SOLID PESTICIDE NANODISPERSION AND ITS PREPARATION

Abstract

A pesticide solid nanodispersion and its preparation method. The said pesticide solid nanodispersion is composed of 0.001-90 parts by weight of pesticide, 0.001-50 parts by weight of surfactants and 5-99.9 parts by weight of water-soluble carriers. The said pesticide is one or more pesticide(s) selected from poorly water-soluble insecticides, fungicides, herbicides or plant growth regulators; the particle size of the said solid nanodispersion is less than 1 m. Compared with the prior art, the pesticide of the present invention has smaller particle size, more uniform dispersibility and better coating effect of surfactants. The content of surfactants may be less than 1%, even less than 0.1%, and can maintain good dispersibility and stability as well.

Claims

1. A pesticide solid nanodispersion, characterized in that it is formed by uniformly dispersing poorly water-soluble pesticide nanoparticles in surfactants and water-soluble carriers, and it has the composition in parts by weight as follows: pesticide 0.001-90; surfactants 0.001-50; water-soluble carriers 5-99.9; wherein, the said pesticide is one or more pesticide(s) selected from poorly water-soluble insecticides, fungicides, herbicides or plant growth regulators; the average particle size of the said pesticide nanoparticles is 1-1000 nm; formulations of the said pesticide solid nanodispersion are powders, tablets granules or microcapsules.

2. The pesticide solid nanodispersion according to claim 1, characterized in that the said insecticide is selected from pyrethrins, carbamates, organophosphorus, organic sulfurs, organic cholines, nereistoxin, neonicotines, phenyl ureide, abamectin, pyridaben, acequinocyl, phenylpyrazole, indoxacarb or diafenthiuron; The said fungicide is selected from aniline pyridine, antibiotics, aromatic hydrocarbons, dinitroaniline, allylamine, benzsulfamide, benzimidazole, benzisothiazole, benzophenone, benzopyrimidine, benzotriazine, benzyl carbamate, carbamate, carboxamide, carboxylic acid diamide, chloronitrile, cyanoimidazole, cyclopropanecarboxamide, ethylaminothiazole carboxamide, imidazole, hydroxyanilide, imidazolidinone, isobenzofuranone, methoxyacrylate, methoxy carbamate, morpholine, N-phenylcarbamate, oxazolidinedione, phenyl acetamide, phenylamide, phenylpyrrole, phenylurea, thiophosphates, phthalamic acid, phthalimide, piperazine, piperidine, propionamide, pyridine, pyridylmethyl amide, toluamide, triazines or triazoles; The said herbicide is selected from amides, aryloxyphenoxy propionates, phenoxy carboxylic acids, organophosphorus, benzamide, benzofuran, benzoic acid, benzothiadiazinone, carbamate, chloroacetamide, pyridine carboxylic acid, chlorocarboxylic acid, cyclohexanedione, dinitroanilines, diphenyl ether, isoxazole, oxazolidinone, N-phenyl phthalimide, oxadiazole, oxazolidinedione, oxyacetamide, phenylcarbamate, phenyl pyridazine, sulfonaminocarboxyl triazolinone, sulfonyl triazolo carboxamide, triazolopyrimidine, triones, uracil or ureas; The said plant growth regulator is selected from maleic hydrazide, methyl naphthacetate, 6-benzylaminopurine, brassinolide, aminoethoxyvinylglycine or paclobutrazol.

3. The pesticide solid nanodispersion according to claim 1, characterized in that the said surfactant is one or more surfactant(s) selected from cationic surfactants, anionic surfactants, nonionic surfactants or amphoteric surfactants; The said cationic surfactant is selected from aliphatic amine salts, ethanolamine salts, polyethylene polyamine salts or quaternary ammonium salts; The said anionic surfactant is selected from sodium dodecyl sulfonate, sodium lauryl sulfate, sodium dodecylbenzenesulfonate, maleic rosin-polyoxypropylene-polyoxyethylene ether sulfonate, alkyl phenol polyoxyethylene ether phosphate salts, monododecyl ether phosphate salt, didodecyl ether phosphate salt, octyl ether phosphate, aliphatic alcohol polyoxyethylene phosphatidates, aliphatic alcohol polyoxyethylene ether carboxylates, polycarboxylates or lignosulfonates; The said nonionic surfactant is selected from alkylphenol polyoxyethylene ether formaldehyde condensates, styrylphenol polyoxyethylene ether formaldehyde condensate, polystyrene phenol polyoxyethylene ether, cumenyl phenol polyoxyethylene ether formaldehyde condensate, benzylphenol polyoxyethylene ether formaldehyde condensate, polyoxyethylene castor oil, polyvinyl pyrrolidone, Tween, sorbitan oleate, polyoxyethylene-polyoxypropylene block copolymer or sucrose monooleate; The said amphoteric surfactant is selected from dodecylhydroxypropyl sulfobetaine, lauryl betaine, octadecyl dihydroxyethyl amine oxide, octadecyl urea or oleyl biuret.

4. The pesticide solid nanodispersion according to claim 1, characterized in that the said water-soluble carrier is selected from urea, sodium sulfate, magnesium sulfate, sodium benzoate, sucrose, lactose, soluble starch, hydroxypropyl methyl cellulose, hydroxyethyl cellulose, sodium carboxymethyl cellulose, hydroxyethyl--cyclodextrin, hydroxypropyl--cyclodextrin, sulfo--cyclodextrin, polyvinyl alcohol, polyethylene glycol, xanthan gum, magnesium aluminum silicate, acacia, sodium acrylate or polyvinylpyrrolidone.

