CN107347881B

CN107347881B - Pesticide nanocapsule and preparation method thereof

Info

Publication number: CN107347881B
Application number: CN201710485630.6A
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: 2021-03-19
Anticipated expiration: 2037-06-23
Also published as: CN107347881A

Abstract

The invention provides a pesticide nanocapsule and a preparation method thereof, wherein the pesticide nanocapsule is prepared from the following components in parts by weight: 0.1-80 parts of pesticide active ingredient, 0.1-40 parts of capsule wall material, 0.2-30 parts of emulsifying dispersant, 10-200 parts of organic solvent, 20-350 parts of water, 0.1-200 parts of excipient and 0-20 parts of adjuvant, wherein the ratio of the pesticide active ingredient to the capsule wall material is 0.1:1-10: 1. The pesticide nanocapsule provided by the invention has the advantages of small particle size, good particle dispersibility, excellent slow release performance, simple preparation process, easiness in operation and good repeatability.

Description

Pesticide nanocapsule and preparation method thereof

Technical Field

The invention belongs to the technical field of pesticides. In particular to a pesticide nanocapsule and a preparation method thereof.

Background

The pesticide is an important material basis for guaranteeing national food safety. Most of traditional pesticide formulations are open systems, from the registration condition of the pesticide formulations, traditional pesticide formulations mainly comprising missible oil, wettable powder, microemulsion and the like account for over 70 percent of the domestic market, most of the traditional pesticide formulations belong to open systems, losses such as dropping, drifting, bouncing, dust drifting and the like exist to different degrees in the using process, the effective utilization rate of the final target of the crop is less than 30 percent, the amount of the pesticide applied to the body of the pest is less than 0.1 percent, and the effective utilization rate of the pesticide is lower.

When the pesticide is prepared into dosage forms with different structures such as spherical and hollow capsule shapes by adopting a high polymer material for wrapping, coupling and inlaying, the wall material can provide a physical barrier effect, so that ultraviolet light can be shielded, the illumination stability of the pesticide is obviously improved, the adsorption of soil is reduced, the degradation, decomposition and loss caused by illumination or other adverse factors are delayed, the toxicity can be reduced, the pollution is reduced, and the prevention and treatment effect of the product is improved. The preparation also has the function of controlling release, and can be divided into a slow release type and a quick release type according to different application scenes. The slow release type is mainly used for soil treatment and seed treatment, while the fast release type is mainly used for stem leaf spraying, ground sealing treatment and airplane control. However, from the registration of the existing pesticide dosage forms, the dosage forms such as spherical pesticide forms and capsule forms account for a smaller proportion of the pesticide compared with other dosage forms, and the development process is relatively complex.

The traditional preparation method of the pesticide microsphere/microcapsule preparation mainly comprises an in-situ polymerization method, an interface polymerization method, a condensation method, a spray drying method and the like. The in-situ polymerization method needs to be heated for a certain time when the capsule wall is formed, so that not only is certain requirement on process equipment required, but also the repeatability of the product is influenced. When the high-concentration microsphere/microcapsule preparation is prepared by adopting an interfacial polymerization method, the crystallization phenomenon is easy to occur, and the crystallized irregular crystals can damage the capsule wall, so that the drug effect cannot be exerted. The spray drying method is a physical preparation method, and the pesticide microsphere/microcapsule preparation prepared by the method has larger grain diameter, and the grain diameter is difficult to realize nano-scale. The pesticide microsphere/microcapsule preparation prepared by the traditional method at present has the following defects: in terms of structure, the particle size of the current commercially available pesticide microsphere/microcapsule preparation is generally about 5 microns, and does not reach the nanometer level, and the large particle size easily causes drop rolling and dust drift, so that the adhesion, permeability and bioavailability to a crop target are poor in the using process, and the activity is low; in the aspect of particle dispersibility, the currently prepared pesticide microsphere/microcapsule preparation has poor monodispersity, serious agglomeration and uneven particle size distribution, and the surface property and the structural morphology of the pesticide microsphere/microcapsule preparation are not effectively regulated and controlled; in the aspect of controllable slow release of pesticide, most of the existing pesticide microsphere/microcapsule preparations can only realize simple and qualitative slow release, and the release rate is unstable and controllable; in the aspect of process flow, the traditional method mostly adopts the processes of heating, heat preservation, gas protection and the like, and has complex process, difficult control and poor repeatability.

Therefore, how to provide a pesticide nanocapsule with small particle size, good particle dispersibility, excellent slow release performance, simple preparation process, easy operation and good repeatability is an urgent problem to be solved in the field.

Disclosure of Invention

In view of the above problems, an object of the present invention is to provide a pesticide nanocapsule which has a small particle size, good particle dispersibility, excellent sustained-release properties, and a simple preparation process, easy operation, and good reproducibility.

Another object of the present invention is to provide a method for preparing the above-mentioned pesticide nanocapsule.

In order to achieve the aim, the invention provides a pesticide nanocapsule which is prepared from the following components in parts by weight:

active ingredients of the pesticide: 0.1 to 80 portions

Capsule wall material: 0.1 to 40 portions

Emulsifying and dispersing agent: 0.2 to 30 portions of

Organic solvent: 10-200 parts of

Water: 20 to 350 portions of

Excipient: 0.1 to 200 portions of

Auxiliary agents: 0 to 20 portions of the components are added,

wherein the ratio of the pesticide active ingredient to the capsule wall material is 0.1:1-10: 1.

In some embodiments, the thickness of the capsule wall of the pesticide nanocapsule is 5 to 50nm, the particle size of the pesticide nanocapsule is 20 to 1000nm, preferably 100nm or less, more preferably less than 50 nm; the pesticide nanocapsule is pesticide nanocapsule powder or a pesticide nanocapsule water suspending agent, the drug-loading rate of the pesticide nanocapsule powder is 0.01-90%, and the drug-loading rate of the pesticide nanocapsule water suspending agent is 0.01-40%.

In some embodiments, the pesticide active ingredient comprises an internal phase active ingredient a and an external phase active ingredient B, the pesticide nanocapsules are pesticide nanocapsule powders, wherein the excipient is a solid filler, and the pesticide nanocapsule powders are made from the following components by weight:

inner phase active ingredient a: 0 to 40 portions of

External phase active ingredient B: 0.1 to 40 portions

Capsule wall material: 0.1 to 40 portions

Emulsifying and dispersing agent: 0.2 to 30 portions of

Organic solvent: 10-200 parts of

Water: 20 to 350 portions of

Solid filler: 0.1 to 200 portions of

Auxiliary agents: 0-20 parts.

Preferably, the pesticide nanocapsule powder is prepared from the following components in parts by weight:

inner phase active ingredient a: 0 to 30 portions of

External phase active ingredient B: 0.5 to 30 portions of

Capsule wall material: 0.5 to 30 portions of

Emulsifying and dispersing agent: 0.5 to 20 portions of

Organic solvent: 10 to 100 portions of

Water: 50-200 parts of

Solid filler: 10-200 parts of

Auxiliary agents: 0-15 parts.

More preferably, the pesticide nanocapsule powder is prepared from the following components by weight:

inner phase active ingredient a: 0 to 20 portions of

External phase active ingredient B: 1-20 parts of

Capsule wall material: 1-20 parts of

Emulsifying and dispersing agent: 0.5 to 10 portions of

Organic solvent: 20-100 parts of

Water: 50-200 parts of

Solid filler: 10-200 parts of

Auxiliary agents: 0-15 parts.

In some embodiments, the pesticide active ingredient comprises an internal phase active ingredient a and an external phase active ingredient B, the pesticide nanocapsules are pesticide nanocapsule aqueous suspensions, wherein the excipient is a thickener, the pesticide nanocapsule aqueous suspensions are made from, by weight:

inner phase active ingredient a: 0 to 40 portions of

External phase active ingredient B: 0.1 to 40 portions

Capsule wall material: 0.1 to 40 portions

Emulsifying and dispersing agent: 0.2 to 30 portions of

Organic solvent: 10-200 parts of

Water: 20 to 350 portions of

Thickening agent: 0.1 to 30 portions

Auxiliary agents: 0-20 parts.

Preferably, the pesticide nanocapsule aqueous suspension is prepared from the following components in percentage by weight:

inner phase active ingredient a: 0 to 30 portions of

External phase active ingredient B: 0.5 to 30 portions of

Capsule wall material: 0.5 to 30 portions of

Emulsifying and dispersing agent: 0.5 to 20 portions of

Organic solvent: 10 to 100 portions of

Water: 50-200 parts of

Thickening agent: 1-20 parts of

Auxiliary agents: 0-15 parts.

inner phase active ingredient a: 0 to 20 portions of

External phase active ingredient B: 1-20 parts of

Capsule wall material: 1-20 parts of

Emulsifying and dispersing agent: 0.5 to 10 portions of

Organic solvent: 20-100 parts of

Water: 50-200 parts of

Thickening agent: 1-10 parts of

Auxiliary agents: 0-15 parts.

In some embodiments, the ratio of the inner phase active ingredient a to the outer phase active ingredient B is from 0.2:1 to 4:1, preferably from 0.2:1 to 0.6:1, more preferably 0.4: 1; preferably, the inner phase active ingredient a and the outer phase active ingredient B are the same or different materials; preferably, the inner phase active ingredient a is a water-soluble substance or a fat-soluble substance, preferably a water-soluble substance, and the outer phase active ingredient B is a fat-soluble substance.

In some embodiments, the inner phase active ingredient a and the outer phase active ingredient B are each selected from one or more of a pesticide, a fungicide, a herbicide, and a plant growth regulator; the capsule wall material is degradable high polymer material.

In some embodiments, the pesticide is selected from one or more of the following: abamectin, emamectin benzoate, lambda-cyhalothrin, chlorantraniliprole, spinosad, indoxacarb, clothianidin, acephate, carbosulfan, triazophos, dinosaur, acanthodol, chlorpyrifos, bifenthrin, cyphenothrin, ethofenprox, deltamethrin, fenvalerate, cyhalothrin, tefluthrin, fosthiazate, phoxim, imidacloprid and thiamethoxam, preferably one or more of thiamethoxam, spinosad, chlorantraniliprole, abamectin, emamectin benzoate and lambda-cyhalothrin.

In some embodiments, the antimicrobial agent is selected from one or more of the following: validamycin, azoxystrobin, pyraclostrobin, thifluzamide, tebuconazole, metconazole, cyenopaus-methyl, fluazinam, cymoxanil, boscalid, etofenprox, cyflumetofen, fenpropathrin, pyraoxystrobin, pefurazoate, prochloraz, propiconazole, difenoconazole, mefenoxam, flusilazole, epoxiconazole, trifloxystrobin and pyraclostrobin, preferably one or more of validamycin, tebuconazole, thifluzamide, metconazole, cyhalothrin, fluazinam, azoxystrobin, pyraclostrobin, cymoxanil and boscalid.

In some embodiments, the herbicide is selected from one or more of the following: pendimethalin, triallate, 2,4-D isooctyl ester, prosulfocarb, cycloxaben, galbanum, clomazone, butralin, metolachlor, trifluralin and prometryn, preferably one or more of pendimethalin and metolachlor.

