CN102106345A - Avermectin microcapsule suspending agent and preparation method thereof - Google Patents
Avermectin microcapsule suspending agent and preparation method thereof Download PDFInfo
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- CN102106345A CN102106345A CN2009102472608A CN200910247260A CN102106345A CN 102106345 A CN102106345 A CN 102106345A CN 2009102472608 A CN2009102472608 A CN 2009102472608A CN 200910247260 A CN200910247260 A CN 200910247260A CN 102106345 A CN102106345 A CN 102106345A
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Abstract
The invention discloses an avermectin microcapsule suspending agent and a preparation method thereof. The avermectin microcapsule suspending agent mainly comprises the following components in percentage by weight: 1 to 10 percent of avermectin, 5 to 40 percent of solvent, 1 to 8 percent of capsule wall material, 0.1 to 3 percent of protection glue, 2 to 5 percent of emulsifier, 3 to 5 percent of dispersant, 0 to 14 percent of adjuvant, and the balance of water. The preparation method for the avermectin microcapsule suspending agent comprises the following steps of: preparing avermectin microcapsules from an avermectin active substance serving as capsule cores and a carbamide resin serving as the capsule wall material by using an interfacial polymerization technology, and finally blending to obtain a microcapsule water suspending agent. Active ingredients of the avermectin microcapsule suspending agent are centralized in the capsule cores, and other media are almost water, so the environmental pollution is reduced and the production cost of products is also effectively reduced. The avermectin microcapsule suspending agent has the release control capacity and can prolong effective duration of pesticides by 3 to 10 times, so that the acute toxicity of technical materials is reduced and the toxicity of a preparation on non-target organisms is also reduced. The avermectin microcapsule suspending agent is safe to use and transport.
Description
Technical field
The invention belongs to formulations of pesticide manufacture field, to be specifically related to the biological pesticide avermectin be capsule-core, be the microcapsules that capsule casing material wraps up with the carbamide resin, and be pesticides new formulation avermectin microcapsule suspending agent of making of basic dispersion medium and preparation method thereof with water.
Background technology
Avermectin (Avermectins): be that a class has desinsection, kills mite, ten hexa-atomic Macrocyclic lactone compounds of eelworm-killing activity, produce by streptomyces griseus fermentation in the streptomycete.Former pharmacology voltinism matter: density 1.16; The smart powder of former medicine is white or yellow crystal (containing B1a 〉=90%), vapour pressure＜200nPa, fusing point 150-155 ℃.25g/L is difficult in 70g/L, the chloroform in 350g/L, the isopropyl alcohol in 100g/L, the toluene in 7.8mg/L, the acetone in solvability such as the water in the time of 21 ℃ decomposes.At 25 ℃, there is not decomposing phenomenon in the solution of pH5-9.
Avermectin is the natural products that separates from edaphon, insect, evil mite is had tag and stomach poison function, crop is had osmosis, but do not have ovicidal action.Insecticidal mechanism mainly is the neurophysiology activity of disturbing insect, thereby causes insect, evil mite paralysis symptom to occur, and inertia is not got food, and is promptly dead through 2-4 days.It is reported that Avermectin (Avermectins) insecticidal spectrum has 84 kinds, can effectively prevent and treat diptera, Homoptera, coleoptera and lepidoptera pest and multiple harmful mite, for example citrus rust mite (blister mite), tangerine Panonychus citri, tangerine bud goitre mite, tangerine short hairs mite, spot true leaf mite, tea half instep mite, unaspis shield kuwana and real hard thrips; Various mite classes of cotton and lyonetid, cotton leaf noctuid; Leaf miner, alfalfa thrips, little Macrosiphus spp class, the black peach aphid of plant tasted in sight; Vegetables liriomyza bryoniae larva, cabbage caterpillar, cauline leaf moth; Colorado potato beetles; Evil mite of kind more than 80 and insects such as fruit tree mites, Aspidiotus, pear sucker and cigarette beetle, day night, Bemisia tabaci.Because Avermectin is fast in degraded in soil, photodissociation is rapid.To crop safety, be difficult for producing poisoning, be one of product most popular in the current biopesticide market therefore.
Existing conventional Avermectin preparation is mainly missible oil, and generally between 0.2%-5%, all the other components mostly are organic solvent and surfactant to content.Both waste raw material, brought the problem of environmental protection again.
Summary of the invention
The present invention with an organic solvent produces pollution problems with emulsifier to environment in a large number in order to solve existing Avermectin preparation, and a kind of avermectin microcapsule suspending agent that provides and preparation method thereof.The present invention develops the novel environment friendly preparation of Avermectin by microencapsulation technology, can reduce employed organic solvent in the conventional formulation missible oil (toluene, dimethylbenzene etc.), and is friendly more to environment, reduces production costs simultaneously.The target insect there is good preventive and therapeutic effect, and effectively reduces the toxicity of preparation, thereby improve safety non-target biology.Owing to the sustained release of active ingredient Avermectin thereby the long lasting period is arranged, reduce the number of times of dispenser, thereby reduce the usage amount of agricultural chemicals.Can effectively reduce Avermectin resolution ratio under ultraviolet light conditions.For the update of adjusting China's formulation products structure with promote the raising of social ecological benefits that remarkable effect is arranged.
