CN105360115A - Method for preparing nanoscale pesticide preparation by means of silicon dioxide aerogel - Google Patents
Method for preparing nanoscale pesticide preparation by means of silicon dioxide aerogel Download PDFInfo
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- CN105360115A CN105360115A CN201510746368.7A CN201510746368A CN105360115A CN 105360115 A CN105360115 A CN 105360115A CN 201510746368 A CN201510746368 A CN 201510746368A CN 105360115 A CN105360115 A CN 105360115A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/12—Powders or granules
- A01N25/14—Powders or granules wettable
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
- A01N43/54—1,3-Diazines; Hydrogenated 1,3-diazines
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N53/00—Biocides, pest repellants or attractants, or plant growth regulators containing cyclopropane carboxylic acids or derivatives thereof
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- General Health & Medical Sciences (AREA)
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- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a method for preparing a nanoscale pesticide preparation by means of silicon dioxide aerogel, belongs to the technical field of pesticides, and particularly relates to the application of silicon dioxide aerogel serving as a novel carrier of a pesticide processing aid. According to the technical scheme, when the silicon dioxide aerogel is used for nanocrystallized preparation processing of a slightly soluble technical material as a carrier, the technical material is dissolved in a solvent or broken, the silicon dioxide aerogel is loaded with liquid containing the solvent through adsorption or mixed with the broken technical material so as to form a nanoparticle drug carrier system with the diameter smaller than 100 nm, water is added to the nanoparticle drug carrier system, stirring or emulsification is conducted for homogenous dispersion, the solvent and water are removed through drying, and then a nanoscale pesticide is obtained. The method has the advantages that environment friendliness is realized, and the gap in the carrier material for nanoscale pesticides at home and abroad is filled.
Description
Technical field
The invention belongs to technical field of pesticide, specifically refer to its application as the novel carriers in pesticide processing auxiliary agent of aerosil.
Background technology
Agricultural chemicals refers in agricultural production, and for ensureing, promoting the growth of plant and crops, a class medicine of the desinsection used, sterilization, kill harmful animal (or weeds) is referred to as.Refer in particular to agriculturally for anti-worm and the medicament such as coordinate plant growth, weeding of curing the disease.Agricultural chemicals, in guarantee agricultural output and quality, ensures that mankind's grain security aspect occupies critical role.Efficiently, low toxicity, low-residual, economy and excellent pesticide species easy to use should be the directions of Agrochemicals.
In real pesticide producing with in using, although be the production and selling having forbidden and limited organic phosphates high toxicity agricultural chemicals, but in the pesticide species of current main flow, still add and have the contour toxic organic solvent of the benzene of a large amount of organic solvents, particularly arene, toluene and dimethylbenzene.Along with socio-economic development and the raising of people's living standard and the enhancing of health perception, people more and more pay attention to quality and the quality problems of agricultural product, more and more pay attention to agricultural chemicals problem to healthy and even on life impact.
Pesticidal products research and development are development in Hi-Tech key areas, and pesticide research person have found in agricultural chemicals the crux of adding organic Solvent, the too low problem of dissolubility of Here it is pesticide original medicine, or perhaps agricultural compound is difficult to dissolve in water.This problem is ubiquity in current biological species agricultural chemicals, bionical class agricultural chemicals and the chemical pesticide used.Even the novel agrochemical in recent years gone on the market still does not address this problem.
Have tablet, capsule, injection etc. different from people by medicine common formulations, agricultural chemicals is normally dispersion medium with water, and common using method is that the water mixing different substances together tens times to thousands of times is in the formulation used farmland, vegetable plot, Orchard Spray.So the size of solvability in water is the key factor determining pesticide efficacy.But be poorly water soluble drugs mostly again at the former medicine of the important kind of agricultural chemicals extensively used now, having to add organic solvent in a large number increases its dissolubility, to reach raising drug effect, the object of prevention and elimination of disease and pests.Medicine as former in Avermectin solvability in water is about 10 μ g/L; The former medicine of ivermectin solvability in water is about 4mg/L; Emamectin-benzoate (emamectin benzoate) former medicine solvability in water is about 300mg/L; The former medicine of Fluoxastrobin solvability in water is about 6mg/L; The former medicine of gamma cyhalothrin is 0.004ppb (when 20 DEG C) in solvability water, according to the classification of medicine dissolving character, the definition of " almost insoluble or insoluble mean that solute 1g (ml) can not dissolve completely in solvent 10000ml ", the former medicine of these medicines all belongs to indissoluble and almost insoluble type.Unfortunately, the good solvent of the toxic organic solvent such as the benzene,toluene,xylene of arene these class pesticide original medicines just, medicine as former in Avermectin solvability in toluene, up to 350g/L, and is only 10 μ g/L in water.Avermectin preparation conventional on agricultural chemicals is abamectin ointment, is the accessory after Avermectin fine powder is refined, and be xylene soluble missible oil dress, content is between 3 ~ 7%.A kind of key component of efficient cyhalothrin emulsifiable concentrate is: gamma cyhalothrin 2.9%, methyl alcohol 20%, dimethylbenzene 40%.
For improving the drug effect of former medicine, alleviate the loss that damage by disease and insect causes agricultural product, add a large amount of organic solvent for increasing former medicine solvability, often being it is believed that and be difficult to avoid, is insoluble technical barrier.And the pesticidal preparations adding a large amount of organic solvent not only endangers physical and mental health, the destruction ecotope of people, be unfavorable for environmental protection, also cause the occupational injury of dispenser peasant.This present situation is badly in need of being solved by the progress of science and technology.
