CN114794139A - Insecticidal water dispersible granule of tetramethrin and dinotefuran and preparation method thereof - Google Patents
Insecticidal water dispersible granule of tetramethrin and dinotefuran and preparation method thereof Download PDFInfo
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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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- 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
- A01N25/02—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 containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- 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
- A01N25/08—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 containing solids as carriers or diluents
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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
- A01N51/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds having the sequences of atoms O—N—S, X—O—S, N—N—S, O—N—N or O-halogen, regardless of the number of bonds each atom has and with no atom of these sequences forming part of a heterocyclic ring
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Abstract
The invention discloses an insecticidal water dispersible granule of tetramethrin and dinotefuran and a preparation method thereof, belonging to the field of preparation of insecticidal medicaments, wherein the water dispersible granule comprises the following raw materials: the invention aims to solve the problems of stickiness and heating when tetramethrin and dinotefuran are mixed to prepare an insecticidal water dispersible granule, and simultaneously solve the problems of low disintegration speed or no disintegration, easy adhesion and poor suspension property of the prepared insecticidal water dispersible granule.
Description
Technical Field
The invention relates to the technical field of pesticide preparation, in particular to an insecticidal water dispersible granule of tetramethrin and dinotefuran and a preparation method thereof.
Background
German cockroach (Blattella germanica) is one of the urban sanitary pests in Blatta order (Blattodea) which has the fastest breeding speed, the widest distribution at home and abroad, is close to human life and is most difficult to control. At present, the prevention and control method of the German cockroach mainly depends on chemical prevention and control, and because people use sanitary pesticides frequently and unreasonably for a long time in the actual prevention and control process and the lack of life habits and prevention and control knowledge of the German cockroach hinders the prevention and control effect of the German cockroach, the drug resistance of the German cockroach to sanitary insecticides such as pyrethroid insecticides and the like is continuously increased. Dinotefuran is the only nicotine pesticide without chlorine atoms and aromatic rings, has a chemical structure which is greatly different from that of the existing nicotine pesticide (such as thiamethoxam, clothianidin, thiacloprid and the like), and has the advantages of contact poisoning, stomach toxicity, strong systemic property, high efficiency, systemic property, broad spectrum, low toxicity, long lasting period, no phytotoxicity to crops, safe use, no cross resistance with conventional pesticides and the like. Tetramethrin, the original drug is white crystalline solid, is a pyrethroid pesticide with high efficiency, low toxicity and quick knockdown, has strong contact poisoning, stomach toxicity, ovicidal action, food refusal and certain repellent action on sanitary pests, and has no systemic absorption and fumigation action. Experiments prove that the composition has the feasibility of compounding.
The water dispersible granule is a new pesticide formulation, also called dry suspending agent, but we find that certain problem defects exist in the compounding process of tetramethrin and dinotefuran, when the water dispersible granule is prepared, the product is easy to bond, is not easy to disintegrate, disperse and suspend in water, is easy to block a spray head, or is easy to cause phenomena of precipitation and the like in a sprayer after standing, causes uneven spraying and easily causes local phytotoxicity of crops, and in addition, the problems of heating and sticking also occur in the process of granulating by adding water, so that the research and development of the compound pesticide formulation for effectively preventing and controlling German cockroach and treating the problem of pesticide resistance has important practical significance and practical value.
Disclosure of Invention
In view of the above, the invention aims to provide an insecticidal water dispersible granule containing tetramethrin and dinotefuran and a preparation method thereof, which solve the problems of stickiness and heating when tetramethrin and dinotefuran are mixed to prepare the insecticidal water dispersible granule, and solve the problems of slow disintegration speed or no disintegration, easy adhesion and poor suspension property of the prepared insecticidal water dispersible granule.
The invention solves the technical problems by the following technical means:
the insecticidal water dispersible granule of tetramethrin and dinotefuran comprises the following raw materials: tetramethrin, dinotefuran, a wetting agent, a dispersing agent, a disintegrating agent and calcined kaolin.
Preferably, the mass percent of the tetramethrin and the mass percent of the dinotefuran in the water dispersible granules are 14.4% and 0.04%.
Preferably, the mass percent of the wetting agent in the water dispersible granule is 4%, the mass percent of the dispersing agent is 10%, the mass percent of the disintegrating agent is 4%, and the calcined kaolin is complemented to 100%.
