CN113519535A - Composition containing pyridalyl and chlorfenapyr - Google Patents
Composition containing pyridalyl and chlorfenapyr Download PDFInfo
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- CN113519535A CN113519535A CN202110955530.1A CN202110955530A CN113519535A CN 113519535 A CN113519535 A CN 113519535A CN 202110955530 A CN202110955530 A CN 202110955530A CN 113519535 A CN113519535 A CN 113519535A
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- lignin
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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
- A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
- A01N43/40—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
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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
- A01N25/08—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
- 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
- A01N25/26—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 in coated particulate form
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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
- A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
- A01N43/36—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom five-membered rings
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/32—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of salts of sulfonic acids
Abstract
The invention discloses a composition containing pyridalyl and chlorfenapyr, which relates to the technical field of pesticide compositions, can generate good synergistic effect after being reasonably compounded by taking pyridalyl and chlorfenapyr as main components, and can achieve good insecticidal effect under the synergistic effect of the pyridalyl and the chlorfenapyr; by adding the modified lignin into the composition, the compound of the pyridalyl and the chlorfenapyr is loaded or coated to achieve a slow release effect, so that the effective components can act on pests for a long time, the probability of insect damage to crops is reduced, and the yield and the quality of the crops are improved; the lignin is easy to biodegrade and has good environmental protection performance as a carrier, but the lignin is still mainly directly discharged into rivers or burnt out after being concentrated as industrial pulping waste along with waste water, so that not only is great resource waste caused, but also the environment is polluted, and the lignin has practical significance for economic development and environmental protection by comprehensively developing and utilizing the lignin.
Description
Technical Field
The invention relates to the technical field of pesticide compositions, and particularly relates to a composition containing pyridalyl and chlorfenapyr.
Background
Triflupirfen is a novel broad-spectrum pesticide developed in recent years, and has good control effect on lepidoptera pests (such as diamond back moths, prodenia litura and the like), thysanoptera pests (such as thrips and the like) and diptera pests (such as liriomyza and the like) on various crops;
the chlorfenapyr is a novel pyrrole compound, acts on mitochondria of cells in an insect body, acts through a multifunctional oxidase in the insect body, mainly inhibits the conversion of Adenosine Diphosphate (ADP) to Adenosine Triphosphate (ATP), and the adenosine triphosphate stores energy necessary for the cells to maintain the vital functions of the cells;
in the actual process of agricultural production, the pest breeding cycle is short, the breeding amount is large, the mobility is small, the self-crossing degree is high, the resistance is particularly easy to generate, and for preventing and controlling the pests generating the resistance in agriculture, a new component without cross resistance with the existing variety is deduced in an effective method; however, the development cost of the new effective components is high, the development period is long, and the new effective components are always faster than the speed of the resistance of pests, and other methods such as crop layout adjustment, different pesticide rotation and the like are difficult to really achieve obvious effects in the actual operation process;
therefore, there is a need for a composition for controlling pests with a long-lasting effect to solve the above problems.
Disclosure of Invention
In order to overcome the technical problems, the invention aims to provide a composition containing pyridalyl and chlorfenapyr: the pyridalyl and the chlorfenapyr are reasonably compounded as main components, so that a good insecticidal effect can be achieved under the synergistic effect of the pyridalyl and the chlorfenapyr, the pyridalyl and the chlorfenapyr compound are loaded or coated by using the modified lignin, a slow-release effect is achieved, and the problems that the existing pyridalyl insecticide and the existing chlorfenapyr insecticide are easy to generate resistance and short in control time effect are solved.
The purpose of the invention can be realized by the following technical scheme:
a composition containing pyridalyl and chlorfenapyr comprises an active ingredient A and an active ingredient B;
the mass ratio of the active component A to the active component B is 1-50: 1 to 50;
the active ingredient A is pyridalyl, and the active ingredient B is chlorfenapyr;
the composition containing pyridalyl and chlorfenapyr is prepared by the following steps:
the method comprises the following steps: dissolving the modified lignin in deionized water to obtain an outer coating solution;
step two: dissolving active ingredient A and active ingredient B in acetone to obtain core solution;
step three: adding the outer wrapping liquid and the inner core liquid into a high-speed shearing machine, shearing for 5-10min under the condition that the stirring speed is 6000-8000r/min, adding isopropanol for defoaming, stirring for 6-8h under the condition that the stirring speed is 300-500r/min, and then evaporating, concentrating, kneading, extruding, granulating, drying and screening to obtain the composition containing the pyridalyl and the chlorfenapyr.
