CN110250197B - Dinotefuran and bifenthrin insecticidal composition and application thereof - Google Patents
Dinotefuran and bifenthrin insecticidal composition and application thereof Download PDFInfo
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- CN110250197B CN110250197B CN201910551785.4A CN201910551785A CN110250197B CN 110250197 B CN110250197 B CN 110250197B CN 201910551785 A CN201910551785 A CN 201910551785A CN 110250197 B CN110250197 B CN 110250197B
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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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- 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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Abstract
The invention discloses a dinotefuran/bifenthrin insecticidal composition and application thereof, wherein the active pharmaceutical ingredients are dinotefuran and bifenthrin, and the mass ratio of the dinotefuran to the bifenthrin is 1-20: 1. The dinotefuran and bifenthrin as the active pharmaceutical ingredients of the insecticidal composition belong to two insecticides with different action mechanisms, and the two insecticides are mixed without conflict, so that the insecticidal spectrum is expanded, the quick action and the lasting effect are improved, and the insecticidal efficiency is improved.
Description
Technical Field
The invention relates to an insecticidal composition, in particular to an insecticidal composition containing dinotefuran and bifenthrin and application of the composition in controlling insect pests of grain crops, fruit trees and vegetables, and belongs to the technical field of pesticides.
Background
Bifenthrin (Bifenthrin) is a high-efficiency synthetic pyrethrin insecticide and acaricide, acts on a sodium ion channel to interfere a nervous system, mainly plays a role in contact killing and stomach poisoning, has no functions of systemic absorption and fumigation, has quick insecticidal action, longer residual period and wide insecticidal spectrum, is effective to various pests such as lepidoptera, hemiptera, coleoptera, thysanoptera and the like, has a certain control effect on acarina pests, and can be used for controlling insects and mites.
Dinotefuran (dinotefuran) is a nicotinic insecticide, which blocks normal conduction of the central nervous system of insects by selectively controlling nicotinic acetylcholinesterase receptors of the insect nervous system, thereby causing paralysis of pests and death. Dinotefuran has the characteristics of contact killing, stomach toxicity, strong root systemic property, high quick effect, long lasting period (3-4 weeks, 43 days of theoretical persistence), wide insecticidal spectrum and the like, has excellent control effect on pests with sucking mouth parts, shows high insecticidal activity at a very low dosage, and has the effect of permeating from the leaf surface to the leaf interior. Dinotefuran is mainly used for preventing and controlling aphids, leafhoppers, plant hoppers, thrips, whiteflies and resistant strains thereof on various crops such as wheat, rice, cotton, vegetables, fruit trees, tobacco leaves and the like, has high efficiency on coleoptera and diptera pests, and has high efficiency on sanitary pests such as cockroaches, termites, houseflies and the like.
Bifenthrin preparations mainly use missible oil as a main component, and a large amount of organic solvents are used, so that the problems of environmental pollution and transportation safety exist; however, dinotefuran is mainly water-soluble granules, and the drug effect is poor in the using process. Moreover, along with the gradual increase of the resistance of pests, the effect of the single pesticide on pest control is gradually reduced, the environmental pollution is aggravated by increasing the application times and the application frequency, and the defects can be effectively overcome by compounding the active ingredients with different action mechanisms. The synergistic effect generated by mixing the two active components can improve the control effect, expand the insecticidal spectrum, delay the generation of the drug resistance of pests and reduce the environmental pollution, and is an important means for comprehensively controlling the pests.
Disclosure of Invention
The invention aims to provide a dinotefuran/bifenthrin insecticidal composition, which is prepared by compounding two active pharmaceutical ingredients of dinotefuran and bifenthrin according to a specific ratio to generate a good synergistic effect, expands an insecticidal spectrum, slows down the generation of drug resistance, overcomes the defects of drug effect reduction and drug resistance generation during single-component insecticidal process, and is beneficial to the sustainable development of the environment.
The invention also aims to provide the application of the insecticidal composition in controlling the insect pests of grain crops such as soybean, vegetables and fruit trees, the preparation process of the insecticidal composition is environment-friendly and safe, the pollution problem is avoided, the insecticidal spectrum is wide, the insecticidal effect is good, and the insecticidal composition has better use experience compared with a single drug active ingredient preparation.
