CN107258778A

CN107258778A - The preparation method of pesticide nano capsules

Info

Publication number: CN107258778A
Application number: CN201710485419.4A
Authority: CN
Inventors: 崔海信; 王琰; 王安琪
Original assignee: Institute of Environment and Sustainable Development in Agriculturem of CAAS
Current assignee: Institute of Environment and Sustainable Development in Agriculturem of CAAS
Priority date: 2017-06-23
Filing date: 2017-06-23
Publication date: 2017-10-20
Anticipated expiration: 2037-06-23
Also published as: CN107258778B

Abstract

The present invention provides a kind of preparation method of pesticide nano capsules, and methods described includes：The component of pesticide nano capsules is formed into colostric fluid through emulsification, pesticide nano capsules then are made through high-pressure homogeneous formation miniemulsion.The preparation method for the pesticide nano capsules that the present invention is provided is simple, easy to operate, reproducible, and the pesticide nano capsules particle diameter prepared is small, particle dispersion is good and sustained release performance is excellent.

Description

The preparation method of pesticide nano capsules

Technical field

The invention belongs to technical field of pesticide.In particular it relates to a kind of preparation method of pesticide nano capsules.

Background technology

Agricultural chemicals is the important substance basis for ensureing national food security.Traditional formulations of pesticide are generally open system, from From the point of view of formulations of pesticide registration situation, the agricultural chemicals conventional dosage forms based on missible oil, wettable powder, microemulsion etc. account for domestic city More than 70% share of field, these conventional dosage forms belong to open system, there is medicine drop to some extent in use mostly Tumble, drift, the loss such as spring and dust drift, eventually arrive at the effective rate of utilization of crop target less than 30%, reach insect It is internal by dose less than 0.1%, the effective rate of utilization of agricultural chemicals is relatively low.

The differences such as globulate, hollow scrotiform are prepared by being wrapped up, being coupled using high polymer material by agricultural chemicals, inlayed etc. During the formulation of structure, wall material can provide physical barrier effect, thus can block ultraviolet light, and the illumination for significantly improving agricultural chemicals is stable Property, the absorption of soil is reduced, delays degraded caused by illumination or other undesirable elements, decompose and be lost in, while poison can be reduced Property, pollution abatement improves the prevention effect of product.Such formulation also has the effect of control release, according to dispenser scene not Together, spacetabs type and quick releasing type can be divided into.Spacetabs type is mainly used in soil treatment and seed treatment, and quick releasing type is mainly used in cauline leaf Spraying, ground surface blockage are administered and Aerial spraying.However, from the point of view of the registration situation of the current formulations of pesticide, relative to other formulations, The formulation proportions such as agricultural chemicals is spherical, scrotiform are less, and it is also relative complex that it researches and develops technique.

The traditional preparation methods of agricultural chemicals microballoon/microcapsule formulation mainly include situ aggregation method, interfacial polymerization, coacervation, Spray drying process etc..Wherein situ aggregation method need to be heated certain time when forming cyst wall, not only have certain to process equipment It is required that, and have an impact to the repeatability of product.Easily occur when preparing high concentration microballoon/microcapsule formulation using interfacial polymerization Crystalline polamer, the irregular crystal crystallized out can destroy cyst wall to lead to not play drug effect.Spray drying process is a kind of thing Preparation method is managed, the particle diameter of the agricultural chemicals microballoon/microcapsule formulation prepared using this method is larger, and particle diameter is difficult to realize nanometer scale. There is following defect in the agricultural chemicals microballoon/microcapsule formulation prepared at present using conventional method：In configuration aspects, presently commercially available agricultural chemicals The particle diameter of microballoon/microcapsule formulation is universal in 5 microns, not up to nanoscale, and thick particle diameter easily causes drop to tumble, powder Dirt drift so that the tack, permeability and bioavilability in use to crop target are poor, at the same activity also compared with It is low；In terms of particle dispersion, the monodispersity of the agricultural chemicals microballoon/microcapsule formulation prepared at present is poor, serious and particle diameter point of reuniting Cloth is uneven, and its surface nature and structure and morphology are not also regulated and controled effectively；It is existing in terms of the controllable sustained-release of agricultural chemicals Agricultural chemicals microballoon/microcapsule formulation can only be realized mostly simply, qualitatively slowly to be discharged, and rate of release is unstable controllable；In technique stream In terms of journey, using techniques, complex process, more difficult control and poor repeatability such as heating and thermal insulation, gas shields more than conventional method.

Therefore, how a kind of preparation side of simple, easy to operate, the reproducible agricultural chemicals microballoon/microcapsule formulation of technique is provided Method, so that it is urgently to be resolved hurrily as this area to prepare the pesticide nano capsules that particle diameter is small, particle dispersion is good and sustained release performance is excellent Problem.

The content of the invention

In view of the above-mentioned problems, it is an object of the invention to provide a kind of preparation method of pesticide nano capsules, the preparation side Method is simple, easy to operate, reproducible, and the pesticide nano capsules particle diameter prepared is small, particle dispersion good and slow release Can be excellent.

To reach above-mentioned purpose, the present invention provides a kind of preparation method of pesticide nano capsules, and methods described includes：By agriculture The component of medicine nano capsule forms colostric fluid through emulsification, and pesticide nano capsules then are made through high-pressure homogeneous formation miniemulsion.

In some embodiments, the preparation method comprises the following steps：

Step a：Pesticide activity component, organic solvent, cyst material, emulsifying dispersant and water are mixed, breast is then carried out Change, obtain colostric fluid；

Step b：By the colostric fluid obtained in step a by high-pressure homogeneous carry out fine crankshaft, miniemulsion is obtained；

Step c：By the miniemulsion obtained in step b stirring, organic solvent is volatilized, obtain Nano capsule mother liquor；

Step d：The Nano capsule mother liquor obtained in step c is mixed with excipient and adjuvant, pesticide nano glue is obtained Capsule.

In some embodiments, the pesticide nano capsules are hollow scrotiform, and the pesticide activity component includes interior phase Active components A and foreign minister's active component B, the step a include：Interior phase active components A is dispersed or dissolved in water, forms interior Foreign minister's active component B is dissolved in organic solvent by the suspension or the aqueous solution of phase active components A as interior aqueous phase, is added Cyst material, obtains oil phase, is added drop-wise in oil phase to obtain W/O (Water-In-Oil) type emulsion by interior aqueous phase under emulsification condition；Will Emulsifying dispersant, which is dissolved in the water, obtains outer aqueous phase, and obtained w/o type emulsion is added drop-wise in outer aqueous phase under emulsification condition, obtained To W/O/W (W/O/W) type colostric fluid.

In some embodiments, the pesticide nano capsules are pesticide nano capsules aqueous suspension agent, and the excipient is Thickener, the step d includes：Thickener and adjuvant are added in the Nano capsule mother liquor obtained in step c, mixing is equal It is even, obtain pesticide nano capsules aqueous suspension agent.

In some embodiments, the pesticide nano capsules are pesticide nano capsules pulvis, and the excipient is solid Filler, the step d includes：The Nano capsule mother liquor obtained in step c is obtained into solid powder after centrifugation and drying, added Solid packing and adjuvant, are well mixed, obtain pesticide nano capsules pulvis.

In some embodiments, " under the emulsification condition " in the step a be " under the conditions of ultrasonic emulsification ", " Under the conditions of emulsification pretreatment " or " under grinding emulsification condition ", preferably " under the conditions of emulsification pretreatment " and " in ultrasonic emulsification condition Under "；The particle diameter of the drop of the colostric fluid is 100-900nm, preferably 100-500nm.

Wherein described " under the conditions of ultrasonic emulsification " is to carry out ultrasonic emulsification, the ultrasonic wave powder using ultrasonic grinder The power of broken machine is 65-650W, more preferably preferably 325-637W, 585W；The time of ultrasonic emulsification is 2-30min, preferably 5- 25min, more preferably 15min.

Wherein described " under the conditions of emulsification pretreatment " is to carry out emulsification pretreatment, the high-speed shearing machine using high-speed shearing machine Shearing rotating speed be 10000-28000rmp, more preferably preferably 22000-28000rmp, 28000rmp；The time of emulsification pretreatment is 3-40min, preferably 3-30min, more preferably 15min.

Wherein described " under grinding emulsification condition " is to be ground emulsification using grinding distribution machine, grinds the frequency of emulsification For 30-50Hz, more preferably preferably 40-50Hz, 50Hz；The time of emulsification is ground for 5-60min, preferably 5-40min, more preferably 15min。

In some embodiments, the high-pressure homogeneous use high pressure homogenizer in the step b is carried out, high-pressure homogeneous pressure Power is 100-1200Pa, preferably 600-1000Pa, more preferably 900Pa；The high-pressure homogeneous time is 10min-2h, preferably 10min- 1h, more preferably 15min；The particle diameter of the drop of the miniemulsion is 10-500nm, preferably 10-100nm.

In some embodiments, it is stirred in the step c using electric mixer, mixing speed is 500- 1500rpm, preferably 1000-1500rpm, more preferably 1500rpm；Mixing time is 5-24h, preferably 10-20h, more preferably 12h.

In some embodiments, when the pesticide nano capsules are pesticide nano capsules pulvis, in the step d, 10-30min is centrifuged under rotating speed 4000-15000rpm using high speed freezing centrifuge；Preferably, using high speed freezing centrifuge 20-30min is centrifuged under rotating speed 4000-15000rpm；It is highly preferred that using high speed freezing centrifuge under rotating speed 15000rpm Centrifuge 20min.

In some embodiments, when the pesticide nano capsules are pesticide nano capsules pulvis, in the step d Dry as spray drying or be freeze-dried, wherein the spray drying is carried out using spray dryer, the condition of spray drying is 30-300 DEG C of EAT, 30-140 DEG C of leaving air temp, drying time 1-1.5s；The freeze-drying is entered using freeze drier OK, the condition of freeze-drying is the precooling 4h at -50 DEG C, keeps 12-24h at -60 DEG C；It is preferred that at -50 DEG C precooling 4h, keeps 12h at -60 DEG C.

In some embodiments, the thickness of the cyst wall of the pesticide nano capsules is 5-50nm, the pesticide nano glue The particle diameter of capsule is 20-1000nm, preferably smaller than equal to 100nm, more preferably less than 50nm；Preferably, the pesticide nano capsules The drugloading rate of pulvis is 0.01-90%, and the drugloading rate of the pesticide nano capsules aqueous suspension agent is 0.01-40%.