In some embodiments, the plant growth regulator is selected from one or more of the following: brassinolide, aminoxyethylvinylglycine and a paclobutrazol plant growth regulator, preferably the paclobutrazol plant growth regulator.

In some embodiments, the wall material is selected from one or more of the following: polyester acrylate and its derivatives, polyvinyl acetate resin, polyacrylonitrile resin, polystyrene resin, polylactic acid, gelatin, modified starch, cellulose and its derivatives, chitosan and acacia, preferably one or more of cellulose and its derivatives, chitosan, polylactic acid and modified starch.

In some embodiments, the emulsifying dispersant is one or more of an agricultural emulsifier and a dispersant, preferably, the agricultural emulsifier is selected from one or more of OP series (octylphenol polyoxyethylene ether, such as OP-10), NP series (nonylphenol polyoxyethylene ether), EL series (castor oil polyoxyethylene ether, such as EL40), Tween series (tweens, such as Tween 80, Tween60, Tween 20), Span series (Span, such as Span 60, Span 80), AEO series (fatty alcohol polyoxyethylene ether, such as AEO-9), emulsifier of the agricultural milk series, polyvinyl alcohol, polyethylene glycol fatty acid ester, polyvinylpyrrolidone, and polyethylene glycol oleate; preferably one or more of Tween series, polyvinyl alcohol and emulsifier of agricultural milk series; more preferably one or more emulsifiers selected from the group consisting of polyvinyl alcohol, Nongru 300 series, Nongru 500 series, Nongru 600 series, Nongru 700 series, and Nongru 1600 series (e.g. Nongru 1601).

In some embodiments, the dispersant is selected from one or more of carboxylate, sulfate, sulfonate, phosphate ester salt, and alkylphenol ethoxylates, preferably, the dispersant is selected from one or more of fatty alcohol-polyoxyethylene ether carboxylate, sodium lauryl sulfate, lignosulfonate, sodium dodecylsulfonate, maleated rosin polyoxyethylene-oxypropylene ether sulfonate, and dodecyl ether phosphate salt, more preferably one or more of lignosulfonate, sodium dodecylsulfate, and sodium dodecylsulfate.

In some embodiments, the adjuvant is selected from one or more of a preservative, a defoamer, an antifreeze, a pH adjuster, and a wetting dispersant, preferably one or more of an antifreeze, a defoamer, and a wetting dispersant (e.g., TERSPERSE2020, TERSPERSE 1004).

In some embodiments, the antifreeze agent is selected from one or more of ethylene glycol, propylene glycol, glycerol, isopropanol, and urea, preferably ethylene glycol.

In some embodiments, the defoamer is selected from one or more of silicone based and lower alcohol defoamers, preferably silicone based defoamers.

In some embodiments, the thickening agent is selected from one or more of xanthan gum, gum arabic, gelatin, cellulose and its derivatives, diatomaceous earth, polyvinyl alcohol, sodium polyacrylate, dextrin, magnesium aluminum silicate, and silica gel, preferably one or more of xanthan gum, gelatin, magnesium aluminum silicate, cellulose and its derivatives, and polyvinyl alcohol.

In some embodiments, the organic solvent is selected from one or more of dichloromethane, chloroform, vegetable oils, petroleum ethers, and aliphatic hydrocarbon solvent oils, preferably dichloromethane.

In some embodiments, the solid filler is selected from one or more of bentonite, diatomaceous earth, kaolin, talc, montmorillonite, silica, corn starch, and sepiolite, preferably one or more of bentonite, kaolin, corn starch, and silica.

The invention further provides a preparation method of the pesticide nanocapsule, which comprises the following steps: emulsifying the components of the pesticide nanocapsule to form primary emulsion, and then homogenizing under high pressure to form miniemulsion to prepare the pesticide nanocapsule.

In some embodiments, the method of making comprises the steps of:

step a: mixing the pesticide active ingredient, the organic solvent, the capsule wall material, the emulsifying dispersant and water, and then emulsifying to obtain a primary emulsion;

step b: b, carrying out fine emulsification on the primary emulsion obtained in the step a through high-pressure homogenization to obtain a fine emulsion;

step c: b, stirring the miniemulsion obtained in the step b to volatilize the organic solvent to obtain a nano-capsule mother solution;

step d: and c, mixing the nano-capsule mother liquor obtained in the step c with an excipient and an auxiliary agent to obtain the pesticide nano-capsule.

In some embodiments, the step a comprises: dispersing or dissolving an internal phase active ingredient A in water to form a suspension or an aqueous solution of the internal phase active ingredient A as an internal aqueous phase, dissolving an external phase active ingredient B in an organic solvent, adding a wall material to obtain an oil phase, and dropwise adding the internal aqueous phase into the oil phase under emulsification conditions to obtain a W/O (water-in-oil) type emulsion; dissolving an emulsifying dispersant into water to obtain an external water phase, and dropwise adding the obtained W/O type emulsion into the external water phase under an emulsifying condition to obtain a W/O/W (water-in-oil-in-water) type primary emulsion.

In some embodiments, the pesticide nanocapsule is a pesticide nanocapsule aqueous suspension, the excipient is a thickener, and step d comprises: and c, adding a thickening agent and an auxiliary agent into the nano-capsule mother liquor obtained in the step c, and uniformly mixing to obtain the pesticide nano-capsule water suspending agent.

In some embodiments, the pesticide nanocapsule is a pesticide nanocapsule powder, the excipient is a solid filler, and step d comprises: and c, centrifuging and drying the nano-capsule mother liquor obtained in the step c to obtain solid powder, adding a solid filler and an auxiliary agent, and uniformly mixing to obtain pesticide nano-capsule powder.

In some embodiments, the "under emulsifying conditions" in step a is "under phacoemulsification conditions", "under shear emulsification conditions" or "under milling emulsification conditions", preferably "under shear emulsification conditions" and "under phacoemulsification conditions"; the particle size of the droplets of the primary emulsion is 100-900nm, preferably 100-500 nm.

Wherein the ultrasonic emulsification is carried out by an ultrasonic crusher under the ultrasonic emulsification condition, and the power of the ultrasonic crusher is 65-650W, preferably 325-637W, and more preferably 585W; the time of ultrasonic emulsification is 2-30min, preferably 5-25min, more preferably 15 min.

Wherein the "under the shearing emulsification condition" is to adopt a high-speed shearing machine to carry out shearing emulsification, and the shearing rotating speed of the high-speed shearing machine is 10000-28000rmp, preferably 22000-28000rmp, and more preferably 28000 rmp; the shearing and emulsifying time is 3-40min, preferably 3-30min, and more preferably 15 min.

Wherein the grinding and emulsifying conditions are grinding and emulsifying by using a grinding and dispersing machine, and the frequency of the grinding and emulsifying is 30-50Hz, preferably 40-50Hz, and more preferably 50 Hz; the time for grinding and emulsifying is 5-60min, preferably 5-40min, and more preferably 15 min.

In some embodiments, the high-pressure homogenization in step b is performed by using a high-pressure homogenizer, and the pressure for the high-pressure homogenization is 100-1200Pa, preferably 600-1000Pa, and more preferably 900 Pa; the high pressure homogenizing time is 10min-2h, preferably 10min-1h, more preferably 15 min; the droplets of the miniemulsion have a particle size of 10 to 500nm, preferably 10 to 100 nm.

In some embodiments, the step c is performed by stirring with an electric stirrer, wherein the stirring speed is 500-; the stirring time is 5-24h, preferably 10-20h, more preferably 12 h.

In some embodiments, when the pesticide nanocapsule is pesticide nanocapsule powder, the step d is performed by centrifuging at 4000-15000rpm for 10-30min by using a high-speed refrigerated centrifuge; preferably, a high-speed refrigerated centrifuge is adopted for centrifuging for 20-30min at the rotating speed of 4000-; more preferably, a high speed refrigerated centrifuge is used for centrifugation at 15000rpm for 20 min.

In some embodiments, when the pesticide nanocapsule is pesticide nanocapsule powder, the drying in the step d is spray drying or freeze drying, wherein the spray drying is performed by using a spray dryer, and the conditions of the spray drying are that the inlet air temperature is 30-300 ℃, the outlet air temperature is 30-140 ℃, and the drying time is 1-1.5 s; the freeze drying is carried out by adopting a freeze dryer, and the condition of freeze drying is pre-freezing for 4h at-50 ℃ and keeping for 12-24h at-60 ℃; preferably pre-frozen at-50 ℃ for 4h and maintained at-60 ℃ for 12 h.

By adopting the method of the invention, the nano-scale pesticide capsule can be obtained, and the pesticide nano-capsule provides a new way for improving the effective utilization rate of the pesticide due to the small size, large specific surface area and modifiability. The unique surface effect and small-size effect of the nano carrier material are utilized, the medicine is loaded in the modes of adsorption, coupling, wrapping or embedding, the efficient loading of the medicine can be realized, the intelligent and accurate release of the medicine in time, space and dosage can be realized by adjusting the fine structure of the nano carrier, the minimum effective target action concentration is maintained in a set period, and the effectiveness and the safety of the medicine are greatly improved. By the functions of carrier loading, water-based dispersion, targeted transmission, controllable release and the like of the nano drug-carrying system, the dispersibility, stability and utilization rate of the pesticide can be improved, the lasting period is prolonged, and the residual pollution is reduced. In addition, compared with a micron-scale microsphere/microcapsule preparation, the granularity of the pesticide nanocapsule reaches the nanometer level, the small-size effect of the nanocapsule can increase the ductility, wettability and target adsorbability of pesticide droplets in the field spraying process, the nanocapsule has the advantages of higher efficiency and environmental protection, the nanocapsule is easier to deposit on plant leaves, the large specific surface area characteristic of the nanocapsule increases the adhesion to the target, and the loss of the pesticide is reduced.

The high-pressure homogenization method is that liquid materials flow through a special homogenization cavity at high speed under the action of ultrahigh pressure to generate fine liquid drops. The high-pressure homogenization method can produce micro/nano-scale particles, and effectively prevent the particles from caking. The invention adopts a new preparation process to prepare the pesticide nanocapsule, and particularly adopts a homogeneous emulsification method to prepare the pesticide nanocapsule. In the preparation method, firstly one or more of ultrasonic emulsification, shearing emulsification and grinding emulsification are adopted to prepare primary emulsion, then a miniemulsion is prepared by adopting a high-pressure homogenization method, and finally an excipient and an auxiliary agent are added to obtain the pesticide nanocapsule with good dispersibility.

The invention adopts a homogeneous emulsification method to prepare the pesticide nanocapsule, and prepares the pesticide nanocapsule with uniform dispersion and excellent performance by adjusting the component formula, the process flow, the parameters in the steps and the like.

