CN102860301A - Azadirachtin preparation using vegetable oil as medium - Google Patents
Azadirachtin preparation using vegetable oil as medium Download PDFInfo
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Abstract
The invention, relating to the field of plant-based insecticides, particularly relates to an Azadirachtin insecticide using plant oil as a medium, characterized by using plant oil as the medium and Azadirachtin as a main insecticidal active component, and adding a certain proportion of various ingredients to prepare four preparations comprising Azadirachtin missible oil, microemulsion, oil flowable formulation, and emulsion in water. According to the invention, the Azadirachtin preparation disclosed herein is prepared by using plant oil as the medium and selecting plant oil to replace aromatic hydrocarbon and other organic solvents to be as the medium, thus the advantages of easy obtainment of raw materials, simple processing, safety, environmental protection, low toxicity, and significant synergic effect are achieved, and the Azadirachtin preparation disclosed herein has excellent control effect on plutella xylostella, prodenia litura, beet armyworm, pieris rapae, rice leaf folder and other insect pests, and is particularly suitable for various insect pests with resistance. The Azadirachtin preparation disclosed herein has various dosage forms, simple preparation method, and high promotional value.
Description
Technical field
The invention belongs to the plant insecticide field, be specifically related to nimbin preparation take vegetable oil as medium and preparation method thereof.
Background technology
Utilize that the exploitation of natural pesticide plant is efficient, low toxicity, vegetable insecticide free from environmental pollution be subject to people's great attention just gradually.In numerous pesticide plants, most study, the most influential seal chinaberry plant that will count the Meliaceae Melia.This plant is the efficient insecticide plant that the world today generally acknowledges, extensively plants in the torrid zone, subtropics, is a kind of energy Fast Growth and evergreen all the year round arbor.Studies show that in a large number that both at home and abroad contain multiple insecticide active substance in the positions such as seed, leaf, bark and branch of seal chinaberry, wherein the insecticidal activity with nimbin is the strongest.
Nimbin is wide spectrum recognized in the world, efficient, low toxicity, the easy insecticide of degraded, noresidue, and there is not resistance, nearly all plant insect is all had repelling and killing efficacy, without any pollution, is a kind of insecticide that has very big exploitation to be worth to people and animals and surrounding environment.Current, the countries in the world scientist is in the research of being devoted to the azadirachtin insecticide product, and the states such as the U.S., Germany, India, Canada successively develop product such as the Margosan-O(U.S. produces), Neemmark(India produces) etc. put on market.But these products all are cream preparations mainly, are widely used the organic solvent such as aromatic hydrocarbons as medium, and this is so that not environmental protection that the plant insecticide nimbin of original environmental protection becomes afterwards in the adding of these organic solvents.And these cream preparations usually only after dispenser in 1～5 day the control efficiency to insect comparatively remarkable, control efficiency then obviously reduces after 5～6 days, the lasting period is short, will force so repeatedly medication of peasant, certainly will cause the increase of production cost.Studies show that in a large number, nimbin is complicated macromolecular substances, many functional groups that can react are arranged in the molecular structure, comprise ester group, epoxy construction etc., but nimbin very easily decomposes in ultraviolet lighting, high temperature or water the time, cause its insecticidal activity to reduce, thereby control of insect is being shown relatively poor lasting effect.Although W.R.Grace(1994) can delay the degraded of nimbin in the pH value method of the certain density nimbin preparation of United States Patent No 5281618 layout of papers and adjusting preparation, but actual effect is unsatisfactory, and substantive solution nimbin product easily decomposes, unsettled method.In addition, nimbin is subject to the pollutions such as aflatoxins and affects its storage-life in process, and there are the shortcomings such as difficult emulsification, nimbin product forms is comparatively single in process of production in nimbin emulsion.For a long time, above-mentioned factor has restricted production and the use of the spread on agricultural of nimbin product.
Vegetable oil is a kind of abundant natural reproducible resource of originating, and its maximum characteristics are nontoxic, water-tolerants and with low cost.Vegetable oil can produce good permeability after mixing with agricultural chemicals, can make the mushroom in the medicine kill tissues or infiltrate in the insect body wall kill pests and pathogen.In addition, after vegetable oil mixes with agricultural chemicals, very strong plate-out ability is arranged, can increase the coverage rate to plant, be difficult for being washed away loss by rainwater, still can keep good drug effect after the rain.Vegetable oil can reduce the characteristics that light decomposes, the strong drift in the time of also can reducing spraying after mixing with agricultural chemicals in addition, overcome water and contained mineral matter, and weakening the phenomenon of pesticide active ingredient, the vegetable oil viscosity is strong, is highly suitable for low-gallonage spraying and ultra low volume spraying.Experiment shows, does the adjuvant spraying with vegetable oil, can save dose 1/8th, even more.Vegetable oil not only can play the effect of petroleum base surface active agent, but also is good anti-volatilizer, can make the liquid of ejection be covered in equably the surface of plant, and guarantees that agricultural chemicals has the longer longevity of residure.In synthetic pyrethrin pesticide, vegetable oil or a kind of best thinner.Make adjuvant with vegetable oil, can avoid because using mineral oil that some sensitive crop is produced poisoning.In existing document, adopt the vegetable oil or derivatives thereof many as the report that pesticide solvent uses, such as soybean oil, corn oil, rapeseed oil, cottonseed oil, soybean oil methyl esters etc.Du Xuelin (2006) can be made into insecticide at CN 1926998A report vegetable oil, and good preventive effect is arranged.Wang Wenzhong (2010) discloses the good purposes of Jatropha curcas oil as a kind of plant source pesticide solvent at CN 101642093A.But it all is not applied on the plant insecticide nimbin, all is as the effective active composition with vegetable oil itself or other organic agricultural chemicals.
