First dimension salt-algae slow-release type microcapsule pesticide and preparation method
Technical field
The invention belongs to first dimension salt pesticide field, specifically a kind of first dimension salt-algae slow-release type microcapsule pesticide and preparation method.
Background technology
Avrmectin, English name Avermectins, be have desinsection, kill mite, ten hexa-atomic Macrocyclic lactone compounds of eelworm-killing activity, 1975 Japanese Kitasato Kenkyusho (JP) 9-1, Shirokane 5-chome, Minato-ku, Tokyo 108, Japan (Kitasato Institute) how separate the pedotheque in city from the Shizuoka,Japan river and obtain.Avermectins is a kind of new antibiotic, has novel structure, the dual-purpose characteristics of farming animals.Along with the raising of people's living standard and to the needs of green food, the usage quantity of Avermectins biological pesticide is increasing.
U.S. Merk﹠amp in 1984; Co. company, beginning A Wei is lead compound with the Avrmectin, synthetic by deriving, the said firm in 1994 optimization improvement is developed novel synthetic pesticide new variety emamectin-benzoate and is claimed first dimension salt (Emamectin benzoate) again, is a kind of of avermectins.Structural formula is:
Effective ingredient is Affirm (Merck Co.) Avrmectin (Emamectin B
1), molecular formula is: B
1aC
49H
75NO
13B
1bC
48H
73NO
13Molecular weight is: B
1a872.11, B
1b886.13.White or off-white color crystalline powder, fusing point 141-146 ℃, be dissolved in acetone, ethanol, methyl alcohol, be slightly soluble in water, be insoluble to hexane, shelf-stable under PH 5.0~7.0 conditions.Have the insecticide efficiency height, to people and animals' low toxicity, noresidue, the nuisanceless advantage that waits biological pesticide.The insecticidal activity of comparing with Avrmectin has improved 1-3 the order of magnitude, and active high to the larva of lepidopterous insects, mite class has stomach toxicity and action of contace poison, and insecticidal spectrum is wide; Under the low-down dosage of 0.084-2g/ha, has good insecticidal effect; , nontoxic in the process of pest control to people and animals to not injury of beneficial insect, be widely used in vegetables, cotton, tobacco, tealeaves, flowers and other crops.
Algae is a biological adsorption agent, and the cell walls of algae forms reticulated structure by cellulosic micro-fibril and constitutes, and contains abundant polysaccharide, pectin, wood sugar, seminose, alginic acid or usnic acid.Algae resource is abundant, and especially blue-green algae has very strong resistance, and it is wide to distribute in the world, and all there is blue-green algae existence on fresh water, ocean and land.
The prior art pesticide formulation mainly are missible oil and pulvis.Missible oil is that former medicine adds emulsifiers dissolve in organic solvents such as toluene or dimethylbenzene, missible oil production, and storage, transportation exists many potential safety hazards, has caused very big destruction to ecotope in the use.Pulvis is because particle is little, and easily drift in the use, brings disadvantageous effect to user and environment on every side.
Sustained release dosage is according to harmful organism pests occurrence rule, harm characteristics and envrionment conditions, by the pesticide processing means, make on demand metering of agricultural chemicals, specific time, continual and steady release to reach economic, safety, to control the technology of harmful organism effectively, its preparation is called sustained release dosage, promptly is the general name with various preparations of sustained release ability.Sustained release dosage has the following advantages: (1) makes that high drugs kind is low to be poisoned, and avoids or alleviates riskiest pesticide in use to people, animal and beneficial microorganism acute poisoning and injury, avoids or alleviates the pollution of agricultural chemicals to environment; (2) make photodissociation, hydrolysis, biological degradation, volatilization, the loss of agricultural chemicals minimizing in environment, dosage reduces, and the lasting period prolongs; (3) medicament release dosage and time can be controlled, and the function of medicament improves.
Pesticide micro capsule agent (Microcapsules, MC) with macromolecular material as cyst membrane, to wrap up as the pesticidal active substance of the capsule heart, form a kind of minigel, and they are stably disperseed, are suspended in the water of external phase with semipermeability cyst membrane.