More preferably, the wetting agent is a wetting agent ProDis6067, the dispersing agent is a dispersing agent LT-SK36, and the disintegrating agent is a disintegrating agent Q303.
When the pesticide is used, the water dispersible granules are mixed with water, when the concentration of a prepared medicament is 1.25-1.45 g/L, the pesticide effect on the German cockroach is 82.92% -97.92%, and the pesticide effect is obvious, so that the water dispersible granules have a better control effect on the German cockroach.
The invention also discloses a preparation method of the insecticidal water dispersible granule containing tetramethrin and dinotefuran, which comprises the following specific steps: mixing all the raw materials, pulverizing in a jet mill, wetting with deionized water (6-8% of the total weight of the raw materials), stirring, granulating in a granulator, drying in a 40 deg.C constant temperature drying oven for 35-40min, and sieving to obtain the final product.
Preferably, the temperature in the pulverizer is less than or equal to 60 ℃ in the pulverizing process of the jet mill.
Before the water dispersible granule is prepared, the calcined kaolin can be obtained by pretreating the kaolin, and the preparation method of the calcined kaolin comprises the following steps:
the method comprises the steps of uniformly mixing kaolin, sodium chloride, poloxamer and water to prepare a mixture with the water content of 25-30%, then placing the mixture in a high-pressure kettle, pressurizing to 0.5-1Mpa, standing for 3-4h, then taking out the mixture, mixing the mixture with montmorillonite, extruding for 10-15min at the pressure of 1-1.5Mpa, taking out the mixture, crushing, placing the mixture in a microwave oscillator for treating for 15-20min at the temperature of 100-110 ℃ and the frequency of 2450MHz, then taking out the mixture for calcining at the temperature of 500-550 ℃ and keeping the temperature for 4h to obtain calcined kaolin.
Preferably, the mass ratio of the kaolin to the sodium chloride to the poloxamer is 100: 1: 5.
preferably, the mass ratio of the mixture to the montmorillonite is 100: 3.
has the advantages that:
(1) the insecticidal water dispersible granule of tetramethrin and dinotefuran provided by the invention can kill German cockroach, the death rate of German cockroach is more than 80%, and the insecticidal water dispersible granule can be used and developed as a novel insecticide for killing cockroach.
(2) The invention solves the problems of stickiness and heating when tetramethrin, dinotefuran and other auxiliary material auxiliaries are mixed to prepare the insecticidal water dispersible granule, reduces the system viscosity, improves the fluidity, and ensures that the prepared product is easy to disintegrate and has high suspension rate.
(3) The prepared insecticidal water dispersible granule has short disintegration time, high suspension rate and dispersibility, stable physicochemical property after high-temperature heat storage, is not easy to block a spray head or cause uneven spraying due to standing precipitation, and can be further explored for application in other fields.
Drawings
FIG. 1: dispersion of the aqueous dispersion prepared in example 4 in water.
Detailed Description
The invention will be described in detail below with reference to specific embodiments and the accompanying drawing 1:
example 1: efficacy test of tetramethrin and dinotefuran
The tetramethrin and the dinotefuran are respectively 14.4% and 0.04% by mass in the water dispersible granule, and a conventional simulated pesticide effect test is carried out on the insecticidal water dispersible granule.
The tested German cockroach is introduced from Chongqing customs health quarantine department of the people's republic of China, the tested cockroach is from the institute of microbial epidemic disease of military medical academy of sciences, indoor isolated breeding is about 25 years to date, and no chemical agent is contacted during the breeding period.
Feeding conditions are as follows: temperature (27 +/-1) DEG C, humidity (60 +/-10)%, no light condition (except operation time); feeding: the mice are fed with complete feed and supplied with tap water.
The water dispersible granules are mixed with water, and prepared into medicaments with the concentrations of 0.45g/L, 0.65g/L, 0.85g/L, 1.05g/L, 1.25g/L and 1.45g/L respectively for carrying out pharmacodynamic tests, 3 times of repetition are set, the number of German cockroaches is 80, the mortality is calculated, and the obtained data are shown in table 1.
TABLE 1
The results in table 1 show that when the content of tetramethrin in the water dispersible granule is 14.4% and the content of dinotefuran is 0.04%, the pesticide composition has a good control effect on the german cockroach, and when the concentration of the pesticide reaches 1.25g/L-1.45g/L, the pesticide effect is remarkable, and the death rate of the german cockroach reaches more than 80%.