The technical scheme that the present invention takes is: the avermectin microcapsule suspending agent, be characterized in, and mainly form by the component of following weight degree:
Avermectin 1～10%,
Solvent 5～40%,
Cyst material 1～8%,
Protection glue 0.1～3%,
Emulsifier 2～5%,
Dispersant 3～5%,
Adjuvant 0～14%,
Water surplus supplies 100%.
Above-mentioned avermectin microcapsule suspending agent, wherein, described solvent is selected from a kind of in toluene, dimethylbenzene, aliphatic solvent oil, cyclohexanone, methylated vegetable oil, vegetable oil, mineral oil, aromatic solvent naphtha, N-Methyl pyrrolidone, carrene, methyl-sulfoxide, the benzinum.
Above-mentioned avermectin microcapsule suspending agent, wherein, described cyst material is a carbamide resin, is to be made by interface polymerization reaction by isocyanates and water or polyamine.
Above-mentioned avermectin microcapsule suspending agent, wherein, described protection glue is selected from wherein a kind of of polyvinyl alcohol, gelatin, gum Arabic, xanthans.
Above-mentioned avermectin microcapsule suspending agent, wherein, described emulsifier is selected lauryl sodium sulfate for use, Nonyl pheno (NP series), alkylphenol-polyethenoxy polyethers and sulphate thereof (or phosphoric acid fat), fatty alcohol-polyoxyethylene ether (AEO series), the polyoxyethylene nonylphenol ether phosphate, polycarboxylate, alkylphenol-polyethenoxy formaldehyde condensation products sulphate, alkylphenol polyoxyethylene formaldehyde condensation products sulphate phosphate, styrene phenol formaldehyde resin polyoxyethylene ether phosphate salt, styryl phenol polyethenoxy polyethenoxy ether, the alkyl naphthalene formaldehyde condensate sulfonates, the dialkyl succinylsuccinate sulfonated ester, this coils SPAN, being used in combination more than two kinds or three kinds among the soil temperature TWEEN.
Above-mentioned avermectin microcapsule suspending agent, wherein, described dispersant is selected naphthalenesulfonic acid-formaldehyde condensate for use, triphenyl vinyl phenol polyethenoxy ether class and derivative eater, fatty alcohol polyethenoxy ether class, the alkylphenol polyoxyethylene class, macromolecule EO-PO block copolymer, lignosulfonates, alkylphenol-polyethenoxy formaldehyde condensation products sulphate, alkylphenol polyoxyethylene formaldehyde condensation products sulphate phosphate, styrene phenol formaldehyde resin polyoxyethylene ether phosphate salt, styryl phenol polyethenoxy polyethenoxy ether, the alkyl naphthalene formaldehyde condensate sulfonates, macromolecule is dredged a dress copolymer of type, being used in combination more than two kinds or three kinds in the polymerization of carboxylic acid salt.
Above-mentioned avermectin microcapsule suspending agent, wherein, described adjuvant is selected from one or more combinations wherein of stabilizing agent, antifreeze, viscosity modifier, PH conditioning agent, sterilization antiseptic, defoamer; Wherein:
Described stabilizing agent is selected from butylhydroxy anisole (BHA), 2, a kind of in 6-BHT (BHT), ditert-butylhydro quinone (TBHQ), epoxidized soybean oil, the epoxychloropropane;
Described antifreeze is selected from a kind of in ethylene glycol, propane diols, glycerine, PEG400, isopropyl alcohol, the urea;
Described viscosity-controlling agent is selected from a kind of in xanthans, cellulose ether and derivative thereof, polyethylene glycol, polyvinyl alcohol, aluminium-magnesium silicate, bentonite, kaolin, diatomite, the attapulgite; 0.05～0.3
Described PH acid-base modifier is selected from a kind of in glacial acetic acid, hydrochloric acid, citric acid, NaOH, ammoniacal liquor, monoethanolamine, the triethanolamine;
Described sterilization antiseptic is selected from a kind of in potassium sorbate, Sodium Benzoate, formaldehyde, the isothiazolinone;
That described defoamer is selected from is silicone based, a kind of in the low-carbon alcohols.