In some embodiments, by weight, the pesticide nano capsules are made up of following components：

Pesticide activity component：0.1-80 parts

Cyst material：0.1-40 parts

Emulsifying dispersant：0.2-30 parts

Organic solvent：10-200 parts

Water：20-350 parts

Excipient：0.1-200 parts

Adjuvant：0-20 parts,

Wherein, the ratio of the pesticide activity component and cyst material is 0.1:1-10:1.

In some embodiments, the pesticide activity component includes interior phase active components A and foreign minister active component B, institute Pesticide nano capsules are stated for pesticide nano capsules pulvis, wherein the excipient is solid packing, by weight, the agricultural chemicals is received Rice capsule powder is made up of following components：

Interior phase active components A：0-40 parts

Foreign minister's active component B：0.1-40 parts

Cyst material：0.1-40 parts

Emulsifying dispersant：0.2-30 parts

Organic solvent：10-200 parts

Water：20-350 parts

Solid packing：0.1-200 parts

Adjuvant：0-20 parts；

Preferably, by weight, the pesticide nano capsules pulvis is made up of following components：

Interior phase active components A：0-30 parts

Foreign minister's active component B：0.5-30 parts

Cyst material：0.5-30 parts

Emulsifying dispersant：0.5-20 parts

Organic solvent：10-100 parts

Water：50-200 parts

Solid packing：10-200 parts

Adjuvant：0-15 parts；

It is highly preferred that by weight, the pesticide nano capsules pulvis is made up of following components：

Interior phase active components A：0-20 parts

Foreign minister's active component B：1-20 parts

Cyst material：1-20 parts

Emulsifying dispersant：0.5-10 parts

Organic solvent：20-100 parts

Water：50-200 parts

Solid packing：10-200 parts

Adjuvant：0-15 parts.

In some embodiments, the pesticide nano capsules are pesticide nano capsules aqueous suspension agent, wherein the figuration Agent is thickener, by weight, and the pesticide nano capsules aqueous suspension agent is made up of following components：

Interior phase active components A：0-40 parts

Foreign minister's active component B：0.1-40 parts

Cyst material：0.1-40 parts

Emulsifying dispersant：0.2-30 parts

Organic solvent：10-200 parts

Water：20-350 parts

Thickener：0.1-30 parts

Adjuvant：0-20 parts；

Preferably, by weight, the pesticide nano capsules aqueous suspension agent is made up of following components：

Interior phase active components A：0-30 parts

Foreign minister's active component B：0.5-30 parts

Cyst material：0.5-30 parts

Emulsifying dispersant：0.5-20 parts

Organic solvent：10-100 parts

Water：50-200 parts

Thickener：1-20 parts

Adjuvant：0-15 parts；

Interior phase active components A：0-20 parts

Foreign minister's active component B：1-20 parts

Cyst material：1-20 parts

Emulsifying dispersant：0.5-10 parts

Organic solvent：20-100 parts

Water：50-200 parts

Thickener：1-10 parts

Adjuvant：0-15 parts.

In some embodiments, the interior phase active components A and foreign minister's active component B ratio are 0.2:1-4:1, it is excellent Select 0.2:1-0.6:1, more preferably 0.4:1；Preferably, the interior phase active components A is identical or different with foreign minister's active component B Material；Preferably, the interior phase active components A is water-soluble substances or liposoluble substance, and preferred water-soluble substances is described outer Phase active component B is liposoluble substance.

In some embodiments, the interior phase active components A and foreign minister's active component B are respectively selected from insecticide, sterilization One or more in agent, herbicide and plant growth regulator；The cyst material is degradable high polymer material.

In some embodiments, the insecticide is selected from following one or more：AVM, methylamino Avermectin Plain benzoate, gamma cyhalothrin, Rynaxypyr, pleocidin, indoxacarb, clothianidin, orthene, fourth sulphur Carbofuran, Hostathion, diazinon, many mite prestige, chlopyrifos, Biphenthrin, cyphenothrin, ethofenprox, decis, the chrysanthemum of cyanogen penta Ester, cyfluthrin, Tefluthrin, lythidathion, phoxim, imidacloprid and Diacloden, preferably Diacloden, pleocidin, chlorine worm benzene One or more in formamide, AVM, emamectin-benzoate and gamma cyhalothrin.

In some embodiments, the bactericide is selected from following one or more：Jinggangmeisu, Fluoxastrobin, pyrazoles Kresoxim-methyl, thifluzamide, Tebuconazole, metconazole, 2-cyano-3-amino-3-phenylancryic acetate, fluazinam, cymoxanil, Boscalid, ethofenprox, fourth fluorine mite Ester, Fenpropathrin, benzothiostrobin, pefurazoate, Prochloraz, propiconazole, Difenoconazoles, Metalaxyl-M, Flusilazole, epoxiconazole, oxime bacterium Ester and pyraclostrobin, preferably jinggangmeisu, Tebuconazole, thifluzamide, metconazole, 2-cyano-3-amino-3-phenylancryic acetate, fluazinam, Fluoxastrobin, pyrazoles One or more in kresoxim-methyl, cymoxanil and Boscalid.

In some embodiments, the herbicide is selected from following one or more：Pendimethalin, tri-allate, 2,4-D Different monooctyl ester, benthiocarb, molinate, cover grass energy, clomazone, butralin, S-metolachlor, trefanocide and prometryn, preferably two One or more in the spirit of first penta and S-metolachlor.

In some embodiments, the plant growth regulator is selected from following one or more：Brassinosteroid, ammonia Oxygen ethyl vinyl glycine and multiple-effect azole plant growth regulator, preferably multiple-effect azole plant growth regulator.

In some embodiments, the cyst material is selected from following one or more：Polyester acrylate and its spread out Biology, polyvinyl acetate resin, polyacrylonitrile resin, polystyrene resin, PLA, gelatin, modified starch, cellulose and its One kind in derivative, chitosan and Arabic gum, preferred cellulose and its derivative, chitosan, PLA and modified starch Or it is a variety of.

In some embodiments, the emulsifying dispersant is the one or more in agricultural emulsifier and dispersant, excellent Selection of land, the agricultural emulsifier is selected from the serial (Nonyl pheno of OP serial (OPEO, such as OP-10), NP Ether), EL serial (castor oil polyoxyethylene ether, such as EL 40), Tween series (tween, such as Tween 80, Tween 60, Tween 20), Span serial (sapn, such as Span 60, Span 80), AEO serial (AEO, such as AEO-9), agriculture breast system One kind or many in row emulsifying agent, polyvinyl alcohol, cithrol, polyvinylpyrrolidone and polyethylene glycol (PEG) oleate Kind；It is preferred that Tween is serial, the one or more in the serial emulsifying agent of polyvinyl alcohol and agriculture breast；More preferably polyvinyl alcohol, agriculture breast In 300 series, the series of agriculture breast 500, the series of agriculture breast 600, Nongru-700 series and serial (such as agriculture breast 1601) emulsifying agent of agriculture breast 1600 One or more.

In some embodiments, the dispersant is selected from carboxylate, sulfate, sulfonate, phosphate ester salt and alkyl phenol One or more in APEO, it is preferable that the dispersant is selected from aliphatic alcohol polyethenoxy ether carboxylate, dodecyl Sodium sulphate, lignosulfonates, dodecyl sodium sulfate, maleated rosin polyethenoxy-oxypropylene ether sulfonate and dodecyl In one or more in ether phosphate salt, more preferably lignosulfonates, lauryl sodium sulfate and dodecyl sodium sulfate One or more.

In some embodiments, the adjuvant is selected from preservative, defoamer, antifreeze, pH adjusting agent and wetting point One or more in powder, preferably antifreeze, defoamer and wetting dispersing agent (such as TERSPERSE 2020, TERSPERSE 1004) one or more in.

In some embodiments, the antifreeze is in ethylene glycol, propane diols, glycerine, isopropanol and urea One or more, preferably ethylene glycol.

In some embodiments, one or more of the defoamer in organic silicon and low-carbon alcohols defoamer, It is preferred that organic silicon defoamer.

In some embodiments, the thickener be selected from xanthans, Arabic gum, gelatin, cellulose and its derivates, It is one or more in diatomite, polyvinyl alcohol, Sodium Polyacrylate, dextrin, aluminium-magnesium silicate and Silica hydrogel, preferably xanthans, bright One or more in glue, aluminium-magnesium silicate, cellulose and its derivates and polyvinyl alcohol.

In some embodiments, the organic solvent is selected from dichloromethane, chloroform, vegetable oil, petroleum ether and fat One or more in fat hydrocarbon solvent oil, preferably dichloromethane.

In some embodiments, the solid packing be selected from bentonite, diatomite, kaolin, talcum powder, montmorillonite, In one or more in white carbon, cornstarch and sepiolite, preferably bentonite, kaolin, cornstarch and white carbon It is one or more.

By using the method for the present invention, can obtain nano level pesticide capsule, pesticide nano capsules due to its small size, Bigger serface and modifiability, the effective rate of utilization for raising agricultural chemicals provide a new approach.Utilize nano-carrier material Expect unique skin effect and small-size effect, both can be real by the mode carrying medicament such as adsorbing, being coupled, wrap up or inlay The high-efficient carrier of existing medicine, can also realize medicine on time, space and dosage by adjusting the fine structure of nano-carrier Intellectuality precisely release, minimum effective target activity is maintained in a period of setting, medicine is significantly increased has Effect property and security., can by the function such as the carrier loaded of nano medicament carrying system, water baseization scattered, targeting delivery, controlled release To improve the dispersiveness, stability and utilization rate of agricultural chemicals, extend the lasting period, reduce residual contamination.In addition, relative to micro-meter scale Microballoon/encapsulated form, the granularity of pesticide nano capsules reaches nanometer scale, and its small-size effect can spray process in field Ductility, wetability, the target adsorptivity of middle increase pesticide droplet, with advantage more efficiently with environmental protection, and nanometre glue Capsule is easier to be deposited on plant leaf blade, and its bigger serface characteristic adds the adhesiveness to target, and then reduces agricultural chemicals Loss.

High pressure homogenization method refers to liquid material under super-pressure effect, special homogeneous chamber generation is flowed through at a high speed tiny Drop.High pressure homogenization method can produce the particle of micro/nano level, effectively prevent particle from caking.The present invention uses new preparation Technique prepares pesticide nano capsules, specifically, and the present invention prepares pesticide nano capsules using emulsifying method.In the system of the present invention In Preparation Method, colostric fluid is prepared using the one or more in ultrasonic emulsification, emulsification pretreatment and grinding emulsification first, is then used High pressure homogenization method prepares miniemulsion, finally adds excipient and adjuvant obtains the pesticide nano capsules of favorable dispersibility.