The existing first dimension salt pesticide formulation are missible oil, microemulsion, wettable powder.In use be subject to the influence of environmental factors light, heat, air, rainwater, soil, microorganism and other chemical substances, cause and decompose and run off, make it be difficult to bring into play the ultra-high efficiency effect, and medication quantity and frequency increase year by year, cost increases.First is tieed up salt be processed into the slow release type minigel and can overcome above-mentioned shortcoming effectively, the performance slow-release function is increased operation rate, and prolongs the lasting period and reduces dosage, makes it become real efficient, nontoxic, free of contamination biological pesticide.
The fertile preparation of medicine is with agricultural chemicals, the fertilizer product that two combine into one, is called for short medicine fertilizer.Can bring into play and fertilize the soil and the double effects of plant protection, its innovative significance shows three aspects: the first, enriched the concrete intension of chemical fertilizer and agricultural chemicals, the functions of use that has expanded original product.The second, with polynary dedicated fertilizer and agricultural chemicals reasonable compatibility, the effect of maximum efficiency ground performance two big agrochemicals.The 3rd, use conveniently, reduce labor intensity.
Comprehensive above-mentioned existing pesticide technology background; in order to protect environment, to improve agricultural production efficiency, invent a kind of with the algae be insecticide efficiency height, the drug effect of carrier long, use conveniently, reduce labor intensity, improve fertilizer and agricultural chemicals utilization ratio, efficient, nontoxic, pollution-free first tie up salt-algae slow-release type microcapsule pesticide and the preparation method is very necessary.
Summary of the invention
The purpose of this invention is to provide a kind ofly, with the algae be that insecticide efficiency height, the drug effect of carrier is long, use conveniently, reduce labor intensity, improve fertilizer and agricultural chemicals utilization ratio, efficient, nontoxic, pollution-free first dimension salt-algae slow-release type microcapsule pesticide in order to protect environment, to improve agricultural production efficiency.
Another object of the present invention provides the preparation method of first dimension salt-algae slow-release type microcapsule pesticide.
For achieving the above object, technical solution of the present invention is as follows:
First dimension salt-algae slow-release type microcapsule pesticide, each components by weight is:
First dimension salt 0.5-10 part
Algae 5-50 part
Tensio-active agent 1-20 part
Easy degraded macromolecular 1-20 part
Stablizer 2-30 part
Little fertile 1-10 part
Plant-growth regulator 1-5 part.
The preparation method of first dimension salt-algae slow-release type microcapsule pesticide comprises the steps:
A. the pre-treatment of algae: algae 50-70 ℃ of dry 4-7h of the above-mentioned processing of 5-50 part fished for, got after centrifugal, the removal of impurities, spraying drying to fresh algae from water;
B. first is tieed up salt and plant-growth regulator and be dissolved in the reaction vessel that organic solvent is housed, and add dried algae, 30 ℃ vibrated immersion down after 24 hours in constant temperature gas bath vibrator;
C. easy degraded macromolecular is added in the above-mentioned reactor;
D. tensio-active agent and stablizer are poured in the redistilled water;
E. step c is mixed with the steps d product, send into high-shear emulsion machine 12000rpm speed and stirred 15 minutes, the speed with 1000rpm stirs again; Temperature steams organic solvent for 40 ℃, solidifies encystation, filters water outlet, and mixes with little fertilizer, promptly gets first dimension salt-algae slow-release type microcapsule pesticide.
Described algae is a kind of in Microcystis aeruginosa, chroococcoid, cytoalgae, capsule ball algae, wedge algae and the chamber ball algae.
Plant-growth regulator is indolebutyric acid or naphthylacetic acid.
Easily the degraded macromolecular compound is one or more in the following material: methyl or carboxymethyl cellulose, polyvinyl acetate (PVA), polyvinylpyrrolidone, polyoxyethylene glycol, Natvosol, polyvinyl alcohol, Zulkovsky starch, W-Gum.
Tensio-active agent is an organic silicon surfactant.