At present, the researcher of pharmaceutical preparation utilizes macromolecular material in existing pharmaceutic adjuvant as PEG (polyethylene glycol) more, and cellulose family and dextrin and liposome etc. carry out the research of drug-loading system technology.But there is more serious technological deficiency in this kind of material, is mainly manifested in the application: drugloading rate is low, and majority is no more than 10%, auxiliary material or auxiliary dosage large; Easy reunion, is difficult to obtain patent medicine product that is micro-, nanostructured; Poor stability, the change of more difficult adaptation temp. and humidity in pesticidal preparations.Leakage, sex change is also there will be during liposome medicine carrying; Only adapt to specific individual drugs, belong to specificity method, there is no universality; Auxiliary material is various, brings the more problem large with quality control difficulty of impurity.Trace it to its cause, key issue does not find suitable drug carrier material.As mostly existing traditional auxiliary material is full particle shape, there is not the space structure of the small scale holding medicine, mostly be by the surface of drug molecule load at fine solid construction, thus very high drugloading rate cannot be realized, the drug content often formed is low, the small scale mixture that auxiliary material amount is very large, is difficult to reach high drug load and the stay-in-grade basic demand of Large ratio surface sum.
Summary of the invention
For solving the above-mentioned problem mentioned, the invention provides pesticidal preparations prepared by a kind of aerosil and preparation method thereof, technology of the present invention is raised difficult questions as follows:
Apply the method that aerosil prepares pesticidal preparations, described application refers to that aerosil is carrying out nanorize preparation processing as carrier to the former medicine of slightly solubility, and procedure of processing is as follows:
1. with dissolution with solvents pesticide original medicine or pulverizing pesticide original medicine;
2. pastille solvent is loaded into containing solvent liquid or be mixed into pulverized former medicine to be less than 100nm nanoparticle drug-loading system with the diameter formed with aerosil absorption, described aerosil is that hydrophilic silicon oxides aeroge or hydrophobic silicon dioxide aerogel after heat treatment have hydrophilic aerosil, the mass ratio of pesticide original medicine and aerosil is 1:0.5 ~ 20, drug molecule bag is loaded in its Nanostructure Network by aerosil, the medicament nano solid dispersions that forming property is stable, the medicinal agent mixing different substances together many times of water formation when using presents transparent watery few precipitation, by the comparative observation with several commercial preparation amount of being watered on an equal basis, pesticidal preparations precipitation prepared by the inventive method is minimum, stabilization time is also the longest,
3. add water nanoparticle drug-loading system homogenous disperse; After this step completes, form a kind of liquid form product that can use.The product agricultural chemicals dilution for many times that directly adds water before administration both can.
4. dry except desolventizing and moisture, obtain Nano medication;
5. Nano medication is prepared various formulation.
Described agricultural chemicals is that one or more are selected from insecticide, bactericide, the weed killer herbicide of slightly solubility.
Insecticide is selected from pyrethroid, carbamate, organic phosphor, organic sulfur, organic choline, nereistoxin, anabasine, phenyl ureide, Avermectin, emamectin-benzoate, pyridaben, acequinocyl, Phenylpyrazole, indoxacarb or diafenthiuron insecticides;
Described bactericide is selected from anilino-pyridine, antibiotic, aromatic hydrocarbon, dinitroaniline, Fluoxastrobin, allylamine, benzsulfamide, benzimidazole, benzisothiazole, benzophenone, benzo yl pyrimidines, phentriazine, benzyq carbamate, carbamate, carboxylic acid amides, carboxylic acid diamides, chlorine nitrile, cyanoimidazole, cyclopropane carboxamide, ethylamino thiazole carboxylic acid amides, imidazoles, hydroxyl anilid, imidazolone, isobenzofuranone, methoxy acrylate, methoxycarbamate, morpholine, N-carbanilate, oxazolidinedione, phenyl-acetamides, phenyl amide, phenylpyrrole, phenylurea, thiophosphate, phthalamic acid, phthalimide, piperazine, piperidines, propionamide, pyridine, pyridylmethyl acid amides, toluamide, triazine or triazole bactericidal agent,
Described weed killer herbicide is selected from acid amides, aryloxyphenoxypropionate, benzene oxycarboxylic acid, organic phosphor, benzamide, benzofuran, benzoic acid, benzothiadiazine ketone, carbamate, chloroacetamide, picolinic acid, chlorine carboxylic acid, cyclohexanedione, dinitroaniline, diphenyl ether, isoxazole, isoxazole alkane ketone, N-phenylphthalimide, oxadiazole, oxazolidinedione, oxygen yl acetamide, carbanilate, phenyl pyridazine, sulfonylamino carboxyl Triazolinones, sulphonyl triazol carboxylic acid amides, triazolo pyrimidine, triketone, uracil or carbamide herbicides,
Inventor is found by research, aerosil is that one has tridimensional network novel nano-material, both there is the particle diameter yardstick being less than 100 nanometers of material science strict difinition, there is again the space structure being independently less than 100 nanometers, every mm of thickness reaches 10000 layers of nano-pore, space (air) volume that can be used for medicine carrying reaches more than 90%, can reach carrying drug ratio the highest in history.It has and improves drug bioavailability thus improve drug effect necessary huge specific surface area and stable nano aperture, nano-dispersed can be carried out by the mode such as " self assembly ", " being cross-linked " to multiclass medicine, with be loaded medicine and form the independence " Nanodispersion " that can not reunite, can realize " nanorize " of the multiclass medicine of " Nano medication " truly and universality, directly crack in Nano medication research and patent medicine, insoluble medicine can not be difficult to the galenic pharmacy difficult problems such as effectively absorption because reuniting.Drugloading rate is large, envelop rate is high, specific surface area is large and quality is the gentliest the essential characteristic of aerosil as pharmaceutical carrier.Aerosil is a kind of brand-new microstructure porous material, utilize " nanorize " that this material can realize former medicine from the physical layer of meso-scale as pharmaceutical carrier, and do not destroy the molecular structure of former medicine, because the molecular size of most medicinal compound is dust level yardstick.Carry out bag by aerosil to drug molecule from the principle to carry, carry out physical dispersion, can keep and give full play to its original biologically active.Embody the feature of small scale, high surface, high bioavilability, reach the drug effect that conventional formulation is difficult to realize.Because this principle is with universality meaning, so inventor thinks, multiclass pesticide original medicine can rely on this technology, convenient, fast, high-quality, low cost prepare Nano medication novel formulation, aerosil carries out nanorize process as medicine carrying material to the former medicine of most slightly solubility, is the technology with general character meaning.
