CN104430394A - Preparation method of ivermectin/emamectin benzoate compound microcapsule suspension - Google Patents
Preparation method of ivermectin/emamectin benzoate compound microcapsule suspension Download PDFInfo
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Abstract
The invention relates to a preparation method of ivermectin/emamectin benzoate compound microcapsule suspension, which belongs to the field of pesticide production. Invermectin and emamectin benzoate are used as main active substances of the pesticide-fertilizer, melamine-formaldehyde resin is adopted as a microcapsule wall material, and a microcapsule is prepared in an in-situ polymerization method. The compound microcapsule has advantages of safety, low toxicity, stability, good preventive effect on root-knot nematode, and the like; pesticide components in the product are coated with the capsule skin material, so that the pesticide components are slow to release, and the service life of the suspension is prolonged. In addition, the ivermectin and enamectin benzoate are easy to decompose in the storage process, so that the decomposition rate of ivermectin and enamectin benzoate can be remarkably reduced by using the microcapsule.
Description
Technical field
The present invention relates to pesticide field, particularly a kind of preparation method containing ivermectin and the composite micro-capsule suspension of emamectin-benzoate
Background technology
The active ingredient rate of release of conventional pesticide is fast, and effective drug duration is short, and availability is low, and traditional agricultural chemicals of 90% all can not meet crop demand in lasting period, release characteristics.Therefore develop pesticides new formulation to improve the availability of agricultural chemicals, reduce toxicity of pesticide, become the vital task of current pesticide research.Current research shows, Microcapsules of Pesticides can overcome the deficiency of conventional pesticide formulation, and enabling agricultural chemicals be agricultural production service safely, efficiently, economically, is most important formulation in pesticide slow-releasing agent.
Microencapsulation of pesticide as appearance the earliest, most study and the most ripe pesticide slow-release formulation, have slow release effect better, the feature such as applied widely.More than 20 kinds such as the active ingredient having made at present microcapsule formulations has sumithion, parathion-methyl, Dalmatian chrysanthemum cruel.
Pesticide micro capsule utilizes microcapsules technology solid, liquid pesticidal isoreactivity material to be coated in cyst material and to form microcapsules exactly.Compared with conventional pesticide, because pesticide activity component is covered by airtight or semipermeable wall film, cyst wall can improve anti-rain, the light resistance of agricultural chemicals, greatly can extend the lasting period of agricultural chemicals, reduce agricultural chemicals to the toxicity of people, animal and excitant simultaneously, expand the scope of application of agricultural chemicals; Both save the consumption of medicament, additionally reduce pollution.
Summary of the invention
The object of the invention is the easy decomposition for alleviating emamectin-benzoate and ivermectin, poor stability, the problem that the lasting period is short.The one control spectrum of development is wide, and drug effect is high, and stability is strong, the ivermectin that environmental pollution is little, the lasting period is long, cost accounting is lower and the composite Microencapsulated Slow pharmaceutical products of emamectin-benzoate.
Object of the present invention is achieved by the following technical programs:
1) a kind of ivermectin and the composite Microencapsulated Slow suspending agent of emamectin-benzoate, this medicament can adopt with the ivermectin of the emamectin-benzoate of 15-25 % by weight and 75-85 % by weight as compounded pesticides active component, both toxic effect ratio is more than 1 spend coefficient together more than 130, weighs for subsequent use.
2) preparation of core-clad material: by step 1) assembly mixture add 10-25% organic solvent mixing, be dissolved into solution, add the emulsifying dispersant of 3-6%, after mixing under high-shearing dispersion emulsifying machine, shear 3-8 minutes for 8000-15000 rev/min, obtained core material composition;
3) in above-mentioned preparation method, step 2) in, described organic solvent, is selected from any class in following substances or its any blend: arene, vegetable oil or improved plant oils, mineral oils, synthesis organic solvent class.
Described arene is selected from any one or its any blend in following substances: toluene, dimethylbenzene, trimethylbenzene; Described vegetable oil or improved plant oils are selected from any one or its blend in following substances: soybean oil, turpentine oil, fatty acid methyl ester; Described mineral oils is selected from any one or its blend in following substances: white oil, deodorized kerosine; Described synthesis organic solvent class is selected from any one or its blend in following substances: dimethyl carbonate, 2-butyl acetate, long chain class.
4) configuration of microcapsules performed polymer: melamine is mixed with the ratio of formaldehyde in 0.5-5:2-7, between adjust ph to 7-10, constant temperature 60-90 DEG C of reaction, obtained melamine formaldehyde resin performed polymer.