As a further scheme of the invention: the adding amount of the modified lignin is 1/2-1 of the total weight of the active ingredient A and the active ingredient B; the volume ratio of the outer wrapping liquid to the inner core liquid is 4-5: 1.
as a further scheme of the invention: the preparation method of the modified lignin comprises the following steps:
s1: adding alkali lignin into a sodium hydroxide solution, stirring at a stirring speed of 200-300r/min until the alkali lignin is completely dissolved, filtering to remove insoluble substances, adjusting the filtrate with a sulfuric acid solution until the pH value is 6-7, centrifuging, washing the precipitate with distilled water to be neutral, then placing the precipitate in a vacuum drying box, and drying at the temperature of 50-55 ℃ for 45-50h to obtain refined lignin;
s2: adding refined lignin and a mixed solvent into a flask provided with a stirrer, stirring and dispersing for 1-2h under the conditions that the temperature is 50-55 ℃ and the stirring speed is 200-300r/min, stopping stirring and standing at a constant temperature for 20-30h, cooling to room temperature, centrifuging to remove insoluble substances, adding into anhydrous ether, stirring for 20-30min, centrifuging under the conditions of 6000-8000r/min to collect precipitate, placing the precipitate in a vacuum drying box, and drying to constant weight under the condition that the temperature is 40-45 ℃ to obtain acetylated lignin;
s3: adding an acetylated lignin and a sodium hydroxide solution into a three-neck flask provided with a stirrer, a constant-pressure dropping funnel, a condensation reflux pipe and a gas guide pipe, stirring at room temperature and a stirring speed of 300-500r/min until the acetylated lignin is completely dissolved, then adding hydrogen peroxide, heating to 80-85 ℃, stirring at constant temperature for reaction for 2-3h, cooling to room temperature, dropwise adding a mixed solution, controlling the dropping speed to be 1-5mL/min, heating to 80-85 ℃, stirring at constant temperature for reaction for 2-3h, adding a benzyl chloride solution after the reaction is finished, introducing nitrogen for protection, stirring at constant temperature for reaction for 2-3h at 75-85 ℃, then adding anhydrous sodium sulfite, adjusting the pH to be 9 by using a hydrochloric acid solution, performing reflux reaction for 2-3h at 90-95 ℃, and after the reaction is finished, cooling the reaction product to room temperature, adding the reaction product into a hydrochloric acid solution, separating out a precipitate, carrying out vacuum filtration, placing a filter cake in a vacuum drying oven, and drying at the temperature of 50-60 ℃ to constant weight to obtain the modified lignin.
The reaction principle is as follows:
as a further scheme of the invention: the mass ratio of the alkali lignin to the sodium hydroxide solution in the step S1 is 1: 10-15 percent of sodium hydroxide solution, and 5-10 percent of sulfuric acid solution.
As a further scheme of the invention: the dosage ratio of the refined lignin, the mixed solvent and the anhydrous ether in the step S2 is 4 g: 100mL of: 300mL, wherein the mixed solvent is acetic anhydride, pyridine and dioxane according to a volume ratio of 1: 1: 1.
As a further scheme of the invention: the dosage ratio of the acetylated lignin, the sodium hydroxide solution and the hydrogen peroxide in the step S3 is 1 g: 10mL of: 10mL, the mass fraction of the sodium hydroxide solution is 10%, the mass fraction of the hydrogen peroxide solution is 4%, the mass fraction of the hydrochloric acid solution is 10%, the benzyl chloride solution is a solution formed by dissolving benzyl chloride in absolute ethyl alcohol, the mixed solution is a mixture of formaldehyde solution and diethylamine, the mass fraction of the formaldehyde solution is 35-40%, and the molar ratio of the acetylated lignin, the formaldehyde, the diethylamine, the benzyl chloride and the absolute sodium sulfite is 1: 1.1: 1.3: 1.3: 0.5.
as a further scheme of the invention: the pesticide formulation prepared by the composition is one of suspending agent, microemulsion, dispersible oil suspending agent and water dispersible granule.