Example 2: preparation of calcined Kaolin
Weighing 100g of kaolin, 1g of sodium chloride, 1885g of poloxamer and 3.18g of montmorillonite according to the following mass.
The calcined kaolin was prepared as follows:
uniformly mixing kaolin and sodium chloride, adding poloxamer 188 and water, uniformly mixing until the water content of the mixture is 25%, then placing the mixture into a high-pressure kettle, pressurizing to 0.5Mpa in the high-pressure kettle, standing for 3h, taking out the mixture, mixing the mixture with montmorillonite, mechanically dispersing uniformly, then placing the mixture into a container, mechanically extruding for 15min at the pressure of 1Mpa, taking out after the extrusion is finished, crushing into powder, treating for 20min in a microwave oscillator with the frequency of 2450MHz and the temperature of 100 ℃, taking out after the treatment is finished, calcining at the temperature of 500 ℃, and keeping the temperature for 4h to obtain calcined kaolin.
Example 3: preparation of calcined Kaolin
Weighing 100g of kaolin, 1g of sodium chloride, 1885g of poloxamer and 3.18g of montmorillonite according to the following mass.
The calcined kaolin was prepared as follows:
uniformly mixing kaolin and sodium chloride, adding poloxamer 188 and water, uniformly mixing until the water content of the mixture is 30%, then placing the mixture into a high-pressure kettle, pressurizing to 1Mpa in the high-pressure kettle, standing for 4h, taking out the mixture, mixing the mixture with montmorillonite, uniformly dispersing mechanically, then placing the mixture into a container, mechanically extruding the mixture for 10min at the pressure of 1.5Mpa, taking out the mixture after the extrusion is finished, crushing the mixture into powder, placing the powder into a microwave oscillator with the frequency of 2450MHz and the temperature of 110 ℃ for treatment for 15min, taking out the powder after the treatment is finished, calcining the temperature of 550 ℃, and keeping the temperature for 4h to obtain calcined kaolin.
Example 4: preparation of pesticidal water dispersible granules
Weighing the following raw materials in parts by weight: 14.4g tetramethrin, 0.04g dinotefuran, 4g wetting agent ProDis6067, 10g dispersant LT-SK36, 4g disintegrant Q303, 67.56g calcined kaolin (prepared in example 2).
The preparation method comprises the steps of uniformly mixing all the raw materials, adding the mixture into a jet mill for grinding, controlling the temperature in the mill to be not higher than 60 ℃ during grinding, grinding to about 5 microns, wetting the ground raw materials with deionized water, adding about 8g of deionized water, uniformly stirring, adding the mixture into a granulator, kneading, extruding and granulating at a rotating speed of 50r/min, drying in a 40 ℃ constant-temperature drying box for 35-40min after granulating, screening to obtain the product, and sieving the obtained insecticidal water dispersible granules with a 20-40-mesh sieve.
Example 5: preparation of pesticidal water dispersible granules
Weighing the following raw materials in parts by weight: 14.4g tetramethrin, 0.04g dinotefuran, 4g wetting agent ProDis6067, 10g dispersant LT-SK36, 4g disintegrant Q303, 67.56g calcined kaolin (prepared in example 3).
The preparation method comprises the steps of uniformly mixing all the raw materials, adding the mixture into a jet mill for grinding, controlling the temperature in the mill to be not higher than 60 ℃ during grinding, grinding to about 5 microns, wetting the ground raw materials with deionized water, adding about 6g of deionized water, uniformly stirring, adding the mixture into a granulator, kneading, extruding and granulating at a rotating speed of 50r/min, drying in a 40 ℃ constant-temperature drying box for 35-40min after granulating, screening to obtain the product, and sieving the obtained insecticidal water dispersible granules with a 20-40-mesh sieve.
Comparative example 1:
the raw materials are weighed according to the mass in the example 2, and the step of preparing the calcined kaolin is different from the step in the example 2 only in that the calcined kaolin is obtained by uniformly mixing kaolin, sodium chloride and montmorillonite, adding poloxamer 188 and water, uniformly mixing, and directly calcining at the constant temperature of 500 ℃ for 4 hours.
Comparative example 2:
weighing 100g of kaolin as a raw material, calcining the kaolin at 500 ℃, and keeping the temperature for 4 hours to obtain calcined kaolin.