The present invention prepares pesticide nano capsules using emulsifying method, and by adjusting component formula, technological process and step In rapid each parameter etc. prepared be uniformly dispersed, the pesticide nano capsules of function admirable.

Compared with prior art, the preparation method for the pesticide nano capsules that the present invention is provided has the advantage that：

1. in terms of preparation method, the present invention prepares pesticide nano capsules using emulsifying method, relative to traditional agriculture Medicine microballoon/microcapsule formulation preparation method, preparation method of the invention is carried out at normal temperatures, and mild condition, technique is relatively easy, more It is easily operated and reproducible, be conducive to industrialization；

2. in terms of particle diameter, pesticide nano capsules of the invention have Nano Particle, particle diameter is smaller than 50nm so that agriculture The specific surface area increase of medicine nano capsule, improves the contact area of agricultural chemicals and crop surface, adds agricultural chemicals on crop blade face Adhesiveness and permeability, be conducive to agricultural chemicals to be embedded into the micro-nano structure on crop blade face, strengthen blade face retention rate, reduce stream Lose, so as to improve the effective rate of utilization and drug effect of agricultural chemicals, reduce spray dosage and number of times；In addition, the pesticide nano of the present invention The particle diameter of capsule is smaller, the contact area increase with insect target, can increase the insecticidal activity to insect target；

3. in terms of particle dispersion, the monodispersity of the pesticide nano capsules prepared using the inventive method is good, grain Footpath is small and is evenly distributed；

4. in terms of the controllable sustained-release of agricultural chemicals, the slow release speed of the pesticide nano capsules prepared using the inventive method is accurate It is adjustable, can be by adjusting one in constituent content, particle size, appearance structure, cavernous structure, total pore volume, duct quantity etc. Plant or a variety of, to realize the control accurate of pesticide slow-release speed；The pesticide slow-release formulation prepared at present using conventional method Sustained release preventing and treating period regulation be limited, and use the inventive method prepare pesticide nano capsules the sustained release phase in -3 months 3 days, can Regulated and controled according to specific dispenser scene demand, effectively extend the sustained release phase of pesticidal preparations, so as to be conducive to improving agriculture The activity and reduction spray number of times and dosage of medicine；

5. in terms of material, the cyst walls of the pesticide nano capsules prepared using the inventive method using safety, low cost and Degradable high polymer material is made, and advantageously reduces the pollution to environment；

6. in terms of drugloading rate, the drugloading rate of the pesticide nano capsules prepared using the inventive method can be in 0.01-90% Between adjust, application is wider；

7. in terms of ultraviolet light degradation property, the anti-purple of pesticide nano capsules can be effectively improved using the inventive method Outer light degradation property, so as to drastically increase effective rate of utilization and bioavilability, reduces spraying times and dosage, is conducive to Environmental protection and ecological safety.

Brief description of the drawings

Fig. 1 is the microscope figure of emamectin-benzoate pesticide nano capsules prepared by the embodiment of the present invention Piece；

Fig. 2 is the elution profiles of avermectin pesticides Nano capsule prepared by the embodiment of the present invention；

Fig. 3 is the ultraviolet photolysis figure of pesticide nano capsules prepared by the embodiment of the present invention.

Embodiment

Illustrate the present invention referring to specific embodiment.It will be appreciated by those skilled in the art that these embodiments are only For illustrating the present invention, it does not limit the scope of the present invention in any way.

Experimental method in following embodiments, is conventional method unless otherwise specified.Medicine used in following embodiments Agent raw material, reagent material etc., unless otherwise specified, are commercially available products.

Instrument

Ultrasonic grinder (SCIENTZ, JY92-IIN)

High-speed shearing machine (FLUKO, FA25)

Grinding distribution machine (SGN, GMSD2000/4)

High pressure homogenizer (ATS, AH-100D)

Electric mixer (IKA, EUROSTAR 60)

High speed freezing centrifuge (Thermo SCIENTIFIC, ST 16R)

Freeze drier (BIOCOOL, Pilot2-4M)

SEM (Hitachi, SU8010)

Environmental scanning electron microscope (FEI, Quanta FEG 250)

Nanometer laser particle size analyzer (Malvern, Nano ZS90)

High performance liquid chromatography (Agilent, 1260)

Agricultural chemicals photo-stability testing case (Xutemp, XT5409-XPC80)

The preparation of the pesticide nano capsules pulvis 1 of embodiment 1

Phase active components A Diacloden in 0.8g is scattered in 20ml water, interior aqueous phase is obtained, by 2g foreign minister's active component B Emamectin-benzoate is dissolved in 50ml organic solvent dichloromethanes, is added 2g cyst material celluloses, is obtained Interior aqueous phase, is added drop-wise in oil phase, ultrasonic emulsification 15min by oil phase using ultrasonic grinder under 585W, obtains w/o type breast Liquid；2g emulsifying dispersants (1g polyvinyl alcohol and 1g dodecyl sodium sulfates) are dissolved in 150ml water and obtain outer aqueous phase, are used Obtained w/o type emulsion is added drop-wise in outer aqueous phase by high shear machine under 28000rmp, and emulsification pretreatment 15min obtains W/O/W The particle diameter of the drop of type colostric fluid, wherein colostric fluid is 300nm.

Using high pressure homogenizer under 900Pa by above-mentioned W/O/W types colostric fluid high pressure homogenizing 15min, obtain miniemulsion, Wherein the particle diameter of the drop of miniemulsion is 100nm.

Above-mentioned miniemulsion is stirred at 1500 rpm by 24h using electric mixer, organic solvent is volatilized, obtains nanometer Capsule mother liquor.

Above-mentioned Nano capsule mother liquor is centrifuged into 20min using high speed freezing centrifuge under 10000rpm, then using cold Lyophilizer precooling 4h at -50 DEG C, 12h is kept at -60 DEG C, obtains solid powder, adds 100g solid packing swellings Soil and 1g adjuvant TERSPERSE2020, are well mixed, obtain pesticide nano capsules pulvis 1.

The preparation of the pesticide nano capsules aqueous suspension agent 2 of embodiment 2

1g thickeners (0.5g xanthans and 0.5g aluminium-magnesium silicates) are added in above-mentioned Nano capsule mother liquor, are well mixed, Obtain pesticide nano capsules aqueous suspension agent 2.

The preparation of the pesticide nano capsules pulvis 3 of embodiment 3

Phase active components A emamectin-benzoate in 0.5g is scattered in 50ml water, interior aqueous phase is obtained, will 2g foreign minister's active component B emamectin-benzoates are dissolved in 100ml organic solvent dichloromethanes, add 3g cyst walls Material PLA, obtains oil phase, interior aqueous phase is added drop-wise in oil phase under 585W using ultrasonic grinder, ultrasonic emulsification 15min, obtains w/o type emulsion；3.5g emulsifying dispersants (1g polyvinyl alcohol, 1.5g agriculture breasts 600 and 1g Nongru-700s) are dissolved in Outer aqueous phase is obtained in 300ml water, obtained w/o type emulsion is added drop-wise to by outer aqueous phase under 28000rmp using high shear machine In, emulsification pretreatment 15min obtains W/O/W type colostric fluids, the wherein particle diameter of the drop of colostric fluid is 300nm.

Above-mentioned Nano capsule mother liquor is centrifuged into 20min using high speed freezing centrifuge under 10000rpm, then using cold Lyophilizer precooling 4h at -50 DEG C, 12h is kept at -60 DEG C, obtains solid powder, adds 100g solid packing swellings Soil and 1g adjuvant TERSPERSE2020, are well mixed, obtain pesticide nano capsules pulvis 3.

The preparation of the pesticide nano capsules aqueous suspension agent 4 of embodiment 4

1g thickeners (0.5g xanthans and 0.5g aluminium-magnesium silicates) are added in above-mentioned Nano capsule mother liquor, are well mixed, Obtain pesticide nano capsules aqueous suspension agent 4.

The preparation of the pesticide nano capsules pulvis 5 of embodiment 5

Phase active components A jinggangmeisu in 1.6g is dissolved in 20ml water, interior aqueous phase is obtained, by 4g foreign minister's active component B thifluzamides are dissolved in 50ml organic solvent dichloromethanes, are added 2g cyst material celluloses, oil phase are obtained, using ultrasound Interior aqueous phase is added drop-wise in oil phase by ripple pulverizer under 585W, and ultrasonic emulsification 15min obtains w/o type emulsion；By 2g emulsion dispersions Agent (1g polyvinyl alcohol and 1g dodecyl sodium sulfates), which is dissolved in 150ml water, obtains outer aqueous phase, is existed using high shear machine Obtained w/o type emulsion is added drop-wise in outer aqueous phase under 28000rmp, emulsification pretreatment 15min, obtains W/O/W type colostric fluids, its The particle diameter of the drop of middle colostric fluid is 300nm.

Above-mentioned Nano capsule mother liquor is centrifuged into 20min using high speed freezing centrifuge under 10000rpm, then using cold Lyophilizer precooling 4h at -50 DEG C, 12h is kept at -60 DEG C, obtains solid powder, adds 100g solid packing swellings Soil and 1g adjuvants TERSPERSE 2020, are well mixed, obtain pesticide nano capsules pulvis 5.

The preparation of the pesticide nano capsules aqueous suspension agent 6 of embodiment 6

1g thickener xanthans is added in above-mentioned Nano capsule mother liquor, is well mixed, pesticide nano capsules water is obtained and hangs Floating agent 6.

The preparation of the pesticide nano capsules pulvis 7 of embodiment 7

Phase active components A AVM in 1.2g is scattered in 20ml water, interior aqueous phase is obtained, by 2g foreign minister's active component B AVMs are dissolved in 50ml organic solvent dichloromethanes, are added 2g cyst material PLAs, oil phase are obtained, using ultrasound Interior aqueous phase is added drop-wise in oil phase by ripple pulverizer under 585W, and ultrasonic emulsification 15min obtains w/o type emulsion；By 3g emulsion dispersions Agent (2g polyvinyl alcohol, 0.5g agriculture breasts 1601 and 0.5g OP-10), which is dissolved in 150ml water, obtains outer aqueous phase, using high shear Obtained w/o type emulsion is added drop-wise in outer aqueous phase by machine under 28000rmp, and emulsification pretreatment 15min obtains W/O/W type colostrums The particle diameter of the drop of liquid, wherein colostric fluid is 300nm.