5. The preparation method for the said pesticide solid nanodispersion according to claim 1 comprises the following steps: A. Preparing the nanodispersion solution Heating 0.001 to 90 parts by weight of the pesticide to the temperature above its melting point while below its decomposition and denaturation temperature, subsequently pouring the said pesticide into the water, then dispersing the said pesticide uniformly in water using a high-speed shear emulsifying machine or a high-pressure homogenizer, subsequently cooling it to room temperature to obtain the dispersion solution of the pesticide solid nanoparticles; and B. Preparing the solid nanodispersion Adding 0.001 to 50 parts by weight of surfactants and 5 to 99.9 parts by weight of water-soluble carriers to the dispersion solution of the pesticide solid nanoparticles obtained in step A, stirring, and then removing water by heating, decompression evaporation, vacuum drying or freeze drying, thus obtaining the said pesticide solid nanodispersion.

6. The preparation method according to claim 5, characterized in that the shearing speed of the said high-speed shear emulsifying machine is 1000-30000 rpm, the pressure of the said high-pressure homogenizer is 50-1500 bar and the said stirring speed is 50-5000 rpm.

7. The preparation method for the pesticide solid nanodispersion according to claim 1, characterized in that the said preparation method comprises the following steps: A. Preparing the nanodispersion solution Heating 0.001 to 90 parts by weight of the pesticide to the temperature above its melting point, subsequently pouring it into a poor solvent of the said pesticide, then dispersing the said pesticide uniformly in the poor solvent using a high-speed shear emulsifying machine or a high-pressure homogenizer, subsequently cooling it to room temperature to obtain the dispersion solution of the pesticide solid nanoparticles; and B. Preparing the solid nanodispersion Adding 0.001 to 50 parts by weight of surfactants and 5 to 99.9 parts by weight of water-soluble carriers to the dispersion solution of the pesticide solid nanoparticles obtained in step A, stirring, and then removing the poor solvent and water by freeze drying, spray drying, centrifugation or distillation, thus obtaining the said pesticide solid nanodispersion.

8. The preparation method according to claim 7, characterized in that the shearing speed of the said high-speed shear emulsifying machine is 1000-30000 rpm, the pressure of the said high-pressure homogenizer is 50-1500 bar and the said stirring speed is 50-5000 rpm.

9. The preparation method for the pesticide solid nanodispersion according to claim 1, characterized in that the said preparation method comprises the following steps: Dissolving 0.001 to 90 parts by weight of the pesticide in the good solvent of the said pesticide, then adding 0.001 to 50 parts by weight of surfactants, 5 to 99.9 parts by weight of water-soluble carriers and 0 to 50 parts by weight of water, mixing, and then dispersing the said pesticide using a high-speed shear emulsifying machine or a high-pressure homogenizer, followed by distillation, decompression evaporation, spray drying, freeze-drying or drying to remove the solvent, thus obtaining the said pesticide solid nanodispersion.

10. The preparation method according to claim 9, characterized in that the shearing speed of the high-speed shear emulsifying machine is 1000-30000 rpm, the pressure of the said high-pressure homogenizer is 50-1500 bar.

Description

EXAMPLES

[0076] It will be able to understand the present invention better by the following examples.

Example 1: Preparation of the Pesticide Solid Nanodispersion of the Present Invention

[0077] The procedures of the example are as follows:

[0078] A. Preparation of a Nanodispersion Solution

[0079] 0.001 parts by weight of lambda-cyhalothrin insecticide was heated to about 10 C. above its melting point 49.2 C. and poured into water. And then lambda-cyhalothrin was uniformly dispersed in water by shearing for 20 min at the speed of 10000 rpm with a high-speed shear emulsifying machine sold by ATS Co. under the trade name C25, subsequently cooled to room temperature, thus obtaining a dispersion solution of lambda-cyhalothrin solid nanoparticles; and

[0080] B. Preparation of Solid Nanodispersion 0.099 parts by weight of dodecanesulfonic acid sodium salt surfactant and 99.9 parts by weight of urea were added into the dispersion solution of lambda-cyhalothrin solid nanoparticles obtained in step A. The resulting mixture was stirred at a rotation speed of 1000 rpm, and then heated at 80 C. to remove water using a drying equipment sold by Shanghai Yiheng Co. under the trade name DHG-9070A, thus preparing the said solid nanodispersion of lambda-cyhalothrin.

[0081] The solid nanodispersion of lambda-cyhalothrin prepared in this example was dispersed in distilled water. It was measured using a laser granularity analyzer sold by Malvern Co. under the trade name Nano ZS90 and its average particle size was 65 nm. Its suspensibility was 99.2%, and wetting time was 25 s.

Example 2: Preparation of the Pesticide Solid Nanodispersion of the Present Invention

[0082] The procedures of the example are as follows:

[0083] A. Preparation of a Nanodispersion Solution

[0084] 10 parts by weight of nitenpyram insecticide was heated to about 10 C. above its melting point 83 C. and poured into water. Then nitenpyram was uniformly dispersed in water by shearing for 20 min at speed of 20000 rpm with a high-speed shear emulsifying machine sold by ATS Co. under the trade name C25, subsequently cooled to room temperature, thus obtaining a dispersion solution of nitenpyram solid nanoparticles; and

[0085] B. Preparation of Solid Nanodispersion

[0086] 50 parts by weight of monododecyl ether phosphate salts anionic surfactant and 40 parts by weight of sodium sulphate water-soluble carrier were added into the dispersion solution of nitenpyram solid nanoparticles obtained in step A. The mixture was stirred well at a rotation speed of 1800 rpm, and then vacuum evaporated to remove water under water bath of 40 C. and vacuum pressure of 10 mbar using a rotary evaporation equipment sold by BUCHI under the trade name R-210, thus obtaining the said nitenpyram solid nanodispersion.

[0087] The nitenpyram solid nanodispersion prepared in this example was dispersed in distilled water. It was measured using a laser granularity analyzer sold by Malvern Co. under the trade name Nano ZS90 and its average particle size was 45 nm. Its suspensibility was 99%, and wetting time was 35 s.