Comparative example 3:
weighing 100g of kaolin and 3.18g of montmorillonite as raw materials, mixing the kaolin and the montmorillonite, mechanically dispersing uniformly, then placing the mixture into a container, mechanically extruding for 15min under the pressure of 1Mpa, taking out the mixture after extrusion, crushing the mixture into powder, treating the powder in a microwave oscillator with the frequency of 2450MHz and the temperature of 100 ℃ for 20min, taking out the powder after treatment, calcining the powder, keeping the temperature at 500 ℃ for 4h, and obtaining calcined kaolin.
Comparative example 4:
weighing 100g of kaolin, 1g of sodium chloride, 1885g of poloxamer and 3.18g of montmorillonite.
The calcined kaolin was prepared as follows:
uniformly mixing kaolin and sodium chloride, adding poloxamer 188 and water, uniformly mixing until the water content of the mixture is 25%, then placing the mixture into a high-pressure kettle, pressurizing to 0.5Mpa in the high-pressure kettle, standing for 3h, taking out the mixture, mixing the mixture with montmorillonite, crushing into powder, placing the powder into a microwave oscillator with the frequency of 2450MHz and the temperature of 100 ℃ for treatment for 20min, taking out after the treatment is finished, calcining at the calcining temperature of 500 ℃, and keeping the temperature for 4h to obtain calcined kaolin.
The calcined kaolin of comparative examples 1 to 4 was used to prepare water dispersible granules according to the method of example 4, to obtain comparative granules 1, 2, 3 and 4, respectively.
The water dispersible granules of comparative granules 1 to 4 and the water dispersible granules of example 4 and example 5 were subjected to disintegration, suspension percentage, wetting time, dispersibility and storage stability, respectively.
Method for measuring disintegratability: at room temperature, after 90ml of water was added to a 100ml stoppered cylinder, a further 0.5g of sample was added and the time required for 99% complete disintegration of the sample particles was recorded, rotating around the centre of the cylinder at a speed of 8 r/min.
The suspension percentage determination method comprises the following steps: reference CIPAC MT15 standard.
The wettability measuring method comprises the following steps: 1g of sample was weighed accurately, poured quickly into a standard graduated cylinder containing 500mL (25 ℃), allowed to settle naturally, and the time for 99% of the sample to settle to the bottom was recorded.
The dispersibility determination method comprises the following steps: reference CIPAC MT174 standard.
Storage stability determination method: the sample is sealed in an ampoule bottle, then placed in a constant-temperature oven at 55 ℃, stored for 14 days and then taken out, and the suspension rate, wettability and disintegrability are measured according to the method.
TABLE 2
From the results in table 2, it can be seen that:
(1) the disintegration time of the insecticidal water dispersible granules prepared in the embodiments 4 and 5 is about 45s, the wetting time is about 55s, the wetting speed is high, the disintegration time is short, and meanwhile, the dispersibility and the suspension property are more than or equal to 90%, so that the insecticidal water dispersible granules are not easy to precipitate, have good suspension property, and are not easy to block a spray head or cause uneven spraying in the using process. After high-temperature heat storage at 55 ℃, the physical and chemical properties of the insecticidal water dispersible granule are basically stable, and the storage stability is better.
(2) Compared with the example 4, the difference lies in the treatment of calcined kaolin, the raw materials such as kaolin, sodium chloride powder and the like are directly calcined at high temperature and then used for preparing the water dispersible granule, and from the test, the disintegration property, the wettability, the suspension rate and the dispersibility of the comparative granule 1 are all poorer than those of the example 4, particularly the disintegration time is 47s higher than that of the example 4, and the physical and chemical properties are obviously reduced after heat storage.
(3) Compared with the embodiment 4, the granule 2 is prepared by using kaolin directly calcined and filler used in the conventional technology, and tests show that the disintegration, wettability, suspension rate and dispersibility of the granule 2 are the worst, the disintegration time is increased by 56s, and the physical and chemical properties after thermal storage are reduced the most obviously.
(4) Compared with the example 4, the difference lies in the treatment of calcined kaolin, the kaolin is not modified by sodium chloride and poloxamer 188, from tests, the disintegration, the wettability, the suspension rate and the dispersibility of the comparative granule 3 are all worse than those of the example 4, and the physicochemical properties after heat storage are reduced because the sodium chloride and the poloxamer are both easily soluble in water, when the poloxamer forms micelles, the kaolin and the sodium chloride are wrapped in the kaolin and the sodium chloride are changed among layers of the kaolin after autoclave and extrusion treatment, the sodium chloride is attached inside, after the water dispersible granules are dissolved in water, the sodium chloride is melted, the water contains sodium ions, the ions adsorbed by the water dispersible granules are increased, the stability of the suspending agent is increased, and after the kaolin is calcined, the dispersibility is also improved.