The present invention is with in the vegetable oil introduced plant insecticide nimbin, as medium, make the plant resource environment-protection pesticide preparation based on plant resource environment-protection pesticide solvent, meet the requirement of environment-friendly type preparation, can use at vegetables, fruit, oil crop, tealeaves, traditional Chinese medicine, with target stronger compatibility is arranged, can give full play to the preventive and therapeutic effect of active ingredient, and need not to add the function that a large amount of synergist improve preparation.In addition, when plant resource environment-protection pesticide solvent is used as the carrier fluid of agricultural chemicals, can make medicament be able to more effective application during the low capacity dispenser, its major advantage is liquid not volatile and drift in the sprinkling process, it is more even that liquid is labeled covering plant, and liquid is difficult for being fallen by rain drop erosion.And research finds that the plant resource active component often exists jointly in plant oiliness composition, often very easily decomposes after separating in the composition from plant, therefore, selects vegetable oil to replace organic solvent as the dissolve medium of nimbin, can strengthen greatly its stability.
Xu Hanhong discloses a kind of plant-type nimbin insecticide in Chinese patent CN 1276161A, but its be with nimbin and neem oil jointly as main active insecticidal components, be configured to nimbin emulsion, wetting powder, three kinds of formulations of suspending agent by adding a certain proportion of multiple batching.Do not relate to vegetable oil as its medium.
Report there are no technology about the nimbin preparation technique scheme take vegetable oil as medium at present.
Summary of the invention
The object of the present invention is to provide the plant-type nimbin insecticide that formulation is various, prescription is original take vegetable oil as medium, possess the machine solvent with acyclics such as the alternative aromatic hydrocarbons of vegetable oil, and the drug effect of enhancing nimbin, solve that nimbin easily decomposes, difficult storage, difficult emulsification, easily pollute, defective that formulation is single, poor to the insect lasting effect, and satisfy the needs that various pests is prevented and treated in the agricultural production.Reach same control efficiency, reduce the pesticide resistance of insect, preserve the ecological environment, improve safety and the export competitiveness of agricultural byproducts.
The present invention provides various preparations of described nimbin take vegetable oil as medium and preparation method thereof simultaneously.
Purpose of the present invention is achieved by the following technical programs:
The nimbin preparation take vegetable oil as medium that the present invention relates to is characterized in that being take vegetable oil as the medium nimbin main active insecticidal components, allocates cosolvent into, emulsifier is configured to the nimbin emulsion preparation; Allocate cosolvent, emulsifier, defoamer and water into and be configured to the nimbin microemulsion formulation; Allocate emulsifier, wetting dispersing agent, suspension stabilizer, defoamer into and be configured to the outstanding preparation of nimbin oil; Allocate cosolvent, emulsifier, thickener, defoamer and water into and be configured to the nimbin water-emulsion preparation.
Described medium vegetable oil is selected from any one or more in neem oil, Jatropha curcas oil, soybean oil, peanut oil, rapeseed oil, palm oil, castor oil, cocoa butter, linseed oil, cottonseed oil, sunflower oil, safflower oil, tung oil, perilla oil, cannabis oil, cashew nut oil, olive oil, the corn oil.
Each component content proportioning is in the described nimbin emulsion preparation: Azadirachtin Cotent is 0.1 %～92 %(weight); Content of vegetable oil is 0.5 %～95 %(weight); Cosolvent content is 0 %～15 %(weight); Emulsifier content is 5 %～15 %(weight); Each component summation is 100 %.
Cosolvent can be selected any one or more in isooctanol, n-octyl alcohol, isobutanol, n-butanol, isopropyl alcohol, ethylene glycol, polyethylene glycol, ethanol, NOP, N-ethyl pyrrolidone, 1-METHYLPYRROLIDONE, the azone; Emulsifier can be selected polyoxyethylene polyoxypropylene block copolymer, the pure APEO in C12～14, sorbitol polyoxyethylene ether, castor oil polyoxyethylene ether, ethylene polyethenoxy ether, anhydrosorbitol acid anhydride oleate, anhydrous sorbitol acid anhydride trioleate, polyoxyethylene sorbitan monolaurate, the alkane polyoxyethylene 20 sorbitan monooleate, sorbierite polyoxy ether, Brij30, aliphatic alcohol polyoxyvinethene phosphate, calcium dodecyl benzene sulfonate, alkyl polyglycol ether phosphate, ethoxylated alkyl phosphate, in the ethoxylated alkyl sulfates any one or more.
Its preparation method is: by ratio requirement nimbin, vegetable oil, cosolvent, emulsifier added in the reactor, and stirring and dissolving, namely being able to vegetable oil is the nimbin emulsion preparation of medium.
Each component content proportioning is in the described nimbin microemulsion formulation: Azadirachtin Cotent is 0.5 %～60 %(weight); Content of vegetable oil is 1 %～30 %(weight); Cosolvent content is 0 %～10 %(weight); Emulsifier content is 5 %～25 %(weight); Antifoam content is 0.1 %～0.3 %(weight); Yu Weishui, each component summation is 100 %.
Cosolvent can be selected any one or more in isooctanol, n-octyl alcohol, isobutanol, n-butanol, isopropyl alcohol, ethylene glycol, polyethylene glycol, ethanol, glycerine, NOP, N-dodecylpyrrolidone, the spectrasolv DMDA; Emulsifier can be selected polyoxyethylene polyoxypropylene block copolymer, the pure APEO in C12～14, sorbitol polyoxyethylene ether, castor oil polyoxyethylene ether, ethylene polyethenoxy ether, anhydrosorbitol acid anhydride oleate, polyoxyethylene sorbitan monolaurate, the alkane polyoxyethylene 20 sorbitan monooleate, the polyoxyethylene polyoxypropylene block copolymer phosphate, C12～14 polyoxyethylene ether phosphates, the straight chain calcium dodecyl benzene sulfonate, straight chain DBSA amine, alkyl polyglycol ether phosphate, in the ethoxylated alkyl phosphate any one or more; Defoamer is selected methyl polysiloxane.
Its preparation method is: by ratio requirement nimbin, vegetable oil, cosolvent, emulsifier, defoamer are added in the reactor, be uniformly dispersed in 2000～5000 rpm/min shearing, the water that adds surplus, high speed shear 20～60 min under 5000～8000 rpm/min, namely being able to vegetable oil is the nimbin microemulsion formulation of medium.