The preparation method of avermectin microcapsule suspending agent is characterized in, according to the material that said components provided, with the Avermectin active substance is capsule-core, the employing carbamide resin is a cyst material, prepares avermectin microcapsule with the interfacial polymerization law technology, is deployed into the microcapsules aqueous suspension agent at last; May further comprise the steps:
A, former medicine of Avermectin and wetting dispersing agent are dropped in the proper amount of solvent, then by the sand mill sand milling;
B, in the good material of sand milling, add an amount of isocyanates cyst material monomer and stir and obtain oil phase;
C, in water, add emulsifier in advance, adjuvant stirs, and adds pre-configured oil phase then, the high speed homogenizing forms the stabilized oil-in-water emulsion;
D, reduction rotating speed under the speed conditions that is fit to, add polyamine or polyatomic alcohol water solution and participate in interface polymerization reaction, and reaction temperature rises to 20 ℃～65 ℃, keeps 2 hours～24 hours, makes cyst material solidify encystation;
E, treat into capsule material and solidify encystation fully after, add an amount of dispersant and adjuvant, stir and promptly make avermectin microcapsule suspending agent;
Above-mentioned technical process is all implemented to finish under atmospheric pressure state.
The preparation method of above-mentioned avermectin microcapsule suspending agent, wherein, the particle mean size of the material described in the step a is at 1um～20um.
The preparation method of above-mentioned avermectin microcapsule suspending agent, wherein, adding adjuvant described in the step e comprises the PH acid-base modifier, be adjusted in the required pH value scope, add viscosity-controlling agent, defoamer, antifreeze, preservative in an amount of dispersant and the adjuvant again, stir and promptly make avermectin microcapsule suspending agent.
The present invention is owing to adopted above technical scheme, and the technique effect of its generation is tangible:
(1) Avermectin is made the suspending agent of the tiny spherical shape microcapsules of being made up of capsule-core that contains the Avermectin active substance and macromolecule cyst material, the active substance in the capsule-core slowly discharges under the condition of control, can satisfy suitable preventive effect requirement;
(2) Avermectin belongs to biogenic agricultural chemicals, is easy to be decomposed in the presence of illumination and oxygen, and for example the light degradation half life period is 12h in the water; In soil, the illumination degrading half life period is 21h; Form the medicine film in environment after, sunshine quickens its decomposition, and causing the half life period only is 4～6h.And by behind the microencapsulation of the present invention, Avermectin is wrapped in the core materials, owing to add stabilizing agents such as suitable antioxidant, UV absorbers, can effectively reduce the decomposition of ultraviolet light to Avermectin again, thereby the raising drug effect, the number of times of minimizing dispenser;
(3) because active ingredient is wrapped in the cyst wall, make preparation reduce toxic grade, therefore some unhappy smells and the skin irritation material can be effectively reduced have improved safety;
(4) owing to reduced by 20%～70% organic solvent and used, thus more friendly to environment;
Embodiment
It is capsule-core that the present invention adopts with the Avermectin active substance, and carbamide resin is a cyst material, prepares avermectin microcapsule with the interfacial polymerization law technology, is deployed into the microcapsules aqueous suspension agent at last, and production cost is low, and process route is simple.The avermectin microcapsule suspending agent mainly is made up of the component of following weight degree:
Avermectin 1～10%,
Solvent 5～40%,
Cyst material 1～8%,
Protection glue 0.1～3%,
Emulsifier 2～5%,
Dispersant 3～5%,
Adjuvant 0～14%,
Water surplus supplies 100%.
Solvent in the component is selected from a kind of in toluene, dimethylbenzene, aliphatic solvent oil, cyclohexanone, methylated vegetable oil, vegetable oil, mineral oil, aromatic solvent naphtha, N-Methyl pyrrolidone, carrene, methyl-sulfoxide, the benzinum, preferred toluene of the present invention and vegetable oil;
Cyst material in the component is a carbamide resin, is to be made by interface polymerization reaction by isocyanates and water (perhaps polyamine);
Protection glue in the component is selected from a kind of in polyvinyl alcohol, gelatin, gum Arabic, the xanthans, preferably polyethylene alcohol of the present invention;
Emulsifier in the component is selected lauryl sodium sulfate for use, Nonyl pheno (NP series), alkylphenol-polyethenoxy polyethers and sulphate thereof (or phosphoric acid fat), fatty alcohol-polyoxyethylene ether (AEO series), the polyoxyethylene nonylphenol ether phosphate, polycarboxylate, alkylphenol-polyethenoxy formaldehyde condensation products sulphate, alkylphenol polyoxyethylene formaldehyde condensation products sulphate phosphate, styrene phenol formaldehyde resin polyoxyethylene ether phosphate salt, styryl phenol polyethenoxy polyethenoxy ether, the alkyl naphthalene formaldehyde condensate sulfonates, the dialkyl succinylsuccinate sulfonated ester, this coils SPAN, being used in combination more than two kinds or three kinds among the soil temperature TWEEN.