Further, in step 4 described Nano medication is passed through 100 order to 200 mesh sieves, in nano pesticide final products, the proterties of solid nano preparation is stabilized in micron order dispersed optimum, this is because too thin particulate easily causes dust-like to fly upward, be unfavorable for Field information, adopt this patent preparation method, can be exactly well select by 200 the orders even particulate in 100 mesh sieve holes, because the medicament nano granule of these thicker particulate package-containeds, meet water can decompose rapidly, do not affect use, and in use greatly reduce dust.
Further, described heat treated temperature is 300 ~ 1000 DEG C.
Inventor is by studying discovery further, and aerosil is carrying out having unique technical advantage in nanorize preparation processing as carrier material to the former medicine of slightly solubility.The chemical inertness that aerosil has as inorganic material self and physics stability, embody the stability of high biologically inert that organic carrier material do not possess and temperature stability and finished product structure.The former medicine of insoluble drug water-soluble very low, but its high-temperature behavior is better, just may decompose when higher temperature, inactivation.The fusing point of medicine as former in Avermectin is: 150 ~ 155 DEG C; The fusing point of the former medicine of emamectin benzoate is 141 ~ 146 DEG C, has pointed out preparation processing to carry out at relatively high temperatures.After former drug solns adsorbed by aerosil, when carrying out dispersion treatment, expensive high pressure homogenizer need not be used, with normal agitation equipment, because aerosil has utilized the nanoscale medicine carrying space of self automatically to carry out highly accurate physical dispersion, isolation to contained former medicine.During processing solid nano dispersion, drying process is carried out to medicine, also there is no need to carry out low temperature drying or freeze drying.
During nano-pesticide formulation is produced, without the need to using expensive process equipment as high-end devices such as freeze drier, low-temperature drier, high pressure homogenizers, will benefit to manufacturing enterprise.The investment that high-end devices uses and operation maintenance and energy consumption, can bring increasing substantially of production cost and human cost.Because agricultural chemicals is large-scale production pattern, select normal agitation machine, dryer, grinding bolting mill just can reach product quality requirement.Can save investment in equipment and maintenance cost in a large number, energy consumption also can significantly reduce.
Further, the porosity of described aerosil is 95 ~ 99%, aperture is 10 ~ 50nm, specific surface area is 200 ~ 1000m
2/ g, density are 3 ~ 300kg/m
3, network consisting colloidal particle diameter be 1 ~ 50nm.
Further, described solvent is ethanol or ethyl acetate, because ethanol or ethyl acetate are low toxicity, therefore has more environment protection significance.
Further, described drying means has oven dry, freeze-drying and spray dry, and bake out temperature is 60 DEG C ~ 120 DEG C; Freeze temperature is-50 DEG C ~-70 DEG C, pressure 0.1 ~ 10pa; The dry temperature of spray is 120 DEG C ~ 220 DEG C, inventor studies discovery further, the former medicine of slightly solubility due to agricultural chemicals and aerosil both have good warm tolerance, the common drying plant of direct use, as a conventional oven just can obtain the block precursor of the dry body of nano-grade medicine, Ordinary pulverization screening machine can be used just can to obtain varigrained nano-grade medicine dispersion, reach Pesticidal products quality requirement and meet and use requirement.The Nano medication that processing technology finally obtains, specific surface area all can reach 300m
2/ g.If use spray dryer, then obtain microspheroidal nano-solid dispersion, specific surface area also can reach 300m
2/ g.
Further, described pesticidal preparations is nano level pesticide solid dispersions, suspension formulation and aqua, and micro mist shape and microspheroidal two class nano level pesticide solid dispersions do not have difference in stability, and manufactured goods are with bottled or packed, do not add desiccant, within more than 3 years, do not reunite.The preparation of two kinds of proterties does not have difference in using, this be due to carrier material adopt be hydrophilic silicon dioxide aeroge, be a kind of similar water miscible carrier, finished medicines is met water and is stirred a little and just can realize high uniformity and disperse, and using the liquid that front high power adds water is water sample transparence.But in the solid state, aerosil drug-loading system shows the physical stability of height, and described pesticide nano solid dispersions is pulvis, tablet, granule or microcapsule formulations.
