machinery Co Ltd
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Qingdao Jiuzhou Thousand Machinery Co Ltd
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Priority to CN201610852358.6A priority Critical patent/CN107864955A/en
Publication of CN107864955A publication Critical patent/CN107864955A/en
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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
    • 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

Abstract

A kind of emamectin benzoate microcapsule suspending agent and preparation method thereof, it 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, utilization rate of active components is further improved, slows down the resistance to the action of a drug growth rate of insect, improve to pest controling effect, is had 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 advantage, the insecticidal activity such as ultra high efficiency, low toxicity (preparation is closely nontoxic), noresidue, nuisanceless to be carried compared with AVM for it The high 1-3 order of magnitude, existing stomach poison function simultaneous action of contace poison again, larva and other many insects and mite to lepidopterous insects Class it is active 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 To be compounded with other active ingredients and the formulations such as missible oil, microemulsion, aqueous emulsion, water dispersible granules are made.
In recent years, the microencapsulation of agricultural chemicals was because it increases the stability of active ingredient, the longevity of residure is long, reduces contact toxicity, different Taste mitigates, reduced the advantage of the pollution of hazardous solvent dosage and reduction to environment etc., by the wide of field of pesticide preparation General concern.Because photodissociation easily occurs for emamectin-benzoate, especially water and some solvents can its significantly accelerated photodissociation, Its drug effect is greatly reduced, microencapsulation formulation, which is made, can weaken its photodissociation characteristic, have necessarily excellent compared with other formulations Gesture.
The content of the invention
, will it is an object of the invention to provide a kind of emamectin benzoate microcapsule suspending agent and preparation method thereof 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, effective ingredient is improved in microcapsule suspension Stability in agent, further improve utilization rate of active components, slow down resistance development.
The purpose of the present invention can be realized using following technical scheme：
A kind of emamectin benzoate microcapsule suspending agent, it is characterised in that：The oil phase of said preparation is using following The material 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 aqueous phase of said preparation is substantially made up of water, and the weight content of water is 15-50%, it can in addition contain including 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：
Emulsifying agent 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.
Emulsifying agent is can be free of in the auxiliary agent.
Described aliphatic hydrocarbon includes one or both of paraffin oil, mineral oil mixture.
Described 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) mixture.
It is mixed that described amine includes one or both of ethylidene -1,2- diamines, diethylenetriamines, trien Compound.
Described emulsifying agent 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.
Described 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.
Described preservative includes one or both of Preventol D2, Preventol D7 (Bayer AG's production) Mixture.
Described 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, it is characterised 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, stir while add cresylene isocyanates and hexamethylene isocyanates, oil phase is made, now reaction temperature raises, Need to be by elevated temperature control at 20-50 DEG C；
(2) aqueous phase is prepared
Polyvinyl alcohol and gum arabic are added to the water aqueous phase is made, heating makes polyvinyl alcohol and gum arabic faster Dissolving, this process should frozen water cools down after 30-100 DEG C, dissolving by temperature control；
(3) microcapsule suspending agent is prepared
By being stirred for dispersion machine, oil phase is dispersed in aqueous phase, speed of agitator is 20000 revs/min, should when disperseing By temperature control at 10-40 DEG C；Treat that temperature is down to less than 15 DEG C, add amine aqueous solution, then heat while stirring, reaching will Stop heating after seeking temperature, and be incubated and continue stirring 20 hours, 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, emulsifying agent, thickener are added, temperature can raise after adding auxiliary agent, should now incite somebody to action Temperature control obtains emamectin benzoate microcapsule suspending agent at 10-50 DEG C.
In the step (2), temperature is preferably controlled in 30-90 DEG C when preparing aqueous phase.
In the step (3), dispersion temperature is preferably controlled in 10-30 DEG C；Heating-up 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, produces 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 resistance to the action of a drug growth rate of worm；(2) significantly improve to pest controling effect, have quick-acting and long-acting, (3) alternative high poison agriculture concurrently Medicine, and field dosage is greatly reduced, effectively reduces environmental pollution and residues of pesticides.
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, 20gAtloxLP and After the grinding of 100g mineral oils, stir while adding 5g cresylenes isocyanates and 3g Cyclohexyl isocyanates, now Reaction temperature raises, by elevated temperature control at 30 DEG C；
(2) aqueous phase is prepared：70 DEG C are heated to, 1g polyvinyl alcohol and 6g gum arabics are dissolved in 130g deionized waters In, frozen water cools down after dissolving；
(3) microcapsule suspending agent is prepared：Oil phase is mixed with water after conjunction and divided with dispersion machine with 20000 revs/min of rotating speed Dissipate, temperature control treats that temperature is down to less than 15 DEG C, add the mixing of 2.8g diethylenetriamines and 2.8g water at 30 DEG C when disperseing Thing, stir while be heated to 50 DEG C, be incubated and stirred 20 hours at 50 DEG C, is cooled under room temperature condition, add 0.3g Preventol D2,0.3g Preventol D7,6g Tersperse 2700,6g Pluronic PE, 8g 2%Kelcan S solution, now temperature rise, by temperature control at 40 DEG C, finally giving 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, stirred after grinding while add 16g cresylenes isocyanates and 12g Cyclohexyl isocyanates, this When reaction temperature raise, by elevated temperature control at 40 DEG C；
(2) aqueous phase is prepared：70 DEG C are heated to, 12g polyvinyl alcohol and 3g gum arabics are dissolved in 350g deionized waters In, frozen water cools down after dissolving；
(3) microcapsule suspending agent is prepared：Oil phase is mixed with water after conjunction and divided with dispersion machine with 20000 revs/min of rotating speed Dissipate, temperature control treats that temperature is down to less than 20 DEG C, 20g50% diethylenetriamines solution is added, while stirring at 40 DEG C when disperseing Mix while be heated to 55 DEG C, maintain the temperature at 55 DEG C and stir 20 hours, be cooled under room temperature condition, add 0.8gPreventol D2,0.8g Preventol D7,30g Baykanol SL, 44g2%Kelcan S solution, it is now warm Degree rise, by temperature control at 30 DEG C, finally give emamectin-benzoate content be 1%, average grain diameter be 11.4 microns of microcapsule suspending agent.