Each component content proportioning is in the outstanding preparation of described nimbin oil: Azadirachtin Cotent is 1 %～50 %(weight); Content of vegetable oil is 1 %～90 %(weight); Emulsifier content is 1 %～10 %(weight); Wetting dispersing agent content is 2 %～10 %(weight); Suspending stabilized agent content is 0 %～5 %(weight); Antifoam content is 0.1 %～0.5 %(weight); Each component summation is 100 %.
Emulsifier can be selected any one or more in polyoxyethylene polyoxypropylene block copolymer, fatty alcohol-polyoxyethylene ether, sorbitol polyoxyethylene ether, polyoxyethylene groups Arrcostab, anhydrosorbitol acid anhydride oleate, sorbitol monooleate, the alkylbenzenesulfonate; Wetting dispersing agent can be selected any one or more in macromolecular grafted lignosulfonates, polycarboxylate, rosin grafting polymer carboxylate, naphthalene and alkylnaphthalene sulfonate formaldehyde condensation products, the oleic acid methylamino ethyl sulfonate; Suspension stabilizer can be selected any one or more in convex-concave rod soil, bentonite, aluminium-magnesium silicate, imvite, the hydroxyethylcellulose; Defoamer is selected from polysiloxanes.
Its preparation method is: after by ratio requirement nimbin, vegetable oil, emulsifier, wetting dispersing agent, suspension stabilizer, defoamer being mixed, place the particle diameter of high speed shear ball-grinding machine ball milling to 90 % less than 4 μ m, namely being able to vegetable oil is the outstanding preparation of nimbin oil of medium.
Each component content proportioning is in the described nimbin water-emulsion preparation: Azadirachtin Cotent is 0.5 %～60 %(weight); Content of vegetable oil is 1 %～30 %(weight); Cosolvent content is 0 %～10 %(weight); Emulsifier content is 5 %～20 %(weight); Amount of thickener is 0 %～1 %(weight); Antifoam content is 0.1 %～0.3 %(weight); Yu Weishui, each component summation is 100 %.
Cosolvent can be selected any one or more in isooctanol, n-octyl alcohol, isobutanol, n-butanol, isopropyl alcohol, ethylene glycol, polyethylene glycol, ethanol, glycerine, propane diols, NOP, the N-dodecylpyrrolidone; Emulsifier can be selected any one or more in polyoxyethylene polyoxypropylene block copolymer, the pure APEO in C12～14, sorbitol polyoxyethylene ether, castor oil polyoxyethylene ether, ethylene polyethenoxy ether, anhydrosorbitol acid anhydride oleate, polyoxyethylene sorbitan monolaurate, polyoxyethylene 20 sorbitan monooleate, polyoxyethylene polyoxypropylene block copolymer phosphate, C12～14 polyoxyethylene ether phosphates; Thickener can be selected any one or more in xanthans, polyvinyl alcohol, aluminium-magnesium silicate, polyvinylpyrrolidone, gum Arabic, the acrylate; Defoamer is selected methyl polysiloxane.
Its preparation method is:
1) oil phase preparation
By ratio requirement nimbin, vegetable oil, emulsifier, cosolvent are added in the reactor, mix, go into oil phase;
2) water preparation
By ratio requirement thickener, defoamer and water are mixed, go into water;
3) high-shear emulsifying
Under stirring condition, water and oil phase are mixed, under 4000～10000 rpm/min conditions, high speed shear emulsification 20～60 min, namely being able to vegetable oil is the nimbin water-emulsion preparation of medium.
The invention has the beneficial effects as follows:
The present invention relates to take vegetable oil as medium the nimbin preparation, changed the technology limitation of traditional insecticidal preparation take organic solvent as medium, using vegetable oil instead is solvent, has following significant progress:
(1) to adopt vegetable oil be carrier in the present invention, and natural origin is renewable resources, does not use the not environmental protection organic solvents such as any aromatic hydrocarbons, and is environmentally friendly, easily biological-degradable, and pollution-free, security performance is good, and the production accumulating is safe and convenient to use;
(2) botanical solvent, good with the nimbin compatibility, solvability is large, good stability, has suitable viscosity, and having good permeability, anti-drift film forming and the emulsion dispersion property opened up, the concentration gradient that has increased between nimbin and insect and plant epidermis helps farm chemical ingredients to improve drug effect to the infiltration of insect and plant tissue semipermeable membrane; Thereby can also effectively reduce simultaneously surface tension improves interaction between droplet and the target and droplet is arrived do not rebound behind the plant leaf surface and be beneficial to its adhesion at plant surface, wetting and sprawl the absorption efficiency that improves liquid;
(3) vegetable oil be difficult for volatile performance, be that pesticide liquid generates the very high liquid crystalline phase of viscosity when dropping in evaporation and concentration, can securely agricultural chemicals be sticked to plant surface and be difficult for being fallen by rain drop erosion, therefore can significantly improve the control efficiency of liquid;
(4) intrinsic active skull cap components makes it have excellent synergistic effect in the vegetable oil, and the generation of pest resistance to insecticide is had retarding action, also can improve simultaneously the resistance level of crop.
The present invention can be used for the control of common insect in the agricultural production, for the production of agricultural, pollution-free food and nuisanceless fruits and vegetables provides safely and efficiently pesticide new variety; Formulation of the present invention is various, and the preparation method is simple, and promotional value is high.
Embodiment
Content for a better understanding of the present invention is described further invention below in conjunction with following specific embodiment, but does not therefore limit protection scope of the present invention.Virulence test and field efficiency test are tested conventional method with reference to this area.
The preparation of embodiment 1 0.5 % nimbin emulsion preparations
In reactor, add successively nimbin 5 kg, neem oil 900 kg, isopropyl alcohol 10 kg, 1-METHYLPYRROLIDONE 10 kg, polyoxyethylene polyoxypropylene block copolymer 25 kg, castor oil polyoxyethylene ether 20 kg, calcium dodecyl benzene sulfonate 30 kg, stirring and dissolving namely gets 1000 kilogram of 0.5 % nimbin emulsion.