Compared with the prior art, the pesticide nanocapsule and the preparation method thereof provided by the invention have the following advantages:

1. in terms of particle size, the pesticide nanocapsule disclosed by the invention has a nanoscale particle size which can be smaller than 50nm, so that the specific surface area of the pesticide nanocapsule is increased, the contact area of the pesticide and the surface of crops is increased, the adhesion and permeability of the pesticide on the leaf surfaces of the crops are increased, the pesticide is favorably embedded into a micro-nano structure of the leaf surfaces of the crops, the retention rate of the leaf surfaces is enhanced, the loss is reduced, the effective utilization rate and the pesticide effect of the pesticide are improved, and the amount and the frequency of pesticide spraying are reduced; in addition, the pesticide nanocapsule has small particle size, increases the contact area with the pest target, and can increase the insecticidal activity on the pest target;

2. in the aspect of particle dispersibility, the pesticide nanocapsule has good monodispersity, small particle size and uniform distribution;

3. in the aspect of controllable slow release of pesticide, the slow release speed of the pesticide nanocapsule is accurate and adjustable, and the accurate regulation and control of the slow release speed of the pesticide can be realized by adjusting one or more of the component content, the particle size, the morphology structure, the pore structure, the total pore volume, the pore canal number and the like; the control period of the traditional slow-release pesticide formulation is limited at present, but the slow-release period of the pesticide nanocapsule disclosed by the invention can be controlled within 3 days to 3 months according to the specific application scene requirements, so that the slow-release period of the pesticide preparation is effectively prolonged, and the activity of the pesticide is improved, and the spraying times and dosage are reduced;

4. in terms of materials, the capsule wall of the pesticide nanocapsule is made of safe, low-cost and degradable high polymer materials, so that the pollution to the environment is reduced;

5. in the aspect of drug loading, the drug loading of the pesticide nanocapsule can be adjusted between 0.01 and 90 percent, and the application range is wide;

6. in the aspect of ultraviolet light degradation resistance, the pesticide nanocapsule can effectively improve the ultraviolet light degradation resistance of the pesticide, thereby greatly improving the effective utilization rate and bioavailability, reducing the application times and dosage and being beneficial to environmental protection and ecological safety;

7. compared with the traditional preparation method of pesticide microspheres/micro-capsules, the preparation method provided by the invention is carried out at normal temperature, has mild conditions, relatively simple process, is easy to operate and has good repeatability, and is beneficial to industrialization.

Drawings

Fig. 1 is a microscope picture of methylamino abamectin benzoate pesticide nanocapsules prepared in the embodiment of the present invention;

FIG. 2 is a slow release curve of the avermectin pesticide nanocapsule prepared by the embodiment of the invention;

fig. 3 is an ultraviolet photolysis diagram of the pesticide nanocapsule prepared by the embodiment of the invention.

Detailed Description

The invention is illustrated below with reference to specific examples. It will be understood by those skilled in the art that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention in any way.

The experimental procedures in the following examples are conventional unless otherwise specified. The raw materials and materials of the reagents used in the following examples are all commercially available products unless otherwise specified.

Instrument for measuring the position of a moving object

Ultrasonic grinder (SCIENTZ, JY92-IIN)

High speed shearer (FLUKO, FA25)

Grinding disperser (SGN, GMSD2000/4)

High pressure homogenizer (ATS, AH-100D)

Electric blender (IKA, EUROSTAR 60)

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

Freeze dryer (BIOCOOL, Pilot2-4M)

Scanning electron microscope (Hitachi, SU8010)

Environment scanning electron microscope (FEI, Quanta FEG 250)

Nanometer laser particle size analyzer (Malvern, Nano ZS90)

High performance liquid chromatography (Agilent, 1260)

Pesticide light stability test box (Xutemp, XT5409-XPC80)

Example 1 preparation of pesticide nanocapsule powder 1

Dispersing 0.8g of an internal phase active ingredient A thiamethoxam in 20ml of water to obtain an internal water phase, dissolving 2g of an external phase active ingredient B emamectin benzoate in 50ml of organic solvent dichloromethane, adding 2g of capsule wall material cellulose to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 585W by adopting an ultrasonic crusher, and ultrasonically emulsifying for 15min to obtain a W/O type emulsion; dissolving 2g of emulsifying dispersant (1g of polyvinyl alcohol and 1g of sodium dodecyl sulfate) in 150ml of water to obtain an external water phase, dropwise adding the obtained W/O type emulsion into the external water phase at 28000rmp by using a high-pressure shearing machine, and shearing and emulsifying for 15min to obtain W/O/W type primary emulsion, wherein the particle size of the droplets of the primary emulsion is 300 nm.

Homogenizing the W/O/W type primary emulsion at 900Pa for 15min by a high-pressure homogenizer to obtain a fine emulsion, wherein the particle size of the droplets of the fine emulsion is 100 nm.

And stirring the miniemulsion for 24 hours at 1500rpm by using an electric stirrer to volatilize the organic solvent, thereby obtaining the nano-capsule mother liquor.

Centrifuging the nano-capsule mother solution for 20min at 10000rpm by using a high-speed refrigerated centrifuge, then pre-freezing for 4h at-50 ℃ by using a freeze dryer, keeping the temperature for 12h at-60 ℃ to obtain solid powder, adding 100g of solid filler bentonite and 1g of adjuvant TERSPERSE2020, and uniformly mixing to obtain the pesticide nano-capsule powder 1.

Example 2 preparation of pesticide nanocapsule aqueous suspension 2

Adding 1g of thickening agent (0.5g of xanthan gum and 0.5g of magnesium aluminum silicate) into the nano-capsule mother liquor, and uniformly mixing to obtain the pesticide nano-capsule water suspending agent 2.

Example 3 preparation of pesticide nanocapsule powder 3

Dispersing 0.5g of internal phase active ingredient A emamectin benzoate in 50ml of water to obtain an internal water phase, dissolving 2g of external phase active ingredient B emamectin benzoate in 100ml of organic solvent dichloromethane, adding 3g of capsule wall material polylactic acid to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 585W by adopting an ultrasonic crusher, and ultrasonically emulsifying for 15min to obtain a W/O type emulsion; dissolving 3.5g emulsifying dispersant (1g polyvinyl alcohol, 1.5g agricultural emulsion 600 and 1g agricultural emulsion 700) in 300ml water to obtain external water phase, dripping the obtained W/O type emulsion into the external water phase at 28000rmp by using a high pressure shearing machine, and shearing and emulsifying for 15min to obtain W/O/W type primary emulsion, wherein the particle size of the primary emulsion is 300 nm.

Centrifuging the nano-capsule mother solution for 20min at 10000rpm by using a high-speed refrigerated centrifuge, then pre-freezing for 4h at-50 ℃ by using a freeze dryer, keeping the temperature for 12h at-60 ℃ to obtain solid powder, adding 100g of solid filler bentonite and 1g of adjuvant TERSPERSE2020, and uniformly mixing to obtain the pesticide nano-capsule powder 3.

Example 4 preparation of pesticide nanocapsule aqueous suspension 4

Adding 1g of thickening agent (0.5g of xanthan gum and 0.5g of magnesium aluminum silicate) into the nano-capsule mother liquor, and uniformly mixing to obtain the pesticide nano-capsule suspension concentrate 4.

Example 5 preparation of pesticide nanocapsule powder 5

Dissolving 1.6g of an internal phase active ingredient A validamycin in 20ml of water to obtain an internal water phase, dissolving 4g of an external phase active ingredient B thifluzamide in 50ml of organic solvent dichloromethane, adding 2g of capsule wall material cellulose to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 585W by using an ultrasonic crusher, and ultrasonically emulsifying for 15min to obtain W/O type emulsion; dissolving 2g of emulsifying dispersant (1g of polyvinyl alcohol and 1g of sodium dodecyl sulfate) in 150ml of water to obtain an external water phase, dropwise adding the obtained W/O type emulsion into the external water phase at 28000rmp by using a high-pressure shearing machine, and shearing and emulsifying for 15min to obtain W/O/W type primary emulsion, wherein the particle size of the droplets of the primary emulsion is 300 nm.

Centrifuging the nano-capsule mother solution for 20min at 10000rpm by using a high-speed refrigerated centrifuge, then pre-freezing for 4h at-50 ℃ by using a freeze dryer, keeping the temperature for 12h at-60 ℃ to obtain solid powder, adding 100g of solid filler bentonite and 1g of adjuvant TERSPERSE2020, and uniformly mixing to obtain the pesticide nano-capsule powder 5.

Example 6 preparation of pesticide nanocapsule aqueous suspension 6

And adding 1g of thickening agent xanthan gum into the nano-capsule mother liquor, and uniformly mixing to obtain the pesticide nano-capsule water suspending agent 6.

Example 7 preparation of pesticide nanocapsule powder 7

Dispersing 1.2g of an internal phase active ingredient A abamectin in 20ml of water to obtain an internal water phase, dissolving 2g of an external phase active ingredient B abamectin in 50ml of organic solvent dichloromethane, adding 2g of a capsule wall material polylactic acid to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 585W by adopting an ultrasonic crusher, and ultrasonically emulsifying for 15min to obtain a W/O type emulsion; dissolving 3g of emulsifying dispersant (2g of polyvinyl alcohol, 0.5g of farm emulsion 1601 and 0.5g of OP-10) in 150ml of water to obtain an external water phase, dropwise adding the obtained W/O type emulsion into the external water phase at 28000rmp by using a high-pressure shearing machine, and shearing and emulsifying for 15min to obtain W/O/W type primary emulsion, wherein the particle size of the primary emulsion is 300 nm.

Centrifuging the nano-capsule mother solution for 20min at 10000rpm by using a high-speed refrigerated centrifuge, then pre-freezing for 4h at-50 ℃ by using a freeze dryer, keeping the temperature for 12h at-60 ℃ to obtain solid powder, adding 50g of solid filler bentonite and 1g of adjuvant TERSPERSE2020, and uniformly mixing to obtain the pesticide nano-capsule powder 7.

Example 8 preparation of pesticide nanocapsule aqueous suspension 8

And adding 2g of thickening agent xanthan gum into the nano-capsule mother liquor, and uniformly mixing to obtain the pesticide nano-capsule water suspending agent 8.

Example 9 preparation of pesticide nanocapsule powder 9

Taking 20ml of pure water as an internal water phase, dissolving 2g of an external phase active ingredient B-cyanoenamid in 50ml of organic solvent dichloromethane, adding 2g of a capsule wall material polylactic acid to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 585W by using an ultrasonic pulverizer, and ultrasonically emulsifying for 15min to obtain a W/O type emulsion; dissolving 2g of emulsifying dispersant Tween 80 in 150ml of water to obtain an external water phase, dropwise adding the obtained W/O type emulsion into the external water phase by adopting a high-pressure shearing machine at 28000rmp, and shearing and emulsifying for 15min to obtain W/O/W type primary emulsion, wherein the particle size of the droplets of the primary emulsion is 300 nm.

Centrifuging the nanometer capsule mother solution at 10000rpm for 20min by a high-speed refrigerated centrifuge, pre-freezing for 4h at-50 ℃ by a freeze dryer, keeping at-60 ℃ for 12h to obtain solid powder, adding 50g of solid filler bentonite and 1g of adjuvant TERSPERSE2020, and mixing uniformly to obtain pesticide nanometer capsule powder 9.