Dispersant in the component is selected naphthalenesulfonic acid-formaldehyde condensate for use, triphenyl vinyl phenol polyethenoxy ether class and derivative eater, fatty alcohol polyethenoxy ether class, the alkylphenol polyoxyethylene class, macromolecule EO-PO block copolymer, lignosulfonates, alkylphenol-polyethenoxy formaldehyde condensation products sulphate, alkylphenol polyoxyethylene formaldehyde condensation products sulphate phosphate, styrene phenol formaldehyde resin polyoxyethylene ether phosphate salt, styryl phenol polyethenoxy polyethenoxy ether, the alkyl naphthalene formaldehyde condensate sulfonates, macromolecule is dredged a dress copolymer of type, being used in combination more than two kinds or three kinds in the polymerization of carboxylic acid salt.
Employed adjuvant comprises in the component: stabilizing agent, antifreeze, viscosity-controlling agent, PH acid-base modifier, sterilization antiseptic, defoamer, wherein:
Described stabilizing agent is selected from butylhydroxy anisole (BHA), 2, a kind of in 6-BHT (BHT), ditert-butylhydro quinone (TBHQ), epoxidized soybean oil, the epoxychloropropane, and its weight percent content for example is 0.1～0.3%.The present invention preferably adopts BHA;
Described antifreeze is selected from a kind of in ethylene glycol, propane diols, glycerine, PEG400, isopropyl alcohol, the urea, and its weight percent content for example is 3～10%.The preferred ethylene glycol of the present invention.
Described viscosity-controlling agent is selected from a kind of in xanthans, cellulose ether and derivative thereof, polyethylene glycol, polyvinyl alcohol, aluminium-magnesium silicate, bentonite, kaolin, diatomite, the attapulgite, and its weight percent content for example is 0.05～0.3%.The preferred xanthans of the present invention or cellulose ether and derivative thereof.
Described PH acid-base modifier is selected from a kind of in glacial acetic acid, hydrochloric acid, citric acid, NaOH, ammoniacal liquor, monoethanolamine, the triethanolamine.
Described sterilization antiseptic is selected from a kind of in potassium sorbate, Sodium Benzoate, formaldehyde, the isothiazolinone.
That described defoamer is selected from is silicone based, a kind of in the low-carbon alcohols.
The water that is adopted in this production technology is deionized water or distilled water.
The method of producing microcapsules at present is of a great variety, generally can be divided into chemical method, physical method and physico-chemical process on principle.Method the most commonly used in the industrial production has interfacial polymerization, situ aggregation method, phase separation method, orifice-coagulating bath method, dry bath method, wraps up in core exchange process, powder bed method, air suspension film forming method, spray drying process, vacuum vapor deposition, static combined techniques and bio-microcapsule method etc.
What the present invention adopted is that interfacial polymerization prepares microcapsules, the advantage of have process stabilizing, being convenient to control.Technical process is summarized as follows: active ingredient and suitable macromolecule cyst material (monomer) are dispersed or dissolved in the solvent; then oil phase is joined under shearing condition in the aqueous phase solution that contains suitable emulsifier and protection glue; become oil-in-water or water in oil form, control certain particle size as required.And adding another kind of water miscible cyst material again at aqueous phase, two kinds of materials react at oil-water interfaces, form the macromolecule cyst wall around the drop that contains active substance.The method generally can be carried out fast, and the cyst wall of formation is rule, homogeneous, and quality is hard.
The preparation method of avermectin microcapsule suspending agent of the present invention is the material that provides according to said components, under atmospheric pressure state, prepares the avermectin microcapsule agent by following concrete process route:
Former medicine of Avermectin and wetting dispersing agent are dropped in the proper amount of solvent, then by the sand mill sand milling,, in the good material of sand milling, add an amount of isocyanates cyst material monomer then and stir and obtain oil phase at 1um～20um up to the particle mean size of material;
Add emulsifier in advance in water, protect glue to stir, add pre-configured oil phase then, the high speed homogenizing forms the stabilized oil-in-water emulsion;
Reduce rotating speed, under the speed conditions that is fit to, add polyamine or polyatomic alcohol water solution and participate in interface polymerization reaction, reaction temperature rises to 20 ℃～65 ℃, keeps making in 2 hours～24 hours cyst material to solidify encystation.After treating into capsule material and solidifying encystation fully, add an amount of PH acid-base modifier, be adjusted in the required pH value scope, add an amount of dispersant, viscosity-controlling agent, defoamer, antifreeze, preservative etc., stir and promptly make avermectin microcapsule suspending agent.
Between the granularity of the resulting avermectin microcapsule suspending agent of the present invention control 1um～20um, possessed the characteristics of pesticide suspension concentrate, can convert the water use of directly spraying.
For better explanation the technology of the present invention, below, describe the present invention in detail with reference to some embodiment, but described embodiment does not mean, should not be understood that limitation of the present invention yet.Any technical staff in the art can be used for a variety of modifications and variations in not departing from the desired spirit and scope of claims of the present invention, so protection scope of the present invention is with being as the criterion that claims scope is defined.
