CN102939970A - Microcapsule suspending agent containing spinosad and cyantraniliprole, and preparation method thereof - Google Patents

Microcapsule suspending agent containing spinosad and cyantraniliprole, and preparation method thereof Download PDF

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Publication number
CN102939970A
CN102939970A CN2012103972754A CN201210397275A CN102939970A CN 102939970 A CN102939970 A CN 102939970A CN 2012103972754 A CN2012103972754 A CN 2012103972754A CN 201210397275 A CN201210397275 A CN 201210397275A CN 102939970 A CN102939970 A CN 102939970A
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China
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suspending agent
microcapsule suspending
insect amide
cyanogen insect
multiple killing
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CN2012103972754A
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Chinese (zh)
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司贤良
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上海沪联生物药业(夏邑)股份有限公司
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Priority to CN2012103972754A priority Critical patent/CN102939970A/en
Publication of CN102939970A publication Critical patent/CN102939970A/en

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Abstract

The invention relates to a microcapsule suspending agent containing spinosad and cyantraniliprole, and a preparation method thereof. The microcapsule suspending agent is mainly composed of spinosad, cyantraniliprole, a capsule wall material, a water-soluble monomer, a dispersing agent, a protective agent, a capsule heart solvent and water. The recovery rate of the obtained microcapsule suspending agent is over 98%; embedding efficiency is higher than 95%; the microcapsules is regular spheres; the particle size is 0.5-5 [mu]m; and the appearance is similar to that of a conventional pesticide suspending agent. The microcapsule suspending agent can be directly mixed with water to carry out spraying. Indoor and field experiments show that the microcapsule suspending agent containing spinosad and cyantraniliprole has very good preventing and treating effects for white flies and thrips on cucumber, paddy rice, cotton and hairy melons, compared with missible oil and a suspending agent; lasting period is significantly prolonged; and the cost is lower than that of missible oil and other preparations. Besides, the microcapsule suspending agent containing employs water as a dispersing medium, has low usage amount of an organic solvent, is safe in storage transportation and use, and reduces pollutions to the environment.

Description

Contain microcapsule suspending agent of multiple killing teichomycin and cyanogen insect amide and preparation method thereof

Technical field

The invention belongs to technical field of compounded pesticide, be specifically related to a kind of microcapsule suspending agent that contains multiple killing teichomycin and cyanogen insect amide and preparation method thereof.

Background technology

Multiple killing teichomycin (Spinosad), molecular formula: C 41H 65NO 10(spinosyn A)+C 42H 67NO 10(spinosyn D).Structural formula:

Multiple killing teichomycin is considered to the acting body of nicotinic acid acetylcholinergic receptor, can sustained activation target insect acetylcholine nicotine receptor, but its binding site is different from nicotine and Imidacloprid.Insect is benumbed rapidly, and paralysis causes death at last.Its desinsection speed can compare favourably with chemical pesticide.Safe, and with present common insecticide be the biological insecticides of low toxicity, efficient, low-residual without cross resistance, existing efficient insecticidal properties has again the characteristic of beneficial insect and mammalian safe is arranged, the most suitable pollution-free vegetable, Production of fruit is used.It is the insecticide of a kind of low toxicity, efficient, wide spectrum.

The mechanism of action: insect had tag fast and stomach poison function, blade is had stronger osmosis, can kill subepidermal insect, the longevity of residure is longer, and some insects are had certain ovicidal action.Without systemic action.Can effectively preventing Lepidoptera, diptera and thrips insect, can prevent and treat well also that some takes food the pest species of blade in a large number in coleoptera and the orthoptera, relatively poor to the control efficiency of sucking pest and mite class.Safer to predatory natural enemy insect, unique because of insecticidal action mechanism, not yet find at present to have mutual drug-fast report with other insecticides.Safe without poisoning to plant.Be suitable for using on vegetables, fruit tree, gardening, the crops.Insecticidal effect be subjected to rain affect less.

Cyanogen insect amide (Cyantraniliprole), molecular formula C 19H 14BrClN 6O 2, chemical name: 3-bromo-1-(3-chloro-2-pyridyl)-N-[4-cyano group-2-methyl-6-[(methylamino) hydroxyl] and phenyl]-1H-pyrazoles-5-formamide.Structural formula:

Cyanogen insect amide is second generation fish fourth acceptor inhibitor insecticides, and permeability, conductivity, chemical stability, high insecticidal activity except having Rynaxypyr also have the activity of very strong interior suction in addition, and desinsection is more thorough.This product is compared with Rynaxypyr, uses crop more extensive, and desinsection is wider, and thrips and flea beetle are also had efficient control efficiency.Simultaneously aphid and downy mildew also there is certain control efficiency.