Through research and experiments, the inventor compounds dinotefuran and bifenthrin, improves the insecticidal effect, reduces the generation of drug resistance, and obtains the dispersible oil suspending agent and wettable powder of dinotefuran and bifenthrin with excellent performance through the selection of an auxiliary agent. The specific technical scheme of the invention is as follows:
the pesticide composition comprises dinotefuran and bifenthrin as active pharmaceutical ingredients, wherein the mass ratio of the dinotefuran to the bifenthrin is 1-20: 1.
Furthermore, the dinotefuran and bifenthrin have stronger synergistic effect and better insecticidal effect when the mass ratio of the dinotefuran to the bifenthrin is 1-10: 1. More preferably, the mass ratio of dinotefuran to bifenthrin is 1-5:1, more preferably 4: 1.
Furthermore, the insecticidal composition also comprises an auxiliary agent besides the medicinal active ingredient, and the content of the medicinal active ingredient in the insecticidal composition is 10-60 wt%, preferably 20-55 wt%.
Further, the above-mentioned pesticidal composition may be formulated into any agriculturally acceptable practical dosage forms, for example, dispersible oil suspensions, wettable powders, according to methods known to those skilled in the art. When the composition is prepared into different dosage forms, the used auxiliary agents are different, and the content of the medicinal active ingredients of different dosage forms can also be different. Wherein, the research and the selection of the auxiliary agent can improve the performance and the using effect of each preparation.
Furthermore, according to the characteristics of the active ingredients of the medicines, the invention researches and screens the formulas of dispersible oil suspending agents and wettable powder of the two active ingredients of the medicines to obtain a preferable dispersible oil suspending agent dosage form and a preferable wettable powder dosage form, and the obtained dosage form has excellent performance. Dinotefuran has high water solubility (39.8g/L), bifenthrin has high molecular weight and low melting point, and the problems of creaming and severe oil bleeding are easy to occur in sanding and hot storage processes when the dispersible oil suspending agent is processed. According to the invention, the coating and dispersion of the original drug particles are improved by selecting the dispersing agent, the original drug particles are prevented from being coagulated, and the oil phase structure is stabilized by selecting the emulsifying agent and the structure stabilizing agent, so that the oil precipitation and creaming are prevented; when dinotefuran and bifenthrin are processed into wettable powder, the low-melting-point raw pesticide is easy to melt and agglomerate raw pesticide particles in the thermal storage process, so that the suspension rate and fineness are reduced, the material is agglomerated and the like.
Further, the preferable dispersible oil suspending agent of the invention comprises the following components in percentage by weight: 10-40% of active pharmaceutical ingredients, 2-5% of dispersing agents, 15.0-25.0% of emulsifying agents, 1-5% of structure stabilizing agents and the balance of oil solvents. The emulsifier, the dispersant, the structure stabilizer and the oil solvent are collectively called as assistants, the emulsifier can enable a liquid oil phase in the dispersible oil suspending agent to be rapidly emulsified and dispersed after being diluted by water, the dispersant can enable dispersed ions to be kept in a single state and eliminate aggregation and agglomeration, the structure stabilizer can enable a product to obtain a long-term stable suspension state, prolong the suspension time of solid particles such as effective components in the oil phase and prevent the solid particles from generating precipitation and agglomeration during storage or environmental change, and the oil solvent is used as a non-aqueous medium to enable the active components to be dispersed in the oil solvent.
Preferably, the dispersible oil suspending agent consists of the following components in percentage by weight: 10-40% of active pharmaceutical ingredients, 2.5-3.5% of dispersing agents, 21.0-25.0% of emulsifying agents, 2.0-2.5% of structure stabilizing agents and the balance of oil solvents.
More preferably, the dispersible oil suspending agent consists of the following components in percentage by weight: 20-30% of active ingredients of the medicine, 3.0-3.5% of dispersing agent, 21.0-25.0% of emulsifying agent, 2.0-2.5% of structure stabilizer and the balance of oil solvent.