Above-mentioned Nano capsule mother liquor is centrifuged into 20min using high speed freezing centrifuge under 10000rpm, then using cold Lyophilizer precooling 4h at -50 DEG C, 12h is kept at -60 DEG C, obtains solid powder, adds 50g solid packing bentonites With 1g adjuvant TERSPERSE2020, it is well mixed, obtains pesticide nano capsules pulvis 7.

The preparation of the pesticide nano capsules aqueous suspension agent 8 of embodiment 8

2g thickener xanthans is added in above-mentioned Nano capsule mother liquor, is well mixed, pesticide nano capsules water is obtained and hangs Floating agent 8.

The preparation of the pesticide nano capsules pulvis 9 of embodiment 9

Using 20ml pure water as interior aqueous phase, 2g foreign minister's active component B 2-cyano-3-amino-3-phenylancryic acetates are dissolved in 50ml organic solvent dichloros In methane, 2g cyst material PLAs are added, oil phase is obtained, interior aqueous phase is added drop-wise to by oil under 585W using ultrasonic grinder Xiang Zhong, ultrasonic emulsification 15min, obtain w/o type emulsion；2g emulsifying dispersants Tween 80 is dissolved in 150ml water and obtains outer Obtained w/o type emulsion, is added drop-wise in outer aqueous phase, emulsification pretreatment 15min by aqueous phase using high shear machine under 28000rmp, W/O/W type colostric fluids are obtained, the wherein particle diameter of the drop of colostric fluid is 300nm.

Above-mentioned Nano capsule mother liquor is centrifuged into 20min using high speed freezing centrifuge under 10000rpm, then using cold Lyophilizer precooling 4h at -50 DEG C, 12h is kept at -60 DEG C, obtains solid powder, adds 50g solid packing bentonites With 1g adjuvant TERSPERSE2020, it is well mixed, obtains pesticide nano capsules pulvis 9.

The preparation of the pesticide nano capsules aqueous suspension agent 10 of embodiment 10

Using 20ml pure water as interior aqueous phase, 2g foreign minister's active component B 2-cyano-3-amino-3-phenylancryic acetates are dissolved in 50ml organic solvent dichloros In methane, 2g cyst material PLAs are added, oil phase is obtained, interior aqueous phase is added drop-wise to by oil under 585W using ultrasonic grinder Xiang Zhong, ultrasonic emulsification 15min, obtain w/o type emulsion；1.5g emulsifying dispersants Tween 80 is dissolved in 150ml water and obtained Obtained w/o type emulsion, is added drop-wise in outer aqueous phase, emulsification pretreatment by outer aqueous phase using high shear machine under 28000rmp 15min, obtains W/O/W type colostric fluids, the wherein particle diameter of the drop of colostric fluid is 300nm.

3g thickeners (2g xanthans and 1g aluminium-magnesium silicates) are added in above-mentioned Nano capsule mother liquor, is well mixed, obtains Pesticide nano capsules aqueous suspension agent 10.

The preparation of the pesticide nano capsules pulvis 11 of embodiment 11

Phase active components A Rynaxypyr in 0.8g is scattered in 20ml water, interior aqueous phase is obtained, by 2g foreign minister's activity Composition B Diaclodens are dissolved in 50ml organic solvent dichloromethanes, are added 2g cyst material celluloses, are obtained oil phase, using super Interior aqueous phase is added drop-wise in oil phase by sonic disintegrator under 585W, and ultrasonic emulsification 15min obtains w/o type emulsion；2.5g is emulsified Dispersant (1g polyvinyl alcohol and 1.5g dodecyl sodium sulfates), which is dissolved in 150ml water, obtains outer aqueous phase, using high shear Obtained w/o type emulsion is added drop-wise in outer aqueous phase by machine under 28000rmp, and emulsification pretreatment 15min obtains W/O/W type colostrums The particle diameter of the drop of liquid, wherein colostric fluid is 300nm.

Above-mentioned Nano capsule mother liquor is centrifuged into 20min using high speed freezing centrifuge under 10000rpm, then using cold Lyophilizer precooling 4h at -50 DEG C, 12h is kept at -60 DEG C, obtains solid powder, adds 150g solid packing swellings Soil and 1g adjuvant TERSPERSE2020, are well mixed, obtain pesticide nano capsules pulvis 11.

The preparation of the pesticide nano capsules aqueous suspension agent 12 of embodiment 12

1g thickener xanthans is added in above-mentioned Nano capsule mother liquor, is well mixed, pesticide nano capsules water is obtained and hangs Floating agent 12.

The preparation of the pesticide nano capsules pulvis 13 of embodiment 13

Phase active components A Rynaxypyr in 1g is scattered in 10ml water, interior aqueous phase is obtained, by 2g foreign minister activity into Divide B gamma cyhalothrins to be dissolved in 20ml organic solvent dichloromethanes, add 2g cyst material celluloses, obtain oil phase, Interior aqueous phase is added drop-wise in oil phase under 585W using ultrasonic grinder, ultrasonic emulsification 15min obtains w/o type emulsion；By 2g Emulsifying dispersant polyvinyl alcohol is dissolved in 150ml water obtains outer aqueous phase, will be obtained under 585W using ultrasonic grinder W/o type emulsion is added drop-wise in outer aqueous phase, ultrasonic emulsification 15min, obtains W/O/W type colostric fluids, the wherein grain of the drop of colostric fluid Footpath is 300nm.

Using high pressure homogenizer under 900Pa by above-mentioned W/O/W types colostric fluid high pressure homogenizing 10min, obtain miniemulsion, Wherein the particle diameter of the drop of miniemulsion is 100nm.

Above-mentioned Nano capsule mother liquor is centrifuged into 20min using high speed freezing centrifuge under 10000rpm, then using cold Lyophilizer precooling 4h at -50 DEG C, 12h is kept at -60 DEG C, obtains solid powder, adds 150g solid packing kaolinites Soil and 2g adjuvant TERSPERSE2020, are well mixed, obtain pesticide nano capsules pulvis 13.

The preparation of the pesticide nano capsules aqueous suspension agent 14 of embodiment 14

1g thickeners (0.5g xanthans and 0.5g aluminium-magnesium silicates) are added in above-mentioned Nano capsule mother liquor, are well mixed, Obtain pesticide nano capsules aqueous suspension agent 14.

The preparation of the pesticide nano capsules pulvis 15 of embodiment 15

Phase active components A emamectin-benzoate in 1g is scattered in 20ml water, interior aqueous phase is obtained, by 2g Foreign minister's active component B gamma cyhalothrins are dissolved in 50ml organic solvent dichloromethanes, add 2g cyst material celluloses, Oil phase is obtained, interior aqueous phase is added drop-wise in oil phase under 28000rmp using high shear machine, emulsification pretreatment 15min obtains W/O Type emulsion；2.5g emulsifying dispersants (1g polyvinyl alcohol and 1.5g EL40) are dissolved in 150ml water and obtain outer aqueous phase, are used Obtained w/o type emulsion is added drop-wise in outer aqueous phase by grinding distribution machine at 50 hz, grinding emulsification 15min, at the beginning of obtaining W/O/W types The particle diameter of the drop of emulsion, wherein colostric fluid is 250nm.

Using high pressure homogenizer under 900Pa by above-mentioned W/O/W types colostric fluid high pressure homogenizing 10min, obtain miniemulsion, Wherein the particle diameter of the drop of miniemulsion is 90nm.

Above-mentioned miniemulsion is stirred at 1500 rpm by 12h using electric mixer, organic solvent is volatilized, obtains nanometer Capsule mother liquor.

Above-mentioned Nano capsule mother liquor is centrifuged into 20min using high speed freezing centrifuge under 10000rpm, then using cold Lyophilizer precooling 4h at -50 DEG C, 12h is kept at -60 DEG C, obtains solid powder, adds 80g solid packing kaolin With 2g adjuvant TERSPERSE2020, it is well mixed, obtains pesticide nano capsules pulvis 15.

The preparation of the pesticide nano capsules aqueous suspension agent 16 of embodiment 16

1.5g thickeners (1g xanthans and 0.5g aluminium-magnesium silicates) are added in above-mentioned Nano capsule mother liquor, are well mixed, Obtain pesticide nano capsules aqueous suspension agent 16.

The preparation of the pesticide nano capsules pulvis 17 of embodiment 17

Phase active components A Diacloden in 0.5g is scattered in 10ml water, interior aqueous phase is obtained, by 2g foreign minister's active component B Gamma cyhalothrin is dissolved in 50ml organic solvent dichloromethanes, is added 2g cyst material PLAs, is obtained oil phase, is used Interior aqueous phase is added drop-wise in oil phase by ultrasonic grinder under 585W, and ultrasonic emulsification 15min obtains w/o type emulsion；3g is emulsified Dispersant (1g polyvinyl alcohol and 2g dodecyl sodium sulfates), which is dissolved in 90ml water, obtains outer aqueous phase, is existed using grinding distribution machine Obtained w/o type emulsion is added drop-wise in outer aqueous phase under 50Hz, grinding emulsification 15min obtains W/O/W type colostric fluids, wherein just The particle diameter of the drop of emulsion is 300nm.

Using high pressure homogenizer under 900Pa by above-mentioned W/O/W types colostric fluid high pressure homogenizing 10min, obtain miniemulsion, Wherein the particle diameter of the drop of miniemulsion is 70nm.

Above-mentioned Nano capsule mother liquor is centrifuged into 20min using high speed freezing centrifuge under 10000rpm, then using cold Lyophilizer precooling 4h at -50 DEG C, 12h is kept at -60 DEG C, obtains solid powder, adds 80g solid packing kaolin With 4g adjuvant TERSPERSE2020, it is well mixed, obtains pesticide nano capsules pulvis 17.

The preparation of the pesticide nano capsules aqueous suspension agent 18 of embodiment 18

1g thickeners (0.5g xanthans and 0.5g aluminium-magnesium silicates) are added in above-mentioned Nano capsule mother liquor, are well mixed, Obtain pesticide nano capsules aqueous suspension agent 18.