Example 3: Preparation of the Pesticide Solid Nanodispersion of the Present Invention

[0088] The procedures of the example are as follows:

[0089] A. Preparation of a Nanodispersion Solution

[0090] 30 parts by weight of spinosad insecticide was heated to about 10 C. above its melting point 84 C. and poured into water. Then spinosad was uniformly dispersed in water by homogenizing for 20 min under the pressure of 600 bar with a high-pressure homogenizer sold by ATS Co. under the trade name AH-100D, subsequently cooled to room temperature, thus obtaining a dispersion solution of spinosad solid nanoparticles; and

[0091] B. Preparation of Solid Nanodispersion

[0092] 0.03 parts by weight of octyl ether phosphate anionic surfactant and 69.97 parts by weight of magnesium sulfate water-soluble carrier were added into the dispersion solution of spinosad solid nanoparticles obtained in step A. The mixture was stirred well at a rotation speed of 1200 rpm, then vacuum dried to remove water at 40 C. using an apparatus sold by Jinghong Co. under the trade name XMTD-822, thus obtaining the said spinosad solid nanodispersion.

[0093] The spinosad solid nanodispersion prepared in this example was dispersed in distilled water. It was measured using a laser granularity analyzer sold by Malvern Co. under the trade name Nano ZS90 and its average particle size was 210 nm. Its suspensibility was 98%, and wetting time was 40 s.

Example 4: Preparation of the Pesticide Solid Nanodispersion of the Present Invention

[0094] The procedures of the example are as follows:

[0095] A. Preparation of a Nanodispersion Solution

[0096] 25 parts by weight of trifluralin herbicide was heated to about 10 C. above its melting point 49 C. and poured into water. Then trifluralin was uniformly dispersed in water by shearing for 12 min at shearing speed of 6000 rpm with a high-speed shear emulsifying machine sold by ATS Co. under the trade name C25, subsequently cooled to room temperature, thus obtaining a dispersion solution of trifluralin solid nanoparticles; and

[0097] B. Preparation of Solid Nanodispersion

[0098] 17 parts by weight of polystyrene phenol polyoxyethylene ether nonionic surfactant and 58 parts by weight of urea water-soluble carrier were added into the dispersion solution of trifluralin solid nanoparticles obtained in step A. The resulting mixture was stirred well at a rotation speed of 5000 rpm, and then freeze-dried under the condition of 10 pa to remove water using an equipment sold by EYELA Co. under the trade name FD-81, thus preparing the said trifluralin solid nanodispersion.

[0099] The trifluralin solid nanodispersion prepared in this example was dispersed in distilled water. It was measured using a laser granularity analyzer sold by Malvern Co. under the trade name Nano ZS90 and its average particle size was 256 nm. Its suspensibility was 98%, and wetting time was 47 s.

Example 5: Preparation of the Pesticide Solid Nanodispersion of the Present Invention

[0100] The procedures of the example are as follows:

[0101] A. Preparation of a Nanodispersion Solution

[0102] 18 parts by weight of propamocarb hydrochloride fungicide was heated to about 10 C. above its melting point 55 C. and poured into water. Then propamocarb hydrochloride was uniformly dispersed in water by homogenizing for 10 min under the pressure of 800 bar with a high-pressure homogenizer sold by ATS Co. under the trade name AH-100D, subsequently cooled to room temperature, thus obtaining a dispersion solution of propamocarb hydrochloride solid nanoparticles; and

[0103] B. Preparation of Solid Nanodispersion

[0104] 12 parts by weight of cumenyl phenol polyoxyethylene ether formaldehyde condensate nonionic surfactant, 64 parts by weight of the mixture of urea and sodium sulphate (weight ratio of 1:1) and 6 parts by weight of the mixture of polyethylene glycol and xanthan gum (weight ratio of 1:2) were added into the dispersion solution of propamocarb hydrochloride solid nanoparticles obtained in step A. The resulting mixture was stirred well at a rotation speed of 1000 rpm, and then heated at 60 C. to remove water using a drying equipment sold by Shanghai Yiheng Co. under the trade name DHG-9070A, thus preparing the said solid nanodispersion of propamocarb hydrochloride.

[0105] The solid nanodispersion of propamocarb hydrochloride prepared in this example was dispersed in distilled water. It was measured using a laser granularity analyzer sold by Malvern Co. under the trade name Nano ZS90 and its average particle size was 324 nm. Its suspensibility was 99%, and wetting time was 42 s.

Example 6: Preparation of the Pesticide Solid Nanodispersion of the Present Invention

[0106] The Procedures of the Example are as Follows:

[0107] A. Preparation of a Nanodispersion Solution 5.9 parts by weight of triflumizole fungicide was heated to about 10 C. above its melting point 63.5 C. and poured into water. Then triflumizole was uniformly dispersed in water by shearing for 18 min at shearing speed of 10000 rpm with a high-speed shear emulsifying machine sold by ATS Co. under the trade name C25, subsequently cooled to room temperature, thus obtaining a dispersion solution of triflumizole solid nanoparticles; and

[0108] B. Preparation of Solid Nanodispersion 0.001 parts by weight of benzylphenol polyoxyethylene ether formaldehyde condensates nonionic surfactant, 70 parts by weight of the mixture of sodium sulphate and magnesium sulphate (weight ratio of 2:3) and 24.099 parts by weight of the mixture of polyethylene glycol and magnesium aluminum silicate (weight ratio of 3:1) water-soluble carriers were added into the dispersion solution of triflumizole solid nanoparticles obtained in step A. The resulting mixture was stirred well at a rotation speed of 3000 rpm, and then vacuum evaporated under water bath of 35 C. and the pressure of 12 mbar to remove water using an apparatus sold by BUCHI Co. under the trade name R-210, thus preparing the said triflumizole solid nanodispersion.