Embodiment one:
The Avermectin of 1g is rolled over the dimethylbenzene (commercial material) that hundred former medicines are dissolved in 15g, toluene di-isocyanate(TDI) TDI (Cangzhou bigization TDI Co., Ltd), the stabilizing agent BHA 0.2g that adds 2g then stir (oil phase); The 10% PVAC polyvinylalcohol aqueous solution of emulsifier polyoxyethylene nonylphenol ether NP-12 (Hai'an petrochemical industry Co., Ltd), the 10g of 2.0g is added in the deionized water of 49g and stir evenly (water); The oil phase that configures to going into water and opening the high speed homogenizing, is formed stable O/W emulsion, and recording average grain diameter is 2.53um; Open to stir (keeping 600 changes/min), then that homogenizing is good emulsion is warming up to 40 ℃, the hexamethylene diamine that slowly adds 0.1g simultaneously, kept stable cyst material solidification temperature 8 hours, xanthans (2%) aqueous solution of the back adding dispersant 5.0g of wooden sodium sulfonate, ethylene glycol 5.0g, 10g, the triethanolamine of 0.1g are transferred about pH value to 7, isothiazolinone compound bactericidal agent shredding 0.1g, silicone defoaming agent 0.3g stir, and promptly make 1% avermectin microcapsule suspending agent.
Embodiment two,
The Avermectin of 5g is rolled over the soybean oil that hundred former medicines are dispersed in 20g, and add stabilizing agent epoxidized soybean oil 5g and stir (oil phase) back, reach about 5um, stop sand milling up to the particle mean size of material by sand mill sand milling; The polyphenyl polymethylene polyisocyanates PAPI (Bayer A.G) that adds 3.0g then stirs with the methyl diphenylene diisocyanate MDI (Yantai Wanhua Polyurethane Co., Ltd) of 1.0g and is oil phase; Gum Arabic (5%) aqueous solution of the emulsifier tween-60 (Hai'an, Jiangsu petrochemical industry Co., Ltd) of 2.0g, 10.0g is added stir evenly in the deionized water of 31g and be water; The oil phase that configures to going into water and opening the high speed homogenizing, is formed stable O/W emulsion, when the average grain diameter of emulsion is about 10um; Open to stir (keeping 700 changes/min), then that homogenizing is good emulsion is warming up to 35 ℃, the triethanolamine that slowly adds 1.0g simultaneously, kept stable cyst material solidification temperature 20 hours, phosphoric acid ester dispersant NP-P (company is changed very much in the Nanjing) propane diols of 8.0g of back adding 3.0g, the Magnesiumaluminumsilicate of 10.0g (2%) aqueous solution, an amount of diluted hydrochloric acid aqueous solution are transferred about pH value to 6.5, preservative formaldehyde 0.05g, silicone defoaming agent 0.3g stir, and promptly make 5% avermectin microcapsule suspending agent.
Embodiment three,
The Avermectin of 10g is rolled over hundred former medicines to be dispersed in the mineral oil of 30g, add BHT 0.3g then and stir (oil phase) back by the sand mill sand milling, reach up to the particle mean size of material and to stop sand milling about 10um, add the polyphenyl polymethylene polyisocyanates PAPI (Bayer A.G) of 5g then and stir with the toluene di-isocyanate(TDI) TDI of 0.9g (Cangzhou bigization TDI Co., Ltd) and be oil phase; Xanthans (2%) aqueous solution of emulsifier NP-10 (Co., Ltd is changed very much in Nanjing), the 5g of 2.0g is added stir evenly in the deionized water of 37g and be water; The oil phase that configures to going into water and opening the high speed homogenizing, is formed stable O/W emulsion, when the average grain diameter of emulsion stops emulsification during in the 18um left and right sides; Open to stir (keeping 800 changes/min), then that homogenizing is good emulsion is warming up to 60 ℃, the diethylenetriamine that slowly adds 0.6g simultaneously, kept stable cyst material solidification temperature 3.0 hours, the glycerine of metal carboxylate dispersant TERSPERSE 2700 (Huntsman company), the 5.0g of back adding 3.0g, the glacial acetic acid of 0.15g are transferred about pH value to 7, preservative sodium benzoate 0.1g, silicone defoaming agent 0.5g stir, and promptly make 10% avermectin microcapsule suspending agent.
The key technical indexes of the present invention such as following table:
| Sequence number | Avermectin content | Outward appearance | Average grain diameter, um | The encystation rate, % | Thermodynamic stability | Freeze and melt examination | Suspensibility, % |
| Embodiment one | 1％ | Coffee-like uniform liquid | 2.53 | 98.3 | Qualified | Qualified | 96.5 |
| Embodiment two | 5％ | The white thick liquid | 10.32 | 92.4 | Qualified | Qualified | 93.2 |
| Embodiment three | 10％ | The white thick liquid | 18.02 | 93.8 | Qualified | Qualified | 90.6 |
Avermectin microcapsule suspending agent content of the present invention can change between 1%～10%, formulates different content according to its different purposes.