Apply a Nano medication prepared by aerosil, described Nano medication drugloading rate > 50%; Envelop rate > 90%; Drug bearing microsphere specific surface area > 300m
2/ g; Drug bearing microsphere particle diameter < 5 μm, can the former medicine particulate of coated multiclass; Study on the stability, soilless sticking time > 3 years, the precedent of international and domestic all not this type of preparations.
Compared with prior art, the present invention has the following advantages:
1, the present invention is that pesticidal preparations neck searches out a kind of new nano carrier material, and this material is nano-particle material popular now or nanometer powder not, but really achieves nano level medicine carrying hole new construction.Achieve the physics medicine carrying yardstick of below 100 nanometers that can realize without any a kind of material in medicinal materials now, fill up the international and domestic blank not having nano level pesticide carrier material so far, as to the formulation innovation of multiclass agricultural chemicals, there is universality meaning.
What 2, utilize the present invention to prepare does not contain organic solvent, particularly not containing the agricultural chemicals novel formulation of benzene.To raising agricultural product quality, ensure food safety and preserve the ecological environment minimizing environmental pollution, has very important realistic meaning.
3, utilize the present invention to prepare nano-pesticide formulation, solve the former medicine of slightly solubility due to solvability too low, have to an organic solvent to disperse the technical barrier of former medicine.This patent only uses the low toxicity such as ethyl acetate, ethanol or nonpoisonous organic solvent as the dissolving medicine carrying to former medicine when preparing nano-pesticide formulation, in drying process subsequently, organic solvent is removed, and obtains not containing the commercially available medicine of organic solvent.Prior art is then add a large amount of organic solvent, particularly aromatic hydrocarbon solvent in preparation preparation.These solvents are sold with commercially available medicine and are used on crops.
Accompanying drawing explanation
Fig. 1 is the electron microscopic picture of silica aerogel material, as can be seen from the figure the nanometer scale space structure of aerosil;
Fig. 2 take aerosil as nano pesticide dispersion prepared by carrier, can find out that pesticide dispersions particle diameter prepared by the present invention is 25nm;
Fig. 3 take aerosil as the electron microscopic picture of drug bearing microsphere prepared by carrier, and can find out that drug bearing microsphere particle diameter prepared by the present invention is less than 2 μm, drug bearing microsphere bag carries a large amount of nano-grade medicine particulate.
Embodiment
Embodiment 1
Nanoscale Avermectin dries preparation technology
1 medicine dissolving and absorption medicine carrying
The former medicine of 1.1 precision weighing Avermectin 250 grams
1.2 precision weighing aerosils 250 grams
1.3 measure solvent ethyl acetate (analyzing pure) 500 milliliters, are dissolved to faint yellow clear liquid, then add absolute ethyl alcohol (analyzing pure) 1500 milliliters dilution.
1.4 add aeroge 250 grams is adsorbed completely to drug solution.
2 Nanodispersions or microballoon preparation
2.1 gained medicine carrying bodies are placed in beaker, add absolute ethyl alcohol 2000 milliliters.
2.2 high-speed emulsifying machine emulsifications, parameter: rotating speed 10000 revs/min, 5 minutes time.
Emulsion uses drying box dry by 2.3, parameter: temperature 100 DEG C, 12 hours time.
Semi-finished product were pulverized 200 mesh sieves by 2.4, obtained nano-avermectin powder.
Embodiment 2
Nanometer emamectin-benzoate (emamectin benzoate) dries preparation technology
1 medicine dissolving and absorption medicine carrying
1.1 precision weighing Methylaminoemamectin benzoates 250 grams
1.2 precision weighing aerosils 250 grams
1.3 take the anti-distintegrant of 7gD902 (Shenzhen Langtai Biotechnology Technology Co., Ltd.), measure solvent absolute ethyl alcohol (analyzing pure) 2000 milliliters, are made into the alcoholic solution that concentration is 0.35%.
1.4 add above-mentioned alcoholic solution dissolves Methylaminoemamectin benzoate to brown clear liquid.
1.4 add aeroge 250 grams is adsorbed completely to drug solution.
2 Nanodispersions or microballoon preparation
2.1 gained medicine carrying bodies are placed in beaker, add pure water 2000 milliliters, stir.
2.2 high-speed emulsifying machine emulsifications, parameter: rotating speed 30000 revs/min, 5 minutes time.
Emulsion uses drying box dry by 2.3, parameter: temperature 120 DEG C, 12 hours time.
Semi-finished product were pulverized 200 mesh sieves by 2.4, obtained nanometer emamectin-benzoate powder.
Embodiment 3
Nanometer ivermectin dries preparation technology
1 medicine dissolving and absorption medicine carrying
The former medicine of 1.1 precision weighing ivermectin 250 grams
1.2 precision weighing aerosils 250 grams
1.3 measure solvent absolute ethyl alcohol (analyzing pure) 2000 milliliters, are dissolved to faint yellow clear liquid.
1.4 add aeroge 250 grams is adsorbed completely to drug solution.
2 Nanodispersions or microballoon preparation
2.1 gained medicine carrying bodies are placed in beaker, add pure water 2000 milliliters, stir.
2.2 high-speed emulsifying machine emulsifications, parameter: rotating speed 28000 revs/min, 5 minutes time.