Further, in the above dispersible oil suspension, the dispersant is one or more of sodium lignosulfonate, maleic acid-acrylic acid copolymer salt, polycarboxylic acid ammonium salt, polyoxyethylene-polyoxypropylene block copolymer, sodium alkylphenol sulfonate, alkyl naphthalene sulfonic acid formaldehyde condensate sodium salt, ethylene oxide-propylene oxide block copolymer and polycarboxylic acid sodium salt, and is preferably formed by mixing alkyl naphthalene sulfonic acid formaldehyde condensate sodium salt and polycarboxylic acid ammonium salt in a mass ratio of 1: 2-4. In the present invention, the ammonium/sodium salts of polycarboxylic acids used are mainly ammonium/sodium salts of polyacrylic acids.
Further, in the dispersible oil suspension agent, the emulsifier is one or more of polyoxyethylene polyoxypropylene block copolymer, fatty alcohol polyoxyethylene ether, polyoxyethylene alkyl ester, alkylphenol polyoxyethylene ether, sorbitol polyoxyethylene ether, sorbitan polyoxyethylene ether, alkylphenol formaldehyde condensate polyoxyethylene ether, calcium dodecyl benzene sulfonate, castor oil polyoxyethylene ether and sodium fatty alcohol polyoxyethylene ether sulfosuccinate, and is preferably formed by mixing calcium dodecyl benzene sulfonate, lauryl alcohol polyoxyethylene ether and castor oil polyoxyethylene ether according to the mass ratio of 3-5:1-2: 1.
Further, in the dispersible oil suspending agent, the structure stabilizer is one or more of white carbon black, organic bentonite, xanthan gum, magnesium aluminum silicate and carboxymethyl cellulose, and is preferably formed by mixing the white carbon black and the organic bentonite according to the mass ratio of 1-2: 1.
Further, in the dispersible oil suspension agent, the oil solvent is one or more of soybean oil, methyl esterified soybean oil, methyl oleate, solvent oil 150#, and solvent oil 200#, preferably a mixture of solvent oil 150#, solvent oil 200#, and methyl oleate, more preferably, the content of solvent oil 150# is 2-3%, the content of solvent oil 200# is 7-8%, and the balance is methyl oleate.
The dispersible oil suspending agent can be prepared by the following method: taking part of the oil solvent, adding the medicinal active ingredient, the dispersing agent and the emulsifying agent into the oil solvent, mixing and stirring, stirring and shearing for 30-40 minutes at the rotating speed of 1000-2000 rpm of a high-speed shearing machine, uniformly mixing, grinding by a sand mill until D90 is less than 8 mu m, adding the rest oil solvent to rinse the sand mill, merging the rinsed oil solvent into the sanded material, adding the structure stabilizing agent into the material, and shearing for 30-40 minutes to obtain the dinotefuran-bifenthrin dispersible oil suspending agent.
Furthermore, the preferable wettable powder of the invention consists of the following components in percentage by weight: 10 to 60 percent of active ingredients of the medicine, 2.0 to 6.0 percent of dispersant, 2.0 to 4.0 percent of wetting agent, 5.0 to 10.0 percent of anti-caking agent and the balance of filler. Wherein, dispersant, wetting agent, anticaking agent, filler are referred to as assistant, the function of dispersant is to prevent the active ingredient fine particles of the medicament from aggregating each other, make it keep dispersing evenly in forming liquid-solid dispersion system with water for a longer time, the function of wetting agent is to reduce the liquid-solid surface tension of the fine particles in water, increase the ability of being wetted by water, the function of anticaking agent is to prevent the powder from agglomerating in the course of storing for a long time, the function of filler is to load or dilute the active ingredient of the medicament, adjust the content of the product to reach the standard.
Preferably, the wettable powder comprises the following components in percentage by weight: 10-60% of active ingredients of the medicine, 2.5% of dispersing agent, 2.5% of wetting agent, 7.0% of anti-caking agent and the balance of filler.
More preferably, the wettable powder comprises the following components in percentage by weight: 45-55% of active ingredients of the medicine, 2.5% of dispersing agent, 2.5% of wetting agent, 7.0% of anti-caking agent and the balance of filler.
Further, in the wettable powder, the dispersant is one or more of sodium lignosulfonate, maleic acid-acrylic acid copolymer salt, polyoxyethylene-polyoxypropylene block copolymer, sodium alkylphenol sulfonate, sodium alkylnaphthalenesulfonic acid-formaldehyde condensate, sodium naphthalenesulfonic acid-formaldehyde condensate, sodium alkylpolyoxyethylene ether sulfate, ethylene oxide-propylene oxide block copolymer and sodium polycarboxylate, and is preferably a mixture of sodium alkylpolyoxyethylene ether sulfate and sodium naphthalenesulfonic acid-formaldehyde condensate in a mass ratio of 1.0-1.5: 1.0. In the present invention, the sodium salt of polycarboxylic acid used is mainly sodium salt of polyacrylic acid. The alkyl group of the sodium alkyl polyoxyethylene ether sulfate is C8-C12 alkyl group.