The preparation of the pesticide nano capsules pulvis 19 of embodiment 19

Using 10ml pure water as interior aqueous phase, 2g foreign minister's active component B Fluoxastrobins are dissolved in 50ml organic solvent dichloromethanes In alkane, 2g cyst material PLAs are added, oil phase is obtained, interior aqueous phase is added drop-wise to by oil under 28000rmp using high shear machine Xiang Zhong, emulsification pretreatment 15min, obtain w/o type emulsion；By 3g emulsifying dispersants (1.5g polyvinyl alcohol and 1.5g dodecyl sulphurs Sour sodium) be dissolved in 150ml water and obtain outer aqueous phase, using high shear machine under 28000rmp by obtained w/o type emulsion droplets It is added in outer aqueous phase, emulsification pretreatment 15min, obtains W/O/W type colostric fluids, the wherein particle diameter of the drop of colostric fluid is 250nm.

Using high pressure homogenizer under 900Pa by above-mentioned W/O/W types colostric fluid high pressure homogenizing 10min, obtain miniemulsion, Wherein the particle diameter of the drop of miniemulsion is 50nm.

Above-mentioned Nano capsule mother liquor is centrifuged into 20min using high speed freezing centrifuge under 10000rpm, then using cold Lyophilizer precooling 4h at -50 DEG C, 12h is kept at -60 DEG C, obtains solid powder, adds 40g solid packing kaolin With 4g adjuvant TERSPERSE2020, it is well mixed, obtains pesticide nano capsules pulvis 19.

The preparation of the pesticide nano capsules aqueous suspension agent 20 of embodiment 20

1g thickeners (0.5g xanthans and 0.5g aluminium-magnesium silicates) are added in above-mentioned Nano capsule mother liquor, are well mixed, Obtain pesticide nano capsules aqueous suspension agent 20.

The preparation of the pesticide nano capsules pulvis 21 of embodiment 21

Using 10ml pure water as interior aqueous phase, 2g foreign minister's active component B pyraclostrobins are dissolved in 50ml organic solvents two In chloromethanes, 2g cyst material PLAs are added, oil phase is obtained, is added drop-wise to interior aqueous phase under 65W using ultrasonic grinder In oil phase, ultrasonic emulsification 30min obtains w/o type emulsion；By 4g emulsifying dispersants (2g polyvinyl alcohol and 2g Tween20) dissolving Outer aqueous phase is obtained in 150ml water, obtained w/o type emulsion is added drop-wise in outer aqueous phase at 50 hz using grinding distribution machine, Grinding emulsification 15min, obtains W/O/W type colostric fluids, the wherein particle diameter of the drop of colostric fluid is 200nm.

Using high pressure homogenizer under 900Pa by above-mentioned W/O/W types colostric fluid high pressure homogenizing 10min, obtain miniemulsion, Wherein the particle diameter of the drop of miniemulsion is 40nm.

Above-mentioned Nano capsule mother liquor is centrifuged into 20min using high speed freezing centrifuge under 10000rpm, then using cold Lyophilizer precooling 4h at -50 DEG C, 12h is kept at -60 DEG C, obtains solid powder, adds 40g solid packing kaolinites Soil, is well mixed, obtains pesticide nano capsules pulvis 21.

The preparation of the pesticide nano capsules aqueous suspension agent 22 of embodiment 22

Using 10ml pure water as interior aqueous phase, 2g foreign minister's active component B pyraclostrobins are dissolved in 50ml organic solvents two In chloromethanes, 2g cyst material PLAs are added, oil phase is obtained, is added drop-wise to interior aqueous phase under 325W using ultrasonic grinder In oil phase, ultrasonic emulsification 25min obtains w/o type emulsion；By 4g emulsifying dispersants (2g polyvinyl alcohol and 2g Tween20) dissolving Outer aqueous phase is obtained in 150ml water, obtained w/o type emulsion is added drop-wise in outer aqueous phase at 50 hz using grinding distribution machine, Grinding emulsification 15min, obtains W/O/W type colostric fluids, the wherein particle diameter of the drop of colostric fluid is 200nm.

1g thickeners (0.5g xanthans and 0.5g aluminium-magnesium silicates) are added in above-mentioned Nano capsule mother liquor, are well mixed, Obtain pesticide nano capsules aqueous suspension agent 22.

The preparation of the pesticide nano capsules pulvis 23 of embodiment 23

Phase active components A imidacloprid in 0.2g is scattered in 2ml water, interior aqueous phase is obtained, by 0.1g foreign minister's active component B AVM is dissolved in 10ml organic solvent chloroforms, is added 0.5g cyst material PLAs, oil phase is obtained, using ultrasound Interior aqueous phase is added drop-wise in oil phase by ripple pulverizer under 585W, and ultrasonic emulsification 15min obtains w/o type emulsion；By 0.2g emulsifications point Powder (0.1g polyvinyl alcohol and 0.1g lignosulfonates), which is dissolved in 18ml water, obtains outer aqueous phase, is existed using high shear machine Obtained w/o type emulsion is added drop-wise in outer aqueous phase under 22000rmp, emulsification pretreatment 30min, obtains W/O/W type colostric fluids, its The particle diameter of the drop of middle colostric fluid is 100nm.

Using high pressure homogenizer under 1200Pa by above-mentioned W/O/W types colostric fluid high pressure homogenizing 2h, obtain miniemulsion, its The particle diameter of the drop of middle miniemulsion is 10nm.

Above-mentioned miniemulsion is stirred under 1300rpm by 20h using electric mixer, organic solvent is volatilized, obtains nanometer Capsule mother liquor.

Above-mentioned Nano capsule mother liquor is centrifuged into 30min using high speed freezing centrifuge under 4000rpm, then using spraying Drying machine is spray-dried 1s at 100 DEG C of EAT, 140 DEG C of leaving air temp, obtains solid powder, adds 0.1g solid packings Diatomite, is well mixed, obtains pesticide nano capsules pulvis 23.

The preparation of the pesticide nano capsules aqueous suspension agent 24 of embodiment 24

Phase active components A imidacloprid in 0.2g is scattered in 2ml water, interior aqueous phase is obtained, by 0.1g foreign minister's active component B AVM is dissolved in 10ml organic solvent chloroforms, is added 0.5g cyst material PLAs, oil phase is obtained, using ultrasound Interior aqueous phase is added drop-wise in oil phase by ripple pulverizer under 585W, and ultrasonic emulsification 15min obtains w/o type emulsion；By 0.2g emulsifications point Powder (0.1g polyvinyl alcohol and 0.1g lignosulfonates), which is dissolved in 18ml water, obtains outer aqueous phase, is existed using high shear machine Obtained w/o type emulsion is added drop-wise in outer aqueous phase under 25000rmp, emulsification pretreatment 20min, obtains W/O/W type colostric fluids, its The particle diameter of the drop of middle colostric fluid is 100nm.

Using high pressure homogenizer under 1000Pa by above-mentioned W/O/W types colostric fluid high pressure homogenizing 1h, obtain miniemulsion, its The particle diameter of the drop of middle miniemulsion is 10nm.

Above-mentioned miniemulsion is stirred under 1000rpm by 22h using electric mixer, organic solvent is volatilized, obtains nanometer Capsule mother liquor.

0.1g thickener xanthans is added in above-mentioned Nano capsule mother liquor, is well mixed, obtains pesticide nano capsules water Suspending agent 24.

The preparation of the pesticide nano capsules pulvis 25 of embodiment 25

Using 10ml pure water as interior aqueous phase, 1g foreign minister's active component B S-metolachlors are dissolved in 20ml organic solvents In dichloromethane, 1g cyst material PLAs are added, oil phase is obtained, interior aqueous phase is added dropwise under 637W using ultrasonic grinder Into oil phase, ultrasonic emulsification 5min obtains w/o type emulsion；By 0.2g emulsifying dispersants (0.1g polyvinyl alcohol and 0.1g lignin Sulfonate) be dissolved in 70ml water and obtain outer aqueous phase, using high shear machine under 28000rmp by obtained w/o type emulsion droplets It is added in outer aqueous phase, emulsification pretreatment 15min, obtains W/O/W type colostric fluids, the wherein particle diameter of the drop of colostric fluid is 500nm.

Using high pressure homogenizer under 600Pa by above-mentioned W/O/W types colostric fluid high pressure homogenizing 50min, obtain miniemulsion, Wherein the particle diameter of the drop of miniemulsion is 50nm.

Above-mentioned miniemulsion is stirred at 1500 rpm by 5h using electric mixer, organic solvent is volatilized, obtains nanometre glue Capsule mother liquor.

Above-mentioned Nano capsule mother liquor is centrifuged into 20min using high speed freezing centrifuge under 10000rpm, then using spray Mist drying machine is spray-dried 1.2s at 300 DEG C of EAT, 100 DEG C of leaving air temp, add 10g solid packings diatomite and 0.05g adjuvant propane diols, is well mixed, obtains pesticide nano capsules pulvis 25.

The preparation of the pesticide nano capsules aqueous suspension agent 26 of embodiment 26

Using 10ml pure water as interior aqueous phase, 1g foreign minister's active component B S-metolachlors are dissolved in 20ml organic solvents In dichloromethane, 1g cyst material celluloses are added, oil phase is obtained, interior aqueous phase is added dropwise under 650W using ultrasonic grinder Into oil phase, ultrasonic emulsification 2min obtains w/o type emulsion；0.5g emulsifying dispersants agriculture breast 1601 is dissolved in 70ml water and obtained To outer aqueous phase, obtained w/o type emulsion is added drop-wise in outer aqueous phase under 28000rmp using high shear machine, emulsification pretreatment 15min, obtains W/O/W type colostric fluids, the wherein particle diameter of the drop of colostric fluid is 500nm.

Using high pressure homogenizer under 100Pa by above-mentioned W/O/W types colostric fluid high pressure homogenizing 50min, obtain miniemulsion, Wherein the particle diameter of the drop of miniemulsion is 50nm.

Above-mentioned miniemulsion is stirred at 500 rpm by 24h using electric mixer, organic solvent is volatilized, obtains nanometre glue Capsule mother liquor.

1g thickeners (0.5g xanthans and 0.5g aluminium-magnesium silicates) are added in above-mentioned Nano capsule mother liquor, are well mixed, Obtain pesticide nano capsules aqueous suspension agent 26.

The preparation of the pesticide nano capsules pulvis 27 of embodiment 27

Phase active components A Tebuconazole in 3g is scattered in 50ml water, interior aqueous phase is obtained, by 30g foreign minister's active component B cyanogen Alkene bacterium ester is dissolved in 130ml organic solvent chloroforms, is added 20g cyst material celluloses, oil phase is obtained, using ultrasonic wave Interior aqueous phase is added drop-wise in oil phase by pulverizer under 585W, and ultrasonic emulsification 15min obtains w/o type emulsion；By 13g emulsion dispersions Agent (6.5g polyvinyl alcohol and 6.5g agriculture breasts 1601), which is dissolved in 220ml water, obtains outer aqueous phase, is existed using high shear machine Obtained w/o type emulsion is added drop-wise in outer aqueous phase under 25000rmp, emulsification pretreatment 22min, obtains W/O/W type colostric fluids, its The particle diameter of the drop of middle colostric fluid is 900nm.