Emulsion uses drying box dry by 2.3, parameter: temperature 120 DEG C, 12 hours time.
Semi-finished product were pulverized 200 mesh sieves by 2.4, obtained nanometer ivermectin powder.
Embodiment 4
Nanoscale Fluoxastrobin dries preparation technology
1 medicine dissolving and absorption medicine carrying
The former medicine of 1.1 precision weighing Fluoxastrobin 250 grams
1.2 precision weighing aerosils 250 grams
1.3 measure solvent ethyl acetate (analyzing pure) 500 milliliters, are dissolved to milky white liquid, then add absolute ethyl alcohol (analyzing pure) 1500 milliliters dilution.
1.4 add aeroge 250 grams is adsorbed completely to drug solution.
2 Nanodispersions or microballoon preparation
2.1 gained medicine carrying bodies are placed in beaker, add absolute ethyl alcohol 2000 milliliters.
2.2 high-speed emulsifying machine emulsifications, parameter: rotating speed 28000 revs/min, 5 minutes time.
Emulsion uses drying box dry by 2.3, parameter: temperature 80 DEG C, 12 hours time.
Semi-finished product were pulverized 200 mesh sieves by 2.4, obtained nanometer Fluoxastrobin powder.
Embodiment 5
Nanometer emamectin-benzoate dries preparation technology
1 medicine dissolving and absorption medicine carrying
1.1 precision weighing Methylaminoemamectin benzoates 25 grams
1.2 precision weighing aerosils 250 grams
1.3 take the anti-distintegrant of 7gD902 (Shenzhen Langtai Biotechnology Technology Co., Ltd.), measure solvent absolute ethyl alcohol (analyzing pure) 2000 milliliters, are made into the alcoholic solution that concentration is 0.35%.
1.4 add above-mentioned alcoholic solution dissolves Methylaminoemamectin benzoate to brown clear liquid.
1.4 add aeroge 250 grams is adsorbed completely to drug solution.
2 Nanodispersions or microballoon preparation
2.1 gained medicine carrying bodies are placed in beaker, add pure water 2000 milliliters, stir.
2.2 high-speed emulsifying machine emulsifications, parameter: rotating speed 25000 revs/min, 2 minutes time.
Emulsion uses drying box dry by 2.3, parameter: temperature 120 DEG C, 12 hours time.
Semi-finished product were pulverized 200 mesh sieves by 2.4, obtained nanometer emamectin-benzoate powder.
Embodiment 5
Efficient nano cyfloxylate dries preparation technology
1 medicine dissolving and absorption medicine carrying
The former medicine of 1.1 precision weighing betacyfluthrin 250 grams
1.2 precision weighing aerosils 250 grams
1.3 measure solvent ethyl acetate (analyzing pure) 500 milliliters, are dissolved to milky white liquid, then add absolute ethyl alcohol (analyzing pure) 1500 milliliters dilution.
1.4 add aeroge 250 grams is adsorbed completely to drug solution.
2 Nanodispersions or microballoon preparation
2.1 gained medicine carrying bodies are placed in beaker, add pure water 2000 milliliters.
2.2 high-speed emulsifying machine emulsifications, parameter: rotating speed 28000 revs/min, 10 minutes time.
Emulsion uses drying box dry by 2.3, parameter: temperature 100 DEG C, 12 hours time.
Semi-finished product were pulverized 150 mesh sieves by 2.4, obtained efficient nano cyfloxylate powder.
Embodiment 6
Nano-avermectin freeze-drying preparation technology
1 medicine dissolving and absorption medicine carrying
The former medicine of 1.1 precision weighing Avermectin 50 grams
1.2 precision weighing aerosils 250 grams
1.3 measure solvent ethyl acetate (analyzing pure) 500 milliliters, are dissolved to faint yellow clear liquid, then add absolute ethyl alcohol (analyzing pure) 1500 milliliters dilution.
1.4 add aeroge 250 grams is adsorbed completely to drug solution.
2 Nanodispersions or microballoon preparation
2.1 gained medicine carrying bodies are placed in beaker, add pure water 2000 milliliters.
2.2 high-speed emulsifying machine emulsifications, parameter: rotating speed 28000 turns points, 5 minutes time.
2.3 high pressure homogenizer homogeneous, parameter: pressure 800bar, 10 minutes time.
2.4 by homogenizing fluid freeze drying, parameter: temperature-70 DEG C, pressure: 5pa, 24 hours time.
Semi-finished product were pulverized 200 mesh sieves by 2.5, obtained nano-avermectin powder.
Embodiment 7
Nanometer emamectin-benzoate freeze-drying preparation technology
1 medicine dissolving and absorption medicine carrying
1.1 precision weighing Methylaminoemamectin benzoates 250 grams
1.2 precision weighing aerosils 250 grams
1.3 take the anti-distintegrant of 7gD902 (Shenzhen Langtai Biotechnology Technology Co., Ltd.), measure solvent absolute ethyl alcohol (analyzing pure) 2000 milliliters, are made into the alcoholic solution that concentration is 0.35%.
1.4 add above-mentioned alcoholic solution dissolves Methylaminoemamectin benzoate to brown clear liquid.
1.4 add aeroge 250 grams is adsorbed completely to drug solution.
2 Nanodispersions or microballoon preparation
2.1 gained medicine carrying bodies are placed in beaker, add pure water 2000 milliliters, stir.