Furthermore, in the wettable powder, the wetting agent is one or more of sodium dodecyl sulfate, a-sulfo fatty acid methyl ester, sodium tetradecyl sulfate, sodium dodecyl benzene sulfonate, sodium alkyl naphthalene sulfonate, sodium a-olefin sulfonate, sodium alkylphenol polyoxyethylene ether sulfate, sodium diisobutyl naphthalene sulfonate, fatty acid sulfate and fatty acid ester sulfate, and preferably, the wettable powder is prepared by mixing the sodium diisobutyl naphthalene sulfonate and the sodium dodecyl sulfonate according to the mass ratio of 1.0-1.5: 1.0.
Further, in the wettable powder, the anti-caking agent is one or more of microcrystalline cellulose, tricalcium phosphate, sodium aluminosilicate and white carbon black, and preferably white carbon black.
Further, in the wettable powder, the filler is one or more of potassium sulfate, potassium chloride, diammonium hydrogen phosphate, urea, anhydrous sodium sulfate, ammonium sulfate, kaolin, bentonite, talcum powder, attapulgite, diatomite, starch and light calcium carbonate, preferably a mixture of kaolin and anhydrous sodium sulfate, more preferably, the content of kaolin is 10-15%, and the balance of anhydrous sodium sulfate is added.
The wettable powder can be prepared by the following method: evenly mixing dinotefuran, bifenthrin, a dispersant, a wetting agent, an anti-blocking agent and a filler in a mixer, crushing the mixture to 20-30 mu m by an airflow crusher, carrying out secondary mixing, and evenly mixing to obtain the dinotefuran-bifenthrin wettable powder.
The dinotefuran and bifenthrin are compounded, so that the insecticidal composition shows a more outstanding insecticidal effect on the basis of keeping the original insecticidal spectrum, is mainly used for controlling insect pests in grain crops such as soybean, vegetables and fruit trees, and can be hemiptera, lepidoptera and homoptera pests such as stinkbug, aphid, whitefly, cabbage caterpillar and the like.
The invention has the beneficial effects that:
1. the dinotefuran and bifenthrin as the active pharmaceutical ingredients of the insecticidal composition belong to two insecticides with different action mechanisms, and the two insecticides are mixed without conflict, so that the insecticidal spectrum is expanded, the quick action and the lasting effect are improved, and the insecticidal efficiency is improved.
2. The insecticidal composition has good synergistic effect in a certain mass ratio, the control effect is higher than that of a single agent, the dosage is small, the drug resistance of insect pests is delayed, and the environmental sustainable development is facilitated.
3. The insecticidal composition can be prepared into dispersible oil suspending agent and wettable powder, and the obtained dosage form has excellent performance and improved drug effect through the selection of the auxiliary agent.
4. The insecticidal composition has special effects on hemipteran, lepidopteran and homopteran pests such as stinkbugs, aphids, whiteflies and cabbage caterpillars on grain crops such as soybeans, vegetables and fruit trees.
Detailed Description
The following specific examples are given to illustrate the technical aspects of the present invention in detail, but the present invention is not limited to these examples. Unless otherwise specified, the following components are contained in weight percent.
The embodiment of the invention adopts a method combining indoor toxicity measurement and field test. Firstly, indoor toxicity measurement is carried out according to the Sun Yunpei method, the cotoxicity coefficient (CTC) of the two medicaments compounded according to a certain proportion is determined, the CTC is less than 80 and is antagonistic, the CTC is more than or equal to 80 and is less than or equal to 120 and is additive, and the CTC is more than 120 and is synergistic, and then field tests are carried out on the basis.
Method for determining indoor toxicity of aphids compounded and paired by dinotefuran and bifenthrin
After the effective inhibition concentration range of each medicament is determined through pre-test, each medicament is respectively treated with a series of concentrations according to the content of effective components, and clear water is used for comparison. The method is carried out according to the standard pesticide for indoor bioassay of pesticides, the lethal medium concentration of the pesticide and the mixed pesticide is measured by adopting an immersion method, and the cotoxicity coefficient is obtained by a method for calculating the combined toxicity provided by Sun Yunpei et al (1960).