The mechanism of action: cyanogen insect amide can efficiently activate the insect ryanodine receptor, and excessively the calcium ion in the calcium storehouse in the release cells causes the insect paralysis dead.The insects such as Lepidoptera, Semiptera and coleoptera are had higher activity, and insecticidal spectrum is wide, and lasting effect is good.Second day just can be seen the sign of insect death, reaches the highest lethality rate after three days, and the lasting period can reach 30 days, real quick-acting holding effects.Controlling object: diamond-back moth, prodenia litura, tomato moth, cotton bollworm, cotten aphid, aphid, thrips, flea beetle, plant hopper, blind Chinese toon silk worm, striped rice borer, paddy stem borer, rice leaf roller, heart-eating worm etc.In addition, downy mildew also there is good control efficiency.

Often there is defective in various degree in the insecticide variety of single-activity component on agricultural insect pests control: use is easily developed immunity to drugs continuously, and insecticidal spectrum is wide not, and environment is caused larger pollution, can not provide comprehensive protection etc. for crop.Can overcome to a certain extent above shortcoming by being mixed of two or more active component.Two or more active component that can produce synergistic effect is mixed, and can improve preventive effect, reduces the consumption of active ingredient, saves cost, delays the generation of pest resistance to insecticide, and reduces the pollution to environment.Prior art discloses multiple killing teichomycin and the composite technical scheme of cyanogen insect amide, a kind of Pesticidal combination is disclosed such as China application CN102308805A, this Pesticidal combination contains multiple killing teichomycin and two kinds of active components of cyanogen insect amide, wherein cyanogen insect amide 1 ~ 40%, multiple killing teichomycin 1 ~ 30%, described Pesticidal combination are suspending agent and water dispersant.But find in the practical application, the disclosed composite suspending agent of this application has the poor shortcoming of physical stability, because the disclosed suspending agent of this application belongs to common suspending agent, it is a kind of coarse dispersion system of thermodynamic instability, preparation of traditional Chinese medicine microparticulate degree is large, make the active ingredient particulate have higher surface free energy and play pendulum, be an impediment to the performance of drug effect; In addition, the active ingredient particulate is generally between 0.5~10 μ m in the disclosed suspending agent of this application, little person can be 0.1 μ m, large person can reach 50 μ m or larger, because it is that form with solia particle exists that this formulation is sprayed at after the crop surface, so the disclosed composite suspending agent of this application is faced with the significant deficiency that active ingredient easily runs off and is difficult for adhering to.In view of this, the present invention proposes the microcapsule suspending agent that a kind of insecticidal effect more preferably contains multiple killing teichomycin and cyanogen insect amide, by selecting unique auxiliary agent and optimizing the preparation method, prepared microcapsule suspending agent has overcome the above-mentioned openly shortcoming of suspending agent fully, because after former medicinal organic solvent dissolves, in carrier, formed oil-in-water emulsion form structure, after being sprayed onto crop surface, active ingredient in the microcapsules slowly discharges, can be fully absorbed by crops, and greatly prolonged the lasting period, reduced operating personnel's contact toxicity, active ingredient and water and the isolation of alkaline agricultural chemicals, with alkaline combined use of pesticides, its stability is unaffected, reduces comprehensive medication number of times and dosage, saving of work and time is worthy of popularization in the agricultural production very much.

Summary of the invention

The first purpose of the present invention is to provide a kind of microcapsule suspending agent that contains multiple killing teichomycin and cyanogen insect amide.

For realizing the first purpose, the present invention adopts following technical scheme:

A kind of microcapsule suspending agent that contains multiple killing teichomycin and cyanogen insect amide; take multiple killing teichomycin and cyanogen insect amide as the capsule heart; described microcapsule suspending agent is comprised of the component of following percentage by weight: multiple killing teichomycin 1~25%; cyanogen insect amide 2~50%, cyst material 0.5~7%, water-soluble monomer 0.5~1%; dispersant 2~5%; protectant 0.5~1%, capsule heart solvent 1~20%, surplus is water.

Further; the preferred described microcapsule suspending agent of the present invention is comprised of the component of following percentage by weight: multiple killing teichomycin 10~15%; cyanogen insect amide 20~35%; cyst material 3~5%; water-soluble monomer 0.6~0.8%, dispersant 3~4%, protectant 0.6~0.8%; capsule heart solvent 5~15%, surplus are water.