[0109] The triflumizole solid nanodispersion prepared in this example was dispersed in distilled water. It was measured using a laser granularity analyzer sold by Malvern Co. under the trade name Nano ZS90 and its average particle size was 67 nm. Its suspensibility was 99.4%, and wetting time was 31 s.

Example 7: Preparation of the Pesticide Solid Nanodispersion of the Present Invention

[0110] The procedures of the example are as follows:

[0111] A. Preparation of a Nanodispersion Solution

[0112] 90.0 parts by weight of alachlor herbicide was heated to about 10 C. above its melting point 41.5 C. and poured into water. Then alachlor was uniformly dispersed in water by homogenizing for 12 min under the pressure of 800 bar with a high-pressure homogenizer sold by ATS Co. under the trade name AH-100D, subsequently cooled to room temperature, thus obtaining a dispersion solution of alachlor solid nanoparticles; and

[0113] B. Preparation of Solid Nanodispersion

[0114] 5.0 parts by weight of dodecylhydroxypropyl sulfobetaine amphoteric surfactant and 5.0 parts by weight of urea water-soluble carrier were added into the dispersion solution of alachlor solid nanoparticles obtained in step A. The mixture was stirred well at a rotation speed of 2000 rpm, then vacuum dried to remove water at 40 C. using an apparatus sold by Jinghong Co. under the trade name XMTD-822, thus obtaining the said alachlor solid nanodispersion.

[0115] The alachlor solid nanodispersion prepared in this example was dispersed in distilled water. It was measured using a laser granularity analyzer sold by Malvern Co. under the trade name Nano ZS90 and its average particle size was 263 nm. Its suspensibility was 98.7%, and wetting time was 37 s.

Example 8: Preparation of the Pesticide Solid Nanodispersion of the Present Invention

[0116] The procedures of the example are as follows:

[0117] A. Preparation of a Nanodispersion Solution

[0118] 20.0 parts by weight of n-triacontanol plant growth regulator was heated to about 5 C. above its melting point 87 C. and poured into water. Then n-triacontanol was uniformly dispersed in water by shearing for 15 min at shearing speed of 18000 rpm with a high-speed shear emulsifying machine sold by ATS Co. under the trade name C25, subsequently cooled to room temperature, thus obtaining a dispersion solution of n-triacontanol solid nanoparticles; and

[0119] B. Preparation of Solid Nanodispersion

[0120] 8.0 parts by weight of lauryl betaine and 72 parts by weight of sodium sulphate water-soluble carrier were added into the dispersion solution of n-triacontanol solid nanoparticles obtained in step A. The resulting mixture was stirred well at a rotation speed of 2600 rpm, and then freeze-dried under the condition of 10 pa to remove water using an apparatus sold by EYELA Co. under the trade name FD-81, thus preparing the said n-triacontanol solid nanodispersion.

[0121] The n-triacontanol solid nanodispersion prepared in this example was dispersed in distilled water. It was measured using a laser granularity analyzer sold by Malvern Co. under the trade name Nano ZS90 and its average particle size was 430 nm. Its suspensibility was 98%, and wetting time was 42 s.

Example 9: Preparation of the Pesticide Solid Nanodispersion of the Present Invention

[0122] The procedures of the example are as follows:

[0123] A. Preparation of a Nanodispersion Solution

[0124] 0.001 parts by weight of deltamethrin insecticide was heated to about 5 C. above its melting point 101 C. and poured into ethylene glycol solvent. Then deltamethrin was uniformly dispersed in ethylene glycol by shearing for 18 min at shearing speed of 25000 rpm with a high-speed shear emulsifying machine sold by ATS Co. under the trade name C25, subsequently cooled to room temperature, thus obtaining a dispersion solution of deltamethrin solid nanoparticles; and

[0125] B. Preparation of Solid Nanodispersion

[0126] 50.0 parts by weight of didodecyl ether phosphate salt anionic surfactant and 49.999 parts by weight of sucrose aqueous solution were added into the dispersion solution of deltamethrin solid nanoparticles obtained in step A. The resulting mixture was stirred well at a rotation speed of 1100 rpm, and then freeze-dried under the condition of 5 pa to remove the solvent using an apparatus sold by EYELA Co. under the trade name FD-81, thus preparing the said deltamethrin solid nanodispersion.

[0127] The deltamethrin solid nanodispersion prepared in this example was dispersed in distilled water. It was measured using a laser granularity analyzer sold by Malvern Co. under the trade name Nano ZS90 and its average particle size was 85 nm. Its suspensibility was 99%, and wetting time was 42 s.

Example 10: Preparation of the Pesticide Solid Nanodispersion of the Present Invention

[0128] The procedures of the example are as follows:

[0129] A. Preparation of a Nanodispersion Solution

[0130] 29.0 parts by weight of buprofezin insecticide was heated to its melting point 105 C. and poured into dimethylformamide. Then buprofezin was uniformly dispersed in dimethylformamide by shearing for 14 min at shearing speed of 16000 rpm with a high-speed shear emulsifying machine sold by ATS Co. under the trade name C25, subsequently cooled to room temperature, thus obtaining a dispersion solution of buprofezin solid nanoparticles; and

[0131] B. Preparation of Solid Nanodispersion

[0132] An aqueous solution containing 10 parts by weight of octyl ether phosphate anionic surfactant, 10 parts by weight of octadecyl dihydroxyethyl amine oxide amphoteric surfactant and 51 parts by weight of lactose water-soluble carrier was added into the dispersion solution of buprofezin solid nanoparticles obtained in step A. The resulting mixture was stirred well at a rotation speed of 2200 rpm, and then freeze-dried under the condition of 5 Pa to remove the solvent using an apparatus sold by EYELA Co. under the trade name FD-81, thus preparing the said buprofezin solid nanodispersion.