The calculation formula is as follows (with dinotefuran as a standard medicament and the virulence index of 100):
LC of bifenthrin with Toxicity Index (TI) of dinotefuran50LC of bifenthrin50×100
LC of actual virulence index (ATI) ═ dinotefuran of M50LC of/M50×100
Theoretical virulence index (TTI) of M-TI XP of dinotefuranDinotefuran+ TI XP of bifenthrinBiphenthrin
Co-toxicity coefficient (CTC) of M-TTI × 100 of ATI/M
In the formula: m is a mixture of dinotefuran and bifenthrin in different proportions;
PdinotefuranIs the proportion of dinotefuran in the compound composition;
PbiphenthrinIs the proportion of bifenthrin in the compound composition.
The test results are shown in table 1:
TABLE 1 toxicity assay results for dinotefuran, bifenthrin and their combined aphids
As shown in Table 1, LC of dinotefuran and bifenthrin against aphids50Are respectively 1.5178mg/L and 0.5021 mg/L. The mass ratio of dinotefuran to bifenthrin is 1:1, 2:1, 4:1, 10:1 and 20:1, the co-toxicity coefficients are respectively 126.84, 130.56, 168.40, 126.65 and 120.43 which are all larger than 120, the dinotefuran and bifenthrin have synergistic effect, and no synergistic effect is generated when the mass ratio exceeds 20: 1. Therefore, the dinotefuran/bifenthrin composite has a good effect when the mass ratio of the dinotefuran to the bifenthrin is 1-20:1, wherein the synergistic effect is obvious when the mass ratio is 1-10:1, and the synergistic effect is the highest when the mass ratio is 4: 1.
After determining the mass ratio of the pharmaceutically active ingredients, the pharmaceutically active ingredients are prepared into wettable powders and dispersible oil suspensions by using appropriate auxiliaries, and a few representative examples are specifically listed below, which are not exhaustive.
Example 110% dinotefuran bifenthrin wettable powder
The formula is as follows: 5 percent of dinotefuran, 5 percent of bifenthrin, 1.25 percent of dispersant alkyl polyoxyethylene ether sodium sulfate, 1.25 percent of naphthalenesulfonic acid formaldehyde condensate sodium salt, 1.5 percent of wetting agent diisobutyl naphthalene sulfonate, 1.0 percent of sodium dodecyl sulfate, 7 percent of anti-caking agent white carbon black, 15 percent of filler kaolin and 100 percent of anhydrous sodium sulfate.
The preparation method comprises the following steps: evenly mixing dinotefuran, bifenthrin, a dispersant, a wetting agent, an anti-blocking agent and a filler in a mixer, crushing the mixture to 20-30 mu m by an airflow crusher, carrying out secondary mixing, and evenly mixing to obtain the dinotefuran-bifenthrin wettable powder.
Example 230% dinotefuran bifenthrin wettable powder
The formula is as follows: 20% of dinotefuran, 10% of bifenthrin, 1.25% of dispersant alkyl polyoxyethylene ether sodium sulfate, 1.25% of naphthalenesulfonic acid formaldehyde condensate sodium salt, 1.25% of wetting agent diisobutyl naphthalene sulfonate, 1.25% of sodium dodecyl sulfate, 7% of anti-caking agent white carbon black, 15% of filler kaolin and 100% of anhydrous sodium sulfate. The preparation method is the same as example 1.
EXAMPLE 345% dinotefuran bifenthrin wettable powder
The formula is as follows: 36% of dinotefuran, 9% of bifenthrin, 1.5% of dispersant alkyl polyoxyethylene ether sodium sulfate, 1.0% of naphthalenesulfonic acid formaldehyde condensate sodium salt, 1.25% of wetting agent diisobutyl naphthalene sulfonate, 1.25% of sodium dodecyl sulfate, 7% of anti-caking agent white carbon black, 15% of filler kaolin and 100% of anhydrous sodium sulfate. The preparation method is the same as example 1.
