CN101999348B - Preparation method of pesticide effervescent tablet - Google Patents
Preparation method of pesticide effervescent tablet Download PDFInfo
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- CN101999348B CN101999348B CN 201010519030 CN201010519030A CN101999348B CN 101999348 B CN101999348 B CN 101999348B CN 201010519030 CN201010519030 CN 201010519030 CN 201010519030 A CN201010519030 A CN 201010519030A CN 101999348 B CN101999348 B CN 101999348B
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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
- A01N25/34—Shaped forms, e.g. sheets, not provided for in any other sub-group of this main group
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Abstract
The invention relates to a preparation method of a pesticide effervescent tablet, comprising the following steps of: (1) with one or the combination of more of bentonite, diatomite, white carbon black, maize starch, white clay, kaolin, superfine silica gel powder and aluminum-magnesium silicate as a carrier, mixing the mixture with pesticide raw materials, freezing at -10DEG C and crushing to obtain the nano carrier pesticide; (2) premixing the nano carrier pesticide with the dried acid source substances, a carbon dioxide source, a caking agent, a wetting dispersant, a disintegrating agent and a lubricating agent, roughly crushing and mixing, crushing by a jet pulverizer and then adding the crushed materials in a conical mixer blender and mixing to allow the materials to completely pass through a standard sieve with over 300 meshes to obtain dry powder; and (3) pressing the dry powder into a tablet with the preset size by using a tablet compression machine in the environment that the temperature is 15-25DEG C and the humidity is below 40 percent, i.e. obtaining the pesticide effervescent tablet. The method is simple, low in cost and environmentally-friendly; and the pesticide effect and the utilization rate of the pesticide of the pesticide effervescent tablet are superior to those of the conventional aqueous emulsion.
Description
Technical field
The invention belongs to the pesticide processing field, particularly a kind of preparation method of effervescent table as agricultural chemical.
Background technology
At present, the formulations of pesticide commonly used have missible oil, suspending agent, wetting powder, pulvis, granula, aqua, poison bait, mother liquor, female powder etc.Most of pesticide species are sold in market mainly with these several dosage form.In these formulations of pesticide, emulsifiable concentrates for agricultural chemicals contains organic solvent, and inflammable, not environmental protection must be strict with fire prevention, leakage-preventing in producing and transporting.Remaining more after suspending agent uses in packing container, container is processed relatively difficulty, and easily layering in storage process, caking, easily corrupt rotten.It is large that wetting powder and water dispersible granules take volume, easily lumps in storage, makes troubles to use.
The open CN1283388A of Chinese patent discloses a kind of effervescent table as agricultural chemical and method for making thereof, and wherein, effervescent table as agricultural chemical is comprised of pesticide original medicine, acid source, carbon dioxide source, waterproofing agent and insecticides adjuvant; The preparation method of effervescent table as agricultural chemical is: at first that acid source material, carbon dioxide source material, waterproofing agent is dry respectively, pulverized 60 mesh sieves, and mix, with isopropyl alcohol or butanols or isobutanol with mixture furnishing pasty state, under vacuum, remove the alcohol of adding, cross 20 mesh sieves, obtain soft material; Then soft material and pesticide original medicine, insecticides adjuvant are mixed and obtain the disintegration shot-like particle, in tablet press machine, the tablet that the disintegration shot-like particle is pressed into suitable size is effervescent table as agricultural chemical at last.Need to adopt organic solvent in the preparation process of this effervescent table as agricultural chemical, preparation process is loaded down with trivial details, and after the effervescent table as agricultural chemical disintegration, the suspensibility of agricultural chemicals in water is not high, affect the availability of agricultural chemicals, in addition, pesticide granules is larger, ductility on the crops surface is bad, affects the performance of pesticide efficacy.
Summary of the invention
Technical problem to be solved by this invention is to overcome the deficiencies in the prior art, and a kind of preparation method of improved effervescent table as agricultural chemical is provided.
For solving above technical problem, the present invention adopts following technical scheme:
A kind of preparation method of effervescent table as agricultural chemical, it comprises the steps:
(1), is combined as carrier with in bentonite, diatomite, White Carbon black, corn starch, carclazyte, kaolin, superfine silica gel powder and the aluminium-magnesium silicate one or more, it is mixed with pesticide original medicine, obtain the nano-carrier agricultural chemicals that size is 100～1000 nanometers in freezing pulverizing below-10 ℃, the weight ratio of carrier and pesticide original medicine is 0.03～10: 1;
(2), with acid source material, carbon dioxide source, binding agent, wetting dispersing agent, disintegrant and the lubricant premixed of step (1) gained nano-carrier agricultural chemicals with drying, through coarse crushing, mix again, join in the cone-type mixer after airslide disintegrating mill is pulverized and mix, make material 100% get dry powder by the standard screen more than 300 orders;
(3), 15 ℃～25 ℃ of temperature, humidity in the environment below 40%, utilize tablet press machine that step (2) gained dry powder is pressed into the tablet of setting size and be described effervescent table as agricultural chemical.