[0133] The buprofezin solid nanodispersion prepared in this example was dispersed in distilled water. It was measured using a laser granularity analyzer sold by Malvern Co. under the trade name Nano ZS90 and its average particle size was 342 nm. Its suspensibility was 97.5%, and wetting time was 48 s.

Example 11: Preparation of the Pesticide Solid Nanodispersion of the Present Invention

[0134] The procedures of the example are as follows:

[0135] A. Preparation of a Nanodispersion Solution

[0136] 90.0 parts by weight of bitertanol fungicide was heated to about 5 C. above its melting point 125 C. and poured into dimethylformamide. Then bitertanol was uniformly dispersed in dimethylformamide by homogenizing for 18 min under the pressure of 800 bar with a high-pressure homogenizer sold by ATS Co. under the trade name AH-100D, subsequently cooled to room temperature, thus obtaining a dispersion solution of bitertanol solid nanoparticles; and

[0137] B. Preparation of Solid Nanodispersion

[0138] An aqueous solution containing 0.001 parts by weight of aliphatic alcohol polyoxyethylene phosphatidates anionic surfactant and 9.999 parts by weight of hydroxypropyl methylcellulose water-soluble carrier were added into the dispersion solution of bitertanol solid nanoparticles obtained in step A. The mixture was stirred well at a rotation speed of 2200 rpm, and then vacuum dried to remove the solvent at 40 C. using an apparatus sold by Jinghong Co. under the trade name XMTD-822, thus obtaining the said bitertanol solid nanodispersion.

[0139] The bitertanol solid nanodispersion prepared in this example was dispersed in distilled water. It was measured using a laser granularity analyzer sold by Malvern Co. under the trade name Nano ZS90 and its average particle size was 560 nm. Its suspensibility was 96.5%, and wetting time was 50 s.

Example 12: Preparation of the Pesticide Solid Nanodispersion of the Present Invention

[0140] The procedures of the example are as follows:

[0141] A. Preparation of a Nanodispersion Solution

[0142] 50.0 parts by weight of simeconazole fungicide was heated to about 5 C. above its melting point 118.5 C. and poured into ethylene glycol. Then simeconazole was uniformly dispersed in ethylene glycol by shearing for 14 min at shearing speed of 16000 rpm with a high-speed shear emulsifying machine sold by ATS Co. under the trade name C25, subsequently cooled to room temperature, thus obtaining a dispersion solution of simeconazole solid nanoparticles; and

[0143] B. Preparation of Solid Nanodispersion

[0144] An aqueous solution containing 45.0 parts by weight of polyvinylpyrrolidone nonionic surfactant and 5.0 parts by weight of hydroxyethyl cellulose water-soluble carrier were added into the dispersion solution of simeconazole solid nanoparticles obtained in step A. The mixture was stirred well at a rotation speed of 3500 rpm, and then freeze-dried under the condition of 5 Pa to remove the solvent using an apparatus sold by EYELA Co. under the trade name FD-81, thus preparing the said simeconazole solid nanodispersion.

[0145] The simeconazole solid nanodispersion prepared in this example was dispersed in distilled water. It was measured using a laser granularity analyzer sold by Malvern Co. under the trade name Nano ZS90 and its average particle size was 350 nm. Its suspensibility was 98%, and wetting time was 33 s.

Example 13: Preparation of the Pesticide Solid Nanodispersion of the Present Invention

[0146] The procedures of the example are as follows:

[0147] A. Preparation of a Nanodispersion Solution

[0148] 0.05 parts by weight of pyrazosulfuron-ethyl herbicide was heated to its melting point 178 C. and poured into ethylene glycol. Then pyrazosulfuron-ethyl was uniformly dispersed in ethylene glycol by homogenizing for 10 min under the pressure of 1200 bar with a high-pressure homogenizer sold by ATS Co. under the trade name AH-100D, subsequently cooled to room temperature, thus obtaining a dispersion solution of pyrazosulfuron-ethyl solid nanoparticles; and

[0149] B. Preparation of Solid Nanodispersion

[0150] An aqueous solution containing 0.05 parts by weight of Tween 80 nonionic surfactant, 49.9 parts by weight of sodium carboxymethyl cellulose and 50 parts by weight of the mixture of polyethylene glycol and xanthan gum (weight ratio of 1:2) were added into the dispersion solution of pyrazosulfuron-ethyl solid nanoparticles obtained in step A. The mixture was stirred well at a rotation speed of 3200 rpm, and then freeze-dried under the condition of 5 Pa to remove the solvent using an apparatus sold by EYELA Co. under the trade name FD-81, thus preparing the said solid nanodispersion of pyrazosulfuron-ethyl.

[0151] The solid nanodispersion of pyrazosulfuron-ethyl prepared in this example was dispersed in distilled water. It was measured using a laser granularity analyzer sold by Malvern Co. under the trade name Nano ZS90 and its average particle size was 482 nm. Its suspensibility was 98%, and wetting time was 35 s.