The invention has the beneficial effects that:
according to the composition containing the pyridalyl and the chlorfenapyr, disclosed by the invention, the pyridalyl and the chlorfenapyr are reasonably compounded as main components, so that both the pyridalyl and the chlorfenapyr have good insecticidal effects, but pests are easy to generate resistance after long-time use, and different varieties of components are compounded, so that the composition is a very common method for preventing and treating resistant pests;
the modified lignin is added into the composition, firstly, the alkali lignin is washed and purified, then, the alkali lignin is acetylated, hydrophilic groups in lignin molecules are reduced, the solubility of the alkali lignin in an organic solvent can be improved, then, substitution reaction is carried out under an alkaline condition to form sulfonated lignin, then, the sulfonated lignin is reacted with formaldehyde to generate 5-hydroxymethyl sulfonated lignin, then, the sulfonated lignin is reacted with diethylamine for dehydration, and then, the sulfonated lignin is reacted with benzyl chloride to form lignin-based ammonium salt, so that the modified lignin is obtained, the molecular structure of the modified lignin simultaneously has cations and anions, the amphoteric characteristic is realized, the solubility of the modified lignin is improved, then, the modified lignin is used for loading or coating active ingredients, the slow release effect is achieved, so that the active ingredients can act on pests for a long time, the probability of insect damage of crops is reduced, and the yield and quality of the crops are improved, the modified lignin is improved in solubility and suitable for preparation of various pesticide formulations, production is carried out according to actual requirements, and the application range is enlarged;
the lignin is the second natural polymer material which is inferior to cellulose in quantity in nature, is rich in resources, easy to biodegrade and good in environmental protection performance as a carrier, but the lignin is still mainly used as industrial pulping waste to be directly discharged into rivers or burnt after being concentrated along with waste water due to the characteristic of a complex amorphous structure of the lignin so far, so that the resource is greatly wasted, the environment is polluted, and the comprehensive development and utilization of the lignin have practical significance on economic development and environmental protection.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the embodiment is a preparation method of modified lignin, which comprises the following steps:
s1: adding 10g of alkali lignin into 150g of a 10% sodium hydroxide solution, stirring at a stirring speed of 200r/min until the alkali lignin is completely dissolved, filtering, adjusting the filtrate with a 5% sulfuric acid solution until the pH value is 6, centrifuging, washing the precipitate with distilled water to be neutral, then placing in a vacuum drying oven, and drying at 50 ℃ for 45 hours to obtain refined lignin;
s2: 4g of refined lignin, 100mL of acetic anhydride, pyridine and dioxane were mixed according to a volume ratio of 1: 1: adding the mixed solvent of 1 into a flask provided with a stirrer, stirring and dispersing for 1h at the temperature of 50 ℃ and the stirring speed of 200r/min, stopping stirring, standing at constant temperature for 20h, cooling to room temperature, centrifuging, adding into 300mL of anhydrous ether, stirring for 20min, centrifuging at 6000r/min, collecting precipitate, placing the precipitate in a vacuum drying oven, and drying at the temperature of 40 ℃ to constant weight to obtain acetylated lignin;
s3: adding 1g of acetylated lignin and 10mL of 10 mass percent sodium hydroxide solution into a three-neck flask provided with a stirrer, a constant-pressure dropping funnel, a condensation reflux pipe and an air guide pipe, stirring at room temperature and a stirring speed of 300r/min until the acetylated lignin is completely dissolved, then adding 10mL of 4 mass percent hydrogen peroxide, heating to 80 ℃, stirring at constant temperature for reaction for 2 hours, cooling to room temperature, dropwise adding a mixed solution of formaldehyde solution and diethylamine, controlling the dropping speed to be 1mL/min, heating to 80 ℃, stirring at constant temperature for reaction for 2 hours, adding benzyl chloride solution after the reaction is finished, introducing nitrogen for protection, stirring at constant temperature for reaction for 2 hours at 75 ℃, then adding anhydrous sodium sulfite, controlling the acetylated lignin, formaldehyde, diethylamine, sodium hydrogen sulfite, sodium hydrogen carbonate, and the like, The molar ratio of benzyl chloride to anhydrous sodium sulfite is 1: 1.1: 1.3: 1.3: 0.5, adjusting the pH value to 9 by using a hydrochloric acid solution with the mass fraction of 10%, performing reflux reaction at the temperature of 90 ℃ for 2 hours, cooling a reaction product to room temperature after the reaction is finished, adding the reaction product into the hydrochloric acid solution with the mass fraction of 10%, separating out a precipitate, performing vacuum filtration, placing a filter cake in a vacuum drying oven, and drying at the temperature of 50 ℃ to constant weight to obtain the modified lignin.