5) 10 minutes are stirred after being mixed with microcapsules performed polymer by core-clad material, between the pH value of polymerizer regulation system to 3-6, under the environment of 25-50 DEG C, isothermal reaction 1-2 hour.Add a certain amount of emulsifying dispersant, under the rotating speed of 600-1000 rev/min, stir 1-3 hour, obtained microcapsules microparticle solution.
6) step 5) described in polymerizer be the one of hydrochloric acid, phosphoric acid or oxalic acid.
7) in microcapsules microparticle solution, add emulsifying dispersant, under the mixing speed of 800-1500 revs/min, mix 70-150min obtain micro-capsule suspension.
8) in above-mentioned preparation method, step 2) with step 7) in, described emulsifying dispersant is selected from any one or its any blend in following substances: non-ionic additive, phosphoric acid ester, sulfuric acid ester, Sulfonates, polyether thiourea acid esters salt, sulphosuccinates class, polycarboxylic acid salt;
Described non-ionic additive is selected from any one or its any blend in following substances: nonyl phenol condensation product, polyarylphenols condensation product, castor oil, vegetable oil acid, sorbitol ester, fatty alcohol, alkylamine, polyethenoxy ether, siloxanes; Described phosphoric acid ester is selected from any one or its any blend in following substances: polyarylphenols ether phosphate, nonyl phenol ether phosphate, fatty alcohol ether phosphate, fatty alcohol phosphate.
9) step 7) described in micro-capsule suspension described in agricultural chemicals, described organic solvent, described emulsifier, described macromolecular material, described water mass ratio be 0.5 ~ 3:5 ~ 20:3 ~ 6:5 ~ 25:35 ~ 70.
Emamectin-benzoate (abbreviation emamectin benzoate) is that Merk & Co. company of the U.S. in 1984 is to 4 of Avermectin, and " result that the hydroxyl on-(-1-olive glycosyl)-1-oleandrose carries out derivatization research is the new and effective antibiotics Insecticidal and acaricidal agent of one synthesized from fermented product AVERMECTIN B1.Its object mainly improves the problem of Avermectin to lepidopteran insecticidal weak effect, the above-mentioned deficiency of Avermectin is solved as the appearance mystery of emamectin benzoate, it is to Lepidoptera, diptera, super-high-efficient, as red tape leaf roller, cigarette aphid noctuid, cotton bollworm, maduca sexta, diamond-back moth mythimna separata, beet armyworm, nonirrigated farmland are coveted noctuid, cabbage looper, cabbage looper, imported cabbageworm, cabbage heart snout moth's larva, wild cabbage horizontal stripe snout moth's larva, tomato hawkmoth, colorado potato beetle, Mexico ladybug etc. and had good preventive effect.And find that it is the highest to lepidopteran insecticidal activity in current known insecticides.
Think carrying out further investigation to emamectin benzoate, it also has good preventive effect to Meloidogyne incognita.
But emamectin benzoate is easily degraded.Be subject to the factor impacts such as acidity is too high or too low, illumination, emamectin benzoate is easy to degraded.
Ivermectin (Ivermectin) is one of structure of modification product of Avermectin, Avermectin be produced by a kind of streptomycete fermentation a kind of there is the material driving Enterozoa activity.This zymotic fluid is cruel compounds in the large ring of a class sixteen-ring, has the component that 8 structures are similar.These 8 components are Ala, Alb, A2a, Alb, Bla, B16, B2a, B2b respectively.Wherein the activity of B1 component is the highest, is widely used in agricultural and livestock breeding as insecticide active substance
Since Avermectin uses in farming and animal husbandry, important effect is played to the control of insect, evil wax.Many scientists, in order to extend the service life of Avermectin and improve biologically active and the stability of Avermectin, have carried out a large amount of structure of modification to Avermectin, have synthesized thousands of alkylation and hydrogenated derivatives.Wherein ivermectin is exactly the B1 component Wilkinson catalyst of Avermectin is carried out selective reduction 22,23 1 unsaturated bonds and obtained.Ivermectin is as the hydrogenated derivatives of Avermectin, and the content of its each composition is very similar to Avermectin, wherein containing ivermectin B1a>80%, Blb<20%.Because ivermectin has good repelling and killing efficacy to the parasite such as nematode and arthropods, be therefore worldwide widely used on livestock breeding and pet care, commercially also achieve huge success simultaneously.
Ivermectin is shown in that light easily decomposes, and very fast in degraded in soil.