The preparation of Comparative Examples 1 0.5 % nimbin emulsion preparations
In reactor, add successively nimbin 5 kg, dimethylbenzene 900 kg, isopropyl alcohol 10 kg, 1-METHYLPYRROLIDONE 10 kg, polyoxyethylene polyoxypropylene block copolymer 25 kg, castor oil polyoxyethylene ether 20 kg, calcium dodecyl benzene sulfonate 30 kg, stirring and dissolving namely gets 1000 kilogram of 0.5 % nimbin emulsion.
Indoor, adopt dip method to measure 0.5 % nimbin emulsion to the control efficiency of diamond-back moth 3 instar larvaes, 24 h " Invest, Then Investigate " lethality, result of the test sees Table 1.
Table 1 adopts dip method to measure 0.5 % nimbin emulsion different formulations to the indoor pharmacodynamic test result of diamond-back moth 3 instar larvaes
Indoor, employing is soaked slide method and is measured 0.5 % nimbin emulsion to the control efficiency of two spotted spider mite (the female one-tenth mite in 3～5 day age), 24 h " Invest, Then Investigate " lethality, and result of the test sees Table 2.
Table 2 employing is soaked slide method and is measured 0.5 % nimbin emulsion different formulations to the indoor pharmacodynamic test result of two spotted spider mite (the female one-tenth mite in 3～5 day age)
Can find that from table 1 and table 2 result the neem oil medium that the present invention relates to is remarkable to 0.5 % nimbin emulsion synergistic effect.
The preparation of embodiment 25 % nimbin emulsion preparations
In reactor, add successively nimbin 50 kg, palm oil 710 kg, NOP 120 kg, alkane polyoxyethylene 20 sorbitan monooleate 45 kg, anhydrous sorbitol acid anhydride oleate 30 kg, ethoxylated alkyl phosphate 45 kg, stirring and dissolving namely gets 1000 kilogram of 5 % nimbin emulsion.
The preparation of embodiment 3 24 % nimbin emulsion preparations
In reactor, add successively nimbin 240 kg, cocoa butter 590 kg, NOP 50 kg, isobutanol 10 kg, ethylene polyethenoxy ether 30 kg, castor oil polyoxyethylene ether 35 kg, alkyl polyglycol ether phosphate 45 kg, stirring and dissolving namely gets 1000 kilogram of 24 % nimbin emulsion.
The preparation of embodiment 4 50 % nimbin emulsion preparations
In reactor, add successively nimbin 500 kg, neem oil 410 kg, polyoxyethylene polyoxypropylene block copolymer 20 kg, polyoxyethylene sorbitan monolaurate 40 kg, calcium dodecyl benzene sulfonate 30 kg, stirring and dissolving namely gets 1000 kilogram of 50 % nimbin emulsion.
The preparation of embodiment 5 90 % nimbin emulsion preparations
In reactor, add successively nimbin 900 kg, Jatropha curcas oil 70 kg, polyethylene glycol 10 kg, castor oil polyoxyethylene ether 10 kg, ethoxylated alkyl sulfates 10 kg, dispersed with stirring is even, namely gets 1000 kilogram of 90 % nimbin emulsion.
The preparation of embodiment 6 0.6 % nimbin microemulsion formulations
In reactor, add successively nimbin 6 kg, neem oil 250 kg, isooctanol 30 kg, polyoxyethylene polyoxypropylene block copolymer 20 kg, castor oil polyoxyethylene ether 20 kg, alkyl polyglycol ether phosphate 40 kg, methyl polysiloxane 1 kg, stirring and dissolving is uniformly dispersed at 2000 rpm/min down cuts; Add deionized water 633 kg again, stir, high speed shear 60 min under 5000 rpm/min namely get 1000 kilogram of 0.6 % micro nimbin emulsion.
The preparation of Comparative Examples 2 0.6 % nimbin microemulsion formulations
In reactor, add successively nimbin 6 kg, dimethylbenzene 250 kg, isooctanol 30 kg, polyoxyethylene polyoxypropylene block copolymer 20 kg, castor oil polyoxyethylene ether 20 kg, alkyl polyglycol ether phosphate 40 kg, methyl polysiloxane 1 kg, dispersed with stirring is even; Add deionized water 633 kg, dispersed with stirring is even again, namely gets 1000 kilogram of 0.6 % micro nimbin emulsion.
Indoor, employing is soaked the worm immersion method and is measured 0.6 % micro nimbin emulsion to the control efficiency of beet armyworm 3 instar larvaes, 24 h " Invest, Then Investigate " lethality, and result of the test sees Table 3.
Table 3 employing is soaked the worm immersion method and is measured 0.6 % micro nimbin emulsion different formulations to the indoor pharmacodynamic test result of beet armyworm 3 instar larvaes
Can find that from table 3 result the neem oil medium that the present invention relates to is remarkable to 0.6 % micro nimbin emulsion synergistic effect.
The preparation of embodiment 7 10 % nimbin microemulsion formulations
In reactor, add successively nimbin 100 kg, soybean oil 200 kg, isopropyl alcohol 40 kg, polyoxyethylene polyoxypropylene block copolymer 50 kg, C12～14 APEOs, 60 kg, straight chain calcium dodecyl benzene sulfonate 50 kg, methyl polysiloxane 2 kg, stirring and dissolving is uniformly dispersed at 3000 rpm/min down cuts; Add deionized water 498 kg again, stir, high speed shear 30 min under 6000 rpm/min namely get 1000 kilogram of 10 % micro nimbin emulsion.
The preparation of embodiment 8 30 % nimbin microemulsion formulations
In reactor, add successively nimbin 300 kg, corn oil 200 kg, polyethylene glycol 20 kg, polyoxyethylene polyoxypropylene block copolymer 60 kg, anhydrosorbitol acid anhydride oleate 40 kg, straight chain calcium dodecyl benzene sulfonate 60 kg, methyl polysiloxane 1 kg, stirring and dissolving is uniformly dispersed at 5000 rpm/min down cuts; Add deionized water 319 kg again, stir, high speed shear 60 min under 8000 rpm/min namely get 1000 kilogram of 30 % micro nimbin emulsion.