According to a concrete aspect of the present invention, in the step (2), the percentage by weight that feeds intake of each material is: nano-carrier agricultural chemicals 5%～60%, acid source 15%～40%, carbon dioxide source 15%～40%, wetting dispersing agent 3%～30%, binding agent 0～10%, disintegrant 0～10%, lubricant 0～10%.
According to the present invention, described acid source, carbon dioxide source, wetting dispersing agent, binding agent, disintegrant, lubricant etc. are makes the used conventional substances of effervescent tablet.For example, acid source can be citric acid, tartaric acid, fumaric acid, adipic acid, succinic acid, citric acid and malic acid etc.; Carbon dioxide source can be sodium carbonate, sodium bicarbonate, potash, saleratus and calcium carbonate etc.; Wetting dispersing agent can be sodium lignin sulfonate, the malonic anhydride polyethers, modification dimethyl siloxane polyethers, sucrose fatty ester, dodecyl sodium sulfate, the trisiloxanes polyethers, sodium phosphate trimer, polycarboxylic acids sodium, the dodecylphenyl polyoxyethylene ether, Negel, sulfonic acid polyformaldehyde condensation product, sldium lauryl sulfate, alkylphenol-polyethenoxy base ether formaldehyde condensation products sodium sulphate, the alkylaryl polyoxyethylene ether, aliphatic alcohol polyethenoxy base ether, sodium pyrophosphate and potassium pyrophosphate etc.; Binding agent can be sodium carboxymethylcellulose, starch, hydroxypropyl cellulose, sucrose etc.; Disintegrant can be sodium carboxymethyl starch, low-substituted hydroxypropyl cellulose, Ac-Di-Sol, PVPP, shitosan, sodium alginate, ammonium sulfate etc.; Lubricant can be dolomol, talcum powder, sldium lauryl sulfate, wheat starch and polyethylene glycol etc.
Term among the present invention " agricultural chemicals " comprises desinsection, kills mite, sterilization, weeding, plant biotechnology regulator etc.Pesticide original medicine can be solid, also can be liquid.When being liquid, the corresponding increase of the amount of carrier.Representational pesticide original medicine has for example Tebuconazole and Difenoconazole.
The temperature of freezing pulverizing is preferably between-15 ℃～-25 ℃ in the step (1), for example-20 ℃.
Because adopt above technical scheme, the present invention compared with prior art has following advantage:
The present invention passes through at first carrier and former medicine mixed freezing crushing technology, can make medicine under thinner particle diameter, be difficult for regrouping, the fineness of dispersion of nano level carrier medicament in water is minimum, greatly improved its suspensibility in water, and its ductility on the crops surface is better, can strengthen agricultural chemicals to the permeability of pathogenic bacteria and plant cell, and absorption ratio is high, improved the availability of control efficiency and agricultural chemicals, effective drug duration is also more permanent than other regular dosage form.In addition, preparation method's operation of the present invention is more easy, not with an organic solvent, is beneficial to environmental protection.
Embodiment
Hereinafter will be take the preparation method of the effervescent tablet of the effervescent tablet of Tebuconazole and Difenoconazole as example, the present invention will be further described in detail, wherein:
Tebuconazole (tebuconazole) is for the seed treatment of Important Economic crop or the efficient germicide of foliage spray, can effectively prevent and treat multiple rust, powdery mildew, net blotch, root rot, the head blight of cereal crop, smut and kind pass zonate spot etc.Tebuconazole mainly is missible oil in the market, aqueous emulsion, and suspending agent, wetting powder, water dispersible granules yet there are no effervescent tablet.
Difenoconazole (difenoconazole) has protection, treatment and systemic activity, is sterol demethylation inhibitor, suppresses the biosynthesis of cell wall sterol, stops the growth of fungi.Fungicidal spectrum is wide, and leaf surface treatment or seed treatment can improve output and the guaranteed quality of crop.Difenoconazole mainly is missible oil in the market, and water dispersible granules yet there are no effervescent tablet.