2.2 high-speed emulsifying machine emulsifications, parameter: rotating speed 28000 revs/min, 5 minutes time.
2.3 high pressure homogenizer homogeneous, parameter: pressure 800bar, 10 minutes time.
2.4 by homogenizing fluid freeze drying, parameter: temperature-70 DEG C, pressure: 5pa, 24 hours time.
Semi-finished product were pulverized 200 mesh sieves by 2.5, obtained nanometer emamectin-benzoate powder.
Embodiment 8
Nanometer ivermectin freeze-drying preparation technology
1 medicine dissolving and absorption medicine carrying
The former medicine of 1.1 precision weighing ivermectin 250 grams
1.2 precision weighing aerosils 250 grams
1.3 measure solvent absolute ethyl alcohol (analyzing pure) 2000 milliliters, are dissolved to faint yellow clear liquid.
1.4 add aeroge 250 grams is adsorbed completely to drug solution.
2 Nanodispersions or microballoon preparation
2.1 gained medicine carrying bodies are placed in beaker, add pure water 2000 milliliters, stir.
2.2 high-speed emulsifying machine emulsifications, parameter: rotating speed 28000 revs/min, 5 minutes time.
2.3 high pressure homogenizer homogeneous, parameter: pressure 800bar, 8 minutes time.
2.4 by homogenizing fluid freeze drying, parameter: temperature-50 DEG C, pressure: 5pa, 24 hours time.
Semi-finished product were pulverized 200 mesh sieves by 2.5, obtained nanometer ivermectin powder.
Embodiment 9
Efficient nano cyfloxylate freeze-drying preparation technology
1 medicine dissolving and absorption medicine carrying
The former medicine of 1.1 precision weighing betacyfluthrin 250 grams
1.2 precision weighing aerosils 250 grams
1.3 measure solvent ethyl acetate (analyzing pure) 500 milliliters, are dissolved to milky white liquid, then add absolute ethyl alcohol (analyzing pure) 1500 milliliters dilution.
1.4 add aeroge 250 grams is adsorbed completely to drug solution.
2 Nanodispersions or microballoon preparation
2.1 gained medicine carrying bodies are placed in beaker, add pure water 2000 milliliters.
2.2 high-speed emulsifying machine emulsifications, parameter: rotating speed 28000 revs/min, 5 minutes time.
2.3 high pressure homogenizer homogeneous, parameter: pressure 800bar, 10 minutes time.
2.4 by homogenizing fluid freeze drying, parameter: temperature-70 DEG C, pressure: 5pa, 24 hours time.
Semi-finished product were pulverized 200 mesh sieves by 2.5, obtained efficient nano cyfloxylate powder.
Embodiment 10
Nanometer Fluoxastrobin freeze-drying preparation technology
1 medicine dissolving and absorption medicine carrying
The former medicine of 1.1 precision weighing Fluoxastrobin 250 grams
1.2 precision weighing aerosils 250 grams
1.3 measure solvent ethyl acetate (analyzing pure) 500 milliliters, are dissolved to milky white liquid, then add absolute ethyl alcohol (analyzing pure) 1500 milliliters dilution.
1.4 add aeroge 250 grams is adsorbed completely to drug solution.
2 Nanodispersions or microballoon preparation
Above-mentioned dried product is placed in beaker by 2.1, adds pure water 2000 milliliters.
2.2 high-speed emulsifying machine emulsifications, parameter: rotating speed 28000 revs/min, 5 minutes time.
2.3 high pressure homogenizer homogeneous, parameter: pressure 1000bar, 10 minutes time.
2.4 by homogenizing fluid freeze drying, parameter: temperature-70 DEG C, pressure: 5pa, 24 hours time.
Semi-finished product were pulverized 200 mesh sieves by 2.5, obtained nanometer Fluoxastrobin powder.
Embodiment 11
The dry preparation technology of nano-avermectin spray
1 medicine dissolving and absorption medicine carrying
The former medicine of 1.1 precision weighing Avermectin 250 grams
1.2 precision weighing aerosils 250 grams
1.3 measure solvent ethyl acetate (analyzing pure) 500 milliliters, are dissolved to faint yellow clear liquid, then add absolute ethyl alcohol (analyzing pure) 1500 milliliters dilution.
1.4 add aeroge 250 grams is adsorbed completely to drug solution.
2 Nanodispersions or microballoon preparation
2.1 gained medicine carrying bodies are placed in beaker, add pure water 2000 milliliters.
2.2 high-speed emulsifying machine emulsifications, parameter: rotating speed 28000 turns points, 5 minutes time.
2.3 high pressure homogenizer homogeneous, parameter: pressure 800bar, 10 minutes time.
2.4 by homogenizing fluid spraying dry, parameter: temperature 120 DEG C, flow velocity 500 mls/hour, shower nozzle 0.75mm.
Namely 2.5 spray dry products obtain nano-avermectin powder.
Embodiment 12
The dry preparation technology of nanometer emamectin-benzoate spray
1 medicine dissolving and absorption medicine carrying
1.1 precision weighing Methylaminoemamectin benzoates 250 grams
1.2 precision weighing aerosils 250 grams
1.3 take the anti-distintegrant of 7gD902 (Shenzhen Langtai Biotechnology Technology Co., Ltd.), measure solvent absolute ethyl alcohol (analyzing pure) 2000 milliliters, are made into the alcoholic solution that concentration is 0.35%.