The preparation of embodiment 9 55 % nimbin microemulsion formulations
In reactor, add successively nimbin 550 kg, tung oil 150 kg, ethylene glycol 10 kg, ethylene polyethenoxy ether 40 kg, C12～14 polyoxyethylene ether phosphates, 50 kg, straight chain calcium dodecyl benzene sulfonate 30 kg, methyl polysiloxane 2 kg, stirring and dissolving is uniformly dispersed at 4000 rpm/min down cuts; Add deionized water 168 kg, high speed shear 30 min under 7000 rpm/min namely get 1000 kilogram of 55 % micro nimbin emulsion again.
The preparation of the outstanding preparation of embodiment 10 2.5 % nimbins oil
In reactor, add successively nimbin 25 kg, neem oil 888 kg, polyoxyethylene polyoxypropylene block copolymer 25 kg, alkylbenzenesulfonate 10 kg, polycarboxylate 20 kg, hydroxyethylcellulose 30 kg, polysiloxanes 2 kg, mix and be placed on particle diameter that high speed shear ball-grinding machine high speed shear balls is milled to 90 % less than 4 um, namely get 1000 kilogram of 2.5 % nimbin oil suspending agent.
The preparation of the outstanding preparation of Comparative Examples 3 2.5 % nimbins oil
In reactor, add successively nimbin 25 kg, neem oil 888 kg, polyoxyethylene polyoxypropylene block copolymer 25 kg, alkylbenzenesulfonate 10 kg, polycarboxylate 20 kg, hydroxyethylcellulose 30 kg, polysiloxanes 2 kg, mix and be placed on sand milling in the sand mill, namely get 1000 kilogram of 2.5 % nimbin oil suspending agent.
Use the 2.5 % nimbin oil suspending agents control rice fulgorid of present embodiment preparation, in rice fulgorid peak period medication in 1～2 age, consumption is 6 g/ mus, adopt field cauline leaf spraying, the control efficiency of 7 days and 15 days is respectively 67.8 % and 98.2 % behind the medicine, and Comparative Examples 3 adopts same method to use according to same dose, and the control efficiency of 7 days and 15 days is respectively 56.7 % and 86.5 % behind the medicine.2.5 % nimbin oil suspending agents of embodiment of the invention preparation are to the preventive effect of rice fulgorid 2.5 % nimbin oil suspending agents significantly better than the preparation of Comparative Examples 3 sanding methods.
The preparation of the outstanding preparation of embodiment 11 15 % nimbins oil
In reactor, add successively nimbin 150 kg, peanut oil 744 kg, polyoxyethylene polyoxypropylene block copolymer 15 kg, anhydrosorbitol acid anhydride oleate 20 kg, polycarboxylate 20 kg, protruding Attapulgite 50 kg, polysiloxanes 1 kg, mix and be placed in the high speed shear ball-grinding machine, the particle diameter of high speed shear ball milling to 90 % namely gets 1000 kilogram of 15 % nimbin oil suspending agent less than 4 um.
The preparation of the outstanding preparation of embodiment 12 20 % nimbins oil
In reactor, add successively nimbin 200 kg, corn oil 663 kg, sorbitol polyoxyethylene ether 100 kg, naphthalene and alkylnaphthalene sulfonate formaldehyde condensation products 10 kg, oleic acid methylamino ethyl sulfonate 10 kg, aluminium-magnesium silicate 15 kg, polysiloxanes 2 kg, mix and be placed on particle diameter that high speed shear ball-grinding machine high speed shear balls is milled to 90 % less than 4 um, namely get 1000 kilogram of 20 % nimbin oil suspending agent.
The preparation of the outstanding preparation of embodiment 13 45 % nimbins oil
In reactor, add successively nimbin 450 kg, cashew nut oil 463 kg, fatty alcohol-polyoxyethylene ether 30 kg, naphthalene and alkylnaphthalene sulfonate formaldehyde condensation products 25 kg, polycarboxylate 30 kg, polysiloxanes 2 kg mix and are placed on particle diameter that high speed shear ball-grinding machine high speed shear balls is milled to 90 % less than 4 um, namely get 1000 kilogram of 45 % nimbin oil suspending agent.
The preparation of embodiment 14 1 % nimbin water-emulsion preparations
Take by weighing nimbin 10 kg, neem oil 300 kg, polyoxyethylene polyoxypropylene block copolymer phosphate 45 kg, pure APEO 50 kg in C12～14, n-octyl alcohol 30 kg mix and obtain oil phase; Take by weighing xanthans 2 kg, methyl polysiloxane 1 kg, water 562 kg mix and obtain water; Under stirring condition, water and oil phase are mixed, under 6000 rpm/min conditions, high speed shear emulsification 50 min namely get 1000 kilogram of 1 % nimbin aqueous emulsion.
The preparation of Comparative Examples 41 % nimbin water-emulsion preparations
Take by weighing nimbin 10 kg, dimethylbenzene 300 kg, polyoxyethylene polyoxypropylene block copolymer phosphate 45 kg, pure APEO 50 kg in C12～14, n-octyl alcohol 30 kg mix and obtain oil phase; Take by weighing xanthans 2 kg, methyl polysiloxane 1 kg, water 562 kg mix and obtain water; Under stirring condition, water and oil phase are mixed, under 6000 rpm/min conditions, high speed shear emulsification 50 min namely get 1000 kilogram of 1 % nimbin aqueous emulsion.
Use the 1 % nimbin aqueous emulsion control paddy rice rice leaf roller of present embodiment preparation, according to active ingredient 40 g/ mu thin up field sprays, the control efficiency of 2 days and 5 days is respectively 80.2 % and 89.7 % behind the medicine, and 1 % nimbin aqueous emulsion of Comparative Examples 4, adopt same method to use according to same dose, the preventive effect of 2 days and 5 days is respectively 62.4 % and 72.8 % behind the medicine.1 % nimbin aqueous emulsion of embodiment of the invention preparation is better than to the preventive effect of rice leaf roller that to use dimethylbenzene be 1 % nimbin aqueous emulsion of the Comparative Examples 4 of solvent, has demonstrated good synergistic effect.