Using high pressure homogenizer under 900Pa by above-mentioned W/O/W types colostric fluid high pressure homogenizing 10min, obtain miniemulsion, Wherein the particle diameter of the drop of miniemulsion is 500nm.

Above-mentioned miniemulsion is stirred at 1500 rpm by 10h using electric mixer, organic solvent is volatilized, obtains nanometer Capsule mother liquor.

Above-mentioned Nano capsule mother liquor is centrifuged into 10min using high speed freezing centrifuge under 15000rpm, then using spray Mist drying machine is spray-dried 1.5s at 30 DEG C of EAT, 30 DEG C of leaving air temp, obtains solid powder, adds 150g solids and fills out Expect diatomite and 15g adjuvants TERSPERSE 2020, be well mixed, obtain pesticide nano capsules pulvis 27.

The preparation of the pesticide nano capsules aqueous suspension agent 28 of embodiment 28

Phase active components A Tebuconazole in 3g is scattered in 50ml water, interior aqueous phase is obtained, by 30g foreign minister's active component B cyanogen Alkene bacterium ester is dissolved in 130ml organic solvent chloroforms, is added 20g cyst material celluloses, oil phase is obtained, using ultrasonic wave Interior aqueous phase is added drop-wise in oil phase by pulverizer under 585W, and ultrasonic emulsification 15min obtains w/o type emulsion；By 13g emulsion dispersions Agent polyvinyl alcohol, which is dissolved in 220ml water, obtains outer aqueous phase, using high shear machine under 25000rmp by obtained w/o type breast Drop is added in outer aqueous phase, emulsification pretreatment 22min, obtains W/O/W type colostric fluids, and the particle diameter of the wherein drop of colostric fluid is 900nm。

4g thickeners (2g xanthans and 2g aluminium-magnesium silicates) and 10g adjuvants are added in above-mentioned Nano capsule mother liquor TERSPERSE 2020, is well mixed, obtains pesticide nano capsules aqueous suspension agent 28.

The preparation of the pesticide nano capsules pulvis 29 of embodiment 29

Phase active components A jinggangmeisu in 3g is dissolved in 40ml water, interior aqueous phase is obtained, by 15g foreign minister's active component B Propiconazole is dissolved in 100ml organic solvent chloroforms, is added 15g cyst material PLAs, oil phase is obtained, using high compression shear Cut machine interior aqueous phase is added drop-wise in oil phase under 28000rmp, emulsification pretreatment 3min obtains w/o type emulsion；By 10g emulsion dispersions Agent (5g polyvinyl alcohol and 5g agriculture breasts 1601), which is dissolved in 160ml water, obtains outer aqueous phase, at 50 hz will using grinding distribution machine Obtained w/o type emulsion is added drop-wise in outer aqueous phase, grinding emulsification 15min, obtains W/O/W type colostric fluids, the wherein liquid of colostric fluid The particle diameter of drop is 400nm.

Above-mentioned Nano capsule mother liquor is centrifuged into 20min using high speed freezing centrifuge under 10000rpm, then using cold Lyophilizer precooling 4h at -50 DEG C, 24h is kept at -60 DEG C, obtains solid powder, adds 150g solid packing kaolinites Soil, is well mixed, obtains pesticide nano capsules pulvis 29.

The preparation of the pesticide nano capsules aqueous suspension agent 30 of embodiment 30

Phase active components A jinggangmeisu in 3g is dissolved in 40ml water, interior aqueous phase is obtained, by 15g foreign minister's active component B Propiconazole is dissolved in 100ml organic solvent chloroforms, is added 15g cyst material PLAs, oil phase is obtained, using high compression shear Cut machine interior aqueous phase is added drop-wise in oil phase under 10000rmp, emulsification pretreatment 40min obtains w/o type emulsion；By 10g emulsifications point Powder (5g polyvinyl alcohol and 5g agriculture breasts 1601), which is dissolved in 160ml water, obtains outer aqueous phase, using grinding distribution machine at 50 hz Obtained w/o type emulsion is added drop-wise in outer aqueous phase, grinding emulsification 15min obtains W/O/W type colostric fluids, wherein colostric fluid The particle diameter of drop is 400nm.

3g thickener xanthans is added in above-mentioned Nano capsule mother liquor, is well mixed, pesticide nano capsules water is obtained and hangs Floating agent 30.

The preparation of the pesticide nano capsules pulvis 31 of embodiment 31

Phase active components A Diacloden in 20g is scattered in 50ml water, interior aqueous phase is obtained, by 20g foreign minister's active component B Emamectin-benzoate is dissolved in 130ml organic solvent dichloromethanes, is added 30g cyst material celluloses, is obtained To oil phase, interior aqueous phase is added drop-wise in oil phase under 585W using ultrasonic grinder, ultrasonic emulsification 15min, obtains w/o type breast Liquid；20g emulsifying dispersants (10g polyvinyl alcohol and 10g dodecyl sodium sulfates) are dissolved in 230ml water and obtain outer aqueous phase, Obtained w/o type emulsion is added drop-wise in outer aqueous phase under 30Hz using grinding distribution machine, grinding emulsification 60min obtains W/O/W The particle diameter of the drop of type colostric fluid, wherein colostric fluid is 400nm.

Above-mentioned Nano capsule mother liquor is centrifuged into 20min using high speed freezing centrifuge under 10000rpm, then using cold Lyophilizer precooling 4h at -50 DEG C, 18h is kept at -60 DEG C, obtains solid powder, adds 150g solid packing swellings Soil and 10g adjuvant TERSPERSE2020, are well mixed, obtain pesticide nano capsules pulvis 31.

The preparation of the pesticide nano capsules aqueous suspension agent 32 of embodiment 32

Phase active components A Diacloden in 20g is scattered in 50ml water, interior aqueous phase is obtained, by 20g foreign minister's active component B Emamectin-benzoate is dissolved in 130ml organic solvent dichloromethanes, is added 30g cyst material celluloses, is obtained To oil phase, interior aqueous phase is added drop-wise in oil phase under 585W using ultrasonic grinder, ultrasonic emulsification 15min, obtains w/o type breast Liquid；20g emulsifying dispersants (10g polyvinyl alcohol and 10g dodecyl sodium sulfates) are dissolved in 230ml water and obtain outer aqueous phase, Obtained w/o type emulsion is added drop-wise in outer aqueous phase under 40Hz using grinding distribution machine, grinding emulsification 40min obtains W/O/W The particle diameter of the drop of type colostric fluid, wherein colostric fluid is 400nm.

10g thickeners (5g xanthans and 5g aluminium-magnesium silicates) and 10g adjuvants are added in above-mentioned Nano capsule mother liquor TERSPERSE 2020, is well mixed, obtains pesticide nano capsules aqueous suspension agent 32.

The preparation of the pesticide nano capsules pulvis 33 of embodiment 33

Phase active components A emamectin-benzoate in 40g is scattered in 40ml water, interior aqueous phase is obtained, will 40g foreign minister's active component B emamectin-benzoates are dissolved in 200ml organic solvent dichloromethanes, add 40g capsules Wall material PLA, obtains oil phase, interior aqueous phase is added drop-wise in oil phase under 65W using ultrasonic grinder, ultrasonic emulsification 30min, obtains w/o type emulsion；30g emulsifying dispersants (10g polyvinyl alcohol, 10g agriculture breasts 600 and 10g Nongru-700s) are dissolved in Outer aqueous phase is obtained in 260ml water, obtained w/o type emulsion is added drop-wise in outer aqueous phase under 45Hz using grinding distribution machine, ground Mill emulsification 20min, obtains W/O/W type colostric fluids, the wherein particle diameter of the drop of colostric fluid is 400nm.

Above-mentioned Nano capsule mother liquor is centrifuged into 25min using high speed freezing centrifuge under 10000rpm, then using cold Lyophilizer precooling 4h at -50 DEG C, 12h is kept at -60 DEG C, obtains solid powder, adds 200g solid packing swellings Soil and 20g adjuvant TERSPERSE2020, are well mixed, obtain pesticide nano capsules pulvis 33.

The preparation of the pesticide nano capsules aqueous suspension agent 34 of embodiment 34

Phase active components A emamectin-benzoate in 40g is scattered in 40ml water, interior aqueous phase is obtained, will 40g foreign minister's active component B emamectin-benzoates are dissolved in 200ml organic solvent dichloromethanes, add 40g capsules Wall material PLA, obtains oil phase, interior aqueous phase is added drop-wise in oil phase under 325W using ultrasonic grinder, ultrasonic emulsification 25min, obtains w/o type emulsion；30g emulsifying dispersants (10g polyvinyl alcohol, 10g agriculture breasts 600 and 10g Nongru-700s) are dissolved in Outer aqueous phase is obtained in 260ml water, obtained w/o type emulsion is added drop-wise in outer aqueous phase at 50 hz using grinding distribution machine, ground Mill emulsification 5min, obtains W/O/W type colostric fluids, the wherein particle diameter of the drop of colostric fluid is 400nm.

30g thickeners (15g xanthans and 15g aluminium-magnesium silicates) and 20g adjuvants are added in above-mentioned Nano capsule mother liquor TERSPERSE 2020, is well mixed, obtains pesticide nano capsules aqueous suspension agent 34.

The preparation of the pesticide nano capsules pulvis 35 of embodiment 35

Phase active components A jinggangmeisu in 0.5g is dissolved in 5ml water, interior aqueous phase is obtained, by 0.5g foreign minister activity into Divide B thifluzamides to be dissolved in 10ml organic solvent dichloromethanes, add 0.1g cyst material celluloses, obtain oil phase, use Interior aqueous phase is added drop-wise in oil phase by ultrasonic grinder under 585W, and ultrasonic emulsification 15min obtains w/o type emulsion；By 0.5g breasts Change dispersant (0.2g polyvinyl alcohol and 0.3g dodecyl sodium sulfates), which is dissolved in 45ml water, obtains outer aqueous phase, using high compression shear Cut machine obtained w/o type emulsion is added drop-wise in outer aqueous phase under 26000rmp, emulsification pretreatment 20min obtains W/O/W type colostrums The particle diameter of the drop of liquid, wherein colostric fluid is 100nm.