Among the present invention, the described microcapsule suspending agent that contains multiple killing teichomycin and cyanogen insect amide can claim again multiple killing teichomycin cyanogen insect amide microcapsule suspending agent.

Cyst material of the present invention is one or more in many many methyl of phenyl polyisocyanates, alkylene diisocyanate, isopropyl myristate, urea, the formaldehyde, preferred many many methyl of phenyl polyisocyanates, urea, formaldehyde.

Water-soluble monomer of the present invention is one or more in deionized water, hydrochloric acid, butanediol, ethohexadiol, glycerine, ethylenediamine, triethylene tetramine, TEPA, the triethanolamine, preferred deionized water, hydrochloric acid, butanediol.

Dispersant of the present invention be in sodium lignin sulfonate, polyoxyethylene polyoxypropylene block copolymer, polyvinyl alcohol, the polyethylene arsenic pyrrolidone any or several, preferred sodium lignin sulfonate, polyethylene arsenic pyrrolidone.

Protectant of the present invention is one or more in gelatin, gum Arabic, polyvinyl alcohol, the polyvinylpyrrolidone, preferred gelatin, gum Arabic, polyvinyl alcohol.

Polyvinyl alcohol not only can be used as dispersant but also can be used as protectant among the present invention, and for obtaining better microcapsule suspending agent, preferred dispersants and protectant are not polyvinyl alcohol simultaneously.

Capsule heart solvent of the present invention is one or more in toluene, dimethylbenzene, ethanol, DMF, cyclohexanone, the acetone, preferred toluene, dimethylbenzene, DMF.

As a kind of preferred forms of the present invention; described microcapsule suspending agent is comprised of the component of following percentage by weight: multiple killing teichomycin 1 ~ 20%; cyanogen insect amide 2 ~ 40%; many methyl of the many phenyl of cyst material polyisocyanates 1 ~ 5%, water-soluble monomer butanediol 0.6 ~ 0.8%, dispersant sodium lignin sulfonate 3 ~ 4%; protectant polyvinyl alcohol 0.6 ~ 0.8%; capsule heart solvent DMF 5 ~ 15%, surplus is water.

The preparation method of the multiple killing teichomycin that the second purpose of the present invention is to provide above-mentioned and the microcapsule suspending agent of cyanogen insect amide, described preparation method is as follows:

In cyst material, add pH adjusting agent pH is transferred to 8 ~ 9, be heated to 60 ~ 80 ℃, the lower reaction of insulation 0.5 ~ 2h, then being diluted with water to the stable cyst material mass percent that contains is 1 ~ 35% the performed polymer aqueous solution; Multiple killing teichomycin and cyanogen insect amide are dissolved in capsule heart solvent; add while stirring dispersant, protectant and above-mentioned cyst material prepolymer solution; speed high-speed stirred 0.5 ~ 1.5h with 1000 ~ 1500 rev/mins; rear reduction rotating speed to 500 ~ 700 rev/mins; add hydrochloric acid solution and regulate pH to 1 ~ 5; polymerisation 1.5 ~ 2.5h adds water-soluble monomer and water again, stirs and namely gets the microcapsule suspending agent that contains multiple killing teichomycin and cyanogen insect amide.

Wherein, preferably add pH adjusting agent in cyst material pH is transferred to 8.5, be heated to 70 ℃, then the lower reaction 1h of insulation is diluted with water to the stable performed polymer aqueous solution that the cyst material mass percent is 1-35% that contains; Multiple killing teichomycin and cyanogen insect amide are dissolved in capsule heart solvent; add while stirring dispersant, protectant and above-mentioned cyst material prepolymer solution; speed high-speed stirred 1h with 1200 rev/mins; rear reduction rotating speed to 600 rev/min; add hydrochloric acid solution and regulate pH to 2.5; polymerisation 2h adds water-soluble monomer and water again, stirs namely to get to contain multiple killing teichomycin and cyanogen insect amide microcapsule suspending agent.

Wherein, described pH adjusting agent can be selected the disclosed various reagent of the present invention that can be used for of prior art, the preferred triethanolamine of the present invention.

Above-mentioned preparation method is scientific and reasonable, and prepared multiple killing teichomycin cyanogen insect amide microcapsule suspending agent has unexpected slow release effect.

The multiple killing teichomycin cyanogen insect amide microcapsule suspending agent of gained of the present invention, the rate of recovery reaches more than 98%, and encapsulation ratio reaches more than 95%, and micro-capsule is regular spherical, and particle diameter is between 0.5~5 μ m, and outward appearance is similar to common agricultural chemicals suspension agent, can directly be watered spraying and use.