Stablizer is one or more in anhydrous sorbitol polyethylene polyethenoxy ether, sorbitan mono-laurate, polypropylene glycol oxyethane ether, Sodium Lauryl Sulphate BP/USP, sodium laurylsulfonate or the polyoxyethylene glycol.
Organic solvent is a kind of in methyl alcohol, ethanol, acetone, sherwood oil, ethyl acetate, methylene dichloride, the chloroform among the step b.
Little fertilizer is one or more in the following material: borax, boric acid, ammonium molybdate, zinc sulfate, manganous sulfate, ferrous sulfate, rare earth nitrate.
The organic solvent that uses among the step b of the present invention is steamed in step e, does not contain organic solvent composition in the product.
Novelty of the present invention is to be carrier with the algae, utilize its physical adsorbability to adsorb former medicine first dimension salt and plant-growth regulator, add easy degraded macromolecular, tensio-active agent and stablizer, mix with little fertilizer after solidifying encystation, be prepared into the microcapsule insecticide-fertilizer preparation---first dimension salt-algae slow-release type microcapsule pesticide.Characteristics of the present invention are: this formulation is sustained release and directed release effectively, increases operation rate; Reduce dosage; The algae bearer resource is abundant, utilizes the algae objectionable impurities to make its resource utilization; Adopt the little fertilizer of agricultural chemicals composite, performance is fertilized the soil and the double effects of plant protection, reach use convenience, reduce labor intensity, saving of labor's abridged edition and make the synergic purpose mutually.Raw material of the present invention is easy to get, complete processing is simple, with low cost, be fit to industrial scale production, be widely used.
Advantage of the present invention is:
1, effectively sustained release and directed release prolongs the lasting period and reduces dosage;
2, the algae bearer resource is abundant, makes objectionable impurities become useful resource, the protection environment;
3, adopt the little fertilizer of agricultural chemicals composite, the double effects of performance infertile field and plant protection;
4, use conveniently, reduce labor intensity;
5, saving of labor, saving agriculture production cost;
6, raw material be easy to get, with low cost; Simple, the suitable industrial scale production of technology.
Embodiment
The present invention will be further described below by embodiment, but never limit the scope of the present invention.
Embodiment 1:
The preparation method of first dimension salt-algae slow-release type microcapsule pesticide comprises the steps:
A. get pretreated 50 ℃ of dry 7h of 20 portions of algaes;
B. with 4 portions of first dimension salt and 1 part of naphthylacetic acid, 0.3 part of indolebutyric acid is dissolved in the reaction vessel of the organic solvent that is equipped with 25 parts, and adds 20 parts of dried algaes, and 30 ℃ vibrated immersion down after 24 hours in constant temperature gas bath vibrator;
C. 2 parts of polymers of easily degrading are added in the above-mentioned reactor;
D. 3 parts tensio-active agent and 4 parts stablizer are poured in 100 parts of redistilled waters;
E. with step c product with after the steps d product mixes, stirred 15 minutes with the speed of high-shear emulsion machine earlier with 12000rpm, speed with 1000rpm stirs again, in temperature is to steam organic solvent under 40 ℃, solidify encystation, filter water outlet, and mix, promptly get first dimension salt-algae slow-release type microcapsule pesticide with 5 parts of zinc sulfate.
The experiment of Toxicity Determination and sub-district, field shows: first dimension salt-algae slow-release type microcapsule pesticide has good slow release effect, insecticidal effect remarkable; Promote vegetable growth, obvious effect of increasing production is arranged.
This 5% first dimension salt-algae slow-release type microcapsule pesticide and the contrast of existing first dimension salt agricultural chemicals do are applied to Toxicity Determination, and method is as follows: with the clear water dilution, place beaker respectively; To put into the different concns dilute liquid medicine and flood 10s for examination diamondback moth larvae in 2 age, take out immediately; Be placed on to inhale on the thieving paper and remove too much soup; Move in the culture dish of each group, the cabbage leaves of giving after fresh clean is made feed, and culture dish mid-one little wet cotton balls to be to preserve moisture, and raises indoor in 28 ℃ of room temperatures, relative humidity 75%~85%.Each handles 3 repetitions, and each repeats 30 larvas, compares with the clear water dipping.24,48, check mortality ratio behind the 72h, gently dial polypide with writing brush during inspection respectively, can bending be with polypide that to join end to end be the worm that lives, calculate mortality ratio with the dead borer population of accumulative total of handling back 72h, and proofread and correct with contrast.Set up virulence regression equation with method of least squares, and calculate LC
50, soup is deposited a Zhou Houzai and is carried out identical experiment.