Avermectin microcapsule aqueous suspension agent of the present invention also is a kind of formulation of controlled active ingredient rate of release simultaneously, and therefore according to its purposes, the thickness of decision softgel shell comes sustained release speed, to reach required effect.
Advantage of the present invention is:
1, because avermectin microcapsule suspending agent active ingredient of the present invention concentrates in the capsule core, other medium is almost water, so effectively reduce the production cost of product.
2, because avermectin microcapsule suspending agent of the present invention has the control releasability, thereby reduced the acute toxicity of former medicine. What avermectin microcapsule suspending agent used simultaneously is the former medicine of AVM crystal rather than preparation " ointment " (contain AbamectinB13%-9%, be generally about 4%) preparation, thereby effectively reduces the toxicity to non-target biology of preparation.
3, photodissociation, oxidation, hydrolysis are the principal elements that affects the agricultural chemicals lasting period. But the active ingredient of avermectin microcapsule suspending agent of the present invention is by the permeability manual control of cyst material, and slow release speed can design in advance. Because the protection of capsule skin, the active ingredient degradation speed slows down, and the agricultural chemicals lasting period can prolong 3-10 doubly. Lasting period prolongs, and just can improve prevention effect, reduces spraying times, reduces agricultural cost.
4, the medium of avermectin microcapsule suspending agent of the present invention is the organic solvents such as water rather than toluene, thus the use amount of effective environmental contamination reduction and reduction organic solvent. And because it is take water as decentralized medium, therefore nonflammable explosive, transportation safety.
Claims (10)
1. the avermectin microcapsule suspending agent is characterized in that, mainly is made up of the component of following weight degree:
Avermectin 1～10%,
Solvent 5～40%,
Cyst material 1～8%,
Protection glue 0.1～3%,
Emulsifier 2～5%,
Dispersant 3～5%,
Adjuvant 0～14%,
Water surplus supplies 100%.
2. avermectin microcapsule suspending agent according to claim 1, it is characterized in that described solvent is selected from a kind of in toluene, dimethylbenzene, aliphatic solvent oil, cyclohexanone, methylated vegetable oil, vegetable oil, mineral oil, aromatic solvent naphtha, N-Methyl pyrrolidone, carrene, methyl-sulfoxide, the benzinum.
3. avermectin microcapsule suspending agent according to claim 1 is characterized in that described cyst material is a carbamide resin, is to be made by interface polymerization reaction by isocyanates and water or polyamine.
4. avermectin microcapsule suspending agent according to claim 1 is characterized in that, described protection glue is selected from wherein a kind of of polyvinyl alcohol, gelatin, gum Arabic, xanthans.
5. avermectin microcapsule suspending agent according to claim 1, it is characterized in that described emulsifier is selected lauryl sodium sulfate for use, the Nonyl pheno of NP series, alkylphenol-polyethenoxy polyethers and sulphate thereof or phosphoric acid fat, the fatty alcohol-polyoxyethylene ether of AEO series, the polyoxyethylene nonylphenol ether phosphate, polycarboxylate, alkylphenol-polyethenoxy formaldehyde condensation products sulphate, alkylphenol polyoxyethylene formaldehyde condensation products sulphate phosphate, styrene phenol formaldehyde resin polyoxyethylene ether phosphate salt, styryl phenol polyethenoxy polyethenoxy ether, the alkyl naphthalene formaldehyde condensate sulfonates, the dialkyl succinylsuccinate sulfonated ester, this coils SPAN, being used in combination more than two kinds or three kinds among the soil temperature TWEEN.
6. avermectin microcapsule suspending agent according to claim 1, it is characterized in that described dispersant is selected naphthalenesulfonic acid-formaldehyde condensate for use, triphenyl vinyl phenol polyethenoxy ether class and derivative eater, fatty alcohol polyethenoxy ether class, the alkylphenol polyoxyethylene class, macromolecule EO-PO block copolymer, lignosulfonates, alkylphenol-polyethenoxy formaldehyde condensation products sulphate, alkylphenol polyoxyethylene formaldehyde condensation products sulphate phosphate, styrene phenol formaldehyde resin polyoxyethylene ether phosphate salt, styryl phenol polyethenoxy polyethenoxy ether, the alkyl naphthalene formaldehyde condensate sulfonates, macromolecule is dredged a dress copolymer of type, being used in combination more than two kinds or three kinds in the polymerization of carboxylic acid salt.