The preparation of embodiment 15 4.5 % nimbin water-emulsion preparations
Take by weighing nimbin 45 kg, linseed oil 60 kg, polyoxyethylene polyoxypropylene block copolymer 15 kg, pure APEO 10 kg in C12～14, sorbitan monooleate 20 kg, ethylene glycol 30 kg mix and obtain oil phase; Take by weighing polyvinylpyrrolidone 20 kg, methyl polysiloxane 3 kg, water 797 kg mix and obtain water; Under stirring condition, water and oil phase are mixed, under 4000 rpm/min conditions, high speed shear emulsification 60 min namely get 1000 kilogram of 4.5 % nimbin aqueous emulsion.
The preparation of embodiment 16 12.5 % nimbin water-emulsion preparations
Take by weighing nimbin 125 kg, castor oil 80 kg, N-dodecylpyrrolidone 50 kg, polyoxyethylene polyoxypropylene block copolymer phosphate 15 kg, pure APEO 15 kg in C12～14, ethylene glycol 20 kg mix and obtain oil phase; Take by weighing polyvinylpyrrolidone 20 kg, methyl polysiloxane 3 kg, water 672 kg mix and obtain water; Under stirring condition, water and oil phase are mixed, under 8000 rpm/min conditions, high speed shear emulsification 30 min namely get 1000 kilogram of 12.5 % nimbin aqueous emulsion.
The preparation of embodiment 17 24 % nimbin water-emulsion preparations
Take by weighing nimbin 240 kg, olive oil 150 kg, NOP 40 kg, polyoxyethylene polyoxypropylene block copolymer phosphate 30 kg, pure APEO 10 kg in C12～14, anhydrosorbitol acid anhydride oleate 30 kg, propane diols 20 kg mix and obtain oil phase; Weighing polyvinyl alcohol 10 kg, methyl polysiloxane 1 kg, water 469 kg mix and obtain water; Under stirring condition, water and oil phase are mixed, under 10000 rpm/min conditions, high speed shear emulsification 60 min namely get 1000 kilogram of 24 % nimbin aqueous emulsion.
The preparation of embodiment 18 50 % nimbin water-emulsion preparations
Take by weighing nimbin 500 kg, neem oil 100 kg, NOP 30 kg, polyoxyethylene sorbitan monolaurate 20 kg, polyoxyethylene 20 sorbitan monooleate 10 kg, polyethylene glycol 20 kg mix and obtain oil phase; Weighing polyvinyl alcohol 20 kg, methyl polysiloxane 2 kg, water 298 kg mix and obtain water; Under stirring condition, water and oil phase are mixed, under 4000 rpm/min conditions, high speed shear emulsification 60 min namely get 1000 kilogram of 50 % nimbin aqueous emulsion.
The preparation of Comparative Examples 5 50 % nimbin water-emulsion preparations
Take by weighing nimbin 500 kg, dimethylbenzene 100 kg, NOP 30 kg, polyoxyethylene sorbitan monolaurate 20 kg, polyoxyethylene 20 sorbitan monooleate 10 kg, polyethylene glycol 20 kg mix and obtain oil phase; Weighing polyvinyl alcohol 20 kg, methyl polysiloxane 2 kg, water 298 kg mix and obtain water; Under stirring condition, water and oil phase are mixed, under 4000 rpm/min conditions, high speed shear emulsification 60 min namely get 1000 kilogram of 50 % nimbin aqueous emulsion.
Use the 50 % nimbin aqueous emulsions control mandarin tree two spotted spider mite of present embodiment preparation, according to active ingredient
2 g/ mu thin up field sprays, the control efficiency of 2 days and 5 days is respectively 78.6 % and 90.7 % behind the medicine,
And 50 % nimbin aqueous emulsions of Comparative Examples 5 adopt same method to use according to same dose, behind the medicine 2 days
Be respectively 62.8 % and 74.1 % with 5 days preventive effect.Embodiment of the invention preparation take neem oil as medium
50 % nimbin aqueous emulsions are better than the 50 % seal that application dimethylbenzene is the Comparative Examples 5 of solvent to the preventive effect of two spotted spider mite
Chinaberry element aqueous emulsion has demonstrated good synergistic effect.
Claims (23)
1. the nimbin preparation take vegetable oil as medium it is characterized in that being take vegetable oil as the medium nimbin main active insecticidal components, allocates cosolvent into, emulsifier is configured to the nimbin emulsion preparation; Allocate cosolvent, emulsifier, defoamer and water into and be configured to the nimbin microemulsion formulation; Allocate emulsifier, wetting dispersing agent, suspension stabilizer, defoamer into and be configured to the outstanding preparation of nimbin oil; Allocate cosolvent, emulsifier, thickener, defoamer and water into and be configured to the nimbin water-emulsion preparation.
2. the nimbin preparation take vegetable oil as medium according to claim 1 is characterized in that described medium vegetable oil is selected from any one or more in neem oil, Jatropha curcas oil, soybean oil, peanut oil, rapeseed oil, palm oil, castor oil, cocoa butter, linseed oil, cottonseed oil, sunflower oil, safflower oil, tung oil, perilla oil, cannabis oil, cashew nut oil, olive oil, the corn oil.
3. the nimbin preparation take vegetable oil as medium according to claim 1, it is characterized in that each component content proportioning is in the described nimbin emulsion preparation: Azadirachtin Cotent is 0.1 %～92 %(weight); Content of vegetable oil is 0.5 %～95 %(weight); Cosolvent content is 0 %～15 %(weight); Emulsifier content is 5 %～15 %(weight); Each component summation is 100 %.
4. the nimbin preparation take vegetable oil as medium according to claim 1, it is characterized in that each component content proportioning is in the described nimbin microemulsion formulation: Azadirachtin Cotent is 0.5 %～60 %(weight); Content of vegetable oil is 1 %～30 %(weight); Cosolvent content is 0 %～10 %(weight); Emulsifier content is 5 %～25 %(weight); Antifoam content is 0.1 %～0.3 %(weight); Yu Weishui, each component summation is 100 %.
5. the nimbin preparation take vegetable oil as medium according to claim 1, it is characterized in that each component content proportioning is in the outstanding preparation of described nimbin oil: Azadirachtin Cotent is 1 %～50 %(weight); Content of vegetable oil is 1 %～90 %(weight); Emulsifier content is 1 %～10 %(weight); Wetting dispersing agent content is 2 %～10 %(weight); Suspending stabilized agent content is 0 %～5 %(weight); Antifoam content is 0.1 %～0.5 %(weight); Each component summation is 100 %.