Multiple killing teichomycin cyanogen insect amide microcapsule suspending agent of the present invention proves through indoor and drug effect test of field zone, for missible oil and suspending agent, multiple killing teichomycin cyanogen insect amide microcapsule suspending agent has good control efficiency to insects such as crop Lepidoptera, diptera and thrips such as vegetables, cotton, paddy rice, the toxic effect no significant difference, but the lasting period obviously prolongs, and cost is lower than other preparations such as present missible oil.

Multiple killing teichomycin cyanogen insect amide microcapsule suspending agent of the present invention has the following advantages:

1. take multiple killing teichomycin and cyanogen insect amide as capsule-core, by the high molecular polymer packing, form slowly-releasing and Controlled release formulation, can satisfy the basic demand of different target chemical controls.

2. because active ingredient is wrapped in the cyst material, preparation toxicity is reduced, reduced the toxicity to beneficial organisms such as honeybee and silkworms.

3. take water as dispersion medium, consumption of organic solvent is low, and storing and use safety have alleviated the pollution to environment.

Description of drawings

Fig. 1 is the release profiles of two kinds of microcapsule suspending agent 1-5d in the test example 2;

Fig. 2 is the release profiles of two kinds of microcapsule suspending agent 5-44d in the test example 2.

Embodiment

In order to understand better the present invention, below the invention will be further described.But the scope of protection of present invention is not limited to the scope that embodiment represents.The following stated only is preferably embodiment of the present invention, only is used for explaining the present invention, can not therefore be interpreted as the restriction to claim of the present invention.

Embodiment 1:2.5% multiple killing teichomycin cyanogen insect amide microcapsule suspending agent

In the there-necked flask that thermometer, agitating device are housed, add urea, formaldehyde, urea: formaldehyde=1:1.5(mol ratio), regulate pH=8 with triethanolamine, be warming up to 70 ℃, stirring at low speed reaction 1h, then being diluted with water to the stable cyst material mass percent that contains is 10% the performed polymer aqueous solution.At normal temperatures the former medicine 1.0g of multiple killing teichomycin and the former medicine 1.5g of cyanogen insect amide are dissolved in 2.5gN, in the dinethylformamide, add while stirring 3g sodium lignin sulfonate, 1g gum Arabic and the above-mentioned urea-formaldehyde performed polymer of the 50g aqueous solution (containing cyst material 5g), speed high-speed stirred 1h with 1200 rev/mins, reduce rotating speed to 600 rev/min after the stable emulsion to be formed, add hydrochloric acid solution and regulate pH value to 2.5, polymerisation 2h, add again 1g butanediol and 40g water, stir and namely make 2.5% multiple killing teichomycin cyanogen insect amide microcapsule suspending agent.

Embodiment 2:5% multiple killing teichomycin cyanogen insect amide microcapsule suspending agent

Method with identical with embodiment 1 makes urea-formaldehyde prepolymer aqueous solution.At normal temperatures, the former medicine 1.6g of multiple killing teichomycin and the former medicine 3.4g of cyanogen insect amide are dissolved in the 2g cyclohexanone, add while stirring 1g gelatin, 2g polyoxyethylene polyoxypropylene block copolymer and the above-mentioned urea-formaldehyde performed polymer of the 49g aqueous solution (containing cyst material 5.6g), speed high-speed stirred 1h with 1200 rev/mins, reduce rotating speed to 600 rev/min after the stable emulsion to be formed, add hydrochloric acid solution and regulate pH value to 2.5, polymerisation 2h, add again 1g hydrochloric acid and 40g water, stir and namely make 5% multiple killing teichomycin cyanogen insect amide microcapsule suspending agent.

Embodiment 3:10% multiple killing teichomycin cyanogen insect amide microcapsule suspending agent

Method with identical with embodiment 1 makes urea-formaldehyde prepolymer aqueous solution.At normal temperatures, the former medicine 5g of multiple killing teichomycin and the former medicine 5g of cyanogen insect amide are dissolved in the mixed liquor of 5g dimethylbenzene and 5g cyclohexanone, add while stirring 0.5g polyvinyl alcohol, 3.5g sodium lignin sulfonate and the above-mentioned urea-formaldehyde performed polymer of the 40g aqueous solution (containing cyst material 3g), speed high-speed stirred 1h with 1200 rev/mins, reduce rotating speed to 600 rev/min after the stable emulsion to be formed, add hydrochloric acid solution and regulate pH value to 2.5, polymerisation 2h, add again 1g triethanolamine and 35g water, stir and namely make 10% multiple killing teichomycin cyanogen insect amide microcapsule suspending agent.