Above-mentioned Nano capsule mother liquor is centrifuged into 30min using high speed freezing centrifuge under 4000rpm, then using spraying Drying machine is spray-dried 1s at 100 DEG C of EAT, 140 DEG C of leaving air temp, obtains solid powder, adds 10g solid packings Bentonite, is well mixed, obtains pesticide nano capsules pulvis 35.

The preparation of the pesticide nano capsules aqueous suspension agent 36 of embodiment 36

1g thickener xanthans is added in above-mentioned Nano capsule mother liquor, is well mixed, pesticide nano capsules water is obtained and hangs Floating agent 36.

The preparation of the pesticide nano capsules pulvis 37 of embodiment 37

Phase active components A Diacloden in 30g is scattered in 50ml water, interior aqueous phase is obtained, by 20g foreign minister's active component B Emamectin-benzoate is dissolved in 130ml organic solvent dichloromethanes, is added 30g cyst material celluloses, is obtained To oil phase, interior aqueous phase is added drop-wise in oil phase under 585W using ultrasonic grinder, ultrasonic emulsification 15min, obtains w/o type breast Liquid；20g emulsifying dispersants (10g polyvinyl alcohol and 10g dodecyl sodium sulfates) are dissolved in 220ml water and obtain outer aqueous phase, Obtained w/o type emulsion is added drop-wise in outer aqueous phase under 30Hz using grinding distribution machine, grinding emulsification 60min obtains W/O/W The particle diameter of the drop of type colostric fluid, wherein colostric fluid is 400nm.

Above-mentioned Nano capsule mother liquor is centrifuged into 20min using high speed freezing centrifuge under 10000rpm, then using cold Lyophilizer precooling 4h at -50 DEG C, 18h is kept at -60 DEG C, obtains solid powder, adds 150g solid packing swellings Soil and 10g adjuvant TERSPERSE2020, are well mixed, obtain pesticide nano capsules pulvis 37.

The preparation of the pesticide nano capsules aqueous suspension agent 38 of embodiment 38

Phase active components A Diacloden in 30g is scattered in 50ml water, interior aqueous phase is obtained, by 20g foreign minister's active component B Emamectin-benzoate is dissolved in 130ml organic solvent dichloromethanes, is added 30g cyst material celluloses, is obtained To oil phase, interior aqueous phase is added drop-wise in oil phase under 585W using ultrasonic grinder, ultrasonic emulsification 15min, obtains w/o type breast Liquid；20g emulsifying dispersants (10g polyvinyl alcohol and 10g dodecyl sodium sulfates) are dissolved in 220ml water and obtain outer aqueous phase, Obtained w/o type emulsion is added drop-wise in outer aqueous phase under 40Hz using grinding distribution machine, grinding emulsification 40min obtains W/O/W The particle diameter of the drop of type colostric fluid, wherein colostric fluid is 400nm.

20g thickeners (10g xanthans and 10g aluminium-magnesium silicates) and 15g adjuvants are added in above-mentioned Nano capsule mother liquor TERSPERSE 2020, is well mixed, obtains pesticide nano capsules aqueous suspension agent 38.

The preparation of the pesticide nano capsules pulvis 39 of embodiment 39

Phase active components A jinggangmeisu in 0.8g is dissolved in 20ml water, interior aqueous phase is obtained, by 0.2g foreign minister activity into Divide B thifluzamides to be dissolved in 30ml organic solvent dichloromethanes, add 10g cyst material celluloses, obtain oil phase, using super Interior aqueous phase is added drop-wise in oil phase by sonic disintegrator under 585W, and ultrasonic emulsification 15min obtains w/o type emulsion；0.5g is emulsified Dispersant (0.25g polyvinyl alcohol and 0.25g dodecyl sodium sulfates), which is dissolved in 80ml water, obtains outer aqueous phase, using high compression shear Cut machine obtained w/o type emulsion is added drop-wise in outer aqueous phase under 28000rmp, emulsification pretreatment 15min obtains W/O/W type colostrums The particle diameter of the drop of liquid, wherein colostric fluid is 300nm.

Above-mentioned Nano capsule mother liquor is centrifuged into 20min using high speed freezing centrifuge under 10000rpm, then using cold Lyophilizer precooling 4h at -50 DEG C, 12h is kept at -60 DEG C, obtains solid powder, adds 20g solid packing bentonites With 0.05g adjuvants TERSPERSE 2020, it is well mixed, obtains pesticide nano capsules pulvis 39.

The preparation of the pesticide nano capsules aqueous suspension agent 40 of embodiment 40

0.1g thickener xanthans is added in above-mentioned Nano capsule mother liquor, is well mixed, obtains pesticide nano capsules water Suspending agent 40.

Pattern, particle diameter and the particle diameter distribution test of the pesticide nano capsules of test case 1

The pattern of the pesticide nano capsules of above-described embodiment preparation is observed using SEM and is swashed using nanometer Light particle size analyzer tests its particle diameter and particle diameter distribution.

Fig. 1 is that emamectin-benzoate pesticide nano capsules prepared by the embodiment of the present invention 3 are amplifying 20,000 times (a) with the microscope photograph under 40,000 times (b).It is seen in fig. 1, that emamectin benzoate benzene first prepared by the embodiment of the present invention Hydrochlorate pesticide nano capsules are in scrotiform, and average grain diameter is about 100nm.

The emamectin-benzoate pesticide nano capsules distribution tests of test case 2

Emamectin-benzoate pesticide nano capsules prepared by above-described embodiment 4 are sprayed, and are sprayed at It is to be dried that point of the pesticide nano capsules on blade is observed using environmental scanning electron microscope afterwards on clean cucumber leaves Cloth.

After tested, the pesticide nano capsules that prepared by embodiment of the present invention favorable dispersibility on cucumber leaves, is evenly distributed.

The sustained release performance test of the avermectin pesticides Nano capsule of test case 3

Avermectin pesticides Nano capsule and commercially available AVM water dispersible granules that respectively prepared by test above-described embodiment 7 The sustained release performance of (Beijing China army are biological, Kai Wei) (is used high performance liquid chromatography, tested in different release time using dialysis The AVM content discharged in pesticide nano capsules), make cumulative release amount-time graph.

Fig. 2 is avermectin pesticides Nano capsule and commercially available AVM water dispersible granules prepared by the embodiment of the present invention 7 Elution profiles in 250 hours, as seen from the figure, avermectin pesticides Nano capsule prepared by the embodiment of the present invention is preceding 13 In hour, cumulative release amount reaches about 15%, and subsequent rate of release slows down, at 250 hours, and cumulative release amount reaches about 81%； And commercially available AVM water dispersible granules, in first 13 hours, cumulative release amount reaches about 95%.Therefore, with commercially available AVM Water dispersible granules are compared, and the release time of avermectin pesticides Nano capsule prepared by the embodiment of the present invention significantly extends, holding effect Phase can extend to more than 10 days, with obvious slow release characteristic.

In addition, after tested, pesticide nano capsules prepared by other embodiments of the invention also have preferably sustained release performance.

The anti-light solution performance test of the avermectin pesticides Nano capsule of test case 4

The avermectin pesticides Nano capsule respectively prepared by above-described embodiment 7 and commercially available AVM water dispersible granules (Beijing China army are biological, Kai Wei) irradiates 12h, 24h, 36h, 48h, 60h and 72h under 500W ultraviolet lamps, and uses agricultural chemicals light Avermectin pesticides Nano capsule and commercially available AVM water dispersible granules prepared by stability test case difference testing example 7 Ultraviolet light degradation property, make photodegradation rate-time graph.

As shown in figure 3, compared with traditional commercially available AVM water dispersible granules, Avermectin prepared by the embodiment of the present invention Photodegradation rate of the plain pesticide nano capsules under ultraviolet light is significantly reduced, with good ultraviolet light degradation property.Need Will especially, it is emphasized that avermectin pesticides preparation for easily occur photodissociation environment sensitive type agricultural chemicals, can by the inventive method Effectively protect it from by light degradation, so as to be greatly enhanced effective rate of utilization and bioavilability, reduce spraying times and agent Amount, is conducive to environmental protection and ecological safety.

In addition, after tested, pesticide nano capsules prepared by other embodiments of the invention also there is excellent ultraviolet light to drop Solve performance.

It is aobvious for those skilled in the art although the preferred embodiments of the invention have been shown and described herein And be clear to is that these embodiments are only provided in an illustrative manner.Those skilled in the art are without departing from the present invention A variety of changes are will now occur, changes and substitutes.It should be understood that the various alternative solutions of embodiment of the present invention specifically described herein It is of the invention available for implementing.Purpose be with the claims below limit the scope of the present invention, and thus cover these rights will Method and structure and its equivalent item in the range of asking.

Claims

1. a kind of preparation method of pesticide nano capsules, methods described includes：The component of pesticide nano capsules is formed through emulsification Colostric fluid, is then made pesticide nano capsules through high-pressure homogeneous formation miniemulsion.

2. preparation method according to claim 1, it is characterised in that the preparation method comprises the following steps：

Step a：Pesticide activity component, organic solvent, cyst material, emulsifying dispersant and water are mixed, is then emulsified, obtained To colostric fluid；

Step d：The Nano capsule mother liquor obtained in step c is mixed with excipient and adjuvant, pesticide nano capsules are obtained.

3. preparation method according to claim 2, it is characterised in that the pesticide nano capsules are hollow scrotiform, described Pesticide activity component includes interior phase active components A and foreign minister's active component B, and the step a includes：By interior phase active components A point Dissipate or be dissolved in the water, the suspension or the aqueous solution of interior phase active components A are formed as interior aqueous phase, by foreign minister's active component B It is dissolved in organic solvent, adds cyst material, obtain oil phase, be added drop-wise in oil phase to obtain by interior aqueous phase under emulsification condition W/o type emulsion；Emulsifying dispersant is dissolved in the water and obtains outer aqueous phase, obtained w/o type emulsion is added dropwise under emulsification condition Into outer aqueous phase, W/O/W type colostric fluids are obtained.

4. the preparation method according to Claims 2 or 3, it is characterised in that the pesticide nano capsules are pesticide nano glue Capsule aqueous suspension agent, the excipient is thickener, and the step d includes：Added in the Nano capsule mother liquor obtained in step c Thickener and adjuvant, are well mixed, obtain pesticide nano capsules aqueous suspension agent.