Example 2:
the embodiment is a preparation method of modified lignin, which comprises the following steps:
s1: adding 10g of alkali lignin into 100g of a 10% sodium hydroxide solution, stirring at a stirring speed of 300r/min until the alkali lignin is completely dissolved, filtering, adjusting the filtrate with a 10% sulfuric acid solution until the pH value is 7, centrifuging, washing the precipitate with distilled water to be neutral, then placing in a vacuum drying oven, and drying at 55 ℃ for 50h to obtain refined lignin;
s2: 4g of refined lignin, 100mL of acetic anhydride, pyridine and dioxane were mixed according to a volume ratio of 1: 1: adding the mixed solvent of 1 into a flask provided with a stirrer, stirring and dispersing for 2h at the temperature of 55 ℃ and the stirring speed of 300r/min, stopping stirring, standing at constant temperature for 30h, cooling to room temperature, centrifuging, adding into 300mL of anhydrous ether, stirring for 30min, centrifuging at 8000r/min, collecting precipitate, placing the precipitate in a vacuum drying oven, and drying at the temperature of 45 ℃ to constant weight to obtain acetylated lignin;
s3: adding 1g of acetylated lignin and 10mL of 10 mass percent sodium hydroxide solution into a three-neck flask provided with a stirrer, a constant-pressure dropping funnel, a condensation reflux pipe and an air guide pipe, stirring at room temperature and a stirring speed of 300-500r/min until the acetylated lignin is completely dissolved, then adding 10mL of 4 mass percent hydrogen peroxide, heating to 85 ℃, stirring at constant temperature for reaction for 3 hours, cooling to room temperature, dropwise adding a mixed solution of formaldehyde solution and diethylamine, controlling the dropwise adding speed to be 5mL/min, heating to 85 ℃, stirring at constant temperature for reaction for 3 hours, adding a benzyl chloride solution after the reaction is finished, introducing nitrogen for protection, stirring at constant temperature for reaction for 3 hours at 85 ℃, then adding anhydrous sodium sulfite, and controlling the acetylated lignin, the formaldehyde, the anhydrous sodium sulfite, The mol ratio of diethylamine to benzyl chloride to anhydrous sodium sulfite is 1: 1.1: 1.3: 1.3: 0.5, adjusting the pH value to 9 by using a hydrochloric acid solution with the mass fraction of 10%, performing reflux reaction at the temperature of 95 ℃ for 3 hours, cooling a reaction product to room temperature after the reaction is finished, adding the reaction product into the hydrochloric acid solution with the mass fraction of 10%, separating out a precipitate, performing vacuum filtration, placing a filter cake in a vacuum drying oven, and drying at the temperature of 60 ℃ to constant weight to obtain the modified lignin.
Example 3:
the embodiment is a preparation method of a composition containing pyridalyl and chlorfenapyr, which comprises the following steps:
the method comprises the following steps: dissolving 20g of modified lignin in 200mL of deionized water to obtain an outer coating solution;
step two: dissolving 1g of pyridalyl and 19g of chlorfenapyr in 50mL of acetone to obtain an inner core solution;
step three: adding the outer wrapping liquid and the inner core liquid into a high-speed shearing machine, shearing for 5min under the condition that the stirring speed is 6000r/min, adding isopropanol, stirring for 6h under the condition that the stirring speed is 300r/min, and then evaporating, concentrating, kneading, extruding, granulating, drying and screening to obtain the composition containing the pyridalyl and the chlorfenapyr.
Example 4:
the embodiment is a preparation method of a composition containing pyridalyl and chlorfenapyr, which comprises the following steps:
the method comprises the following steps: dissolving 10g of modified lignin in 200mL of deionized water to obtain an outer coating solution;
step two: dissolving 10g of pyridalyl and 10g of chlorfenapyr in 50mL of acetone to obtain an inner core solution;
step three: adding the outer wrapping liquid and the inner core liquid into a high-speed shearing machine, shearing for 8min under the condition that the stirring speed is 7000r/min, adding isopropanol, stirring for 7h under the condition that the stirring speed is 400r/min, and then evaporating, concentrating, kneading, extruding, granulating, drying and screening to obtain the composition containing pyridalyl and chlorfenapyr.