Embodiment 4:15% multiple killing teichomycin cyanogen insect amide microcapsule suspending agent

Method with identical with embodiment 1 makes urea-formaldehyde prepolymer aqueous solution.At normal temperatures, the former medicine 5g of multiple killing teichomycin and the former medicine 10g of cyanogen insect amide are dissolved in 10g dimethylbenzene and 2g N, in the mixed liquor of dinethylformamide, add while stirring the above-mentioned performed polymer aqueous solution of 1g polyvinylpyrrolidone, 5g sodium lignin sulfonate and 40g (containing cyst material 5g), speed high-speed stirred 1h with 1200 rev/mins, reduce rotating speed to 600 rev/min after the stable emulsion to be formed, add hydrochloric acid solution and regulate pH value to 2.5, polymerisation 2h, add again 2g butanediol and 25g water, stir and namely make 15% multiple killing teichomycin cyanogen insect amide microcapsule suspending agent.

Embodiment 5:20% multiple killing teichomycin cyanogen insect amide microcapsule suspending agent

Method with identical with embodiment 1 makes urea-formaldehyde prepolymer aqueous solution.At normal temperatures, the former medicine 7g of multiple killing teichomycin and the former medicine 13g of cyanogen insect amide are dissolved in 10g dimethylbenzene and 5g N, in the mixed liquor of dinethylformamide, add while stirring the above-mentioned performed polymer aqueous solution of 0.5g gum Arabic, 5g sodium lignin sulfonate and 34.5g (containing cyst material 2.5g), speed high-speed stirred 1h with 1500 rev/mins, reduce rotating speed to 500 rev/min after the stable emulsion to be formed, add hydrochloric acid solution and regulate pH value to 2.5, polymerisation 2h, add again 1g ethohexadiol and 24g water, stir and namely make 20% multiple killing teichomycin cyanogen insect amide microcapsule suspending agent.

Embodiment 6:25% multiple killing teichomycin cyanogen insect amide microcapsule suspending agent

With the method identical with embodiment 1, make many many methyl of phenyl polyisocyanates-isopropyl myristates (the two mole dosage is than being 1:1.2) performed polymer aqueous solution.At normal temperatures, the former medicine 8.3g of multiple killing teichomycin and the former medicine 16.7g of cyanogen insect amide are dissolved in 10g dimethylbenzene and 10gN, in the mixed liquor of dinethylformamide, add while stirring the 0.6g gum Arabic, the above-mentioned performed polymer aqueous solution of 4g sodium lignin sulfonate and 25.4g (containing cyst material 0.5g), speed high-speed stirred 1h with 1000 rev/mins, reduce rotating speed to 700 rev/min after the stable emulsion to be formed, add hydrochloric acid solution and regulate pH value to 2.5, polymerisation 2h, add again 1g glycerine and 24g water, stir and namely make 25% multiple killing teichomycin cyanogen insect amide microcapsule suspending agent.

Embodiment 7:30% multiple killing teichomycin cyanogen insect amide microcapsule suspending agent

Method with identical with embodiment 1 makes urea-formaldehyde prepolymer aqueous solution.At normal temperatures, the former medicine 10g of multiple killing teichomycin and the former medicine 20g of cyanogen insect amide are dissolved in the mixed liquor of 10g toluene and 10g acetone, add while stirring the above-mentioned performed polymer aqueous solution of 3g sodium lignin sulfonate, 0.8g gelatin and 25.2g (containing cyst material 1g), speed high-speed stirred 1h with 1200 rev/mins, reduce rotating speed to 600 rev/min after the stable emulsion to be formed, add hydrochloric acid solution and regulate pH value to 2.5, polymerisation 2h, add again 1g ethylenediamine and 20g water, stir and namely make 40% multiple killing teichomycin cyanogen insect amide microcapsule suspending agent.

Embodiment 8:40% multiple killing teichomycin cyanogen insect amide microcapsule suspending agent

With the method identical with embodiment 1, make many many methyl of phenyl polyisocyanates-alkylene diisocyanates (the two mole dosage is than being 1:1.5) performed polymer aqueous solution.At normal temperatures, the former medicine 13.3g of multiple killing teichomycin and the former medicine 26.7g of cyanogen insect amide are dissolved in the mixed liquor of 6g toluene and 4g acetone, add while stirring the above-mentioned performed polymer aqueous solution of 5g sodium lignin sulfonate, 0.5g gelatin and 20g (containing cyst material 3g), speed high-speed stirred 1h with 1200 rev/mins, reduce rotating speed to 600 rev/min after the stable emulsion to be formed, add hydrochloric acid solution and regulate pH value to 2.5, polymerisation 2h, add again 0.5g triethylene tetramine and 24g water, stir and namely make 40% multiple killing teichomycin cyanogen insect amide microcapsule suspending agent.