Example 14: Preparation of the Pesticide Solid Nanodispersion of the Present Invention

[0152] The procedures of the example are as follows:

[0153] A. Preparation of a Nanodispersion Solution

[0154] 17.0 parts by weight of daminozide plant growth regulator was heated to about 5 C. above its melting point 157 C. and poured into ethylene glycol. Then daminozide was uniformly dispersed in ethylene glycol by shearing for 15 min at shearing speed of 15000 rpm with a high-speed shear emulsifying machine sold by ATS Co. under the trade name C25, subsequently cooled to room temperature, thus obtaining a dispersion solution of daminozide solid nanoparticle; and

[0155] B. Preparation of Solid Nanodispersion

[0156] An aqueous solution containing 8.0 parts by weight of sorbitan oleate nonionic surfactant, 70 parts by weight of hydroxyethyl--cyclodextrin and 5 parts by weight of the mixture of polyethylene glycol and magnesium aluminum silicate (weight ratio of 3:1) were added into the dispersion solution of daminozide solid nanoparticles obtained in step A. The mixture was stirred well at a rotation speed of 1800 rpm, and then freeze-dried under the condition of 5 Pa to remove the solvent using an apparatus sold by EYELA Co. under the trade name FD-81, thus preparing the said daminozide solid nanodispersion.

[0157] The daminozide solid nanodispersion prepared in this example was dispersed in distilled water. It was measured using a laser granularity analyzer sold by Malvern Co. under the trade name Nano ZS90 and its average particle size was 490 nm. Its suspensibility was 98.5%, and wetting time was 40 s.

Example 15: Preparation of the Pesticide Solid Nanodispersion of the Present Invention

[0158] The procedures of the example are as follows:

[0159] 25 parts by weight of avermectin insecticide was dissolved in acetone. Subsequently, an aqueous solution of 25 parts by weight of aliphatic alcohol polyoxyethylene ether carboxylate anionic surfactant and 50 parts by weight of lactose water-soluble carrier was added into the resulting solution. The mixture thus obtained was mixed well and then sheared for 12 min at shearing speed of 18000 rpm with a high-speed shear emulsifying machine sold by ATS Co. under the trade name C25, then removed the solvent at 45 C. using a rotary evaporation equipment sold by EYELA Co. under the trade name N-2100, thus obtaining an avermectin solid nanodispersion.

[0160] The avermectin solid nanodispersion prepared in this example was dispersed in distilled water.

[0161] It was measured using a laser granularity analyzer sold by Malvern Co. under the trade name Nano ZS90 and its average particle size was 95 nm. Its suspensibility was 99%, and wetting time was 25 s.

Example 16: Preparation of the Pesticide Solid Nanodispersion of the Present Invention

[0162] The procedures of the example are as follows:

[0163] 45 parts by weight of emamectin benzoate insecticide was dissolved in ethyl acetate. Subsequently, an aqueous solution of 25 parts by weight of maleic rosin-polyoxypropylene-polyoxyethylene ether sulfonate, 15 parts by weight of sodium dodecylbenzenesulfonate anionic surfactants and 15 parts by weight of urea water-soluble carrier was added into the resulting solution. The mixture thus obtained was mixed well and then homogenized for 12 min under the pressure of 800 bar with a high-pressure homogenizer sold by ATS Co. under the trade name AH-100D, and then removed the solvent under the condition of inlet temperature of 45 C., outlet temperature of 95 C., spray pressure of 20 kPa and inlet velocity of 0.09 L/h using a spray drying equipment sold by EYELA Co. under the trade name SD-1000, thus obtaining the solid nanodispersion of emamectin benzoate.

[0164] The solid nanodispersion of emamectin benzoate prepared in this example was dispersed in distilled water. It was measured using a laser granularity analyzer sold by Malvern Co. under the trade name Nano ZS90 and its average particle size was 87 nm. Its suspensibility was 99%, and wetting time was 23 s.

Example 17: Preparation of the Pesticide Solid Nanodispersion of the Present Invention

[0165] The procedures of the example are as follows:

[0166] 90.0 parts by weight of prochloraz fungicide was dissolved in chloroform. Subsequently, an aqueous solution of 3.5 parts by weight of didodecyl ether phosphate salt, 1.5 parts by weight of sodium dodecylbenzenesulfonate anionic surfactant and 5.0 parts by weight of sucrose water-soluble carrier was added into the resulting solution. The mixture thus obtained was mixed well and then sheared for 18 min at a shearing speed of 10000 rpm with a high-speed shear emulsifying machine sold by ATS Co. under the trade name C25, then removed the solvent at 30 C. using a rotary evaporation equipment sold by EYELA Co. under the trade name N-2100, thus obtaining a prochloraz solid nanodispersion.

[0167] The prochloraz solid nanodispersion prepared in this example was dispersed in distilled water. It was measured using a laser granularity analyzer sold by Malvern Co. under the trade name Nano ZS90 and its average particle size was 550 nm. Its suspensibility was 97.5%, and wetting time was 42 s.

Example 18: Preparation of the Pesticide Solid Nanodispersion of the Present Invention

[0168] The procedures of the example are as follows:

[0169] 0.05 parts by weight of thifluzamide fungicide was dissolved in chloroform. Subsequently, 0.05 parts by weight of oleyl biuret amphoteric surfactant and 99.9 parts by weight of the mixture of urea and sodium sulphate (weight ratio of 3:1) were added into the resulting solution. The mixture thus obtained was mixed well at a rotation speed of 4200 rpm, and then removed the solvent at 30 C. using a rotary evaporation equipment sold by EYELA Co. under the trade name N-2100, thus obtaining a thifluzamide solid nanodispersion.

[0170] The thifluzamide solid nanodispersion prepared in this example was dispersed in distilled water. It was measured using a laser granularity analyzer sold by Malvern Co. under the trade name Nano ZS90 and its average particle size was 620 nm. Its suspensibility was 97%, and wetting time was 48 s.

Example 19: Preparation of the Pesticide Solid Nanodispersion of the Present Invention

[0171] The procedures of the example are as follows:

[0172] 65 parts by weight of diclofop-methyl herbicide was dissolved in acetone. Subsequently, 11.0 parts by weight of octadecyl dihydroxyethyl amine oxide amphoteric surfactant, 12.0 parts by weight of magnesium sulphate and 12.0 parts by weight of magnesium aluminum silicate were added into the resulting solution. The mixture thus obtained was mixed well at a rotation speed of 5000 rpm, and then freeze-dried to remove the solvent under the condition of 10 pa using an apparatus sold by EYELA Co. under the trade name FD-81, thus obtaining a diclofop-methyl solid nanodispersion.