Example 10 preparation of pesticide nanocapsule aqueous suspension 10

Taking 20ml of pure water as an internal water phase, dissolving 2g of an external phase active ingredient B-cyanoenamid in 50ml of organic solvent dichloromethane, adding 2g of a capsule wall material polylactic acid to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 585W by using an ultrasonic pulverizer, and ultrasonically emulsifying for 15min to obtain a W/O type emulsion; dissolving 1.5g of emulsifying dispersant Tween 80 in 150ml of water to obtain an external water phase, dropwise adding the obtained W/O type emulsion into the external water phase by adopting a high-pressure shearing machine under 28000rmp, and shearing and emulsifying for 15min to obtain W/O/W type primary emulsion, wherein the particle size of the droplets of the primary emulsion is 300 nm.

And adding 3g of thickening agent (2g of xanthan gum and 1g of magnesium aluminum silicate) into the nano-capsule mother liquor, and uniformly mixing to obtain the pesticide nano-capsule water suspending agent 10.

Example 11 preparation of pesticide nanocapsule powder 11

Dispersing 0.8g of an internal phase active ingredient A, namely chlorantraniliprole, in 20ml of water to obtain an internal water phase, dissolving 2g of an external phase active ingredient B, namely thiamethoxam, in 50ml of organic solvent dichloromethane, adding 2g of cellulose serving as a capsule wall material to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 585W by using an ultrasonic pulverizer, and ultrasonically emulsifying for 15min to obtain a W/O type emulsion; dissolving 2.5g of emulsifying dispersant (1g of polyvinyl alcohol and 1.5g of sodium dodecyl sulfate) in 150ml of water to obtain an external water phase, dropwise adding the obtained W/O type emulsion into the external water phase at 28000rmp by using a high-pressure shearing machine, and shearing and emulsifying for 15min to obtain W/O/W type primary emulsion, wherein the particle size of the droplets of the primary emulsion is 300 nm.

Centrifuging the nano-capsule mother solution for 20min at 10000rpm by using a high-speed refrigerated centrifuge, then pre-freezing for 4h at-50 ℃ by using a freeze dryer, keeping the temperature for 12h at-60 ℃ to obtain solid powder, adding 150g of solid filler bentonite and 1g of adjuvant TERSPERSE2020, and uniformly mixing to obtain the pesticide nano-capsule powder 11.

Example 12 preparation of pesticide nanocapsule aqueous suspension 12

And adding 1g of thickening agent xanthan gum into the nano-capsule mother liquor, and uniformly mixing to obtain the pesticide nano-capsule water suspending agent 12.

Example 13 preparation of pesticide nanocapsule powder 13

Dispersing 1g of an internal phase active ingredient A, namely chlorantraniliprole, in 10ml of water to obtain an internal water phase, dissolving 2g of an external phase active ingredient B, namely efficient cyhalothrin, in 20ml of organic solvent dichloromethane, adding 2g of capsule wall material cellulose to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 585W by using an ultrasonic crusher, and ultrasonically emulsifying for 15min to obtain W/O type emulsion; dissolving 2g of emulsifying dispersant polyvinyl alcohol in 150ml of water to obtain an external water phase, dropwise adding the obtained W/O type emulsion into the external water phase at 585W by using an ultrasonic pulverizer, and ultrasonically emulsifying for 15min to obtain a W/O/W type primary emulsion, wherein the particle size of the droplets of the primary emulsion is 300 nm.

Homogenizing the W/O/W type primary emulsion at 900Pa for 10min by a high-pressure homogenizer to obtain a fine emulsion, wherein the particle size of the droplets of the fine emulsion is 100 nm.

Centrifuging the nano-capsule mother solution for 20min at 10000rpm by using a high-speed refrigerated centrifuge, then pre-freezing for 4h at-50 ℃ by using a freeze dryer, keeping the temperature for 12h at-60 ℃ to obtain solid powder, adding 150g of solid filler kaolin and 2g of auxiliary agent TERSPERSE2020, and uniformly mixing to obtain the pesticide nano-capsule powder 13.

Example 14 preparation of pesticide nanocapsule aqueous suspension 14

Adding 1g of thickening agent (0.5g of xanthan gum and 0.5g of magnesium aluminum silicate) into the nano-capsule mother liquor, and uniformly mixing to obtain the pesticide nano-capsule water suspending agent 14.

Example 15 preparation of pesticide nanocapsule powder 15

Dispersing 1g of internal phase active ingredient A emamectin benzoate in 20ml of water to obtain an internal water phase, dissolving 2g of external phase active ingredient B high-efficiency cyhalothrin in 50ml of organic solvent dichloromethane, adding 2g of capsule wall material cellulose to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 28000rmp by using a high-pressure shearing machine, and shearing and emulsifying for 15min to obtain a W/O type emulsion; dissolving 2.5g emulsifying dispersant (1g polyvinyl alcohol and 1.5g EL40) in 150ml water to obtain external water phase, dripping the obtained W/O type emulsion into the external water phase at 50Hz by using a grinding disperser, and grinding and emulsifying for 15min to obtain W/O/W type primary emulsion, wherein the particle diameter of the droplet of the primary emulsion is 250 nm.

Homogenizing the W/O/W type primary emulsion at 900Pa for 10min by a high-pressure homogenizer to obtain a fine emulsion, wherein the particle size of the droplets of the fine emulsion is 90 nm.

And stirring the miniemulsion for 12 hours at 1500rpm by using an electric stirrer to volatilize the organic solvent to obtain the nano-capsule mother liquor.

Centrifuging the nano-capsule mother solution for 20min at 10000rpm by using a high-speed refrigerated centrifuge, then pre-freezing for 4h at-50 ℃ by using a freeze dryer, keeping the temperature for 12h at-60 ℃ to obtain solid powder, adding 80g of solid filler kaolin and 2g of auxiliary agent TERSPERSE2020, and uniformly mixing to obtain the pesticide nano-capsule powder 15.

EXAMPLE 16 preparation of pesticide nanocapsule aqueous suspension 16

And adding 1.5g of thickening agent (1g of xanthan gum and 0.5g of magnesium aluminum silicate) into the nano-capsule mother liquor, and uniformly mixing to obtain the pesticide nano-capsule water suspending agent 16.

Example 17 preparation of pesticide nanocapsule powder 17

Dispersing 0.5g of an internal phase active ingredient A thiamethoxam in 10ml of water to obtain an internal water phase, dissolving 2g of an external phase active ingredient B efficient cyhalothrin in 50ml of organic solvent dichloromethane, adding 2g of wall material polylactic acid to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 585W by adopting an ultrasonic crusher, and ultrasonically emulsifying for 15min to obtain W/O type emulsion; dissolving 3g of emulsifying dispersant (1g of polyvinyl alcohol and 2g of sodium dodecyl sulfate) in 90ml of water to obtain an external water phase, dropwise adding the obtained W/O type emulsion into the external water phase at 50Hz by using a grinding dispersion machine, and grinding and emulsifying for 15min to obtain W/O/W type primary emulsion, wherein the particle size of the droplets of the primary emulsion is 300 nm.

Homogenizing the W/O/W type primary emulsion at 900Pa for 10min by a high-pressure homogenizer to obtain a fine emulsion, wherein the particle size of the droplets of the fine emulsion is 70 nm.

Centrifuging the nano-capsule mother solution for 20min at 10000rpm by using a high-speed refrigerated centrifuge, then pre-freezing for 4h at-50 ℃ by using a freeze dryer, keeping for 12h at-60 ℃ to obtain solid powder, adding 80g of solid filler kaolin and 4g of auxiliary agent TERSPERSE2020, and uniformly mixing to obtain the pesticide nano-capsule powder 17.

EXAMPLE 18 preparation of pesticide nanocapsule aqueous suspension 18

Adding 1g of thickening agent (0.5g of xanthan gum and 0.5g of magnesium aluminum silicate) into the nano-capsule mother liquor, and uniformly mixing to obtain the pesticide nano-capsule water suspending agent 18.

EXAMPLE 19 preparation of pesticide nanocapsule powder 19

Taking 10ml of pure water as an inner water phase, dissolving 2g of azoxystrobin serving as an outer phase active ingredient B in 50ml of organic solvent dichloromethane, adding 2g of polylactic acid serving as a capsule wall material to obtain an oil phase, dropwise adding the inner water phase into the oil phase at 28000rmp by using a high-pressure shearing machine, and shearing and emulsifying for 15min to obtain a W/O type emulsion; dissolving 3g of emulsifying dispersant (1.5g of polyvinyl alcohol and 1.5g of sodium dodecyl sulfate) in 150ml of water to obtain an external water phase, dropwise adding the obtained W/O type emulsion into the external water phase at 28000rmp by using a high-pressure shearing machine, and shearing and emulsifying for 15min to obtain W/O/W type primary emulsion, wherein the particle size of the droplets of the primary emulsion is 250 nm.

Homogenizing the W/O/W type primary emulsion at 900Pa for 10min by a high-pressure homogenizer to obtain a fine emulsion, wherein the particle size of the droplets of the fine emulsion is 50 nm.

Centrifuging the nano-capsule mother solution for 20min at 10000rpm by using a high-speed refrigerated centrifuge, then pre-freezing for 4h at-50 ℃ by using a freeze dryer, keeping for 12h at-60 ℃ to obtain solid powder, adding 40g of solid filler kaolin and 4g of auxiliary agent TERSPERSE2020, and uniformly mixing to obtain the pesticide nano-capsule powder 19.

EXAMPLE 20 preparation of pesticide nanocapsule aqueous suspension 20

Adding 1g of thickening agent (0.5g of xanthan gum and 0.5g of magnesium aluminum silicate) into the nano-capsule mother liquor, and uniformly mixing to obtain the pesticide nano-capsule water suspending agent 20.

EXAMPLE 21 preparation of pesticide Nanocoapsule powder 21

Taking 10ml of pure water as an internal water phase, dissolving 2g of pyraclostrobin serving as an external phase active ingredient B in 50ml of organic solvent dichloromethane, adding 2g of polylactic acid serving as a capsule wall material to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 65W by using an ultrasonic pulverizer, and ultrasonically emulsifying for 30min to obtain a W/O type emulsion; dissolving 4g of emulsifying dispersant (2g of polyvinyl alcohol and 2g of Tween 20) in 150ml of water to obtain an external water phase, dropwise adding the obtained W/O type emulsion into the external water phase at 50Hz by using a grinding dispersion machine, and grinding and emulsifying for 15min to obtain W/O/W type primary emulsion, wherein the particle size of the droplets of the primary emulsion is 200 nm.

Homogenizing the W/O/W type primary emulsion at 900Pa for 10min by a high-pressure homogenizer to obtain a fine emulsion, wherein the particle size of the droplets of the fine emulsion is 40 nm.