Embodiment 1
Present embodiment provides the preparation method of a kind of 25% Tebuconazole effervescent tablet (the quality percentage composition of Tebuconazole in the 25% expression effervescent tablet), comprises the steps:
(1), carclazyte 14 weight portions are mixed with Tebuconazole 25 weight portions, at-20 ℃ of freezing nanoscales that are crushed to, cross 1200 mesh standard sieves and get nano-carrier Tebuconazole 39 weight portions;
(2), with fumaric acid 15 part, the sodium bicarbonate 26 part of nano-carrier Tebuconazole 39 weight portions with drying, 5 parts of Fluhyzon formaldehyde sodium sulfonates, 4 parts of sodium phosphate trimers, 2 parts of sldium lauryl sulfates, 3 parts of trisiloxanes polyethers, 1 part of PVPP, 5 parts of premixeds of dolomol, coarse crushing, mix again, airslide disintegrating mill is pulverized, and the material after the pulverizing joins cone-type mixer again to be mixed, and batch mixing 100% gets dry powder by 300 mesh standard sieves;
(3), step (2) gained dry powder is suppressed in multiple tablet press machine in flakes, the compressing tablet environmental condition is about 20 ℃ of temperature, and humidity is below 40%, and the size of tablet is determined as required.
Embodiment 2
Present embodiment provides a kind of preparation method of 16% Tebuconazole effervescent tablet, comprises the steps:
(1), kaolin 8 weight portions are mixed with Tebuconazole 16 weight portions, at-20 ℃ of freezing nanoscales that are crushed to, cross 1200 mesh standard sieves and get nano-carrier Tebuconazole 24 weight portions;
(2), with 24 weight portion nano-carrier Tebuconazoles of step (1) gained and dry tartaric acid 25 weight portions, sodium bicarbonate 25 weight portions, low-substituted hydroxypropyl cellulose 5 weight portions, sodium lignin sulfonate 6 weight portions, sodium phosphate trimer 4 weight portions, Negel 5 weight portions, talcum powder 6 weight portion premixeds, coarse crushing, again mixing, airslide disintegrating mill are pulverized, material after the pulverizing joins in the cone-type mixer and mixes, and makes batch mixing 100% get dry powder by 300 mesh standard sieves;
(3), step (2) gained dry powder is suppressed in multiple tablet press machine in flakes, the compressing tablet environmental condition is about 20 ℃ of temperature, and humidity is below 40%, and the size of tablet is determined as required.
Embodiment 3
Present embodiment provides a kind of preparation method of 50% Tebuconazole effervescent tablet, and it comprises the steps:
(1), with 3 parts of corn starchs and Tebuconazole 50 weight portions at-20 ℃ of freezing nanoscales that are crushed to, cross 1200 mesh standard sieves and get nano-carrier Tebuconazole 53 weight portions;
(2), with 53 weight portion nano-carrier Tebuconazoles of step (1) gained and dry fumaric acid 19 weight portions, sodium carbonate 15 weight portions, alkylphenol-polyethenoxy base ether formaldehyde condensation products sodium sulphate 3 weight portions, alkylaryl polyoxyethylene ether 1 weight portion, sodium phosphate trimer 4 weight portions, sldium lauryl sulfate 5 weight portion premixeds, coarse crushing, again mixing, airslide disintegrating mill are pulverized, material after the pulverizing joins in the cone-type mixer and mixes, and makes batch mixing 100% get dry powder by 300 mesh standard sieves;
(3), step (2) gained dry powder is suppressed in multiple tablet press machine in flakes, the compressing tablet environmental condition is about 20 ℃ of temperature, and humidity is below 40%, and the size of tablet is determined as required.
Embodiment 4
Present embodiment provides a kind of preparation method of 10% Difenoconazole effervescent tablet, comprises the steps:
(1), kaolin 10 weight portions, White Carbon black 5 weight portions, superfine silica gel powder 3 weight portions are mixed with Difenoconazole 10 weight portions, at-20 ℃ of freezing nanoscales that are crushed to, cross 1200 mesh standard sieves and get nano-carrier Difenoconazole 28 weight portions;
(2), with fumaric acid 20 weight portions, sodium bicarbonate 40 weight portions of 28 weight portion nano-carrier Difenoconazoles with drying, Negel 2 weight portions, trisiloxanes polyethers 4 weight portions, sodium phosphate trimer 1 weight portion, low-substituted hydroxypropyl cellulose 3 weight portions, dolomol 2 weight portion premixeds, coarse crushing mixes again, and airslide disintegrating mill is pulverized, material after the pulverizing joins in the cone-type mixer and mixes, and makes batch mixing 100% get dry powder by 300 mesh standard sieves;
(3), step (2) gained dry powder suppressed in multiple tablet press machine be in flakes 10% Difenoconazole effervescent tablet, the compressing tablet environmental condition is about 20 ℃ of temperature, humidity is below 40%, the size of tablet is determined as required.