[0173] The diclofop-methyl solid nanodispersion prepared in this example was dispersed in distilled water. It was measured using a laser granularity analyzer sold by Malvern Co. under the trade name Nano ZS90 and its average particle size was 190 nm. Its suspensibility was 98%, and wetting time was 38 s.

Example 20: Preparation of the Pesticide Solid Nanodispersion of the Present Invention

[0174] The procedures of the example are as follows:

[0175] 20 parts by weight of amidosulfuron herbicide was dissolved in methanol. Subsequently, 50 parts by weight of oleyl biuret amphoteric surfactant, 25 parts by weight of the mixture of urea and sodium sulphate (weight ratio of 3:1) and 5 parts by weight of aqueous solution of the mixture of polyethylene glycol and magnesium aluminum silicate (weight ratio 3:5) were added into the resulting solution. The mixture thus obtained was sheared for 8 min at a shearing speed of 10000 rpm using a high-speed shear emulsifying machine sold by ATS Co. under the trade name C25, and then freeze-dried to remove the solvent under the condition of 10 pa using an apparatus sold by EYELA Co. under the trade name FD-81, thus obtaining a amidosulfuron solid nanodispersion.

[0176] The amidosulfuron solid nanodispersion prepared in this example was dispersed in distilled water. It was measured using a laser granularity analyzer sold by Malvern Co. under the trade name Nano ZS90 and its average particle size was 220 nm. Its suspensibility was 98%, and wetting time was 33 s.

Example 21: Preparation of the Pesticide Solid Nanodispersion of the Present Invention

[0177] The procedures of the example are as follows:

[0178] 0.001 parts by weight of benzylaminopurine plant growth regulator was dissolved in methanol. Subsequently, an aqueous solution of 25 parts by weight of cremophorel nonionic surfactant, 25 parts by weight of lauryl betaine amphoteric surfactants, 30 parts by weight of the mixture of urea and sucrose (weight ratio 1:1) and 19.999 parts by weight of polyethylene glycol water-soluble carrier was added into the resulting solution. The mixture thus obtained was mixed well at a rotation speed of 4200 rpm, and then removed the solvent under the condition of inlet temperature of 120 C., outlet temperature of 95 C., spray pressure of 20 kPa and inlet velocity of 0.1 L/h using a spray drying equipment sold by EYELA Co. under the trade name SD-1000, thus obtaining the solid nanodispersion of benzylaminopurine.

[0179] The solid nanodispersion of benzylaminopurine prepared in this example was dispersed in distilled water. It was measured using a laser granularity analyzer sold by Malvern Co. under the trade name Nano ZS90 and its average particle size was 85 nm. Its suspensibility was 99%, and wetting time was 22 s.

Example 22: Preparation of the Pesticide Solid Nanodispersion of the Present Invention

[0180] The procedures of the example are as follows:

[0181] 42.0 parts by weight of pyripropanol plant growth regulator was dissolved in chloroform. Subsequently, an aqueous solution of 0.001 parts by weight of aliphatic alcohol polyoxyethylene ether carboxylate anionic surfactant, 57.999 parts by weight of sucrose water-soluble carrier was added into the resulting solution. The mixture thus obtained was sheared for 15 min at a shearing speed of 10000 rpm with a high-speed shear emulsifying machine sold by ATS Co. under the trade name C25, thus obtaining a pyripropanol solid nanodispersion.

[0182] The pyripropanol solid nanodispersion prepared in this example was dispersed in distilled water. It was measured using a laser granularity analyzer sold by Malvern Co. under the trade name Nano ZS90 and its average particle size was 250 nm. Its suspensibility was 98%, and wetting time was 32 s.

Example 23: Preparation of the Pesticide Solid Nanodispersion of the Present Invention

[0183] The procedures of the example are as follows:

[0184] A. Preparation of a Nanodispersion Solution

[0185] 10 parts by weight of lambda-cyhalothrin insecticide and 5 parts by weight of spinosad insecticide were heated to 90 C. and poured into water. Then lambda-cyhalothrin and spinosad were uniformly dispersed in water by shearing for 20 min at shearing speed of 10000 rpm with a high-speed shear emulsifying machine sold by ATS Co. under the trade name C25, subsequently cooled to room temperature, thus obtaining a dispersion solution containing the above insecticide solid nanoparticles; and

[0186] B. Preparation of Solid Nanodispersion

[0187] 15.0 parts by weight of dodecanesulfonic acid sodium, 15.0 parts by weight of polycarboxylate anionic surfactant and 45 parts by weight of urea were added into the dispersion solution obtained in step A. The mixture was stirred well at a rotation speed of 1000 rpm, and then freeze-dried under the condition of 5 pa to remove the water using an apparatus sold by EYELA Co. under the trade name FD-81, thus preparing the said lambda-cyhalothrinspinosad solid nanodispersion.

[0188] The lambda-cyhalothrinspinosad solid nanodispersion prepared in this example was dispersed in distilled water. It was measured using a laser granularity analyzer sold by Malvern Co. under the trade name Nano ZS90 and its average particle size was 175 nm. Its suspensibility was 99%, and wetting time was 35 s.