EXAMPLE 450% dinotefuran bifenthrin wettable powder
The formula is as follows: 40% of dinotefuran, 10% of bifenthrin, 1.5% of dispersant alkyl polyoxyethylene ether sodium sulfate, 1.0% of naphthalenesulfonic acid formaldehyde condensate sodium salt, 1.5% of wetting agent diisobutyl naphthalene sulfonate, 1.0% of sodium dodecyl sulfate, 7% of anti-caking agent white carbon black, 15% of filler kaolin and 100% of anhydrous sodium sulfate. The preparation method is the same as example 1.
Example 560% dinotefuran bifenthrin wettable powder
The formula is as follows: 54.5 percent of dinotefuran, 5.5 percent of bifenthrin, 1.5 percent of dispersant alkyl polyoxyethylene ether sodium sulfate, 1.0 percent of naphthalenesulfonic acid formaldehyde condensate sodium salt, 1.5 percent of wetting agent diisobutyl naphthalene sulfonate, 1.0 percent of sodium dodecyl sulfate, 7 percent of anti-caking agent white carbon black, 10 percent of filler kaolin and 100 percent of anhydrous sodium sulfate. The preparation method is the same as example 1.
Example 610% dinotefuran bifenthrin wettable powder
The formula is as follows: the preparation method is the same as that of example 1 when the dinotefuran is 5%, the bifenthrin is 5%, the sodium salt of the naphthalene sulfonic acid formaldehyde condensate serving as the dispersant is 6.0%, the wetting agent sodium dodecyl sulfate is 2.5%, the anti-blocking agent white carbon black is 5%, the microcrystalline cellulose is 5%, the filler talcum powder is 10%, and the anhydrous sodium sulfate is added to 100%.
EXAMPLE 730% dinotefuran bifenthrin wettable powder
The formula is as follows: 20.0 percent of dinotefuran, 10.0 percent of bifenthrin, 2 percent of dispersant sodium polyacrylate, 2 percent of sodium lignosulfonate, 1 percent of wetting agent sodium dodecyl sulfate, 1 percent of sodium dodecyl benzene sulfonate, 5 percent of anti-caking agent sodium aluminosilicate, 5 percent of white carbon black, 35 percent of filler ammonium sulfate and 100 percent of diatomite. The preparation method is the same as example 1.
EXAMPLE 845% dinotefuran bifenthrin wettable powder
The formula is as follows: 36 percent of dinotefuran, 9 percent of bifenthrin, 1.5 percent of dispersant polyoxyethylene-polyoxypropylene segmented copolymer, 1.5 percent of alkyl naphthalene sulfonic acid formaldehyde condensate sodium salt, 2.5 percent of wetting agent diisobutyl naphthalene sulfonic acid sodium salt, 10 percent of anti-caking agent white carbon black, 15 percent of filler attapulgite and 100 percent of potassium sulfate. The preparation method is the same as example 1.
EXAMPLE 950% dinotefuran bifenthrin wettable powder
The formula is as follows: 40% of dinotefuran, 10% of bifenthrin, 1.0% of sodium salt of maleic acid-acrylic acid copolymer serving as a dispersant, 1.0% of sodium alkyl polyoxyethylene ether sulfate, 1.5% of sodium a-olefin sulfonate serving as a wetting agent, 1.5% of sodium sulfate of fatty acid, 5% of tricalcium phosphate serving as an anti-blocking agent, 5% of white carbon black, 30% of diammonium hydrogen phosphate serving as a filler and 100% of bentonite. The preparation method is the same as example 1.
EXAMPLE 1060% dinotefuran bifenthrin wettable powder
The formula is as follows: 54.5 percent of dinotefuran, 5.5 percent of bifenthrin, 2.0 percent of dispersant ethylene oxide-propylene oxide block copolymer, 1.5 percent of wetting agent a-sulfo fatty acid methyl ester, 1 percent of alkylphenol polyoxyethylene ether sodium sulfate, 5 percent of anti-caking agent white carbon black, 20 percent of filler urea and 100 percent of light calcium carbonate. The preparation method is the same as example 1.