Pesticide micro capsule utilizes microcapsules technology solid, liquid pesticidal isoreactivity material to be coated in cyst material and to form microcapsules exactly.Compared with conventional pesticide, because pesticide activity component is covered by airtight or semipermeable wall film, cyst wall can improve anti-rain, the light resistance of agricultural chemicals, greatly can extend the lasting period of agricultural chemicals, alleviates the degradation speed of active ingredient.
Reduce agricultural chemicals to the toxicity of people, animal and excitant simultaneously, expand the scope of application of agricultural chemicals; Both save the consumption of medicament, additionally reduce pollution.
Embodiment
Below by specific embodiment, method of the present invention is described, but the present invention is not limited thereto.
The encapsulation rate of microcapsules prepared by described embodiment is 20%-60%.Encapsulation rate method of testing is: the microcapsules getting certain mass pulverize post-drying, and gravimetry changes, and goes out encapsulation rate after obtaining maximum weight-loss ratio according to the ratiometric conversion of water and agricultural chemicals.
Experimental technique described in following embodiment, if no special instructions, is conventional method; Described reagent and material, if no special instructions, all can obtain from commercial channels.
Following embodiment is evaluated the envelop rate of gained microencapsulation of pesticide all by the following method:
Following embodiment is evaluated the sustained release performance of gained microencapsulation of pesticide all by the following method:
By microcapsules centrifugal 15min on the centrifuge of 4500r/min of preparation, abandoning supernatant, by washed with de-ionized water three times, washed with methanol without optical absorption peak, obtains microcapsules sample to 254nm place.Precisely take microcapsules sample prepared by 1.0000g, be wrapped in the bag filter that 600 object double gauzes are prepared from, add 20ml methyl alcohol, make methyl alcohol soak into bag filter completely.Be positioned in 25 DEG C of environment, get 1mL sustained-release liquid at regular intervals, after being diluted to l0mL with ethanol, measure light absorption value with high performance liquid chromatography at 245nm place.The 1mL sustained-release liquid 1mL ethanol taken out is supplied.Calculated the content of sustained-release liquid Pesticides by calibration curve, measure the cumulative release amount of microcapsules with this:
Embodiment 1, prepare 5% emamectin benzoate ivermectin micro-capsule suspension
3.000g emamectin benzoate and the former medicine of 1.000 ivermectins are dissolved in 18g toluene, add 4.5g agriculture breast 603,38.5g water.The high-shearing dispersion emulsifying machine down cut 3min being 1000r/min in speed makes emamectin benzoate ivermectin emulsifier.
Mixed with 12g formaldehyde by 4g melamine, adjust ph, to 8, adds thermal response 10 minutes in the water-bath of 65 DEG C, and after system clarification, cool to room temperature, namely obtains melamine formaldehyde resin performed polymer.
Be prepared from emamectin benzoate ivermectin emulsifier with the melamine formaldehyde resin performed polymer Hybrid Heating be prepared to 30 DEG C, the pH value of the hydrochloric acid regulation system with 25%, to 5.0, fully reacts 1.5h.
4gNH is added in above-mentioned system
4after Cl reacts 30 minutes, adjust ph is to 6.3, and fully reaction 2.5 hours, obtains emamectin benzoate ivermectin microcapsules.
The microcapsules prepared are added 2g xanthans, fully mixes, obtained 5% emamectin benzoate ivermectin micro-capsule suspension.
The envelop rate of microencapsulation of pesticide prepared by the present embodiment is 48.3%, and average grain diameter is 4 microns, and slow-release period is 14 days.
Embodiment 2, prepare 5% emamectin benzoate ivermectin micro-capsule suspension
3.000g emamectin benzoate and the former medicine of 2.000g ivermectin are dissolved in 20g dimethylbenzene, add 4.5g agriculture breast 603,36.5g water.The high-shearing dispersion emulsifying machine down cut 3min being 10000r/min in speed makes emamectin benzoate ivermectin emulsifier.
Mixed with 12g formaldehyde by 4g melamine, adjust ph, to 8, adds thermal response 10 minutes in the water-bath of 65 DEG C, and after system clarification, cool to room temperature, namely obtains melamine formaldehyde resin performed polymer.
Be prepared from emamectin benzoate ivermectin emulsifier with the melamine formaldehyde resin performed polymer Hybrid Heating be prepared to 30 DEG C, the pH value of the hydrochloric acid regulation system with 25%, to 5.0, fully reacts 1.5h.
4gNH is added in above-mentioned system
4after Cl reacts 30 minutes, adjust ph is to 6.3, and fully reaction 2.5 hours, obtains emamectin benzoate ivermectin microcapsules.