Embodiment 9:50% multiple killing teichomycin cyanogen insect amide microcapsule suspending agent

Method with identical with embodiment 1 makes urea-formaldehyde prepolymer aqueous solution.At normal temperatures, multiple killing teichomycin 17g and the former medicine of cyanogen insect amide 33g are dissolved in the mixed liquor of 5g DMF and 5g dimethylbenzene, add while stirring the 2.5g sodium lignin sulfonate, 2.5g polyoxyethylene polyoxypropylene block copolymer, the above-mentioned performed polymer aqueous solution of 1g polyvinylpyrrolidone and 30g, speed high-speed stirred 1h with 1200 rev/mins, reduce rotating speed to 600 rev/min after the stable emulsion to be formed, add hydrochloric acid solution and regulate pH value to 2.5, polymerisation 2h, add again 0.5g TEPA and 3.5g water, stir and namely make 50% multiple killing teichomycin cyanogen insect amide microcapsule suspending agent.

In order further to verify the superiority of gained multiple killing teichomycin cyanogen insect amide microcapsule suspending agent of the present invention, the inventor has launched a series of special items experiments to this, and length is limit, and only exemplifies the most representative herein and part test convincingness.

The field control effectiveness test of test example 1 multiple killing teichomycin cyanogen insect amide microcapsule suspending agent control joint melon trialeurodes vaporariorum and thrips:

Test in Shouguang, Shandong Vegetable Base and carry out, according to 5 of multiple killing teichomycin among the embodiment 1~5 and cyanogen insect amide microcapsule suspending agents different content, and the disclosed embodiment 1(5% of CN102308805A multiple killing teichomycin cyanogen insect amide suspending agent) 60g/ mu is made saving the field trial of melon trialeurodes vaporariorum and thrips of 15% multiple killing teichomycin cyanogen insect amide microcapsule suspending agent 20g/ mu of interfacial polymerization preparation.Other establishes the clear water blank.Totally 8 processing, every processing repeats 4 times, the residential quarter randomized arrangement.Spray medicine when the joint melon is in full-bloom stage and trialeurodes vaporariorum, thrips occurrence in peak period is investigated radix before the spray medicine, adopt conventional spray-on process, carries out respectively efficacy survey behind the spray medicine in 7 days, 15 days, 30 days.Result of the test sees Table 1.

Table 1 multiple killing teichomycin cyanogen insect amide microcapsule suspending agent is to the efficiency test result of joint melon trialeurodes vaporariorum and thrips

Table 1 result shows: 15% multiple killing teichomycin cyanogen insect amide microcapsule suspending agent has more significant control efficiency to joint melon thrips, compare with two kinds of contrast medicaments, 15% multiple killing teichomycin cyanogen insect amide missible oil is better than 5% multiple killing teichomycin cyanogen insect amide suspending agent 60g/ mu, and with the control efficiency of 15% multiple killing teichomycin cyanogen insect amide microcapsule suspending agent 20g/ mu of interfacial polymerization preparation, evidence, the multiple killing teichomycin that the preparation method who provides with the present invention makes and cyanogen insect amide microcapsule suspending agent, obviously prolonged the lasting period to trialeurodes vaporariorum and thrips, dosage and drug cost have been reduced, to joint melon safety, be worth applying from now on.

Test example 2 multiple killing teichomycin cyanogen insect amide microcapsule suspending agent sustained release performances characterize

Release performance is the key property of reflection pesticide micro capsule slow release effect, has extremely important reference value to estimating pesticide micro capsule.This test example has been done following comparative trial to the slow release effect of the embodiment of the invention 1 gained multiple killing teichomycin cyanogen insect amide microcapsule suspending agent and the disclosed embodiment 1 of CN102027904A:

Test method: place respectively experimental group to be measured and control group in the chromatographic column, in the situation that keep extraneous as temperature, pressure, reach the constant core-clad material that makes of moisture condition and perform to outside the capsule, use at regular intervals eluent solvent, measure the active constituent content in the leacheate, and then obtain the release profiles of multiple killing teichomycin in two kinds of microcapsule suspending agents.(test method herein can be with reference to [Scientia Agricultura Sinica 2007,40(12): the 2753-2758] column chromatography in " chlorpyrifos microcapsule and release performance characterize ", also can select the additive method of the conventional usefulness of those skilled in the art to measure dispose procedure, concrete selection and be determined as those skilled in the art and grasp.)