Example 24: Preparation of the Pesticide Solid Nanodispersion of the Present Invention

[0189] The procedures of the example are as follows:

[0190] A. Preparation of a Nanodispersion Solution

[0191] 30 parts by weight of spinosad insecticide and 30 parts by weight of trifluralin herbicide were heated to 90 C. and poured into water. Then spinosad and trifluralin were uniformly dispersed in water by homogenizing for 20 min under the pressure of 1200 bar with a high-pressure homogenizer sold by ATS Co. under the trade name AH-100D, subsequently cooled to room temperature, thus obtaining a dispersion solution of spinosad and trifluralin solid nanoparticles; and

[0192] B. Preparation of Solid Nanodispersion

[0193] 10.0 parts by weight of dodecanesulfonic acid sodium, 5.0 parts by weight of polycarboxylate anionic surfactant and 22 parts by weight of urea water-soluble carrier were added into the dispersion solution of solid nanoparticles obtained in step A. The mixture was stirred well at a rotation speed of 1200 rpm, then removed the water under the condition of inlet temperature of 120 C., outlet temperature of 95 C., spray pressure of 20 kPa and inlet velocity of 0.1 L/h using a spray drying equipment sold by EYELA Co. under the trade name SD-1000, thus obtaining the said spinosadtrifluralin solid nanodispersion.

[0194] The spinosadtrifluralin solid nanodispersion prepared in this example was dispersed in distilled water. It was measured using a laser granularity analyzer sold by Malvern Co. under the trade name Nano ZS90 and its average particle size was 320 nm. Its suspensibility was 98.7%, and wetting time was 43 s.

Example 25: Preparation of the Pesticide Solid Nanodispersion of the Present Invention

[0195] The procedures of the example are as follows:

[0196] A. Preparation of a nanodispersion solution

[0197] 6 parts by weight of propamocarb hydrochloride fungicide and 24 parts by weight of alachlor herbicide were heated to 65 C. and poured into water. The said propamocarb hydrochloride and alachlor were uniformly dispersed in water by homogenizing for 20 min under the pressure of 1000 bar with a high-pressure homogenizer sold by ATS Co. under the trade name AH-100D, subsequently cooled to room temperature, thus obtaining a dispersion solution containing the above fungicide and herbicide solid nanoparticles; and

[0198] B. Preparation of Solid Nanodispersion

[0199] 12.0 parts by weight of dodecanesulfonic acid sodium anionic surfactant, 8.0 parts by weight of cumenyl phenol polyoxyethylene ether formaldehyde condensate nonionic surfactant and 50 parts by weight of the mixture of urea and sodium sulphate (weight ratio of 1:1) were added into the dispersion solution of solid nanoparticles obtained in step A. The resulting mixture was stirred well at a rotation speed of 1000 rpm, and then freeze-dried under the condition of 5 pa with a freeze drying apparatus sold by EYELA Co. under the trade name FD-81, thus preparing the said solid nanodispersion of propamocarb hydrochloridealachlor.

[0200] The solid nanodispersion of propamocarb hydrochloridealachlor prepared in this example was dispersed in distilled water. It was measured using a laser granularity analyzer sold by Malvern Co. under the trade name Nano ZS90 and its average particle size was 255 nm. Its suspensibility was 98.2%, and wetting time was 29 s.

Example 26: Preparation of the Pesticide Solid Nanodispersion of the Present Invention

[0201] The procedures of the example are as follows:

[0202] A. Preparation of a Nanodispersion Solution

[0203] 27.0 parts by weight of deltamethrin insecticide and 20 parts by weight of simeconazole fungicide were heated to 120 C. and poured into octane. Then deltamethrin and simeconazole were uniformly dispersed in octane by shearing for 15 min at shearing speed of 15000 rpm with a high-speed shear emulsifying machine sold by ATS Co. under the trade name C25, subsequently cooled to room temperature, thus obtaining a dispersion solution containing the above insecticide and fungicide solid nanoparticles; and

[0204] B. Preparation of Solid Nanodispersion

[0205] 13.0 parts by weight of octadecyl dihydroxyethyl amine oxide amphoteric surfactant, 32 parts by weight of magnesium sulphate and 8 parts by weight of magnesium aluminum silicate water-soluble carriers were added into the dispersion solution of solid nanoparticles obtained in step A. The resulting mixture was stirred well at a rotation speed of 4000 rpm, and then distilled to remove the solvent under the condition of 150 C. with a distillation equipment sold by Kaifeng Hongxing Co. under the trade name S212, thus obtaining the said solid nanodispersion of deltamethrinsimeconazole.

[0206] The deltamethrinsimeconazole solid nanodispersion prepared in this example was dispersed in distilled water. It was measured using a laser granularity analyzer sold by Malvern Co. under the trade name Nano ZS90 and its average particle size was 172 nm. Its suspensibility was 98.5%, and wetting time was 34 s.

Example 27: Preparation of the Pesticide Solid Nanodispersion of the Present Invention

[0207] The procedures of the example are as follows:

[0208] 18 parts by weight of lambda-cyhalothrin insecticide and 18 parts by weight of avermectin insecticide were dissolved in acetone. Subsequently, an aqueous solution of 15 parts by weight of maleic rosin-polyoxypropylene-polyoxyethylene ether sulfonate anionic surfactant, 15 parts by weight of cumenyl phenol polyoxyethylene ether formaldehyde condensate nonionic surfactant and 34 parts by weight of sucrose water-soluble carrier was added into the resulting solution. The mixture thus obtained was sheared for 15 min at a shearing speed of 10000 rpm using a high-speed shear emulsifying machine sold by ATS Co. under the trade name C25, and then freeze-dried to remove the solvent under the condition of 5 pa using an apparatus sold by EYELA Co. under the trade name FD-81, thus obtaining a solid nanodispersion of lambda-cyhalothrinavermectin.

[0209] The solid nanodispersion of lambda-cyhalothrinavermectin prepared in this example was dispersed in distilled water. It was measured using a laser granularity analyzer sold by Malvern Co. under the trade name Nano ZS90 and its average particle size was 67 nm. Its suspensibility was 99.5%, and wetting time was 21 s.