The microcapsules prepared are added 2g xanthans, fully mixes, obtained 5% emamectin benzoate ivermectin micro-capsule suspension.
The envelop rate of microencapsulation of pesticide prepared by the present embodiment is 45.9%, and average grain diameter is 6.3 microns, and slow-release period is 12 days.
Embodiment 3, prepare 5% emamectin benzoate ivermectin micro-capsule suspension
3.000g emamectin benzoate and the former medicine of 2.000g ivermectin are dissolved in 20g dimethylbenzene, add 4.5g agriculture breast 603,36.5g water.The high-shearing dispersion emulsifying machine down cut 5min being 15000r/min in speed makes emamectin benzoate ivermectin emulsifier.
Mixed with 12g formaldehyde by 4g melamine, adjust ph, to 8, adds thermal response 10 minutes in the water-bath of 65 DEG C, and after system clarification, cool to room temperature, namely obtains melamine formaldehyde resin performed polymer.
Be prepared from emamectin benzoate ivermectin emulsifier with the melamine formaldehyde resin performed polymer Hybrid Heating be prepared to 30 DEG C, the pH value of the hydrochloric acid regulation system with 25%, to 5.0, fully reacts 1.5h.
4gNH is added in above-mentioned system
4after Cl reacts 30 minutes, adjust ph is to 6.3, and fully reaction 2.5 hours, obtains emamectin benzoate ivermectin microcapsules.
The microcapsules prepared are added 2g xanthans, fully mixes, obtained 5% emamectin benzoate ivermectin micro-capsule suspension.
The envelop rate of microencapsulation of pesticide prepared by the present embodiment is 47.12%, and average grain diameter is 4.3 microns, and slow-release period is 14 days.
Embodiment 4, prepare 5% emamectin benzoate ivermectin micro-capsule suspension
3.000g emamectin benzoate and the former medicine of 2.000g ivermectin are dissolved in 20g dimethylbenzene, add 4.5g agriculture breast 603,36.5g water.The high-shearing dispersion emulsifying machine down cut 5min being 20000r/min in speed makes emamectin benzoate ivermectin emulsifier.
Mixed with 12g formaldehyde by 4g melamine, adjust ph, to 8, adds thermal response 10 minutes in the water-bath of 65 DEG C, and after system clarification, cool to room temperature, namely obtains melamine formaldehyde resin performed polymer.
Be prepared from emamectin benzoate ivermectin emulsifier with the melamine formaldehyde resin performed polymer Hybrid Heating be prepared to 30 DEG C, the pH value of the hydrochloric acid regulation system with 25%, to 5.0, fully reacts 1.5h.
4gNH is added in above-mentioned system
4after Cl reacts 30 minutes, adjust ph is to 6.3, and fully reaction 2.5 hours, obtains emamectin benzoate ivermectin microcapsules.
The microcapsules prepared are added 2g xanthans, fully mixes, obtained 5% emamectin benzoate ivermectin micro-capsule suspension.
The envelop rate of microencapsulation of pesticide prepared by the present embodiment is 42.33%, and average grain diameter is 3.5 microns, and slow-release period is 10 days.
Embodiment 5, prepare 5% emamectin benzoate ivermectin micro-capsule suspension
3.000g emamectin benzoate and the former medicine of 2.000g ivermectin are dissolved in 20g dimethylbenzene, add 4.5g agriculture breast 603,36.5g water.The high-shearing dispersion emulsifying machine down cut 5min being 20000r/min in speed makes emamectin benzoate ivermectin emulsifier.
Mixed with 12g formaldehyde by 4g melamine, adjust ph, to 8, adds thermal response 10 minutes in the water-bath of 65 DEG C, and after system clarification, cool to room temperature, namely obtains melamine formaldehyde resin performed polymer.
Be prepared from emamectin benzoate ivermectin emulsifier with the melamine formaldehyde resin performed polymer Hybrid Heating be prepared to 40 DEG C, the pH value of the hydrochloric acid regulation system with 25%, to 5.0, fully reacts 1.5h.
4gNH is added in above-mentioned system
4after Cl reacts 30 minutes, adjust ph is to 6.3, and fully reaction 2.5 hours, obtains emamectin benzoate ivermectin microcapsules.
The microcapsules prepared are added 2g xanthans, fully mixes, obtained 5% emamectin benzoate ivermectin micro-capsule suspension.