1.4 add above-mentioned alcoholic solution dissolves Methylaminoemamectin benzoate to brown clear liquid.
1.4 add aeroge 250 grams is adsorbed completely to drug solution.
2 Nanodispersions or microballoon preparation
2.1 gained medicine carrying bodies are placed in beaker, add pure water 2000 milliliters, stir.
2.2 high-speed emulsifying machine emulsifications, parameter: rotating speed 28000 revs/min, 5 minutes time.
2.3 high pressure homogenizer homogeneous, parameter: pressure 500bar, 10 minutes time.
2.4 by homogenizing fluid spraying dry, parameter: temperature 120 DEG C, flow velocity 500 mls/hour, shower nozzle 0.75mm.
Namely 2.5 spray dry products obtain nanometer emamectin-benzoate powder.
Embodiment 13
The dry technique of nanometer ivermectin preparation spray
1 medicine dissolving and absorption medicine carrying
The former medicine of 1.1 precision weighing ivermectin 250 grams
1.2 precision weighing aerosils 250 grams
1.3 measure solvent absolute ethyl alcohol (analyzing pure) 2000 milliliters, are dissolved to faint yellow clear liquid.
1.4 add aeroge 250 grams is adsorbed completely to drug solution.
2 Nanodispersions or microballoon preparation
2.1 gained medicine carrying bodies are placed in beaker, add pure water 2000 milliliters, stir.
2.2 high-speed emulsifying machine emulsifications, parameter: rotating speed 28000 revs/min, 5 minutes time.
2.3 high pressure homogenizer homogeneous, parameter: pressure 800bar, 10 minutes time.
2.4 by homogenizing fluid spraying dry, parameter: temperature 120 DEG C, flow velocity 500 mls/hour, shower nozzle 0.75mm.
Namely 2.5 spray dry products obtain nanometer ivermectin powder.
Embodiment 14
The dry preparation technology of nanometer Fluoxastrobin spray
1 medicine dissolving and absorption medicine carrying
The former medicine of 1.1 precision weighing Fluoxastrobin 250 grams
1.2 precision weighing aerosils 250 grams
1.3 measure solvent ethyl acetate (analyzing pure) 500 milliliters, are dissolved to milky white liquid, then add absolute ethyl alcohol (analyzing pure) 1500 milliliters dilution.
1.4 add aeroge 250 grams is adsorbed completely to drug solution.
2 Nanodispersions or microballoon preparation
Above-mentioned dried product is placed in beaker by 2.1, adds pure water 2000 milliliters.
2.2 high-speed emulsifying machine emulsifications, parameter: rotating speed 28000 revs/min, 5 minutes time.
2.3 high pressure homogenizer homogeneous, parameter: pressure 800bar, 10 minutes time.
2.4 by homogenizing fluid spraying dry, parameter: temperature 120 DEG C, flow velocity 500 mls/hour, shower nozzle 0.75mm.
Namely 2.5 spray dry products obtain nanometer Fluoxastrobin powder.
Embodiment 15
The dry preparation technology of efficient nano cyfloxylate spray
1 medicine dissolving and absorption medicine carrying
The former medicine of 1.1 precision weighing betacyfluthrin 250 grams
1.2 precision weighing aerosils 250 grams
1.3 measure solvent ethyl acetate (analyzing pure) 500 milliliters, are dissolved to milky white liquid, then add absolute ethyl alcohol (analyzing pure) 1500 milliliters dilution.
1.4 add aeroge 250 grams is adsorbed completely to drug solution.
2 Nanodispersions or microballoon preparation
2.1 gained medicine carrying bodies are placed in beaker, add pure water 2000 milliliters.
2.2 high-speed emulsifying machine emulsifications, parameter: rotating speed 28000 revs/min, 5 minutes time.
2.3 high pressure homogenizer homogeneous, parameter: pressure 800bar, 10 minutes time.
2.4 by homogenizing fluid spraying dry, parameter: temperature 120 DEG C, flow velocity 500 mls/hour, shower nozzle 0.75mm.
Namely 2.5 spray dry products obtain efficient nano cyfloxylate powder.
The nano level pesticide utilizing the present invention to prepare, in field efficacy experiment, has obtained satisfied effect, and formulation used is not containing the water dispersible granules of organic solvent, and the stoving process in the embodiment provided by this patent obtains; Using method is all be watered rear spraying.
In field control effectiveness test, the nano level pesticide of this patent and Vegetable Sold insecticide doubly interior prestige (10% bromine cyanogen insect amide dispersibles oil-suspending agent) have carried out comparison, the multispectral type insecticide of a new generation that Bei Neiweishi du pont company releases in May, 2015 in China's listing.
Field control effectiveness test is independently carried out by Gan County, Jiangxi Province plant protection unit, and three groups of data are as follows:
Field control effectiveness test 1
Field control effectiveness test 2
Field control effectiveness test 3
Claims (10)
1. apply the method that aerosil prepares nano level pesticide preparation, described application refers to that aerosil is carrying out nanorize preparation processing as carrier to the former medicine of slightly solubility, and procedure of processing is as follows:
1. with dissolution with solvents pesticide original medicine or pulverizing pesticide original medicine;
2. be loaded into pastille solvent liquid with aerosil absorption or be mixed into pulverized former medicine and be less than the nanoparticle drug-loading system of 100nm with the diameter formed, described aerosil is that hydrophilic silicon oxides aeroge or hydrophobic silicon dioxide aerogel after heat treatment have hydrophilic aerosil, the mass ratio of former medicine and aerosil is 1:0.5 ~ 20, and described heat treated temperature is 300 ~ 1000 DEG C;
3. added water by nanoparticle drug-loading system, stirring or emulsification make it homogenous disperse;
4. dry except desolventizing and moisture, obtain Nano medication.