Claims (2)

  1. A kind of 1. emamectin benzoate microcapsule suspending agent, it is characterised in that:The oil phase of said preparation is using following heavy The material 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%；
    Described aliphatic hydrocarbon includes one or both of paraffin oil, mineral oil mixture；
    Described oil-soluble polymerization dispersant includes alkyl vinyl pyrrolidinone copolymer class, phosphoric acid ester, polymerization hydroxy stearate One or both of acids mixture；
    Described amine includes the mixing of one or both of ethylidene -1,2- diamines, diethylenetriamines, trien Thing；
    The aqueous phase of said preparation is made up of water, and the weight content of water is 15-50%, comprises additionally in 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：
    Emulsifying agent 1-8%；
    Dispersant 1-8%；
    Preservative 0.05-0.5%；
    Thickener 0.01-0.2%；
    Said preparation is made up 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, Stir while add cresylene isocyanates and hexamethylene isocyanates, oil phase be made, now reaction temperature raises, need by Elevated temperature control is at 20-50 DEG C；(2) aqueous phase is prepared
    Polyvinyl alcohol and gum arabic are added to the water aqueous phase is made, heating makes polyvinyl alcohol and gum arabic faster molten Solution, this process should frozen water cools down after 30-100 DEG C, dissolving by temperature control；
    (3) microcapsule suspending agent is prepared
    By being stirred for dispersion machine, oil phase is dispersed in aqueous phase, speed of agitator is 20000 revs/min, should be by temperature when scattered Degree control is at 10-40 DEG C；Treat that temperature is down to less than 15 DEG C, add amine aqueous solution, then heat while stir, reach requirement temperature Stop heating after degree, and be incubated and continue stirring 20 hours, this process heating and temperature control is at 40-80 DEG C；It is cooled to room temperature bar Under part, preservative, dispersant, emulsifying agent, thickening agent aid are added, temperature can raise after adding auxiliary agent, now should be by temperature control System obtains emamectin benzoate microcapsule suspending agent at 10-50 DEG C.
  2. A kind of 2. emamectin benzoate microcapsule suspending agent according to claim 1, it is characterised in that：The system The oil phase of agent uses the material 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 aqueous phase of said preparation is made up of water, and the weight content of water is 15-50%, comprises additionally in 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：
    Emulsifying agent 2-5%；
    Dispersant 2-5%；
    Preservative 0.1-0.3%；
    Thickener 0.05-0.15%.
CN201610852358.6A 2016-09-26 2016-09-26 A kind of emamectin benzoate microcapsule suspending agent and preparation method thereof Pending CN107864955A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114532335A (en) * 2022-03-04 2022-05-27 上海师范大学 Ionic liquid type pesticide microcapsule and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114532335A (en) * 2022-03-04 2022-05-27 上海师范大学 Ionic liquid type pesticide microcapsule and preparation method thereof

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