The envelop rate of microencapsulation of pesticide prepared by the present embodiment is 48.75%, and average grain diameter is 7.1 microns, and slow-release period is 15 days.
Embodiment 6, prepare 5% emamectin benzoate ivermectin micro-capsule suspension
3.000g emamectin benzoate and the former medicine of 2.000g ivermectin are dissolved in 20g dimethylbenzene, add 4.5g agriculture breast 603,36.5g water.The high-shearing dispersion emulsifying machine down cut 5min being 20000r/min in speed makes emamectin benzoate ivermectin emulsifier.
Mixed with 12g formaldehyde by 4g melamine, adjust ph, to 8, adds thermal response 10 minutes in the water-bath of 65 DEG C, and after system clarification, cool to room temperature, namely obtains melamine formaldehyde resin performed polymer.
Be prepared from emamectin benzoate ivermectin emulsifier with the melamine formaldehyde resin performed polymer Hybrid Heating be prepared to 50 DEG C, the pH value of the hydrochloric acid regulation system with 25%, to 5.0, fully reacts 1.5h.
4gNH is added in above-mentioned system
4after Cl reacts 30 minutes, adjust ph is to 6.3, and fully reaction 2.5 hours, obtains emamectin benzoate ivermectin microcapsules.
The microcapsules prepared are added 2g xanthans, fully mixes, obtained 5% emamectin benzoate ivermectin micro-capsule suspension.
The envelop rate of microencapsulation of pesticide prepared by the present embodiment is 49.12%, and average grain diameter is 7.6 microns, and slow-release period is 15 days.
Embodiment 7, prepare 5% emamectin benzoate ivermectin micro-capsule suspension
3.000g emamectin benzoate and the former medicine of 2.000g ivermectin are dissolved in 20g dimethylbenzene, add 4.5g agriculture breast 603,36.5g water.The high-shearing dispersion emulsifying machine down cut 5min being 20000r/min in speed makes emamectin benzoate ivermectin emulsifier.
Mixed with 12g formaldehyde by 4g melamine, adjust ph, to 8, adds thermal response 10 minutes in the water-bath of 65 DEG C, and after system clarification, cool to room temperature, namely obtains melamine formaldehyde resin performed polymer.
Be prepared from emamectin benzoate ivermectin emulsifier with the melamine formaldehyde resin performed polymer Hybrid Heating be prepared to 30 DEG C, the pH value of the phosphoric acid regulation system with 45%, to 5.0, fully reacts 1.5h.
4gNH is added in above-mentioned system
4after Cl reacts 30 minutes, adjust ph is to 6.3, and fully reaction 2.5 hours, obtains emamectin benzoate ivermectin microcapsules.
The microcapsules prepared are added 2g xanthans, fully mixes, obtained 5% emamectin benzoate ivermectin micro-capsule suspension.
The envelop rate of microencapsulation of pesticide prepared by the present embodiment is 57.93%, and average grain diameter is 5.3 microns, and slow-release period is 13 days.
Embodiment 8, prepare 5% emamectin benzoate ivermectin micro-capsule suspension
3.000g emamectin benzoate and the former medicine of 2.000g ivermectin are dissolved in 20g dimethylbenzene, add 4.5g agriculture breast 603,36.5g water.The high-shearing dispersion emulsifying machine down cut 5min being 20000r/min in speed makes emamectin benzoate ivermectin emulsifier.
Mixed with 12g formaldehyde by 4g melamine, adjust ph, to 8, adds thermal response 10 minutes in the water-bath of 65 DEG C, and after system clarification, cool to room temperature, namely obtains melamine formaldehyde resin performed polymer.
Be prepared from emamectin benzoate ivermectin emulsifier with the melamine formaldehyde resin performed polymer Hybrid Heating be prepared to 30 DEG C, the pH value of the hydrochloric acid regulation system with 25%, to 4.0, fully reacts 1.5h.
4gNH is added in above-mentioned system
4after Cl reacts 30 minutes, adjust ph is to 6.3, and fully reaction 2.5 hours, obtains emamectin benzoate ivermectin microcapsules.
The microcapsules prepared are added 2g xanthans, fully mixes, obtained 5% emamectin benzoate ivermectin micro-capsule suspension.
The envelop rate of microencapsulation of pesticide prepared by the present embodiment is 35.49%, and average grain diameter is 5.8 microns, and slow-release period is 9 days.
Embodiment 9, prepare 5% emamectin benzoate ivermectin micro-capsule suspension
3.000g emamectin benzoate and the former medicine of 2.000g ivermectin are dissolved in 20g dimethylbenzene, add 4.5g agriculture breast 603,36.5g water.The high-shearing dispersion emulsifying machine down cut 5min being 20000r/min in speed makes emamectin benzoate ivermectin emulsifier.