Centrifuging the nanometer capsule mother liquor at 10000rpm for 20min by a high-speed refrigerated centrifuge, pre-freezing for 4h at-50 ℃ by a freeze dryer, keeping at-60 ℃ for 12h to obtain solid powder, adding 40g of solid filler kaolin, and mixing uniformly to obtain pesticide nanometer capsule powder 21.

EXAMPLE 22 preparation of pesticide nanocapsule aqueous suspension 22

Taking 10ml of pure water as an internal water phase, dissolving 2g of pyraclostrobin serving as an external phase active ingredient B in 50ml of organic solvent dichloromethane, adding 2g of polylactic acid serving as a capsule wall material to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 325W by adopting an ultrasonic pulverizer, and ultrasonically emulsifying for 25min to obtain a W/O type emulsion; dissolving 4g of emulsifying dispersant (2g of polyvinyl alcohol and 2g of Tween 20) in 150ml of water to obtain an external water phase, dropwise adding the obtained W/O type emulsion into the external water phase at 50Hz by using a grinding dispersion machine, and grinding and emulsifying for 15min to obtain W/O/W type primary emulsion, wherein the particle size of the droplets of the primary emulsion is 200 nm.

Adding 1g of thickening agent (0.5g of xanthan gum and 0.5g of magnesium aluminum silicate) into the nano-capsule mother liquor, and uniformly mixing to obtain the pesticide nano-capsule water suspending agent 22.

EXAMPLE 23 preparation of pesticide Nanocoapsule powder 23

Dispersing 0.2g of an internal phase active ingredient A imidacloprid in 2ml of water to obtain an internal water phase, dissolving 0.1g of an external phase active ingredient B abamectin in 10ml of organic solvent trichloromethane, adding 0.5g of capsule wall material polylactic acid to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 585W by adopting an ultrasonic crusher, and ultrasonically emulsifying for 15min to obtain a W/O type emulsion; dissolving 0.2g of emulsifying dispersant (0.1g of polyvinyl alcohol and 0.1g of lignosulfonate) in 18ml of water to obtain an external water phase, dripping the obtained W/O type emulsion into the external water phase at 22000rmp by using a high-pressure shearing machine, and shearing and emulsifying for 30min to obtain W/O/W type primary emulsion, wherein the particle size of the droplets of the primary emulsion is 100 nm.

Homogenizing the W/O/W type primary emulsion for 2h at 1200Pa by a high-pressure homogenizer to obtain a fine emulsion, wherein the particle size of the droplets of the fine emulsion is 10 nm.

And stirring the miniemulsion for 20 hours at 1300rpm by using an electric stirrer to volatilize the organic solvent to obtain the nano-capsule mother liquor.

And (3) centrifuging the nano-capsule mother solution for 30min at 4000rpm by using a high-speed refrigerated centrifuge, then performing spray drying for 1s at the air inlet temperature of 100 ℃ and the air outlet temperature of 140 ℃ by using a spray dryer to obtain solid powder, adding 0.1g of solid filler diatomite, and uniformly mixing to obtain pesticide nano-capsule powder 23.

EXAMPLE 24 preparation of pesticide nanocapsule aqueous suspension 24

Dispersing 0.2g of an internal phase active ingredient A imidacloprid in 2ml of water to obtain an internal water phase, dissolving 0.1g of an external phase active ingredient B abamectin in 10ml of organic solvent trichloromethane, adding 0.5g of capsule wall material polylactic acid to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 585W by adopting an ultrasonic crusher, and ultrasonically emulsifying for 15min to obtain a W/O type emulsion; dissolving 0.2g emulsifying dispersant (0.1g polyvinyl alcohol and 0.1g lignosulfonate) in 18ml water to obtain an external water phase, dripping the obtained W/O type emulsion into the external water phase at 25000rmp by using a high-pressure shearing machine, and shearing and emulsifying for 20min to obtain W/O/W type primary emulsion, wherein the particle size of the droplets of the primary emulsion is 100 nm.

Homogenizing the W/O/W type primary emulsion at 1000Pa for 1h by a high-pressure homogenizer to obtain a fine emulsion, wherein the particle size of the droplets of the fine emulsion is 10 nm.

And stirring the miniemulsion for 22 hours at 1000rpm by using an electric stirrer to volatilize the organic solvent to obtain the nano-capsule mother liquor.

0.1g of thickening agent xanthan gum is added into the nano-capsule mother liquor and uniformly mixed to obtain the pesticide nano-capsule water suspending agent 24.

EXAMPLE 25 preparation of pesticide nanocapsule powder 25

Taking 10ml of pure water as an internal water phase, dissolving 1g of external phase active ingredient B s-metolachlor in 20ml of organic solvent dichloromethane, adding 1g of capsule wall material polylactic acid to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 637W by adopting an ultrasonic pulverizer, and ultrasonically emulsifying for 5min to obtain a W/O type emulsion; dissolving 0.2g emulsifying dispersant (0.1g polyvinyl alcohol and 0.1g lignosulfonate) in 70ml water to obtain an external water phase, dropwise adding the obtained W/O type emulsion into the external water phase at 28000rmp by using a high-pressure shearing machine, and shearing and emulsifying for 15min to obtain W/O/W type primary emulsion, wherein the particle size of the droplets of the primary emulsion is 500 nm.

Homogenizing the W/O/W type primary emulsion at 600Pa for 50min to obtain fine emulsion with droplet size of 50 nm.

And stirring the miniemulsion for 5 hours at 1500rpm by using an electric stirrer to volatilize the organic solvent to obtain the nano-capsule mother liquor.

And (3) centrifuging the nano-capsule mother solution for 20min at 10000rpm by using a high-speed refrigerated centrifuge, then performing spray drying for 1.2s at the air inlet temperature of 300 ℃ and the air outlet temperature of 100 ℃ by using a spray dryer, adding 10g of solid filler diatomite and 0.05g of auxiliary agent propylene glycol, and uniformly mixing to obtain the pesticide nano-capsule powder 25.

EXAMPLE 26 preparation of pesticide nanocapsule aqueous suspension 26

Taking 10ml of pure water as an internal water phase, dissolving 1g of external phase active ingredient B s-metolachlor in 20ml of organic solvent dichloromethane, adding 1g of capsule wall material cellulose to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 650W by adopting an ultrasonic pulverizer, and ultrasonically emulsifying for 2min to obtain a W/O type emulsion; dissolving 0.5g of emulsification dispersant agricultural emulsion 1601 in 70ml of water to obtain an external water phase, dropwise adding the obtained W/O type emulsion into the external water phase at 28000rmp by using a high-pressure shearing machine, and shearing and emulsifying for 15min to obtain W/O/W type primary emulsion, wherein the particle size of the droplets of the primary emulsion is 500 nm.

Homogenizing the W/O/W type primary emulsion at 100Pa for 50min to obtain fine emulsion with droplet size of 50 nm.

And stirring the miniemulsion for 24 hours at 500rpm by using an electric stirrer to volatilize the organic solvent to obtain the nano-capsule mother liquor.

Adding 1g of thickening agent (0.5g of xanthan gum and 0.5g of magnesium aluminum silicate) into the nano-capsule mother liquor, and uniformly mixing to obtain the pesticide nano-capsule water suspending agent 26.

EXAMPLE 27 preparation of pesticide Nanocoapsule powder 27

Dispersing 3g of an internal phase active ingredient A tebuconazole in 50ml of water to obtain an internal water phase, dissolving 30g of an external phase active ingredient B cyanodinioxystrobin in 130ml of organic solvent trichloromethane, adding 20g of capsule wall material cellulose to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 585W by adopting an ultrasonic crusher, and ultrasonically emulsifying for 15min to obtain a W/O type emulsion; dissolving 13g of emulsifying dispersant (6.5g of polyvinyl alcohol and 6.5g of agricultural emulsion 1601) in 220ml of water to obtain an external water phase, dropwise adding the obtained W/O type emulsion into the external water phase at 25000rmp by using a high-pressure shearing machine, and shearing and emulsifying for 22min to obtain W/O/W type primary emulsion, wherein the particle size of the droplets of the primary emulsion is 900 nm.

Homogenizing the W/O/W type primary emulsion at 900Pa for 10min by a high-pressure homogenizer to obtain a fine emulsion, wherein the particle size of the droplets of the fine emulsion is 500 nm.

And stirring the miniemulsion for 10 hours at 1500rpm by using an electric stirrer to volatilize the organic solvent to obtain the nano-capsule mother liquor.

Centrifuging the nano-capsule mother solution at 15000rpm for 10min by using a high-speed refrigerated centrifuge, then spray-drying for 1.5s at the air inlet temperature of 30 ℃ and the air outlet temperature of 30 ℃ by using a spray dryer to obtain solid powder, adding 150g of solid filler diatomite and 15g of adjuvant TERSPERSE2020, and uniformly mixing to obtain the pesticide nano-capsule powder 27.

EXAMPLE 28 preparation of pesticide nanocapsule aqueous suspension 28

Dispersing 3g of an internal phase active ingredient A tebuconazole in 50ml of water to obtain an internal water phase, dissolving 30g of an external phase active ingredient B cyanodinioxystrobin in 130ml of organic solvent trichloromethane, adding 20g of capsule wall material cellulose to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 585W by adopting an ultrasonic crusher, and ultrasonically emulsifying for 15min to obtain a W/O type emulsion; dissolving 13g of emulsifying dispersant polyvinyl alcohol in 220ml of water to obtain an external water phase, dropwise adding the obtained W/O type emulsion into the external water phase at 25000rmp by using a high-pressure shearing machine, and shearing and emulsifying for 22min to obtain W/O/W type primary emulsion, wherein the particle size of the droplets of the primary emulsion is 900 nm.

4g of thickening agent (2g of xanthan gum and 2g of magnesium aluminum silicate) and 10g of auxiliary agent TERSPERSE2020 are added into the nano-capsule mother liquor and uniformly mixed to obtain the pesticide nano-capsule water suspending agent 28.

Example 29 preparation of pesticide nanocapsule powder 29

Dissolving 3g of an internal phase active ingredient A validamycin in 40ml of water to obtain an internal water phase, dissolving 15g of an external phase active ingredient B propiconazole in 100ml of organic solvent trichloromethane, adding 15g of wall material polylactic acid to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 28000rmp by adopting a high-pressure shearing machine, and shearing and emulsifying for 3min to obtain W/O type emulsion; dissolving 10g of emulsifying dispersant (5g of polyvinyl alcohol and 5g of agricultural emulsion 1601) in 160ml of water to obtain an external water phase, dropwise adding the obtained W/O type emulsion into the external water phase at 50Hz by using a grinding dispersion machine, and grinding and emulsifying for 15min to obtain W/O/W type primary emulsion, wherein the particle size of the droplets of the primary emulsion is 400 nm.

Centrifuging the nanometer capsule mother liquor at 10000rpm for 20min by a high-speed refrigerated centrifuge, pre-freezing for 4h at-50 ℃ by a freeze dryer, keeping at-60 ℃ for 24h to obtain solid powder, adding 150g of solid filler kaolin, and mixing uniformly to obtain pesticide nanometer capsule powder 29.