Example 5:
the embodiment is a preparation method of a composition containing pyridalyl and chlorfenapyr, which comprises the following steps:
the method comprises the following steps: dissolving 10g of modified lignin in 200mL of deionized water to obtain an outer coating solution;
step two: dissolving 7g of pyridalyl and 13g of chlorfenapyr in 40mL of acetone to obtain an inner core solution;
step three: adding the outer wrapping liquid and the inner core liquid into a high-speed shearing machine, shearing for 10min under the condition that the stirring speed is 8000r/min, adding isopropanol for defoaming, stirring for 8h under the condition that the stirring speed is 500r/min, and then performing evaporation concentration, kneading, extrusion granulation, drying and screening to obtain the composition containing pyridalyl and chlorfenapyr.
Comparative example 1:
comparative example 1 differs from example 5 in that no modified lignin was added.
Comparative example 2:
comparative example 2 is the insecticidal composition containing chlorfenapyr provided in CN 201910418978.2.
The performance of the compositions containing pyridalyl and chlorfenapyr of examples 3-5 was tested for 30 days to control thrips in the subjects, and the test results were as follows:
| sample (I) | 1d average control efficacy/%) | 7d average control efficacy/%) | 14d average control efficacy/%) | 30d average control efficacy% |
| Example 3 | 83.9 | 90.1 | 95.6 | 91.9 |
| Example 4 | 85.1 | 93.9 | 96.2 | 92.8 |
| Example 5 | 84.7 | 91.8 | 95.7 | 92.4 |
| Comparative example 1 | 86.2 | 90.3 | 62.1 | 41.1 |
| Comparative example 2 | 66.2 | 92.2 | 80.0 | 49.7 |
Referring to the data in the table, it can be seen that the composition of the present invention has a long-lasting effect compared to the comparative example, wherein it can be seen that the control time can be significantly increased by adding the modified lignin by comparing the example with the comparative example 1, and it can be seen that the composition of the present invention has a better effect compared to the composition of the prior art by comparing the example with the comparative example 2.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (7)
1. A composition containing pyridalyl and chlorfenapyr is characterized by comprising an active ingredient A and an active ingredient B;
the mass ratio of the active component A to the active component B is 1-50: 1 to 50;
the active ingredient A is pyridalyl, and the active ingredient B is chlorfenapyr;
the composition containing pyridalyl and chlorfenapyr is prepared by the following steps:
the method comprises the following steps: dissolving the modified lignin in deionized water to obtain an outer coating solution;
step two: dissolving active ingredient A and active ingredient B in acetone to obtain core solution;
step three: adding the outer wrapping liquid and the inner core liquid into a high-speed shearing machine, shearing for 5-10min under the condition that the stirring speed is 6000-8000r/min, adding isopropanol, stirring for 6-8h under the condition that the stirring speed is 300-500r/min, and then carrying out evaporation concentration, kneading, extrusion granulation, drying and screening to obtain the composition containing the pyridalyl and the chlorfenapyr.
2. The composition containing pyridalyl and chlorfenapyr according to claim 1, wherein the addition amount of the modified lignin is 1/2-1 of the total weight of the active ingredient A and the active ingredient B; the volume ratio of the outer wrapping liquid to the inner core liquid is 4-5: 1.
3. the composition containing pyridalyl and chlorfenapyr according to claim 1, wherein the modified lignin is prepared by the following method:
s1: adding alkali lignin into a sodium hydroxide solution, stirring at the stirring speed of 200-300r/min until the alkali lignin is completely dissolved, filtering, adjusting the filtrate with a sulfuric acid solution until the pH value is 6-7, centrifuging, washing the precipitate with distilled water to be neutral, then placing the precipitate in a vacuum drying box, and drying at the temperature of 50-55 ℃ for 45-50h to obtain refined lignin;
s2: adding refined lignin and a mixed solvent into a flask provided with a stirrer, stirring and dispersing for 1-2h under the conditions that the temperature is 50-55 ℃, the stirring speed is 200-300r/min, stopping stirring, standing at a constant temperature for 20-30h, cooling to room temperature, centrifuging, adding into anhydrous ether, stirring for 20-30min, centrifuging under the conditions of 6000-8000r/min, placing the precipitate into a vacuum drying box, and drying to constant weight under the condition that the temperature is 40-45 ℃ to obtain acetylated lignin;
s3: adding an acetylated lignin and a sodium hydroxide solution into a three-neck flask provided with a stirrer, a constant-pressure dropping funnel, a condensation reflux pipe and a gas guide pipe, stirring at room temperature and a stirring speed of 300-500r/min until the acetylated lignin is completely dissolved, then adding hydrogen peroxide, heating to 80-85 ℃, stirring at constant temperature for reaction for 2-3h, cooling to room temperature, dropwise adding a mixed solution, controlling the dropping speed to be 1-5mL/min, heating to 80-85 ℃, stirring at constant temperature for reaction for 2-3h, adding a benzyl chloride solution after the reaction is finished, introducing nitrogen for protection, stirring at constant temperature for reaction for 2-3h at 75-85 ℃, then adding anhydrous sodium sulfite, adjusting the pH to be 9 by using a hydrochloric acid solution, performing reflux reaction for 2-3h at 90-95 ℃, and after the reaction is finished, cooling the reaction product to room temperature, adding the reaction product into a hydrochloric acid solution, separating out a precipitate, carrying out vacuum filtration, placing a filter cake in a vacuum drying oven, and drying at the temperature of 50-60 ℃ to constant weight to obtain the modified lignin.