Mixed with 12g formaldehyde by 4g melamine, adjust ph, to 8, adds thermal response 10 minutes in the water-bath of 65 DEG C, and after system clarification, cool to room temperature, namely obtains melamine formaldehyde resin performed polymer.
Be prepared from emamectin benzoate ivermectin emulsifier with the melamine formaldehyde resin performed polymer Hybrid Heating be prepared to 30 DEG C, the pH value of the hydrochloric acid regulation system with 25%, to 3.0, fully reacts 1.5h.
4gNH is added in above-mentioned system
4after Cl reacts 30 minutes, adjust ph is to 6.3, and fully reaction 2.5 hours, obtains emamectin benzoate ivermectin microcapsules.
The microcapsules prepared are added 2g xanthans, fully mixes, obtained 5% emamectin benzoate ivermectin micro-capsule suspension.
The envelop rate of microencapsulation of pesticide prepared by the present embodiment is 23.31%, and average grain diameter is 6.7 microns, and slow-release period is 7 days.
Embodiment 10, prepare 5% emamectin benzoate ivermectin micro-capsule suspension
3.000g emamectin benzoate and the former medicine of 2.000g ivermectin are dissolved in 20g dimethylbenzene, add 4.5g agriculture breast 603,36.5g water.The high-shearing dispersion emulsifying machine down cut 5min being 20000r/min in speed makes emamectin benzoate ivermectin emulsifier.
Mixed with 12g formaldehyde by 4g melamine, adjust ph, to 8, adds thermal response 10 minutes in the water-bath of 65 DEG C, and after system clarification, cool to room temperature, namely obtains melamine formaldehyde resin performed polymer.
Be prepared from emamectin benzoate ivermectin emulsifier with the melamine formaldehyde resin performed polymer Hybrid Heating be prepared to 30 DEG C, the pH value of the hydrochloric acid regulation system with 25%, to 5.0, fully reacts 1.5h.
4gNH is added in above-mentioned system
4after Cl reacts 30 minutes, adjust ph is to 6.3, and fully reaction 2.5 hours, obtains emamectin benzoate ivermectin microcapsules.
The microcapsules prepared are added 2g xanthans, fully mixes, obtained 5% emamectin benzoate ivermectin micro-capsule suspension.
The envelop rate of microencapsulation of pesticide prepared by the present embodiment is 23.31%, and average grain diameter is 6.7 microns, and slow-release period is 7 days.
Embodiment 11, prepare 5% emamectin benzoate ivermectin micro-capsule suspension
3.000g emamectin benzoate and the former medicine of 2.000g ivermectin are dissolved in 20g dimethylbenzene, add 4.0g agriculture breast 0203B, 37.00g water.The high-shearing dispersion emulsifying machine down cut 5min being 20000r/min in speed makes emamectin benzoate ivermectin emulsifier.
Mixed with 12g formaldehyde by 4g melamine, adjust ph, to 8, adds thermal response 10 minutes in the water-bath of 65 DEG C, and after system clarification, cool to room temperature, namely obtains melamine formaldehyde resin performed polymer.
Be prepared from emamectin benzoate ivermectin emulsifier with the melamine formaldehyde resin performed polymer Hybrid Heating be prepared to 30 DEG C, the pH value of the hydrochloric acid regulation system with 25%, to 5.0, fully reacts 1.5h.
4gNH is added in above-mentioned system
4after Cl reacts 30 minutes, adjust ph is to 6.3, and fully reaction 2.5 hours, obtains emamectin benzoate ivermectin microcapsules.
The microcapsules prepared are added 2g xanthans, fully mixes, obtained 5% emamectin benzoate ivermectin micro-capsule suspension.
The envelop rate of microencapsulation of pesticide prepared by the present embodiment is 39.66%, and average grain diameter is 3.2 microns, and slow-release period is 8 days.
Embodiment 12, prepare 5% emamectin benzoate ivermectin micro-capsule suspension
3.000g emamectin benzoate and the former medicine of 2.000g ivermectin are dissolved in 20g dimethylbenzene, add 3.5g agriculture breast 0203B, 0.5g agriculture breast 500#, 37.00g water.The high-shearing dispersion emulsifying machine down cut 5min being 20000r/min in speed makes emamectin benzoate ivermectin emulsifier.