7. avermectin microcapsule suspending agent according to claim 1 is characterized in that, described adjuvant is selected from one or more combinations wherein of stabilizing agent, antifreeze, viscosity modifier, PH conditioning agent, sterilization antiseptic, defoamer; Wherein:
Described stabilizing agent is selected from butylhydroxy anisole (BHA), 2, a kind of in 6-BHT (BHT), ditert-butylhydro quinone (TBHQ), epoxidized soybean oil, the epoxychloropropane;
Described antifreeze is selected from a kind of in ethylene glycol, propane diols, glycerine, PEG400, isopropyl alcohol, the urea;
Described viscosity-controlling agent is selected from a kind of in xanthans, cellulose ether and derivative thereof, polyethylene glycol, polyvinyl alcohol, aluminium-magnesium silicate, bentonite, kaolin, diatomite, the attapulgite;
Described PH acid-base modifier is selected from a kind of in glacial acetic acid, hydrochloric acid, citric acid, NaOH, ammoniacal liquor, monoethanolamine, the triethanolamine;
Described sterilization antiseptic is selected from a kind of in potassium sorbate, Sodium Benzoate, formaldehyde, the isothiazolinone;
That described defoamer is selected from is silicone based, a kind of in the low-carbon alcohols.
8. the preparation method of avermectin microcapsule suspending agent is characterized in that, according to the material that said components provided, with the Avermectin active substance is capsule-core, the employing carbamide resin is a cyst material, prepares avermectin microcapsule with the interfacial polymerization law technology, is deployed into the microcapsules aqueous suspension agent at last; May further comprise the steps:
A, former medicine of Avermectin and wetting dispersing agent are dropped in the proper amount of solvent, then by the sand mill sand milling;
B, in the good material of sand milling, add an amount of isocyanates cyst material monomer and stir and obtain oil phase;
C, in water, add emulsifier in advance, adjuvant stirs, and adds pre-configured oil phase then, the high speed homogenizing forms the stabilized oil-in-water emulsion;
D, reduction rotating speed under the speed conditions that is fit to, add polyamine or polyatomic alcohol water solution and participate in interface polymerization reaction, and reaction temperature rises to 20 ℃～65 ℃, keeps 2 hours～24 hours, makes cyst material solidify encystation;
E, treat into capsule material and solidify encystation fully after, add an amount of dispersant and adjuvant, stir and promptly make avermectin microcapsule suspending agent;
Above-mentioned technical process is all implemented to finish under atmospheric pressure state.
9. the preparation method of avermectin microcapsule suspending agent according to claim 8 is characterized in that, the particle mean size of the material described in the step a is at 1um～20um.
10. the preparation method of avermectin microcapsule suspending agent according to claim 8, it is characterized in that, adding adjuvant described in the step e comprises the PH acid-base modifier, be adjusted in the required pH value scope, add an amount of dispersant and the adjuvant that comprises viscosity-controlling agent, defoamer, antifreeze, preservative again, stir and promptly make avermectin microcapsule suspending agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102472608A CN102106345A (en) | 2009-12-28 | 2009-12-28 | Avermectin microcapsule suspending agent and preparation method thereof |
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| CN102349509A (en) * | 2011-07-01 | 2012-02-15 | 华南农业大学 | Method for preparing lignin urea-formaldehyde pesticide microcapsule |
| CN102379286A (en) * | 2011-09-20 | 2012-03-21 | 中国科学院化学研究所 | Pesticide microcapsule and preparation method thereof |
| CN102578118A (en) * | 2012-01-30 | 2012-07-18 | 华南理工大学 | Microcapsule pesticide compounding sucrose ester with abamectin and preparation method of microcapsule pesticide |
| CN102812967A (en) * | 2012-09-03 | 2012-12-12 | 江苏宝灵化工股份有限公司 | Nematode killing composition micro-capsule suspending agent, and production method and application thereof |
| CN103229772A (en) * | 2013-03-07 | 2013-08-07 | 河南好年景生物发展有限公司 | Microcapsule suspending agent containing avermectin and dimehypo |
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| CN104839177A (en) * | 2015-03-31 | 2015-08-19 | 陕西康禾立丰生物科技药业有限公司 | Microencapsulated pesticide formulation |
| CN105010362A (en) * | 2015-07-27 | 2015-11-04 | 华南理工大学 | Abamectin microcapsule powder prepared from lignin-based wall material and method for preparing abamectin microcapsule powder by use of lignin-based wall material |