Embodiment 5
Present embodiment provides a kind of preparation method of 1% Difenoconazole effervescent tablet, comprises the steps:
(1), aluminium-magnesium silicate 9 weight portions are mixed with Difenoconazole 1 weight portion, at-20 ℃ of freezing nanoscales that are crushed to, cross 1200 mesh standard sieves and get nano-carrier Difenoconazole 10 weight portions;
(2), with tartaric acid 35 weight portions of 10 weight portion nano-carrier Difenoconazoles with drying, sodium bicarbonate 35 weight portions, sucrose 5 weight portions, low-substituted hydroxypropyl cellulose 9 weight portions, polycarboxylate 3 weight portions, alkylnaphthalene sulfonate 2 weight portions, talcum powder 1 weight portion premixed, coarse crushing, mix again, airslide disintegrating mill is pulverized, and the material after the pulverizing joins in the cone-type mixer and mixes, and makes batch mixing 100% get dry powder by 300 mesh standard sieves;
(3), step (2) gained dry powder suppressed in multiple tablet press machine be in flakes 1% Difenoconazole effervescent tablet, the compressing tablet environmental condition is about 20 ℃ of temperature, humidity is below 40%, the size of tablet is determined as required.
Embodiment 6
Present embodiment provides a kind of preparation method of 25% Difenoconazole effervescent tablet, comprises the steps:
(1), superfine silica gel powder 5 weight portions are mixed with Difenoconazole 25 weight portions, at-20 ℃ of freezing nanoscales that are crushed to, cross 1200 mesh standard sieves and get nano-carrier Difenoconazole 30 weight portions;
(2), with fumaric acid 30 weight portions of 30 weight portion nano-carrier Difenoconazoles with drying, sodium carbonate 25 weight portions, dolomol 2 weight portions, Negel 2 weight portions, aliphatic alcohol polyethenoxy base ether 1 weight portion, sodium phosphate trimer 6 weight portions, sodium lignin sulfonate 3 weight portions, PVPP 1 weight portion premixed, coarse crushing mixes again, and airslide disintegrating mill is pulverized, material after the pulverizing joins in the cone-type mixer and mixes, and makes batch mixing 100% get dry powder by 300 mesh standard sieves;
(3), step (2) gained dry powder suppressed in multiple tablet press machine be in flakes 25% Difenoconazole effervescent tablet, the compressing tablet environmental condition is about 20 ℃ of temperature, humidity is below 40%, the size of tablet is determined as required.
Above-described embodiment 1-6 gained effervescent tablet produces bubble after dropping in the water immediately, and tablet is disintegration gradually, and after the disintegration, farm chemical ingredients is distributed in the water equably.Therefore, effervescent tablet can impose on various crops by spraying, or can directly throw in the paddy field, does not need special medical instruments.
Take the 10% Difenoconazole effervescent tablet of the 25% Tebuconazole effervescent tablet of embodiment 1 and embodiment 4 as representative, carry out respectively preventing and treating the stripe rust of wheat field control effectiveness test and prevented and treated the early blight of tomato field control effectiveness test, and compare with the control efficiency of corresponding aqueous emulsion simultaneously, the result sees Table respectively 1 and table 2.
Table 1, chemical control stripe rust of wheat field control effectiveness test result of the present invention
Table 2, chemical control early blight of tomato field control effectiveness test result of the present invention
From table 1,2 as seen, compare conventional aqueous emulsion, the drug effect of Tebuconazole effervescent tablet of the present invention and Difenoconazole effervescent tablet improves, and effective drug duration prolongs, thereby can reduce spraying times, is beneficial to environmental protection.