Mixed with 12g formaldehyde by 4g melamine, adjust ph, to 8, adds thermal response 10 minutes in the water-bath of 65 DEG C, and after system clarification, cool to room temperature, namely obtains melamine formaldehyde resin performed polymer.
Be prepared from emamectin benzoate ivermectin emulsifier with the melamine formaldehyde resin performed polymer Hybrid Heating be prepared to 30 DEG C, the pH value of the hydrochloric acid regulation system with 25%, to 5.0, fully reacts 1.5h.
4gNH is added in above-mentioned system
4after Cl reacts 30 minutes, adjust ph is to 6.3, and fully reaction 2.5 hours, obtains emamectin benzoate ivermectin microcapsules.
The microcapsules prepared are added 2g xanthans, fully mixes, obtained 5% emamectin benzoate ivermectin micro-capsule suspension.
The envelop rate of microencapsulation of pesticide prepared by the present embodiment is 41.00%, and average grain diameter is 3.5 microns, and slow-release period is 10 days.
5.0% ivermectin emamectin-benzoate microcapsules medicament field efficacy: test site is that test soil is red soil in banana nursery, Xin Xu town, Nanning, nematode worm amount is large and even, before dispenser, investigate root-knot nematode second instar larvae insect population is 400/100g soil, ensure to infect, 4 concentration established by medicament: 10g/ mu, 20g/ mu, 40g/ mu, 80g/ mu, lythidathion field recommended dose 2g/ mu, separately establishes CK blank, amount to 6 process, often process 5 repetitions.Each process randomized arrangement, rich water quality management is consistent.Before field planting, the medicament be prepared from evenly is sprayed in preprepared sick soil, stirs, field planting of transplanting seedlings, normal field management.After dispenser, 45d investigates soil nematodes density, is separated root-knot nematode 2 instar larvae in soil sample by the graceful funnel method of shellfish and counts.45d after dispenser, slowly take out plant root and clean, record incidence, calculates disease index, relative control effect.
5.0% ivermectin emamectin-benzoate micro-capsule suspension refers to table 1 to Meloidogyne incognita control efficiency result of the test.
Table 15.0% ivermectin emamectin-benzoate micro-capsule suspension amount of application is prevented and treated Meloidogyne incognita second instar larvae
The impact of effect, root knot index and index of reproduction
As can be seen from Table 1,45d after medicine, 5 kinds of process are all good to Meloidogyne incognita second instar larvae preventive effect, preventive effect the best for formulation rate be 80g/ mu, reach 98.49%, secondly for formulation rate is 40g/ mu, 20g/ mu, 10g/ mu and lythidathion, its preventive effect is respectively 96.08%, 94.77%, 93.93%, 83.11%.Meanwhile, 5.0% ivermectin emamectin-benzoate micro-capsule suspension has good root knot control efficiency to Meloidogyne incognita disease, preventive effect the best for formulation rate be 80g/ mu, reach 99.70%, secondly for formulation rate is 40g/ mu, 20g/ mu, 10g/ mu and lythidathion, its preventive effect is respectively 95.12%, 84.38%, 82.03%.; From index of reproduction and root knot index, four kinds of formulation rates of microcapsules all significantly can suppress the root knot of Meloidogyne incognita and the formation of pieces of an egg, its index of reproduction is only respectively: 0.30,0.10,0.09,0.00, this shows that 5.0% ivermectin emamectin-benzoate micro-capsule suspension can control the Population of Meloidogyne incognita effectively, thus reaches the object controlling Meloidogyne incognita disease.
The aforementioned description to concrete exemplary of the present invention is to illustrate and the object of illustration.These descriptions not want the present invention to be defined as disclosed precise forms, and obviously, according to above-mentioned instruction, can much change and change.The object selected exemplary embodiment and describe is to explain certain principles of the present invention and practical application thereof, thus those skilled in the art can be realized and utilize various different exemplary of the present invention and various different selection and change.Scope of the present invention is intended to limited by claims and equivalents thereof.
Claims (10)
1. one kind contains the preparation method of ivermectin and the composite micro-capsule suspension of emamectin-benzoate, it is characterized in that: described microcapsules with the ivermectin of the emamectin-benzoate of 15-25 % by weight and 75-85 % by weight for activated feedstock, first be dissolved in organic solvent, and add emulsifying dispersant, in the shear action down cut emulsification of high-shearing dispersion emulsifying machine, be prepared into emulsion, add melamine formaldehyde resin performed polymer, add polymerizer, the pH value of regulation system is to suitable scope, constant temperature is polymerized, be prepared into microcapsules, add emulsifying dispersant and high-speed stirred, make stable micro-capsule suspension.