(5) The comparative granule 4 is compared with example 4, except that the mixture is not treated by mechanical extrusion during the treatment of calcined kaolin, and only autoclave treatment is used, and from the test, the disintegration, wettability, suspension percentage and dispersibility of the comparative granule 4 are all inferior to those of example 4, and the physicochemical properties after heat storage are reduced. Compared with the comparative granule 2, the disintegration property, the suspension property and the dispersibility of the granules are improved, but the physicochemical properties of the granules can not achieve the effect of example 4 without extrusion treatment.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims. The techniques, shapes, and configurations not described in detail in the present invention are all known techniques.
Claims (10)
1. The insecticidal water dispersible granule containing tetramethrin and dinotefuran is characterized by comprising the following raw materials: tetramethrin, dinotefuran, a wetting agent, a dispersing agent, a disintegrating agent and calcined kaolin.
2. The insecticidal water dispersible granule containing tetramethrin and dinotefuran according to claim 1, wherein the mass percent of tetramethrin in the water dispersible granule is 14.4%, and the mass percent of dinotefuran is 0.04%.
3. The insecticidal water dispersible granule of tetramethrin and dinotefuran according to claim 2, wherein the water dispersible granule comprises 4% by mass of a wetting agent, 10% by mass of a dispersing agent, 4% by mass of a disintegrating agent, and calcined kaolin to make up to 100%.
4. The insecticidal water dispersible granule of tetramethrin and dinotefuran according to claim 3, wherein the wetting agent is ProDis6067, the dispersing agent is LT-SK36, and the disintegrating agent is Q303.
5. The insecticidal water dispersible granule containing tetramethrin and dinotefuran according to claim 4, wherein the concentration of the insecticide in the water dispersible granule is 1.25g/L-1.45 g/L.
6. The preparation method of the insecticidal water dispersible granule of tetramethrin and dinotefuran according to any one of claims 1 to 5, which is characterized by comprising the following steps: mixing all the raw materials, pulverizing in a jet mill, wetting with deionized water, stirring, granulating in a granulator, drying at 40 deg.C for 35-40min, and sieving to obtain the final product.
7. The preparation method of the insecticidal water dispersible granule containing tetramethrin and dinotefuran according to claim 6, wherein the temperature in the pulverizer is less than or equal to 60 ℃ in the pulverizing process of the jet mill.
8. The preparation method of tetramethrin and dinotefuran insecticidal water dispersible granules according to claim 7, wherein kaolin is pretreated to obtain calcined kaolin before the water dispersible granules are prepared, and the preparation method of the calcined kaolin is as follows:
the method comprises the steps of uniformly mixing kaolin, sodium chloride, poloxamer and water to prepare a mixture with the water content of 25-30%, then placing the mixture in a high-pressure kettle, pressurizing to 0.5-1Mpa, standing for 3-4h, then taking out the mixture, mixing the mixture with montmorillonite, extruding for 10-15min at the pressure of 1-1.5Mpa, taking out the mixture, crushing, placing the mixture in a microwave oscillator for treating for 15-20min at the temperature of 100-110 ℃ and the frequency of 2450MHz, then taking out the mixture for calcining at the temperature of 500-550 ℃ and keeping the temperature for 4h to obtain calcined kaolin.
9. The preparation method of tetramethrin and dinotefuran insecticidal water dispersible granules according to claim 8, wherein the mass ratio of kaolin to sodium chloride to poloxamer is 100: 1: 5.
10. the preparation method of tetramethrin and dinotefuran insecticidal water dispersible granules according to claim 9, wherein the mass ratio of the mixture to montmorillonite is 100: 3.
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| 刘育超等: "胺菊酯与呋虫胺对德国小蠊的联合毒力测定", 《中国媒介生物学及控制杂志》, vol. 32, no. 1, pages 26 - 29 * |
| 李宝智,徐星佩: "煅烧高岭土表面改性", 非金属矿, vol. 25, no. 1, pages 48 - 49 * |
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