Example 1110% dinotefuran bifenthrin dispersible oil suspension
The formula is as follows: 5% of dinotefuran, 5% of bifenthrin, 0.5% of dispersant alkyl naphthalene sulfonic acid formaldehyde condensate sodium salt, 2.0% of polyacrylic ammonium salt, 15.0% of emulsifier dodecyl benzene sulfonic acid calcium salt, 3.0% of lauryl alcohol polyoxyethylene ether, 3.0% of castor oil polyoxyethylene ether, 1.0% of structure stabilizer white carbon black HTB-260B, 1.0% of organic bentonite, 2.0% of oil solvent oil 150#2, 7.0% of solvent oil 200# and 100% of methyl oleate.
The preparation method comprises the following steps: adding the original drug, the emulsifier and the dispersant into the oil solvent, mixing, stirring and shearing for 30-40 minutes at the rotating speed of 1000-2000 rpm of a high-speed shearing machine, uniformly mixing, grinding by a sand mill until D90 is less than 8 mu m, adding the rest oil solvent to rinse the sand mill, transferring into a sanded preparation, adding the structure stabilizer, and shearing for 30-40 minutes to obtain the dinotefuran/bifenthrin dispersible oil suspending agent product.
Example 1218% dinotefuran bifenthrin dispersible oil suspension
The formula is as follows: 12% of dinotefuran, 6% of bifenthrin, 0.6% of sodium alkyl naphthalene sulfonate formaldehyde condensate as a dispersant, 2.4% of ammonium polyacrylate, 15.0% of calcium dodecyl benzene sulfonate as an emulsifier, 4.0% of lauryl alcohol polyoxyethylene ether, 4.0% of castor oil polyoxyethylene ether, 1.6% of white carbon black HTB-260B as a structure stabilizer, 0.8% of organic bentonite, 2.0% of oil solvent oil 150#2, 8.0% of solvent oil 200#8, and 100% of methyl oleate. The preparation method is the same as example 11.
Example 1326% dinotefuran bifenthrin dispersible oil suspension
The formula is as follows: 20.8% of dinotefuran, 5.2% of bifenthrin, 1.0% of sodium alkyl naphthalene sulfonic acid formaldehyde condensate serving as a dispersant, 2.3% of polyacrylic ammonium salt, 15.5% of calcium dodecyl benzene sulfonate serving as an emulsifier, 4.5% of lauryl alcohol polyoxyethylene ether, 4.0% of castor oil polyoxyethylene ether, 1.6% of white carbon black HTB-260B serving as a structure stabilizer, 0.8% of organic bentonite, 2.5% of oil-solvent oil 150#, 8.0% of solvent oil 200#, and the total amount of methyl oleate to 100%. The preparation method is the same as example 11.
Example 1430% dinotefuran bifenthrin dispersible oil suspension
24% of dinotefuran, 6% of bifenthrin, 0.7% of dispersant alkyl naphthalene sulfonic acid formaldehyde condensate sodium salt, 2.8% of polyacrylic ammonium salt, 15.0% of emulsifier dodecyl benzene sulfonic acid calcium salt, 5.0% of lauryl alcohol polyoxyethylene ether, 5.0% of castor oil polyoxyethylene ether, 1.5% of structure stabilizer white carbon black HTB-260B, 1.0% of organic bentonite, 3.0% of oil solvent oil 150#, 8.0% of solvent oil 200#, and 100% of methyl oleate. The preparation method is the same as example 11. The preparation method is the same as example 11.
Example 1540% dinotefuran bifenthrin dispersible oil suspension
36.4% of dinotefuran, 3.6% of bifenthrin, 1.0% of dispersant alkyl naphthalene sulfonic acid formaldehyde condensate sodium salt, 2.5% of polyacrylic ammonium salt, 16.0% of emulsifier dodecyl benzene sulfonic acid calcium salt, 5.0% of lauryl alcohol polyoxyethylene ether, 4.0% of castor oil polyoxyethylene ether, 1.5% of structure stabilizer white carbon black HTB-260B, 1.0% of organic bentonite, 3.0% of oil solvent oil 150#, 8.0% of solvent oil 200#, and the total amount of methyl oleate to 100%. The preparation method is the same as example 11.
Example 1610% dinotefuran bifenthrin dispersible oil suspension
5% of dinotefuran, 5% of bifenthrin, 0.6% of dispersant alkyl naphthalene sulfonic acid formaldehyde condensate sodium salt, 1.4% of polyacrylic acid sodium salt, 9% of emulsifier dodecyl benzene sulfonic acid calcium salt, 3.0% of fatty alcohol polyoxyethylene ether AEO-93.0% of alkylphenol formaldehyde condensate polyoxyethylene ether, 1.0% of structure stabilizer xanthan gum, 5.0% of oil solvent oil 150#, 5.0% of solvent oil 200#, and 100% of methyl esterified soybean oil. The preparation method is the same as example 11.