2. according to the preparation method of the ivermectin described in claim 1 and the composite micro-capsule suspension of emamectin-benzoate, it is characterized in that: described melamine formaldehyde resin performed polymer is that melamine mixes with the ratio of formaldehyde in 0.5-5:2-7, between adjust ph to 7-10, constant temperature 60-90 DEG C of reaction, obtained melamine formaldehyde resin performed polymer.
3. according to the preparation method of the ivermectin described in claim 1 and the composite micro-capsule suspension of emamectin-benzoate, it is characterized in that: the amount ratio of described ivermectin and Methylaminoemamectin benzoate, described organic solvent, described emulsifier, described melamine formaldehyde resin, described water is 0.5 ~ 6:5 ~ 20:3 ~ 6:5 ~ 25:35 ~ 70.
4. according to the preparation method of the ivermectin described in claim 1 and the composite micro-capsule suspension of emamectin-benzoate, it is characterized in that, described organic solvent, is selected from any class in following substances or its any blend: arene, vegetable oil or improved plant oils, mineral oils, synthesis organic solvent class.
5. the preparation method of ivermectin according to claim 3 and the composite micro-capsule suspension of emamectin-benzoate, is characterized in that: described arene is selected from any one or its any blend in following substances: toluene, dimethylbenzene, trimethylbenzene; Described vegetable oil or improved plant oils are selected from any one or its blend in following substances: soybean oil, turpentine oil, fatty acid methyl ester; Described mineral oils is selected from any one or its blend in following substances: white oil, deodorized kerosine; Described synthesis organic solvent class is selected from any one or its blend in following substances: dimethyl carbonate, 2-butyl acetate, long chain class.
6. according to the preparation method of the micro-capsule suspension described in claim 1, it is characterized in that: described emulsifying dispersant is selected from any one or its any blend in following substances: non-ionic additive, phosphoric acid ester, sulfuric acid ester, Sulfonates, polyether thiourea acid esters salt, sulphosuccinates class, polycarboxylic acid salt.
7. according to the preparation method of the micro-capsule suspension described in claim 5, it is characterized in that: described non-ionic additive is selected from any one or its any blend in following substances: nonyl phenol condensation product, polyarylphenols condensation product, castor oil, vegetable oil acid, sorbitol ester, fatty alcohol, alkylamine, polyethenoxy ether, siloxanes; Described phosphoric acid ester is selected from any one or its any blend in following substances: polyarylphenols ether phosphate, nonyl phenol ether phosphate, fatty alcohol ether phosphate, fatty alcohol phosphate.
8. according to the preparation method of the micro-capsule suspension described in claim 1, it is characterized in that: the shearing of described high-shearing dispersion emulsifying machine, shear time is 3-8 minute, and shear rate is 8000-15000 rev/min.
9. according to the preparation method of the micro-capsule suspension described in claim 1, it is characterized in that: described polymerizer is the one of hydrochloric acid, phosphoric acid or oxalic acid.
10. according to the preparation method of the micro-capsule suspension described in claim 1, it is characterized in that: the suitable scope of the pH value of institute's regulation system is 3-6; The temperature of described constant temperature polymerization controls between 25-50 DEG C; Described interpolation emulsifying dispersant the stir speed (S.S.) of high-speed stirred is 600-1500 rev/min, mixing time is 1-3 hour.
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| CN104521949A (en) * | 2014-12-15 | 2015-04-22 | 广西大学 | Microcapsule suspension agent |
| CN105028023A (en) * | 2015-07-24 | 2015-11-11 | 广西大学 | Seedling cultivation substrate for preventing meloidogyne incognita chitwood of bananas |
| CN105732199A (en) * | 2016-02-15 | 2016-07-06 | 中国农业大学 | Insecticide microcapsule suspension type liquid medicine fertilizer and preparation method and application thereof |
| CN106277902A (en) * | 2016-08-17 | 2017-01-04 | 常熟理工学院 | A kind of preparation method of time controlled released type cement mortar coagulant microcapsule |
| CN106561643A (en) * | 2016-10-25 | 2017-04-19 | 北京明德立达农业科技有限公司 | Microcapsule suspension-suspending agent containing bifenazate and abamectin and preparation method of microcapsule suspension-suspending agent |
| CN108432751A (en) * | 2018-03-27 | 2018-08-24 | 江苏邦盛生物科技有限责任公司 | A kind of pesticide microcapsule suspending agent and its preparation method and application |
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