The result shows: the embodiment of the invention 5% first dimension salt-algae slow-release type microcapsule pesticide and existing first dimension salt 5% water dispersible granules LC
50Be more or less the same, be respectively 6.88mg/l, 6.91mg/l; Soup is deposited a Zhou Houzai and is experimentized, LC
50Differ bigger, be respectively 8.98mg/l, 13.76mg/l illustrates that duration of efficacy of the present invention is long.
This 5% first dimension salt-algae slow-release type microcapsule pesticide and the contrast of existing first dimension salt 5% water dispersible granules do are applied to field plot trial, carry out according to " test rule () is asked in the agricultural chemicals field " that medicine inspecting institute of the Ministry of Agriculture issues, use the recommended dose dilute with water of existing first dimension salt 5% water dispersible granules to carry out routine spraying processing respectively, formulation rate 4.0gai/ha, and the soup after will diluting deposits a Zhou Houzai and carries out routine spraying and handle, and every sub-district area is 50m
2, each is handled and repeats 4 times, establishes the clear water contrast, and each is handled random alignment and distributes, every sub-district fixed point investigation 20 strain wild cabbages.Investigation insect population radix before the medicine behind the medicine 1,3, the residual borer population alives of 7d investigation, calculates insect population go down rate, prevention effect, looks into the weightening finish situation of wild cabbage after 30 days by the title fresh weight.
The result shows: the present invention's 5% first dimension salt-algae slow-release type microcapsule pesticide is suitable with existing first dimension salt 5% water dispersible granules prevention effect; Soup is deposited a Zhou Houzai and is carried out routine spraying processing, and prevention effect is significantly better than existing first dimension salt 5% water dispersible granules.Claim the wild cabbage fresh weight after 30 days, the 5% first dimension salt-algae slow-release type microcapsule pesticide of medication is than the weightening finish 20-30% of existing first dimension salt 5% water dispersible granules wild cabbage.Illustrate that first of the present invention dimension salt-algae slow-release type microcapsule pesticide has good slow release effect, duration of efficacy long, has obvious insecticidal action; Can promote vegetable growth, effect of increasing production is obvious.
Embodiment 2:
The preparation technology of first dimension salt-algae slow-release type microcapsule pesticide comprises the steps:
A. get 70 ℃ of dry 4h of pretreated 25 portions of algaes;
B. with 5 portions of first dimension salt and 2 parts of naphthylacetic acids, 0.5 part of indolebutyric acid is dissolved in the reaction vessel of the organic solvent that is equipped with 30 parts, and adds 25 parts of dried algaes, and 20 ℃ vibrated immersion down after 24 hours in constant temperature gas bath vibrator;
C. 3 parts of polymers of easily degrading are added in the above-mentioned reactor;
D. 3 parts tensio-active agent and 5 parts stablizer are poured in 150 parts of redistilled waters;
E. with steps d, after e mixes, stirred 15 minutes with the speed of high-shear emulsion machine earlier with 10000rpm, speed with 800rpm stirs again, in temperature is to steam organic solvent under 50 ℃, solidifies encystation, filters water outlet, and mix with 7 parts of rare earth nitrates, promptly get first dimension salt-algae slow-release type microcapsule pesticide.
Toxicity Determination and the experiment of sub-district, field, method is with embodiment 1.The result shows: first dimension salt-algae slow-release type microcapsule pesticide has good slow releasing function, insecticidal effect obvious; Can promote vegetable growth, obvious effect of increasing production is arranged.