4. The composition containing pyridalyl and chlorfenapyr according to claim 3, wherein the mass ratio of the alkali lignin to the sodium hydroxide solution in the step S1 is 1: 10-15 percent of sodium hydroxide solution, and 5-10 percent of sulfuric acid solution.
5. The composition containing pyridalyl and chlorfenapyr according to claim 3, wherein the amount ratio of the refined lignin, the mixed solvent and the anhydrous ether in the step S2 is 4 g: 100mL of: 300mL, wherein the mixed solvent is acetic anhydride, pyridine and dioxane according to a volume ratio of 1: 1: 1.
6. The composition containing pyridalyl and chlorfenapyr according to claim 3, wherein the dosage ratio of the acetylated lignin, the sodium hydroxide solution and the hydrogen peroxide in the step S3 is 1 g: 10mL of: 10mL, the mass fraction of the sodium hydroxide solution is 10%, the mass fraction of the hydrogen peroxide solution is 4%, the mass fraction of the hydrochloric acid solution is 10%, the benzyl chloride solution is a solution formed by dissolving benzyl chloride in absolute ethyl alcohol, the mixed solution is a mixture of formaldehyde solution and diethylamine, the mass fraction of the formaldehyde solution is 35-40%, and the molar ratio of the acetylated lignin, the formaldehyde, the diethylamine, the benzyl chloride and the absolute sodium sulfite is 1: 1.1: 1.3: 1.3: 0.5.
7. the composition containing pyridalyl and chlorfenapyr according to claim 1, wherein the pesticide formulation prepared from the composition is one of a suspending agent, a microemulsion, a dispersible oil suspending agent and a water dispersible granule.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000169305A (en) * | 1998-12-03 | 2000-06-20 | Sumitomo Chem Co Ltd | Composition for insecticide and miticide |
| CN101664032A (en) * | 2009-09-08 | 2010-03-10 | 深圳诺普信农化股份有限公司 | Pesticide combination |
| CN104381261A (en) * | 2014-11-25 | 2015-03-04 | 广东中迅农科股份有限公司 | Insecticide composition containing chlorine chlorfenapyr and pyridalyl |
| CN110037033A (en) * | 2019-05-20 | 2019-07-23 | 海南博士威农用化学有限公司 | A kind of Pesticidal combination and its preparation containing capillary |
-
2021
- 2021-08-19 CN CN202110955530.1A patent/CN113519535A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000169305A (en) * | 1998-12-03 | 2000-06-20 | Sumitomo Chem Co Ltd | Composition for insecticide and miticide |
| CN101664032A (en) * | 2009-09-08 | 2010-03-10 | 深圳诺普信农化股份有限公司 | Pesticide combination |
| CN104381261A (en) * | 2014-11-25 | 2015-03-04 | 广东中迅农科股份有限公司 | Insecticide composition containing chlorine chlorfenapyr and pyridalyl |
| CN110037033A (en) * | 2019-05-20 | 2019-07-23 | 海南博士威农用化学有限公司 | A kind of Pesticidal combination and its preparation containing capillary |
Non-Patent Citations (1)
| Title |
|---|
| 艾青 等: "以二甲基--正丁基--磺化木质素基氯化铵为模板剂制备多孔钛材料", 《北京林业大学学报》 * |
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