6. the nimbin preparation take vegetable oil as medium according to claim 1, it is characterized in that each component content proportioning is in the described nimbin water-emulsion preparation: Azadirachtin Cotent is 0.5 %～60 %(weight); Content of vegetable oil is 1 %～30 %(weight); Cosolvent content is 0 %～10 %(weight); Emulsifier content is 5 %～20 %(weight); Amount of thickener is 0 %～1 %(weight); Antifoam content is 0.1 %～0.3 %(weight); Yu Weishui, each component summation is 100 %.
According to claim 1 with 3 described nimbin preparations take vegetable oil as medium, it is characterized in that co-solvent component in the described nimbin emulsion preparation is to be selected from isooctanol, n-octyl alcohol, isobutanol, n-butanol, isopropyl alcohol, ethylene glycol, polyethylene glycol, ethanol, NOP, N-ethyl pyrrolidone, 1-METHYLPYRROLIDONE, the azone any one or more.
According to claim 1 with 3 described nimbin preparations take vegetable oil as medium, it is characterized in that emulsifier component is to be selected from polyoxyethylene polyoxypropylene block copolymer in the described nimbin emulsion preparation, the pure APEO in C12～14, sorbitol polyoxyethylene ether, castor oil polyoxyethylene ether, ethylene polyethenoxy ether, anhydrosorbitol acid anhydride oleate, anhydrous sorbitol acid anhydride trioleate, polyoxyethylene sorbitan monolaurate, the alkane polyoxyethylene 20 sorbitan monooleate, sorbierite polyoxy ether, Brij30, aliphatic alcohol polyoxyvinethene phosphate, calcium dodecyl benzene sulfonate, alkyl polyglycol ether phosphate, ethoxylated alkyl phosphate, in the ethoxylated alkyl sulfates any one or more.
According to claim 1 with 4 described nimbin preparations take vegetable oil as medium, it is characterized in that co-solvent component in the described nimbin microemulsion formulation is to be selected from isooctanol, n-octyl alcohol, isobutanol, n-butanol, isopropyl alcohol, ethylene glycol, polyethylene glycol, ethanol, glycerine, NOP, N-dodecylpyrrolidone, the spectrasolv DMDA any one or more.
According to claim 1 with 4 described nimbin preparations take vegetable oil as medium, it is characterized in that emulsifier component is to be selected from polyoxyethylene polyoxypropylene block copolymer in the described nimbin microemulsion formulation, the pure APEO in C12～14, sorbitol polyoxyethylene ether, castor oil polyoxyethylene ether, ethylene polyethenoxy ether, anhydrosorbitol acid anhydride oleate, polyoxyethylene sorbitan monolaurate, the alkane polyoxyethylene 20 sorbitan monooleate, the polyoxyethylene polyoxypropylene block copolymer phosphate, C12～14 polyoxyethylene ether phosphates, the straight chain calcium dodecyl benzene sulfonate, straight chain DBSA amine, alkyl polyglycol ether phosphate, in the ethoxylated alkyl phosphate any one or more.
11. with 4 described nimbin preparations take vegetable oil as medium, it is characterized in that component of antifoam agent is to be selected from methyl polysiloxane in the described nimbin microemulsion formulation according to claim 1.
12. according to claim 1 with 5 described nimbin preparations take vegetable oil as medium, it is characterized in that emulsifier component in the outstanding preparation of described nimbin oil is to be selected from polyoxyethylene polyoxypropylene block copolymer, fatty alcohol-polyoxyethylene ether, sorbitol polyoxyethylene ether, polyoxyethylene groups Arrcostab, anhydrosorbitol acid anhydride oleate, sorbitol monooleate, the alkylbenzenesulfonate any one or more.
13. according to claim 1 with 5 described nimbin preparations take vegetable oil as medium, it is characterized in that wetting dispersing agent component in the outstanding preparation of described nimbin oil is to be selected from macromolecular grafted lignosulfonates, polycarboxylate, rosin grafting polymer carboxylate, naphthalene and alkylnaphthalene sulfonate formaldehyde condensation products, the oleic acid methylamino ethyl sulfonate any one or more.
14. according to claim 1 with 5 described nimbin preparations take vegetable oil as medium, it is characterized in that suspension stabilizer component in the outstanding preparation of described nimbin oil is to be selected from protruding Attapulgite, bentonite, aluminium-magnesium silicate, imvite, the hydroxyethylcellulose any one or more.
15. according to claim 1 with 5 described nimbin preparations take vegetable oil as medium, it is characterized in that defoamer is to be selected from polysiloxanes in the outstanding preparation of described nimbin oil.
16. according to claim 1 with 6 described nimbin preparations take vegetable oil as medium, it is characterized in that co-solvent component in the described nimbin water-emulsion preparation is to be selected from isooctanol, n-octyl alcohol, isobutanol, n-butanol, isopropyl alcohol, ethylene glycol, polyethylene glycol, ethanol, glycerine, propane diols, NOP, the N-dodecylpyrrolidone any one or more.
17. with 6 described nimbin preparations take vegetable oil as medium, it is characterized in that emulsifier component is to be selected from polyoxyethylene polyoxypropylene block copolymer in the described nimbin water-emulsion preparation according to claim 1, the pure APEO in C12～14, sorbitol polyoxyethylene ether, castor oil polyoxyethylene ether, ethylene polyethenoxy ether, anhydrosorbitol acid anhydride oleate, polyoxyethylene sorbitan monolaurate, polyoxyethylene 20 sorbitan monooleate, the polyoxyethylene polyoxypropylene block copolymer phosphate, in C12～14 polyoxyethylene ether phosphates any one or more.
18. according to claim 1 with 6 described nimbin preparations take vegetable oil as medium, it is characterized in that thickener component in the described nimbin water-emulsion preparation is to be selected from xanthans, polyvinyl alcohol, aluminium-magnesium silicate, polyvinylpyrrolidone, gum Arabic, the acrylate any one or more.