EXAMPLE 30 preparation of pesticide nanocapsule aqueous suspension 30

Dissolving 3g of an internal phase active ingredient A validamycin in 40ml of water to obtain an internal water phase, dissolving 15g of an external phase active ingredient B propiconazole in 100ml of organic solvent trichloromethane, adding 15g of wall material polylactic acid to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 10000rmp by using a high-pressure shearing machine, and shearing and emulsifying for 40min to obtain W/O type emulsion; dissolving 10g of emulsifying dispersant (5g of polyvinyl alcohol and 5g of agricultural emulsion 1601) in 160ml of water to obtain an external water phase, dropwise adding the obtained W/O type emulsion into the external water phase at 50Hz by using a grinding dispersion machine, and grinding and emulsifying for 15min to obtain W/O/W type primary emulsion, wherein the particle size of the droplets of the primary emulsion is 400 nm.

And 3g of thickening agent xanthan gum is added into the nano-capsule mother liquor and uniformly mixed to obtain the pesticide nano-capsule water suspending agent 30.

EXAMPLE 31 preparation of pesticide Nanocoapsule powder 31

Dispersing 20g of an internal phase active ingredient A thiamethoxam in 50ml of water to obtain an internal water phase, dissolving 20g of an external phase active ingredient B emamectin benzoate in 130ml of organic solvent dichloromethane, adding 30g of capsule wall material cellulose to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 585W by adopting an ultrasonic pulverizer, and ultrasonically emulsifying for 15min to obtain a W/O type emulsion; dissolving 20g of emulsifying dispersant (10g of polyvinyl alcohol and 10g of sodium dodecyl sulfate) in 230ml of water to obtain an external water phase, dropwise adding the obtained W/O type emulsion into the external water phase at 30Hz by using a grinding dispersion machine, and grinding and emulsifying for 60min to obtain W/O/W type primary emulsion, wherein the particle size of the droplets of the primary emulsion is 400 nm.

Centrifuging the nano-capsule mother solution for 20min at 10000rpm by using a high-speed refrigerated centrifuge, then pre-freezing for 4h at-50 ℃ by using a freeze dryer, keeping the temperature for 18h at-60 ℃ to obtain solid powder, adding 150g of solid filler bentonite and 10g of adjuvant TERSPERSE2020, and uniformly mixing to obtain the pesticide nano-capsule powder 31.

EXAMPLE 32 preparation of pesticide nanocapsule aqueous suspension 32

Dispersing 20g of an internal phase active ingredient A thiamethoxam in 50ml of water to obtain an internal water phase, dissolving 20g of an external phase active ingredient B emamectin benzoate in 130ml of organic solvent dichloromethane, adding 30g of capsule wall material cellulose to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 585W by adopting an ultrasonic pulverizer, and ultrasonically emulsifying for 15min to obtain a W/O type emulsion; dissolving 20g of emulsifying dispersant (10g of polyvinyl alcohol and 10g of sodium dodecyl sulfate) in 230ml of water to obtain an external water phase, dropwise adding the obtained W/O type emulsion into the external water phase at 40Hz by using a grinding dispersion machine, and grinding and emulsifying for 40min to obtain W/O/W type primary emulsion, wherein the particle size of the droplets of the primary emulsion is 400 nm.

And adding 10g of thickening agent (5g of xanthan gum and 5g of magnesium aluminum silicate) and 10g of auxiliary agent TERSPERSE2020 into the nano-capsule mother liquor, and uniformly mixing to obtain the pesticide nano-capsule water suspending agent 32.

EXAMPLE 33 preparation of pesticide nanocapsule powder 33

Dispersing 40g of internal phase active ingredient A emamectin benzoate in 40ml of water to obtain an internal water phase, dissolving 40g of external phase active ingredient B emamectin benzoate in 200ml of organic solvent dichloromethane, adding 40g of capsule wall material polylactic acid to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 65W by adopting an ultrasonic crusher, and ultrasonically emulsifying for 30min to obtain W/O type emulsion; dissolving 30g of emulsifying dispersant (10g of polyvinyl alcohol, 10g of agricultural emulsion 600 and 10g of agricultural emulsion 700) in 260ml of water to obtain an external water phase, dropwise adding the obtained W/O type emulsion into the external water phase at 45Hz by using a grinding and dispersing machine, and grinding and emulsifying for 20min to obtain W/O/W type primary emulsion, wherein the particle size of the droplets of the primary emulsion is 400 nm.

Centrifuging the nano-capsule mother solution at 10000rpm for 25min by using a high-speed refrigerated centrifuge, pre-freezing for 4h at-50 ℃ by using a freeze dryer, keeping the temperature at-60 ℃ for 12h to obtain solid powder, adding 200g of solid filler bentonite and 20g of adjuvant TERSPERSE2020, and uniformly mixing to obtain the pesticide nano-capsule powder 33.

EXAMPLE 34 preparation of pesticide nanocapsule aqueous suspension 34

Dispersing 40g of internal phase active ingredient A emamectin benzoate in 40ml of water to obtain an internal water phase, dissolving 40g of external phase active ingredient B emamectin benzoate in 200ml of organic solvent dichloromethane, adding 40g of capsule wall material polylactic acid to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 325W by adopting an ultrasonic crusher, and ultrasonically emulsifying for 25min to obtain W/O type emulsion; dissolving 30g of emulsifying dispersant (10g of polyvinyl alcohol, 10g of agricultural emulsion 600 and 10g of agricultural emulsion 700) in 260ml of water to obtain an external water phase, dropwise adding the obtained W/O type emulsion into the external water phase at 50Hz by using a grinding and dispersing machine, and grinding and emulsifying for 5min to obtain W/O/W type primary emulsion, wherein the particle size of the droplets of the primary emulsion is 400 nm.

30g of thickening agent (15g of xanthan gum and 15g of magnesium aluminum silicate) and 20g of auxiliary agent TERSPERSE2020 are added into the nano-capsule mother liquor and mixed uniformly to obtain the pesticide nano-capsule water suspending agent 34.

EXAMPLE 35 preparation of pesticide nanocapsule powder 35

Dissolving 0.5g of an internal phase active ingredient A validamycin in 5ml of water to obtain an internal water phase, dissolving 0.5g of an external phase active ingredient B thifluzamide in 10ml of organic solvent dichloromethane, adding 0.1g of capsule wall material cellulose to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 585W by adopting an ultrasonic crusher, and ultrasonically emulsifying for 15min to obtain a W/O type emulsion; dissolving 0.5g emulsifying dispersant (0.2g polyvinyl alcohol and 0.3g sodium dodecyl sulfate) in 45ml water to obtain an external water phase, dripping the obtained W/O type emulsion into the external water phase at 26000rmp by a high-pressure shearing machine, and shearing and emulsifying for 20min to obtain W/O/W type primary emulsion, wherein the particle size of the droplets of the primary emulsion is 100 nm.

Centrifuging the nano-capsule mother liquor for 30min at 4000rpm by using a high-speed refrigerated centrifuge, then performing spray drying for 1s at the air inlet temperature of 100 ℃ and the air outlet temperature of 140 ℃ by using a spray dryer to obtain solid powder, adding 10g of solid filler bentonite, and uniformly mixing to obtain the pesticide nano-capsule powder 35.

EXAMPLE 36 preparation of pesticide nanocapsule aqueous suspension 36

And adding 1g of thickening agent xanthan gum into the nano-capsule mother liquor, and uniformly mixing to obtain the pesticide nano-capsule water suspending agent 36.

Example 37 preparation of pesticide nanocapsule powder 37

Dispersing 30g of an internal phase active ingredient A thiamethoxam in 50ml of water to obtain an internal water phase, dissolving 20g of an external phase active ingredient B emamectin benzoate in 130ml of organic solvent dichloromethane, adding 30g of capsule wall material cellulose to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 585W by adopting an ultrasonic pulverizer, and ultrasonically emulsifying for 15min to obtain a W/O type emulsion; dissolving 20g of emulsifying dispersant (10g of polyvinyl alcohol and 10g of sodium dodecyl sulfate) in 220ml of water to obtain an external water phase, dropwise adding the obtained W/O type emulsion into the external water phase at 30Hz by using a grinding dispersion machine, and grinding and emulsifying for 60min to obtain W/O/W type primary emulsion, wherein the particle size of the droplets of the primary emulsion is 400 nm.

Centrifuging the nano-capsule mother solution for 20min at 10000rpm by using a high-speed refrigerated centrifuge, pre-freezing for 4h at-50 ℃ by using a freeze dryer, keeping the temperature at-60 ℃ for 18h to obtain solid powder, adding 150g of solid filler bentonite and 10g of adjuvant TERSPERSE2020, and uniformly mixing to obtain pesticide nano-capsule powder 37.

EXAMPLE 38 preparation of pesticide nanocapsule aqueous suspension 38

Dispersing 30g of an internal phase active ingredient A thiamethoxam in 50ml of water to obtain an internal water phase, dissolving 20g of an external phase active ingredient B emamectin benzoate in 130ml of organic solvent dichloromethane, adding 30g of capsule wall material cellulose to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 585W by adopting an ultrasonic pulverizer, and ultrasonically emulsifying for 15min to obtain a W/O type emulsion; dissolving 20g of emulsifying dispersant (10g of polyvinyl alcohol and 10g of sodium dodecyl sulfate) in 220ml of water to obtain an external water phase, dropwise adding the obtained W/O type emulsion into the external water phase at 40Hz by using a grinding dispersion machine, and grinding and emulsifying for 40min to obtain W/O/W type primary emulsion, wherein the particle size of the droplets of the primary emulsion is 400 nm.

20g of thickening agent (10g of xanthan gum and 10g of magnesium aluminum silicate) and 15g of auxiliary agent TERSPERSE2020 are added into the nano-capsule mother liquor and uniformly mixed to obtain the pesticide nano-capsule water suspending agent 38.

Example 39 preparation of pesticide nanocapsule powder 39

Dissolving 0.8g of an internal phase active ingredient A validamycin in 20ml of water to obtain an internal water phase, dissolving 0.2g of an external phase active ingredient B thifluzamide in 30ml of organic solvent dichloromethane, adding 10g of capsule wall material cellulose to obtain an oil phase, dropwise adding the internal water phase into the oil phase at 585W by using an ultrasonic crusher, and ultrasonically emulsifying for 15min to obtain a W/O type emulsion; dissolving 0.5g emulsifying dispersant (0.25g polyvinyl alcohol and 0.25g sodium dodecyl sulfate) in 80ml water to obtain an external water phase, dripping the obtained W/O type emulsion into the external water phase at 28000rmp by using a high-pressure shearing machine, and shearing and emulsifying for 15min to obtain W/O/W type primary emulsion, wherein the particle size of the droplets of the primary emulsion is 300 nm.

Centrifuging the nano-capsule mother solution for 20min at 10000rpm by using a high-speed refrigerated centrifuge, then pre-freezing for 4h at-50 ℃ by using a freeze dryer, keeping the temperature for 12h at-60 ℃ to obtain solid powder, adding 20g of solid filler bentonite and 0.05g of adjuvant TERSPERSE2020, and uniformly mixing to obtain pesticide nano-capsule powder 39.