| CN106035327A (en) * | 2016-06-16 | 2016-10-26 | 周启新 | Preparation method of biological pesticide microcapsules |
| CN106070354A (en) * | 2016-06-08 | 2016-11-09 | 芜湖福民生物药业有限公司 | abamectin insecticide and preparation method thereof |
| CN106818735A (en) * | 2017-01-13 | 2017-06-13 | 华南理工大学 | A kind of avermectin microcapsule suspending agent and preparation method with anti-photolytic efficiency |
| CN106900703A (en) * | 2017-01-13 | 2017-06-30 | 华南理工大学 | A kind of lignin-base polyureas pesticide micro capsule and preparation method thereof |
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| CN110839623A (en) * | 2019-11-28 | 2020-02-28 | 南通德益化工有限公司 | Abamectin microcapsule suspending agent capable of improving insecticidal efficiency and preparation method thereof |
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| CN102349509A (en) * | 2011-07-01 | 2012-02-15 | 华南农业大学 | Method for preparing lignin urea-formaldehyde pesticide microcapsule |
| CN102349509B (en) * | 2011-07-01 | 2013-07-31 | 华南农业大学 | Method for preparing lignin urea-formaldehyde pesticide microcapsule |
| CN103732219A (en) * | 2011-08-16 | 2014-04-16 | 巴斯夫欧洲公司 | Method for encapsulating substances with formation of capsule shell by interfacial reaction in centrifugal reactor |
| CN102379286A (en) * | 2011-09-20 | 2012-03-21 | 中国科学院化学研究所 | Pesticide microcapsule and preparation method thereof |
| CN102578118A (en) * | 2012-01-30 | 2012-07-18 | 华南理工大学 | Microcapsule pesticide compounding sucrose ester with abamectin and preparation method of microcapsule pesticide |
| CN103250711A (en) * | 2012-02-18 | 2013-08-21 | 张秋芳 | High-efficiency environment-friendly pesticide complex composition |
| CN102812967A (en) * | 2012-09-03 | 2012-12-12 | 江苏宝灵化工股份有限公司 | Nematode killing composition micro-capsule suspending agent, and production method and application thereof |
| CN103229772A (en) * | 2013-03-07 | 2013-08-07 | 河南好年景生物发展有限公司 | Microcapsule suspending agent containing avermectin and dimehypo |
| CN103229772B (en) * | 2013-03-07 | 2015-04-08 | 河南好年景生物发展有限公司 | Microcapsule suspending agent containing avermectin and dimehypo |
| CN104273122A (en) * | 2013-07-03 | 2015-01-14 | 上海追光科技有限公司 | Preparation method of long-acting polyurethane pesticide microcapsule |
| CN104273122B (en) * | 2013-07-03 | 2016-08-10 | 上海追光科技有限公司 | The preparation method of long-acting polyurethane pesticide micro capsule |
| CN104782623A (en) * | 2015-03-25 | 2015-07-22 | 塔里木大学 | Trifluralin micro-capsule granule and preparation method thereof |
| CN104839177A (en) * | 2015-03-31 | 2015-08-19 | 陕西康禾立丰生物科技药业有限公司 | Microencapsulated pesticide formulation |
| CN105010362A (en) * | 2015-07-27 | 2015-11-04 | 华南理工大学 | Abamectin microcapsule powder prepared from lignin-based wall material and method for preparing abamectin microcapsule powder by use of lignin-based wall material |
| CN106070354A (en) * | 2016-06-08 | 2016-11-09 | 芜湖福民生物药业有限公司 | abamectin insecticide and preparation method thereof |
| CN106035327A (en) * | 2016-06-16 | 2016-10-26 | 周启新 | Preparation method of biological pesticide microcapsules |
| CN106818735A (en) * | 2017-01-13 | 2017-06-13 | 华南理工大学 | A kind of avermectin microcapsule suspending agent and preparation method with anti-photolytic efficiency |
| CN106900703A (en) * | 2017-01-13 | 2017-06-30 | 华南理工大学 | A kind of lignin-base polyureas pesticide micro capsule and preparation method thereof |
| CN107125241A (en) * | 2017-04-01 | 2017-09-05 | 西南大学 | Cyflumetofen capsule sustained-release and preparation method thereof |
| CN107047609A (en) * | 2017-04-20 | 2017-08-18 | 深圳诺普信农化股份有限公司 | A kind of microcapsule suspending agent |
| US11382330B2 (en) | 2017-12-25 | 2022-07-12 | Dow Global Technologies Llc | Micro-encapsulation of an insecticide |
| CN110050788A (en) * | 2018-05-08 | 2019-07-26 | 华东理工大学 | Gamma cyhalothrin poly-dopamine micro-capsule suspension and preparation method thereof |
| CN109122734A (en) * | 2018-08-31 | 2019-01-04 | 镇江鑫源达园艺科技有限公司 | A kind of sustained-release pesticides insecticide and preparation method thereof |
| CN109452272A (en) * | 2018-12-21 | 2019-03-12 | 江苏艾津农化有限责任公司 | A kind of avermectin microcapsule agent and preparation method thereof |
| CN109691444A (en) * | 2018-12-25 | 2019-04-30 | 江苏精禾界面科技有限公司 | A kind of pH response type controlled release pesticide microcapsule suspending agent and preparation method thereof |
| CN110839623A (en) * | 2019-11-28 | 2020-02-28 | 南通德益化工有限公司 | Abamectin microcapsule suspending agent capable of improving insecticidal efficiency and preparation method thereof |
| CN113016815A (en) * | 2021-02-23 | 2021-06-25 | 沈阳化工大学 | Abamectin B2 microcapsule suspending agent and preparation method thereof |
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