19. with 6 described nimbin preparations take vegetable oil as medium, it is characterized in that component of antifoam agent is to be selected from methyl polysiloxane in the described nimbin water-emulsion preparation according to claim 1.
20. according to claim 1 with 3 described nimbin preparations take vegetable oil as medium, the preparation method who it is characterized in that described nimbin emulsion preparation is: by ratio requirement nimbin, vegetable oil, cosolvent, emulsifier are added in the reactor, stirring and dissolving, namely being able to vegetable oil is the nimbin emulsion preparation of medium.
21. according to claim 1 with 4 described nimbin preparations take vegetable oil as medium, the preparation method who it is characterized in that described nimbin microemulsion formulation is: by ratio requirement nimbin, vegetable oil, cosolvent, emulsifier, defoamer are added in the reactor, be uniformly dispersed in 2000～5000 rpm/min shearing, the water that adds surplus, high speed shear 20～60 min under 5000～8000 rpm/min, namely being able to vegetable oil is the nimbin microemulsion formulation of medium.
22. according to claim 1 with 5 described nimbin preparations take vegetable oil as medium, the preparation method who it is characterized in that the outstanding preparation of described nimbin oil is: after by ratio requirement nimbin, vegetable oil, emulsifier, wetting dispersing agent, suspension stabilizer, defoamer being mixed, place the particle diameter of high speed shear ball-grinding machine ball milling to 90 % less than 4 μ m, namely being able to vegetable oil is the outstanding preparation of nimbin oil of medium.
23. with 6 described nimbin preparations take vegetable oil as medium, it is characterized in that the preparation method of described nimbin water-emulsion preparation is according to claim 1:
1) oil phase preparation
By ratio requirement nimbin, vegetable oil, emulsifier, cosolvent are added in the reactor, mix, go into oil phase;
2) water preparation
By ratio requirement thickener, defoamer and water are mixed, go into water;
3) high-shear emulsifying
Under stirring condition, water and oil phase are mixed, under 4000～10000 rpm/min conditions, high speed shear emulsification 20～60 min, namely being able to vegetable oil is the nimbin water-emulsion preparation of medium.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103299992A (en) * | 2013-06-20 | 2013-09-18 | 中国林业科学研究院资源昆虫研究所 | Azadirachtin microemulsion and preparation method thereof |
| CN104255747A (en) * | 2014-09-02 | 2015-01-07 | 石家庄市青冠化工有限公司 | Environment-friendly azadirachtin missible oil and preparation method thereof |
| CN104872114A (en) * | 2014-06-13 | 2015-09-02 | 中国日用化学工业研究院 | Environmentally friendly insecticidal microemulsion and preparation technology thereof |
| CN105660664A (en) * | 2016-02-19 | 2016-06-15 | 河北岗恩生物科技有限公司 | Azadirachtin aromatic-free missible oil and preparation method thereof |
| CN109315413A (en) * | 2018-11-15 | 2019-02-12 | 深圳职业技术学院 | A kind of nimbin ultra low volume liquids and preparation method thereof |
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| CN112243347A (en) * | 2018-06-04 | 2021-01-19 | 特瑞美睿股份有限公司 | Pesticidal compositions with improved physical characteristics |
| CN113518555A (en) * | 2018-12-31 | 2021-10-19 | 特瑞美睿股份有限公司 | Emulsifier system for agricultural compositions comprising pesticidal natural oils |
| CN113841691A (en) * | 2021-11-09 | 2021-12-28 | 成都绿金生物科技有限责任公司 | Oil suspending agent containing azadirachtin and preparation method thereof |
| WO2022248293A1 (en) * | 2021-05-26 | 2022-12-01 | Basf Se | New method for controlling pests |
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| CN1276161A (en) * | 2000-04-27 | 2000-12-13 | 华南农业大学 | Plant-type nimbin insecticide |
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| CN103299992A (en) * | 2013-06-20 | 2013-09-18 | 中国林业科学研究院资源昆虫研究所 | Azadirachtin microemulsion and preparation method thereof |
| CN104872114A (en) * | 2014-06-13 | 2015-09-02 | 中国日用化学工业研究院 | Environmentally friendly insecticidal microemulsion and preparation technology thereof |
| CN104255747A (en) * | 2014-09-02 | 2015-01-07 | 石家庄市青冠化工有限公司 | Environment-friendly azadirachtin missible oil and preparation method thereof |
| CN105660664A (en) * | 2016-02-19 | 2016-06-15 | 河北岗恩生物科技有限公司 | Azadirachtin aromatic-free missible oil and preparation method thereof |
| US11980193B2 (en) | 2018-04-10 | 2024-05-14 | Terramera, Inc. | Natural oil pesticidal compositions |
| CN112243347A (en) * | 2018-06-04 | 2021-01-19 | 特瑞美睿股份有限公司 | Pesticidal compositions with improved physical characteristics |
| CN112272520A (en) * | 2018-06-04 | 2021-01-26 | 特瑞美睿股份有限公司 | Improved natural oil pesticidal compositions |
| CN112272520B (en) * | 2018-06-04 | 2023-10-17 | 特瑞美睿股份有限公司 | Improved natural oil pesticide composition |
| CN112243347B (en) * | 2018-06-04 | 2023-10-20 | 特瑞美睿股份有限公司 | Pesticidal compositions with improved physical characteristics |
| CN109452273A (en) * | 2018-11-13 | 2019-03-12 | 钟祥品红植物免疫科技有限公司 | A kind of agricultural builder of safflower seed oil and its preparation method and application |
| CN109315413A (en) * | 2018-11-15 | 2019-02-12 | 深圳职业技术学院 | A kind of nimbin ultra low volume liquids and preparation method thereof |
| CN113518555A (en) * | 2018-12-31 | 2021-10-19 | 特瑞美睿股份有限公司 | Emulsifier system for agricultural compositions comprising pesticidal natural oils |
| WO2022248293A1 (en) * | 2021-05-26 | 2022-12-01 | Basf Se | New method for controlling pests |
| CN113841691A (en) * | 2021-11-09 | 2021-12-28 | 成都绿金生物科技有限责任公司 | Oil suspending agent containing azadirachtin and preparation method thereof |
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