Above-described embodiment only is explanation technical conceive of the present invention and characteristics; its purpose is to allow the personage who is familiar with technique can understand content of the present invention and according to this enforcement; can not limit protection scope of the present invention with this; all equivalences that Spirit Essence is done according to the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (7)
1. the preparation method of an effervescent table as agricultural chemical, it is characterized in that: described preparation method comprises the steps:
(1), with in bentonite, diatomite, White Carbon black, corn starch, carclazyte, kaolin, superfine silica gel powder and the aluminium-magnesium silicate one or more be combined as carrier, it is mixed with pesticide original medicine, obtain the nano-carrier agricultural chemicals that size is 100～1000 nanometers-15 ℃～-25 ℃ lower freezing pulverizing, wherein the weight ratio of carrier and pesticide original medicine is 0.03～10:1, and described pesticide original medicine is Tebuconazole or Difenoconazole;
(2), with the acid source material of step (1) gained nano-carrier agricultural chemicals with drying, carbon dioxide source, binding agent, wetting dispersing agent, disintegrant and lubricant premixed, through coarse crushing, mix again, join in the cone-type mixer after airslide disintegrating mill is pulverized and mix, make material 100% get dry powder by the standard screen more than 300 orders, wherein, the percentage by weight that feeds intake of each material is: nano-carrier agricultural chemicals 5%～60%, acid source 15%～40%, carbon dioxide source 15%～40%, wetting dispersing agent 3%～30%, binding agent 0～10%, disintegrant 0～10%, lubricant 0～10%;
(3), 15 ℃～25 ℃ of temperature, humidity in the environment below 40%, utilize tablet press machine that step (2) gained dry powder is pressed into the tablet of setting size and be described effervescent table as agricultural chemical.
2. the preparation method of described effervescent table as agricultural chemical according to claim 1 is characterized in that: described acid source is one or more the combination in citric acid, tartaric acid, fumaric acid, hexanedioic acid, succinic acid, citric acid and the malic acid.
3. the preparation method of effervescent table as agricultural chemical according to claim 1 is characterized in that: described carbon dioxide source is one or more the combination in sodium carbonate, sodium bicarbonate, potash, saleratus and the calcium carbonate.
4. the preparation method of effervescent table as agricultural chemical according to claim 1 is characterized in that: described wetting dispersing agent is one or more the combination in sodium lignin sulfonate, modification dimethyl siloxane polyethers, sucrose fatty ester, dodecyl sodium sulfate, trisiloxanes polyethers, sodium phosphate trimer, polycarboxylic acids sodium, Negel, sldium lauryl sulfate, alkylphenol-polyethenoxy base ether, formaldehyde condensation products sodium sulphate, alkylaryl polyoxyethylene ether, aliphatic alcohol polyethenoxy base ether, sodium pyrophosphate and the potassium pyrophosphate.
5. the preparation method of effervescent table as agricultural chemical according to claim 1 is characterized in that: described binding agent is one or more the combination in sodium carboxymethylcellulose, starch, hydroxypropyl cellulose, the sucrose.
6. the preparation method of effervescent table as agricultural chemical according to claim 1 is characterized in that: described disintegrant is one or more the combination in sodium carboxymethyl starch, low-substituted hydroxypropyl cellulose, Ac-Di-Sol, PVPP, shitosan, sodium alginate, the ammonium sulfate.
7. the preparation method of effervescent table as agricultural chemical according to claim 1 is characterized in that: described lubricant is one or more combination in dolomol, talcum powder, sldium lauryl sulfate, wheat starch and the polyethylene glycol.
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| CN 201010519030 CN101999348B (en) | 2010-10-26 | 2010-10-26 | Preparation method of pesticide effervescent tablet |
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| CN101999348B true CN101999348B (en) | 2013-01-02 |
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| CN102524279A (en) * | 2011-12-22 | 2012-07-04 | 广东中迅农科股份有限公司 | Pyrazosulfuron effervescent tablet and preparation method thereof |
| CN103098802B (en) * | 2013-02-02 | 2016-05-11 | 广东中迅农科股份有限公司 | penoxsuam effervescent tablet and preparation method thereof |
| CN103111210A (en) * | 2013-02-26 | 2013-05-22 | 杭州海虹精细化工有限公司 | Technology for modifying ADC foaming agent |
| CN106490021A (en) * | 2016-10-31 | 2017-03-15 | 郑州思辩科技有限公司 | A kind of effervescent tablet of preventing and treating Caulis Zizaniae caduciflorae striped rice borer and preparation method thereof |
| CN106490029A (en) * | 2016-10-31 | 2017-03-15 | 郑州思辩科技有限公司 | A kind of effervescent tablet of preventing and treating rice grub and preparation method thereof |
| CN106978133A (en) * | 2017-04-21 | 2017-07-25 | 广州惠利电子材料有限公司 | LED packaging silicon rubbers and its preparation method and application |
| CN109792986A (en) * | 2018-06-27 | 2019-05-24 | 贵州大学 | A kind of short-chain amylose nano pesticide and preparation method thereof |
| CN112189676B (en) * | 2020-10-15 | 2022-03-11 | 德强生物股份有限公司 | Biopesticide effervescent tablet for preventing and treating rice sheath blight disease and preparation method thereof |
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