Experimental group (series 1): the embodiment of the invention 1;

Control group (series 2): the disclosed embodiment 1 of CN102027904A.

Result of the test: see Fig. 1 and Fig. 2.Wherein, the result of the test of Fig. 1 shows, the 1st day multiple killing teichomycin burst size of experimental group (being the present invention) is 12.58%, and it is 38.56% that front 5 days accumulative total discharges percentage composition, shows that there is a comparatively desirable dispose procedure at the initial stage of microcapsule suspending agent of the present invention.And control group is 18.98% the 1st day multiple killing teichomycin burst size, and front 5 days accumulative total discharges percentage composition up to 55.87%.The result of the test of Fig. 2 shows, after the 5th day, the release behavior of the embodiment of the invention 1 microcapsule suspending agent enters the Stable Release stage, be the zero level release dynamics, finally make multiple killing teichomycin within longer a period of time, keep stable rate of release, discharge fate and reach 44d, when drug effect played a role, the short time medicine discharged the too fast harmful effect that plant itself is caused when having avoided the insects such as crop Lepidoptera, diptera and thrips such as vegetables, cotton, paddy rice are prevented and treated.And control group multiple killing teichomycin in front 20d has been finished whole releases, and duration of efficacy is short, and early stage, drug concentration was too high, was unfavorable for the control of insect.

In addition, CN102308805A embodiment 1 disclosed multiple killing teichomycin cyanogen insect amide suspending agent and the embodiment of the invention 1 multiple killing teichomycin cyanogen insect amide microcapsule suspending agent are done the comparative trial of dispose procedure, the result shows, it is long that the present invention has duration of efficacy, delay pest resistance, to advantages such as crop safeties, visible multiple killing teichomycin cyanogen insect amide is made microcapsules can obtain best releasing effect.And the disclosed multiple killing teichomycin cyanogen insect amide of CN102308805A suspending agent rate of release in early stage is too fast, and effective drug duration is too short, and dispose procedure is not ideal enough.

Although, above used general explanation, embodiment and test, the present invention is described in detail, on basis of the present invention, can make some modifications or improvements it, and this will be apparent to those skilled in the art.Therefore, these that make are without departing from theon the basis of the spirit of the present invention revised and are all belonged to the scope of protection of present invention.

Claims (9)