2. method according to claim 1, is characterized in that, in step, 3 adopt mulser emulsification, and rotating speed is rotating speed 10000 ~ 30000 revs/min, 2 ~ 10 minutes time.
3. method according to claim 1, is characterized in that, in step, 3 adopt homogenizer homogeneous, pressure 500bar ~ 1500bar, 5 ~ 15 minutes time.
4. method according to claim 1, is characterized in that, in steps of 5 described Nano medication is passed through 100 order to 200 mesh sieves.
5. method according to claim 1, is characterized in that, the porosity of described aerosil is 95 ~ 99%, aperture is 10 ~ 50nm, specific surface area is 200 ~ 1000m
2/ g, density are 3 ~ 300kg/m
3, network consisting colloidal particle diameter be 1 ~ 50nm.
6. method according to claim 1, is characterized in that, described solvent is ethanol or ethyl acetate.
7. method according to claim 1, is characterized in that, described drying means has oven dry, freeze-drying and spray dry, and bake out temperature is 60 DEG C ~ 120 DEG C; Freeze temperature is-50 DEG C ~-70 DEG C, pressure 0.1 ~ 10pa; The dry temperature of spray is 120 DEG C ~ 220 DEG C.
8. method according to claim 1, is characterized in that, described Nano medication prepares various formulation, and described formulation includes nano level pesticide solid dispersions, suspension formulation and aqua.
9. the Nano medication applied aerosil and prepare.
10. Nano medication as claimed in claim 9, is characterized in that, described Nano medication drugloading rate > 50%; Envelop rate > 90%; Drug bearing microsphere specific surface area > 300m
2/ g; Drug bearing microsphere particle diameter < 5 μm.
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| CN109010250A (en) * | 2017-06-12 | 2018-12-18 | 天津城建大学 | Galapectite-silicon dioxide composite aerogel material and preparation method thereof |
| CN111096317A (en) * | 2019-12-31 | 2020-05-05 | 江西宏柏新材料股份有限公司 | Preparation method of drug-loaded silicon dioxide aerogel powder |
| CN111149797A (en) * | 2020-01-07 | 2020-05-15 | 仲恺农业工程学院 | Preparation method of pesticide aqueous solution |
| CN111631213A (en) * | 2020-06-22 | 2020-09-08 | 中国农业科学院植物保护研究所 | Drug-loaded gel and preparation method thereof |
| CN111991349A (en) * | 2020-09-02 | 2020-11-27 | 江西省科达动物药业有限公司 | Ivermectin sustained-release microsphere injection |
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| CN112007014A (en) * | 2020-09-02 | 2020-12-01 | 江西省科达动物药业有限公司 | Polylactic acid-coated silicon dioxide aerogel-doramectin microcapsule particle |
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| CN109006850A (en) * | 2017-06-10 | 2018-12-18 | 广东中迅农科股份有限公司 | A kind of pyraclostrobin nanometer formulation and preparation method thereof |
| CN109010250A (en) * | 2017-06-12 | 2018-12-18 | 天津城建大学 | Galapectite-silicon dioxide composite aerogel material and preparation method thereof |
| CN111096317A (en) * | 2019-12-31 | 2020-05-05 | 江西宏柏新材料股份有限公司 | Preparation method of drug-loaded silicon dioxide aerogel powder |
| CN111096317B (en) * | 2019-12-31 | 2021-07-02 | 江西宏柏新材料股份有限公司 | Preparation method of drug-loaded silicon dioxide aerogel powder |
| CN111149797A (en) * | 2020-01-07 | 2020-05-15 | 仲恺农业工程学院 | Preparation method of pesticide aqueous solution |
| CN111631213B (en) * | 2020-06-22 | 2021-04-06 | 中国农业科学院植物保护研究所 | Drug-loaded gel and preparation method thereof |
| CN111631213A (en) * | 2020-06-22 | 2020-09-08 | 中国农业科学院植物保护研究所 | Drug-loaded gel and preparation method thereof |
| CN111991357A (en) * | 2020-09-01 | 2020-11-27 | 江西省科达动物药业有限公司 | Silicon dioxide aerogel loaded ivermectin drug-loaded particle |
| CN111991348A (en) * | 2020-09-01 | 2020-11-27 | 江西省科达动物药业有限公司 | Doramectin sustained-release microcapsule injection |
| CN111991357B (en) * | 2020-09-01 | 2023-02-21 | 江西省科达动物药业有限公司 | Silicon dioxide aerogel loaded ivermectin drug-loaded particle |
| CN112007014A (en) * | 2020-09-02 | 2020-12-01 | 江西省科达动物药业有限公司 | Polylactic acid-coated silicon dioxide aerogel-doramectin microcapsule particle |
| CN111991349A (en) * | 2020-09-02 | 2020-11-27 | 江西省科达动物药业有限公司 | Ivermectin sustained-release microsphere injection |
| CN111991349B (en) * | 2020-09-02 | 2022-11-15 | 江西省科达动物药业有限公司 | Ivermectin sustained-release microsphere injection |
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Application publication date: 20160302 |