Embodiment 3:
The preparation technology of first dimension salt-algae slow-release type microcapsule pesticide comprises the steps:
A. get 60 ℃ of dry 6h of pretreated 15 portions of algaes;
B. with 2.5 portions of first dimension salt and 1.5 parts of naphthylacetic acids, 0.4 part of indolebutyric acid is dissolved in the reaction vessel of the organic solvent that is equipped with 35 parts, and adds 15 parts of dried algaes, and 25 ℃ vibrated immersion down after 24 hours in constant temperature gas bath vibrator;
C. 1.5 parts of polymers of easily degrading are added in the above-mentioned reactor;
D. 2 parts tensio-active agent and 4 parts stablizer are poured in 100 parts of redistilled waters;
E. with steps d, after e mixes, stirred 15 minutes with the speed of high-shear emulsion machine earlier with 8000rpm, speed with 700rpm stirs again, in temperature is to steam organic solvent under 55 ℃, solidifies encystation, filters water outlet, and mix with 3 parts of ferrous sulfate, promptly get first dimension salt-algae slow-release type microcapsule pesticide.
Toxicity Determination and the experiment of sub-district, field, method is with embodiment 1.The result shows: first dimension salt-algae slow-release type microcapsule pesticide has good slow releasing function, insecticidal effect obvious; Can promote vegetable growth, obvious effect of increasing production is arranged.
Embodiment 4:
The preparation technology of first dimension salt-algae slow-release type microcapsule pesticide comprises the steps:
A. get 70 ℃ of dry 5h of pretreated 20 portions of algaes;
B. with 3 portions of first dimension salt and 2 parts of naphthylacetic acids, 0.4 part of indolebutyric acid is dissolved in the reaction vessel of the organic solvent that is equipped with 25 parts, and adds 20 parts of dried algaes, and 30 ℃ vibrated immersion down after 24 hours in constant temperature gas bath vibrator;
C. 1.5 parts of polymers of easily degrading are added in the above-mentioned reactor;
D. 2 parts tensio-active agent and 5 parts stablizer are poured in 100 parts of redistilled waters;
E. with steps d, after e mixes, stirred 15 minutes with the speed of high-shear emulsion machine earlier with 8000rpm, speed with 900rpm stirs again, in temperature is to steam organic solvent under 50 ℃, solidifies encystation, filters water outlet, and mix with 5 parts of rare earth nitrates, promptly get first dimension salt-algae slow-release type microcapsule pesticide.
Toxicity Determination and the experiment of sub-district, field, method is with embodiment 1.The result shows: first dimension salt-algae slow-release type microcapsule pesticide has good slow releasing function, insecticidal effect obvious; Can promote vegetable growth, obvious effect of increasing production is arranged.
Embodiment 5:
The preparation technology of first dimension salt-algae slow-release type microcapsule pesticide comprises and states step:
A. get 70 ℃ of dry 7h of pretreated 10 portions of algaes;
B. 1 portion of first dimension salt and 0.5 part of naphthylacetic acid are dissolved in the reaction vessel of the organic solvent that is equipped with 15 parts, and add 10 parts of dried algaes, 25 ℃ vibrated immersion down after 24 hours in constant temperature gas bath vibrator;
C. 1 part of polymer of easily degrading is added in the above-mentioned reactor;
D. 1 part tensio-active agent and 3 parts stablizer are poured in 50 parts of redistilled waters;
E. with steps d, after e mixes, stirred 10 minutes with the speed of high-shear emulsion machine earlier with 5000rpm, speed with 600rpm stirs again, in temperature is to steam organic solvent under 45 ℃, solidifies encystation, filters water outlet, and mix with 2 parts of rare earth nitrates, promptly get first dimension salt-algae slow-release type microcapsule pesticide.
Toxicity Determination and the experiment of sub-district, field, method is with embodiment 1.The result shows: first dimension salt-algae slow-release type microcapsule pesticide has good slow releasing function, insecticidal effect obvious; Can promote vegetable growth, obvious effect of increasing production is arranged.
The foregoing description only is a preference of the present invention, is not used for limiting the present invention, and all within principle of the present invention, any modifications and variations of being done are all within protection scope of the present invention.