1. microcapsule suspending agent that contains multiple killing teichomycin and cyanogen insect amide; it is characterized in that: take multiple killing teichomycin and cyanogen insect amide as the capsule heart; described microcapsule suspending agent is comprised of the component of following percentage by weight: multiple killing teichomycin 1~50%; cyanogen insect amide 1~50%, cyst material 0.5~7%, water-soluble monomer 0.5~1%; dispersant 2~5%; protectant 0.5~1%, capsule heart solvent 1~20%, surplus is water.
2. the microcapsule suspending agent that contains multiple killing teichomycin and cyanogen insect amide according to claim 1, it is characterized in that: described cyst material is one or more in many many methyl of phenyl polyisocyanates, alkylene diisocyanate, isopropyl myristate, urea, the formaldehyde, and preferred described cyst material is many many methyl of phenyl polyisocyanates, urea and/or formaldehyde.
3. the microcapsule suspending agent that contains multiple killing teichomycin and cyanogen insect amide according to claim 1, it is characterized in that: described water-soluble monomer is one or more in deionized water, hydrochloric acid, butanediol, ethohexadiol, glycerine, ethylenediamine, triethylene tetramine, TEPA, the triethanolamine, and preferred described water-soluble monomer is deionized water, hydrochloric acid and/or butanediol.
4. the microcapsule suspending agent that contains multiple killing teichomycin and cyanogen insect amide according to claim 1, it is characterized in that: described dispersant is one or more in sodium lignin sulfonate, polyoxyethylene polyoxypropylene block copolymer, polyvinyl alcohol, the polyvinylpyrrolidone, and preferred described dispersant is sodium lignin sulfonate and/or polyvinylpyrrolidone.
5. the microcapsule suspending agent that contains multiple killing teichomycin and cyanogen insect amide according to claim 1; it is characterized in that: described protectant is one or more in gelatin, gum Arabic, polyvinyl alcohol, the polyvinylpyrrolidone, and preferred described protectant is gelatin, gum Arabic and/or polyvinyl alcohol.
6. the microcapsule suspending agent that contains multiple killing teichomycin and cyanogen insect amide according to claim 1, it is characterized in that: described capsule heart solvent is toluene, dimethylbenzene, ethanol, N, in dinethylformamide, cyclohexanone, the acetone one or more, be preferably toluene, dimethylbenzene and/or DMF.
7. the microcapsule suspending agent that contains multiple killing teichomycin and cyanogen insect amide according to claim 1; it is characterized in that: described microcapsule suspending agent is comprised of the component of following percentage by weight: multiple killing teichomycin 1 ~ 20%; cyanogen insect amide 2 ~ 40%; many methyl of the many phenyl of cyst material polyisocyanates 1 ~ 5%, water-soluble monomer butanediol 0.6 ~ 0.8%, dispersant sodium lignin sulfonate 3 ~ 4%; protectant polyvinyl alcohol 0.6 ~ 0.8%; capsule heart solvent DMF 5 ~ 15%, surplus is water.
8. each described preparation method who contains the microcapsule suspending agent of multiple killing teichomycin and cyanogen insect amide of claim 1-7, it is characterized in that: in cyst material, add pH adjusting agent pH is transferred to 8 ~ 9, be heated to 60 ~ 80 ℃, the lower reaction of insulation 0.5 ~ 2h, then being diluted with water to the stable cyst material mass percent that contains is 1 ~ 35% the performed polymer aqueous solution; Multiple killing teichomycin and cyanogen insect amide are dissolved in capsule heart solvent; add while stirring dispersant, protectant and above-mentioned cyst material prepolymer solution; speed high-speed stirred 0.5 ~ 1.5h with 1000 ~ 1500 rev/mins; rear reduction rotating speed to 500 ~ 700 rev/mins; add hydrochloric acid solution and regulate pH to 1 ~ 5; polymerisation 1.5 ~ 2.5h adds water-soluble monomer and water again, stirs and namely gets the microcapsule suspending agent that contains multiple killing teichomycin and cyanogen insect amide.
9. preparation method according to claim 8 is characterized in that: add pH adjusting agent in cyst material pH is transferred to 8.5, be heated to 70 ℃, the lower reaction 1h of insulation; Then being diluted with water to the stable cyst material mass percent that contains is 10% the performed polymer aqueous solution; Multiple killing teichomycin and cyanogen insect amide are dissolved in capsule heart solvent; add while stirring dispersant, protectant and above-mentioned cyst material prepolymer solution; speed high-speed stirred 1h with 1200 rev/mins; rear reduction rotating speed to 600 rev/min; add hydrochloric acid solution and regulate pH to 2.5; polymerisation 2h adds water-soluble monomer and water again, stirs namely to get to contain multiple killing teichomycin and cyanogen insect amide microcapsule suspending agent.
CN2012103972754A 2012-10-18 2012-10-18 Microcapsule suspending agent containing spinosad and cyantraniliprole, and preparation method thereof CN102939970A (en)

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Publication number Priority date Publication date Assignee Title
CN102027904A (en) * 2011-01-06 2011-04-27 北京燕化永乐农药有限公司 Spinosad microcapsule suspending agent
CN102308805A (en) * 2011-10-19 2012-01-11 北京燕化永乐农药有限公司 Compound pesticide
CN102326538A (en) * 2011-10-31 2012-01-25 湖南化工研究院 Thiofluoximate capsule suspension, preparation method and application
CN102362591A (en) * 2011-11-18 2012-02-29 山东海利尔化工有限公司 Insecticidal composition containing spinetoram and amide pesticides
CN102396475A (en) * 2011-12-20 2012-04-04 广西田园生化股份有限公司 Pesticide composition containing cyantraniliprole and abamectin

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102027904A (en) * 2011-01-06 2011-04-27 北京燕化永乐农药有限公司 Spinosad microcapsule suspending agent
CN102308805A (en) * 2011-10-19 2012-01-11 北京燕化永乐农药有限公司 Compound pesticide
CN102326538A (en) * 2011-10-31 2012-01-25 湖南化工研究院 Thiofluoximate capsule suspension, preparation method and application
CN102362591A (en) * 2011-11-18 2012-02-29 山东海利尔化工有限公司 Insecticidal composition containing spinetoram and amide pesticides
CN102396475A (en) * 2011-12-20 2012-04-04 广西田园生化股份有限公司 Pesticide composition containing cyantraniliprole and abamectin

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Application publication date: 20130227