EXAMPLE 40 preparation of pesticide nanocapsule aqueous suspension 40

And adding 0.1g of thickening agent xanthan gum into the nano-capsule mother liquor, and uniformly mixing to obtain the pesticide nano-capsule water suspending agent 40.

Test example 1 measurement of morphology, particle size and particle size distribution of pesticide nanocapsules

The morphology of the pesticide nanocapsule prepared in the above example was observed by a scanning electron microscope and the particle size and particle size distribution thereof were measured by a nanometer laser particle sizer.

Fig. 1 is a microscope picture of the emamectin benzoate pesticide nanocapsule prepared in example 3 of the present invention under 2 ten thousand times (a) and 4 ten thousand times (b) magnification. As seen from figure 1, the emamectin benzoate pesticide nanocapsules prepared by the embodiment of the invention are in a capsule shape, and the average particle size is about 100 nm.

Test example 2 emamectin benzoate pesticide nanocapsule distribution test

The emamectin benzoate pesticide nanocapsule prepared in the above example 4 is sprayed on clean cucumber leaves, and after drying, the distribution of the pesticide nanocapsule on the leaves is observed by using an environmental scanning electron microscope.

Tests prove that the pesticide nanocapsules prepared by the embodiment of the invention have good dispersibility and uniform distribution on cucumber leaves.

Test example 3 sustained release Performance test of Avermectin pesticide nanocapsules

The avermectin pesticide nanocapsules prepared in example 7 and the commercially available avermectin water dispersible granules (Beijing Huajon biology, Kaiwei) were tested for their sustained release performance (the content of avermectin released in the pesticide nanocapsules was tested by dialysis at different release times using high performance liquid chromatography) respectively to prepare cumulative release-time curves.

Fig. 2 is a slow release curve of the avermectin pesticide nanocapsule prepared in embodiment 7 of the present invention and the commercially available avermectin water dispersible granules in 250 hours, and it is seen from the graph that the avermectin pesticide nanocapsule prepared in the embodiment of the present invention has an accumulated release amount of about 15% in the first 13 hours, and then the release rate is slowed down, and the accumulated release amount reaches about 81% in 250 hours; and the accumulated release amount of the commercial abamectin water dispersible granule reaches about 95 percent within the first 13 hours. Therefore, compared with the abamectin water dispersible granule sold in the market, the abamectin pesticide nano-capsule prepared by the embodiment of the invention has the advantages that the release time is obviously prolonged, the lasting period can be prolonged to more than 10 days, and the abamectin pesticide nano-capsule has an obvious slow release characteristic.

In addition, tests show that the pesticide nanocapsule prepared by the other embodiments of the invention also has excellent slow release performance.

Test example 4 anti-photolysis Performance test of Avermectin pesticide nanocapsules

The avermectin pesticide nanocapsule prepared in the above example 7 and the commercially available avermectin water dispersible granule (Beijing Huajon biology, Kaiwei) are respectively irradiated under 500W ultraviolet light for 12h, 24h, 36h, 48h, 60h and 72h, and ultraviolet degradation resistance of the avermectin pesticide nanocapsule prepared in the example 7 and the commercially available avermectin water dispersible granule is respectively tested by adopting a pesticide light stability test box, and a light degradation rate-time curve is prepared.

As shown in fig. 3, compared with the traditional commercially available abamectin water dispersible granule, the abamectin pesticide nanocapsule prepared by the embodiment of the invention has a significantly reduced photodegradation rate under ultraviolet light irradiation and has good ultraviolet light degradation resistance. The method can effectively protect the abamectin pesticide from photodegradation, thereby greatly improving the effective utilization rate and bioavailability, reducing the application frequency and dosage and being beneficial to environmental and ecological safety.

In addition, tests show that the pesticide nanocapsules prepared by the other embodiments of the invention also have excellent ultraviolet degradation resistance.

While preferred embodiments of the present invention have been shown and described herein, it will be obvious to those skilled in the art that such embodiments are provided by way of example only. Numerous variations, changes, and substitutions will now occur to those skilled in the art without departing from the invention. It should be understood that various alternatives to the embodiments of the invention described herein may be employed in practicing the invention. It is intended that the following claims define the scope of the invention and that methods and structures within the scope of these claims and their equivalents be covered thereby.

Claims

1. A pesticide nanocapsule is prepared from the following components in parts by weight:

active ingredients of the pesticide: 0.1 to 80 portions

Capsule wall material: 0.1 to 40 portions

Emulsifying and dispersing agent: 0.2 to 30 portions of

Organic solvent: 10-200 parts of

Water: 20 to 350 portions of

Excipient: 0.1 to 200 portions of

Auxiliary agents: 0 to 20 portions of the components are added,

wherein the ratio of the pesticide active ingredient to the capsule wall material is 0.1:1-10: 1; the pesticide active ingredients comprise an inner phase active ingredient A and an outer phase active ingredient B, and the ratio of the inner phase active ingredient A to the outer phase active ingredient B is 0.2:1-4: 1; the capsule wall material is a degradable high polymer material; the slow release period of the pesticide nano capsule is within 3 days to 3 months; the capsule wall of the pesticide nanocapsule is 5-50nm thick;

the preparation method of the pesticide nanocapsule comprises the following steps:

step a: dispersing or dissolving an internal phase active ingredient A in water to form a suspension or an aqueous solution of the internal phase active ingredient A as an internal water phase, dissolving an external phase active ingredient B in an organic solvent, adding a capsule wall material to obtain an oil phase, and dropwise adding the internal water phase into the oil phase under an emulsification condition to obtain a W/O type emulsion; dissolving an emulsifying dispersant into water to obtain an external water phase, and dropwise adding the obtained W/O type emulsion into the external water phase under an emulsifying condition to obtain a W/O/W type primary emulsion;

step d: mixing the nano-capsule mother liquor obtained in the step c with an excipient and an auxiliary agent to obtain a pesticide nano-capsule;

the particle size of the droplets of the primary emulsion in the step a under the emulsification condition is 100-900nm under the ultrasonic emulsification condition, the shearing emulsification condition or the grinding emulsification condition; wherein under the ultrasonic emulsification condition, an ultrasonic crusher is adopted for ultrasonic emulsification, the power of the ultrasonic crusher is 65-650W, and the ultrasonic emulsification time is 2-30 min; wherein the shearing emulsification is carried out by adopting a high-speed shearing machine under the shearing emulsification condition, the shearing rotating speed of the high-speed shearing machine is 10000-28000rmp, and the shearing emulsification time is 3-40 min; wherein the grinding and emulsifying are carried out by adopting a grinding dispersion machine under the grinding and emulsifying conditions, the frequency of the grinding and emulsifying is 30-50Hz, and the time of the grinding and emulsifying is 5-60 min;

the high-pressure homogenization in the step b is carried out by adopting a high-pressure homogenizer, the pressure of the high-pressure homogenization is 100-1200Pa, the time of the high-pressure homogenization is 10min-2h, and the particle size of the droplets of the miniemulsion is 10-500 nm;

in the step c, an electric stirrer is adopted for stirring, the stirring speed is 500-1500rpm, and the stirring time is 5-24 h.

2. The pesticide nanocapsule of claim 1, wherein the pesticide nanocapsule has a particle size of 20 to 1000 nm;

the pesticide nanocapsule is pesticide nanocapsule powder or a pesticide nanocapsule water suspending agent, the drug-loading rate of the pesticide nanocapsule powder is 0.01-90%, and the drug-loading rate of the pesticide nanocapsule water suspending agent is 0.01-40%.

3. The pesticide nanocapsule of claim 2, wherein the particle size of the pesticide nanocapsule is 100nm or less.

4. The pesticide nanocapsule of claim 3, wherein the pesticide nanocapsule has a particle size of less than 50 nm.

5. The pesticide nanocapsule of claim 1, wherein the pesticide nanocapsule is a pesticide nanocapsule powder, wherein the excipient is a solid filler, and wherein the pesticide nanocapsule powder is prepared from the following components by weight:

inner phase active ingredient a: 0 to 40 portions of

External phase active ingredient B: 0.1 to 40 portions

Capsule wall material: 0.1 to 40 portions

Emulsifying and dispersing agent: 0.2 to 30 portions of

Organic solvent: 10-200 parts of

Water: 20 to 350 portions of

Solid filler: 0.1 to 200 portions of

Auxiliary agents: 0-20 parts.

6. The pesticide nanocapsule of claim 5, wherein the pesticide nanocapsule powder is made of, by weight:

inner phase active ingredient a: 0 to 30 portions of

External phase active ingredient B: 0.5 to 30 portions of

Capsule wall material: 0.5 to 30 portions of

Emulsifying and dispersing agent: 0.5 to 20 portions of

Organic solvent: 10 to 100 portions of

Water: 50-200 parts of

Solid filler: 10-200 parts of

Auxiliary agents: 0-15 parts.

7. The pesticide nanocapsule of claim 6, wherein the pesticide nanocapsule powder is made of, by weight:

inner phase active ingredient a: 0 to 20 portions of

External phase active ingredient B: 1-20 parts of

Capsule wall material: 1-20 parts of

Emulsifying and dispersing agent: 0.5 to 10 portions of

Organic solvent: 20-100 parts of

Water: 50-200 parts of

Solid filler: 10-200 parts of

Auxiliary agents: 0-15 parts.

8. The pesticide nanocapsule of claim 1, wherein the pesticide nanocapsule is a pesticide nanocapsule aqueous suspension concentrate, wherein the excipient is a thickener, and wherein the pesticide nanocapsule aqueous suspension concentrate is prepared from, by weight:

inner phase active ingredient a: 0 to 40 portions of

External phase active ingredient B: 0.1 to 40 portions

Capsule wall material: 0.1 to 40 portions

Emulsifying and dispersing agent: 0.2 to 30 portions of

Organic solvent: 10-200 parts of

Water: 20 to 350 portions of

Thickening agent: 0.1 to 30 portions

Auxiliary agents: 0-20 parts.

9. The pesticide nanocapsule of claim 8, wherein the pesticide nanocapsule aqueous suspension is prepared from, by weight:

inner phase active ingredient a: 0 to 30 portions of

External phase active ingredient B: 0.5 to 30 portions of

Capsule wall material: 0.5 to 30 portions of

Emulsifying and dispersing agent: 0.5 to 20 portions of

Organic solvent: 10 to 100 portions of

Water: 50-200 parts of

Thickening agent: 1-20 parts of

Auxiliary agents: 0-15 parts.

10. The pesticide nanocapsule of claim 9, wherein the pesticide nanocapsule aqueous suspension is made of, by weight:

inner phase active ingredient a: 0 to 20 portions of

External phase active ingredient B: 1-20 parts of

Capsule wall material: 1-20 parts of

Emulsifying and dispersing agent: 0.5 to 10 portions of

Organic solvent: 20-100 parts of

Water: 50-200 parts of

Thickening agent: 1-10 parts of

Auxiliary agents: 0-15 parts.