5. the preparation method according to Claims 2 or 3, it is characterised in that the pesticide nano capsules are pesticide nano glue Capsule pulvis, the excipient is solid packing, and the step d includes：By the Nano capsule mother liquor obtained in step c through centrifugation and Solid powder is obtained after drying, solid packing and adjuvant is added, is well mixed, obtains pesticide nano capsules pulvis.

6. the preparation method according to any one of claim 2-5, it is characterised in that emulsifying bar in the step a It is under the conditions of ultrasonic emulsification, under the conditions of emulsification pretreatment or under grinding emulsification condition, preferably in emulsification pretreatment condition under part Down and under the conditions of ultrasonic emulsification；The particle diameter of the drop of the colostric fluid is 100-900nm, preferably 100-500nm；

Wherein described is to carry out ultrasonic emulsification using ultrasonic grinder under the conditions of ultrasonic emulsification, the ultrasonic grinder Power is 65-650W, preferably 325-637W, more preferably 585W；The time of ultrasonic emulsification be 2-30min, preferably 5-25min, more It is preferred that 15min；

Wherein described is to carry out emulsification pretreatment, the shearing of the high-speed shearing machine using high-speed shearing machine under the conditions of emulsification pretreatment Rotating speed is 10000-28000rmp, preferably 22000-28000rmp, more preferably 28000rmp；The time of emulsification pretreatment is 3- 40min, preferably 3-30min, more preferably 15min；

Wherein described is to be ground emulsification using grinding distribution machine under grinding emulsification condition, and the frequency of grinding emulsification is 30- 50Hz, preferably 40-50Hz, more preferably 50Hz；The time of grinding emulsification is 5-60min, more preferably preferably 5-40min, 15min；

Preferably, the high-pressure homogeneous use high pressure homogenizer in the step b is carried out, and high-pressure homogeneous pressure is 100- 1200Pa, preferably 600-1000Pa, more preferably 900Pa；The high-pressure homogeneous time be 10min-2h, preferably 10min-1h, it is more excellent Select 15min；The particle diameter of the drop of the miniemulsion is 10-500nm, preferably 10-100nm；

Preferably, it is stirred in the step c using electric mixer, mixing speed is 500-1500rpm, preferably 1000- 1500rpm, more preferably 1500rpm；Mixing time is 5-24h, preferably 10-20h, more preferably 12h；

Preferably, when the pesticide nano capsules are pesticide nano capsules pulvis, in the step d, using high speed freeze from Scheming centrifuges 10-30min under rotating speed 4000-15000rpm；Preferably, using high speed freezing centrifuge in rotating speed 4000- 20-30min is centrifuged under 15000rpm；It is highly preferred that centrifuging 20min under rotating speed 15000rpm using high speed freezing centrifuge；

Preferably, when the pesticide nano capsules are pesticide nano capsules pulvis, the drying in the step d is spray drying Or freeze-drying, wherein the spray drying is carried out using spray dryer, the condition of spray drying is EAT 30-300 DEG C, 30-140 DEG C of leaving air temp, drying time 1-1.5s；The freeze-drying is carried out using freeze drier, freeze-drying Condition is the precooling 4h at -50 DEG C, keeps 12-24h at -60 DEG C；It is preferred that at -50 DEG C precooling 4h, keep at -60 DEG C 12h。

7. the preparation method according to any one of the claims, it is characterised in that the capsule of the pesticide nano capsules The thickness of wall is 5-50nm, and the particle diameter of the pesticide nano capsules is 20-1000nm, more preferably small preferably smaller than equal to 100nm In 50nm；Preferably, the drugloading rate of the pesticide nano capsules pulvis is 0.01-90%, the pesticide nano capsules aqueous suspension The drugloading rate of agent is 0.01-40%.

8. the preparation method according to any one of the claims, it is characterised in that by weight, the pesticide nano Capsule is made up of following components：

Pesticide activity component：0.1-80 parts

Cyst material：0.1-40 parts

Emulsifying dispersant：0.2-30 parts

Organic solvent：10-200 parts

Water：20-350 parts

Excipient：0.1-200 parts

Adjuvant：0-20 parts,

9. preparation method according to claim 8, it is characterised in that the pesticide activity component includes interior phase active component A and foreign minister's active component B, the pesticide nano capsules are pesticide nano capsules pulvis, wherein the excipient is solid packing, By weight, the pesticide nano capsules pulvis is made up of following components：

Interior phase active components A：0-40 parts

Foreign minister's active component B：0.1-40 parts

Cyst material：0.1-40 parts

Emulsifying dispersant：0.2-30 parts

Organic solvent：10-200 parts

Water：20-350 parts

Solid packing：0.1-200 parts

Adjuvant：0-20 parts；

Or, the pesticide nano capsules are pesticide nano capsules aqueous suspension agent, wherein the excipient is thickener, by weight Meter, the pesticide nano capsules aqueous suspension agent is made up of following components：

Interior phase active components A：0-40 parts

Foreign minister's active component B：0.1-40 parts

Cyst material：0.1-40 parts

Emulsifying dispersant：0.2-30 parts

Organic solvent：10-200 parts

Water：20-350 parts

Thickener：0.1-30 parts

Adjuvant：0-20 parts.

10. the preparation method according to any one of claim 3-9, it is characterised in that the interior phase active components A with it is outer Phase active component B ratio is 0.2:1-4:1, preferably 0.2:1-0.6:1, more preferably 0.4:1；

Preferably, the interior phase active components A and foreign minister's active component B are identical or different material；

Preferably, the interior phase active components A is water-soluble substances or liposoluble substance, preferably water-soluble substances, the foreign minister Active component B is liposoluble substance.

11. the preparation method according to any one of claim 3-10, it is characterised in that the interior phase active components A and Foreign minister's active component B is respectively selected from the one or more in insecticide, bactericide, herbicide and plant growth regulator；

The cyst material is degradable high polymer material.

12. preparation method according to claim 11, it is characterised in that the insecticide is selected from following one kind or many Kind：AVM, emamectin-benzoate, gamma cyhalothrin, Rynaxypyr, pleocidin, indenes worm Prestige, clothianidin, orthene, carbosulfan, Hostathion, diazinon, many mite prestige, chlopyrifos, Biphenthrin, benzene cyanogen chrysanthemum Ester, ethofenprox, decis, fenvalerate, cyfluthrin, Tefluthrin, lythidathion, phoxim, imidacloprid and Diacloden, it is excellent Select Diacloden, pleocidin, Rynaxypyr, AVM, emamectin-benzoate and efficient cyhalothrin One or more in ester；

The bactericide is selected from following one or more：Jinggangmeisu, Fluoxastrobin, pyraclostrobin, thifluzamide, penta azoles Alcohol, metconazole, 2-cyano-3-amino-3-phenylancryic acetate, fluazinam, cymoxanil, Boscalid, ethofenprox, cyflumetofen, Fenpropathrin, benzothiostrobin, Pefurazoate, Prochloraz, propiconazole, Difenoconazoles, Metalaxyl-M, Flusilazole, epoxiconazole, trifloxystrobin and pyraclostrobin, optimizing well ridge Mycin, Tebuconazole, thifluzamide, metconazole, 2-cyano-3-amino-3-phenylancryic acetate, fluazinam, Fluoxastrobin, pyraclostrobin, cymoxanil and pyridine acyl bacterium One or more in amine；

The herbicide is selected from following one or more：The different monooctyl ester of pendimethalin, tri-allate, 2,4-D, benthiocarb, molinate, In cover grass energy, clomazone, butralin, S-metolachlor, trefanocide and prometryn, preferably pendimethalin and S-metolachlor One or more；

The plant growth regulator is selected from following one or more：Brassinosteroid, ammonia oxygen ethyl vinyl glycine and Multiple-effect azole plant growth regulator, preferably multiple-effect azole plant growth regulator；

Preferably, the cyst material is selected from following one or more：Polyester acrylate and its derivative, polyvinyl acetate Resin, polyacrylonitrile resin, polystyrene resin, PLA, gelatin, modified starch, cellulose and its derivates, chitosan and One or more in Arabic gum, preferred cellulose and its derivative, chitosan, PLA and modified starch.

13. the preparation method according to any one of claim 2-12, it is characterised in that the emulsifying dispersant is agricultural One or more in emulsifying agent and dispersant, it is preferable that the agricultural emulsifier be selected from OP series, NP series, EL series, Tween series, Span series, AEO series, the serial emulsifying agent of agriculture breast, polyvinyl alcohol, cithrol, polyethylene pyrrole One or more in pyrrolidone and polyethylene glycol (PEG) oleate；It is preferred that Tween is serial, in the serial emulsifying agent of polyvinyl alcohol and agriculture breast One or more；More preferably polyvinyl alcohol, the series of agriculture breast 300, the series of agriculture breast 500, the series of agriculture breast 600, Nongru-700 series and One or more in the serial emulsifying agent of agriculture breast 1600；

Preferably, the dispersant is in carboxylate, sulfate, sulfonate, phosphate ester salt and APES It is one or more, it is preferable that the dispersant is selected from aliphatic alcohol polyethenoxy ether carboxylate, lauryl sodium sulfate, lignin In sulfonate, dodecyl sodium sulfate, maleated rosin polyethenoxy-oxypropylene ether sulfonate and dodecyl ether phosphate salt One or more in one or more, more preferably lignosulfonates, lauryl sodium sulfate and dodecyl sodium sulfate；

Preferably, one kind in preservative, defoamer, antifreeze, pH adjusting agent and wetting dispersing agent of the adjuvant or It is a variety of, the one or more preferably in antifreeze, defoamer and wetting dispersing agent；

Preferably, one or more of the antifreeze in ethylene glycol, propane diols, glycerine, isopropanol and urea, preferably Ethylene glycol；

Preferably, one or more of the defoamer in organic silicon and low-carbon alcohols defoamer, preferably organic silicon disappears Infusion；

Preferably, the thickener is selected from xanthans, Arabic gum, gelatin, cellulose and its derivates, diatomite, polyethylene One or more in alcohol, Sodium Polyacrylate, dextrin, aluminium-magnesium silicate and Silica hydrogel, preferably xanthans, gelatin, aluminium-magnesium silicate, fibre One or more in dimension element and its derivative and polyvinyl alcohol；

Preferably, the organic solvent is in dichloromethane, chloroform, vegetable oil, petroleum ether and aliphatic solvent oil One or more, preferably dichloromethane；

Preferably, the solid packing is selected from bentonite, diatomite, kaolin, talcum powder, montmorillonite, white carbon, cornstarch With the one or more in sepiolite, the preferably one or more in bentonite, kaolin, cornstarch and white carbon.