11. The pesticide nanocapsule of claim 1, wherein the ratio of the inner phase active ingredient a to the outer phase active ingredient B is from 0.2:1 to 0.6: 1;

the inner phase active ingredient A and the outer phase active ingredient B are the same or different substances;

the inner phase active component A is a water-soluble substance or a fat-soluble substance, and the outer phase active component B is a fat-soluble substance.

12. The pesticide nanocapsule of claim 11, wherein the ratio of the inner phase active ingredient a to the outer phase active ingredient B is 0.4: 1;

the inner phase active ingredient A is a water-soluble material.

13. The pesticide nanocapsule of claim 1, wherein the inner phase active ingredient a and the outer phase active ingredient B are each selected from one or more of an insecticide, a fungicide, a herbicide, and a plant growth regulator.

14. The pesticide nanocapsule of claim 13, wherein the pesticide is selected from one or more of the following: abamectin, emamectin benzoate, lambda-cyhalothrin, chlorantraniliprole, spinosad, indoxacarb, clothianidin, acephate, carbosulfan, triazophos, dinosaur, acanthodol, chlorpyrifos, bifenthrin, cyphenothrin, ethofenprox, deltamethrin, fenvalerate, cyhalothrin, tefluthrin, fosthiazate, phoxim, imidacloprid and thiamethoxam;

the bactericide is selected from one or more of the following: validamycin, azoxystrobin, pyraclostrobin, thifluzamide, tebuconazole, metconazole, cyenopyram, fluazinam, cymoxanil, boscalid, ethofenprox, cyflumetofen, fenpropathrin, benzothiostrobin, pefurazoate, prochloraz, propiconazole, difenoconazole, mefenoxam, flusilazole, epoxiconazole, trifloxystrobin and pyraclostrobin;

the herbicide is selected from one or more of the following: pendimethalin, triallate, 2,4-D isooctyl ester, prosulfocarb, cycloxaben, galapetalum, clomazone, butralin, metolachlor, trifluralin and prometryn;

the plant growth regulator is selected from one or more of the following: brassinolide, aminoxyethylvinylglycine and a paclobutrazol plant growth regulator;

the wall material is selected from one or more of the following: polyester acrylate and its derivatives, polyvinyl acetate resin, polyacrylonitrile resin, polystyrene resin, polylactic acid, gelatin, modified starch, cellulose and its derivatives, chitosan and acacia.

15. The pesticide nanocapsule of claim 14, wherein the pesticide is selected from one or more of thiamethoxam, spinosad, chlorantraniliprole, abamectin, emamectin benzoate, and lambda-cyhalothrin;

the bactericide is selected from one or more of validamycin, tebuconazole, thifluzamide, metconazole, cyhalothrin, fluazinam, azoxystrobin, pyraclostrobin, cymoxanil and boscalid;

the herbicide is selected from one or more of pendimethalin and metolachlor;

the plant growth regulator is a paclobutrazol plant growth regulator;

the capsule wall material is selected from one or more of cellulose and derivatives thereof, chitosan, polylactic acid and modified starch.

16. The pesticide nanocapsule of claim 5, wherein the emulsifying dispersant is one or more of an agricultural emulsifier and a dispersant, and the agricultural emulsifier is one or more selected from OP series, NP series, EL series, Tween series, Span series, AEO series, agricultural emulsion series emulsifier, polyvinyl alcohol, polyethylene glycol fatty acid ester, polyvinylpyrrolidone, and polyethylene glycol oleate;

the dispersing agent is selected from one or more of carboxylate, sulfate, sulfonate, phosphate ester salt and alkylphenol polyoxyethylene;

the auxiliary agent is selected from one or more of a preservative, a defoaming agent, an antifreeze agent, a pH regulator and a wetting dispersant;

the antifreeze is selected from one or more of ethylene glycol, propylene glycol, glycerol, isopropanol and urea;

the defoaming agent is selected from one or more of organic silicon defoaming agents and low-carbon alcohol defoaming agents;

the organic solvent is selected from one or more of dichloromethane, trichloromethane, vegetable oil, petroleum ether and aliphatic hydrocarbon solvent oil;

the solid filler is selected from one or more of bentonite, diatomite, kaolin, talcum powder, montmorillonite, white carbon black, corn starch and sepiolite.

17. The pesticide nanocapsule of claim 8, wherein the thickener is selected from one or more of xanthan gum, gum arabic, gelatin, cellulose and its derivatives, diatomaceous earth, polyvinyl alcohol, sodium polyacrylate, dextrin, magnesium aluminum silicate, and silica gel.

18. The pesticide nanocapsule of claim 16, wherein the agricultural emulsifier is selected from one or more of Tween series, polyvinyl alcohol and agricultural dairy series emulsifiers;

the dispersing agent is selected from one or more of fatty alcohol polyoxyethylene ether carboxylate, lauryl sodium sulfate, lignosulfonate, sodium dodecyl sulfonate, maleic rosin polyoxyethylene-oxypropylene ether sulfonate and dodecyl ether phosphate;

the auxiliary agent is selected from one or more of an antifreeze agent, a defoaming agent and a wetting dispersant;

the antifreeze agent is ethylene glycol;

the defoaming agent is an organic silicon defoaming agent;

the organic solvent is dichloromethane;

the solid filler is selected from one or more of bentonite, kaolin, corn starch and white carbon black.

19. The pesticide nanocapsule of claim 17, wherein the thickener is selected from one or more of xanthan gum, gelatin, magnesium aluminum silicate, cellulose and its derivatives, and polyvinyl alcohol.

20. The pesticide nanocapsule of claim 18, wherein the agricultural emulsifier is selected from one or more of the group consisting of polyvinyl alcohol, agricultural milk 300 series, agricultural milk 500 series, agricultural milk 600 series, agricultural milk 700 series, and agricultural milk 1600 series emulsifiers;

the dispersant is selected from one or more of lignosulfonate, sodium dodecyl sulfate and sodium dodecyl sulfate.

21. The method for preparing a pesticide nanocapsule as claimed in any one of claims 1 to 20, the method comprising: emulsifying the components of the pesticide nanocapsule to form primary emulsion, and then homogenizing under high pressure to form miniemulsion to prepare the pesticide nanocapsule.

22. The method of manufacturing of claim 21, comprising the steps of:

23. The method for preparing a composite material according to claim 22, wherein the step a comprises: dispersing or dissolving an internal phase active ingredient A in water to form a suspension or an aqueous solution of the internal phase active ingredient A as an internal water phase, dissolving an external phase active ingredient B in an organic solvent, adding a capsule wall material to obtain an oil phase, and dropwise adding the internal water phase into the oil phase under an emulsification condition to obtain a W/O type emulsion; dissolving an emulsifying dispersant into water to obtain an external water phase, and dropwise adding the obtained W/O type emulsion into the external water phase under an emulsifying condition to obtain the W/O/W type primary emulsion.

24. The method for preparing the pesticide nanocapsule of claim 23, wherein the pesticide nanocapsule is a pesticide nanocapsule aqueous suspension, the excipient is a thickener, and the step d comprises: c, adding a thickening agent and an auxiliary agent into the nano-capsule mother liquor obtained in the step c, and uniformly mixing to obtain a pesticide nano-capsule water suspending agent;

or, the pesticide nanocapsule is pesticide nanocapsule powder, the excipient is a solid filler, and the step d comprises: and c, centrifuging and drying the nano-capsule mother liquor obtained in the step c to obtain solid powder, adding a solid filler and an auxiliary agent, and uniformly mixing to obtain pesticide nano-capsule powder.

25. The method of claim 24, wherein the emulsifying conditions in step a are under shear emulsifying conditions and under ultrasonic emulsifying conditions; the particle size of the primary emulsion liquid drop is 100-500 nm;

wherein the ultrasonic emulsification is carried out by adopting an ultrasonic crusher under the ultrasonic emulsification condition, and the power of the ultrasonic crusher is 325-637W; the ultrasonic emulsification time is 5-25 min;

wherein the shearing emulsification is carried out by adopting a high-speed shearing machine under the shearing emulsification condition, and the shearing rotating speed of the high-speed shearing machine is 22000-28000 rmp; shearing and emulsifying for 3-30 min;

wherein the grinding and emulsifying are carried out by adopting a grinding dispersion machine under the grinding and emulsifying conditions, and the frequency of the grinding and emulsifying is 40-50 Hz; grinding and emulsifying for 5-40 min;

the high-pressure homogenization in the step b is carried out by adopting a high-pressure homogenizer, and the pressure of the high-pressure homogenization is 600-1000 Pa; the high-pressure homogenization time is 10min-1 h; the particle size of the droplets of the miniemulsion is 10-100 nm;

stirring by adopting an electric stirrer in the step c at the stirring speed of 1000-; stirring for 10-20 h;

when the pesticide nanocapsule is pesticide nanocapsule powder, in the step d, a high-speed refrigerated centrifuge is adopted to centrifuge for 10-30min at the rotation speed of 4000-15000 rpm;

when the pesticide nanocapsule is pesticide nanocapsule powder, the drying in the step d is spray drying or freeze drying, wherein the spray drying is carried out by adopting a spray dryer, the conditions of the spray drying are that the air inlet temperature is 30-300 ℃, the air outlet temperature is 30-140 ℃, and the drying time is 1-1.5 s; the freeze drying is carried out by adopting a freeze dryer, and the condition of freeze drying is pre-freezing for 4h at-50 ℃ and keeping for 12-24h at-60 ℃.

26. The method of claim 25, wherein the subjecting is carried out under the condition of ultrasonic emulsification with an ultrasonic pulverizer having a power of 585W; the ultrasonic emulsification time is 15 min;

under the condition of shearing emulsification, a high-speed shearing machine is adopted for shearing emulsification, and the shearing rotating speed of the high-speed shearing machine is 28000 rmp; the shearing and emulsifying time is 15 min;

under the grinding and emulsifying conditions, a grinding dispersion machine is adopted for grinding and emulsifying, and the frequency of grinding and emulsifying is 50 Hz; grinding and emulsifying for 15 min;

the high-pressure homogenization in the step b is carried out by adopting a high-pressure homogenizer, and the pressure of the high-pressure homogenization is 900 Pa; homogenizing under high pressure for 15 min;

stirring by adopting an electric stirrer in the step c, wherein the stirring speed is 1500 rpm; the stirring time is 12 h;

when the pesticide nanocapsule is pesticide nanocapsule powder, in the step d, a high-speed refrigerated centrifuge is adopted to centrifuge for 20-30min at the rotation speed of 4000-15000 rpm;

when the pesticide nanocapsule is pesticide nanocapsule powder, the freeze drying is carried out by adopting a freeze dryer, and the condition of freeze drying is pre-freezing for 4 hours at-50 ℃ and keeping for 12 hours at-60 ℃.

27. The method for preparing a pesticide nanocapsule as claimed in claim 26, wherein the step d comprises centrifuging the pesticide nanocapsule powder using a high-speed refrigerated centrifuge at 15000rpm for 20 min.