Example 1718% dinotefuran bifenthrin dispersible oil suspension
12.0 percent of dinotefuran, 6.0 percent of bifenthrin, 1.0 percent of dispersant maleic acid-acrylic acid copolymer salt, 1.5 percent of ethylene oxide-propylene oxide block copolymer, 12.0 percent of emulsifier calcium dodecyl benzene sulfonate, 4.0 percent of fatty alcohol polyoxyethylene ether sodium sulfosuccinate, 4.0 percent of alkylphenol polyoxyethylene, 1.5 percent of white carbon black HTB-260B as a structure stabilizer, 2.3 percent of oil solvent oil 150, 8.0 percent of solvent oil 200 and 100 percent of soybean oil. The preparation method is the same as example 11.
Example 1826% dinotefuran bifenthrin dispersible oil suspension
The formula is as follows: 20.8% of dinotefuran, 5.2% of bifenthrin, 2.0% of sodium alkylphenol sulfonate serving as a dispersant, 2.0% of ammonium polyacrylate, 15.0% of polyoxyethylene polyoxypropylene block copolymer serving as an emulsifier, 5.0% of polyoxyethylene sorbitol, 4.0% of polyoxyethylene castor oil, 1.0% of white carbon black HTB-260B serving as a structure stabilizer, 1.0% of magnesium aluminum silicate, 2.0% of solvent oil 150# serving as an oil solvent, 8.0% of methyl esterified soybean oil and 100% of methyl oleate. The preparation method is the same as example 11.
Example 1933% dinotefuran bifenthrin dispersible oil suspension
The formula is as follows: 30.0 percent of dinotefuran, 3.0 percent of bifenthrin, 2.0 percent of dispersant sodium lignosulfonate, 2.5 percent of polyacrylic ammonium salt, 15.8 percent of emulsifier calcium dodecyl benzene sulfonate, 4.6 percent of alkylphenol formaldehyde condensation product polyoxyethylene ether, 4.0 percent of castor oil polyoxyethylene ether, 1.5 percent of white carbon black HTB-260B as a structure stabilizer, 2.0 percent of xanthan gum, 10.0 percent of oil solvent methyl esterified soybean oil and 100 percent of methyl oleate. The preparation method is the same as example 11.
Example 2040% dinotefuran bifenthrin dispersible oil suspension
The formula is as follows: 38.1% of dinotefuran, 1.9% of bifenthrin, 2.5% of a dispersant polyoxyethylene-polyoxypropylene block copolymer, 2.5% of a polyacrylic ammonium salt, 16.0% of emulsifier calcium dodecyl benzene sulfonate, 5.0% of alkylphenol formaldehyde condensate polyoxyethylene ether, 4.0% of castor oil polyoxyethylene ether, 2.5% of a structure stabilizer white carbon black HTB-260B, 2.5% of carboxymethyl cellulose, 10.0% of an oil solvent oil 150# and 100% of methyl esterified soybean oil. The preparation method is the same as example 11.
Comparative example 150% dinotefuran bifenthrin wettable powder
The formula is as follows: 40% of dinotefuran, 10% of bifenthrin, 0.5% of dispersant sodium lignosulfonate, 2% of dioctyl sodium sulfosuccinate, 1.5% of wetting agent alkylphenol polyoxyethylene formaldehyde condensate succinic acid half ester sulfonic acid sodium salt, 1% of lauryl alcohol ether sodium sulfate, 7% of anti-caking agent white carbon black, 15% of filler anhydrous sodium sulfate and 100% of argil. The preparation method is the same as example 1.
Comparative example 226% dinotefuran bifenthrin dispersible oil suspending agent
The formula is as follows: 20.8% of dinotefuran, 5.2% of bifenthrin, 1.0% of a dispersant styrene acrylic copolymer, 2.3% of fatty alcohol polyoxyethylene ether phosphate, 15.5% of an emulsifier dodecyl benzene sulfonic acid isopropyl ammonium salt, 4.5% of fatty acid polyoxyethylene ester, 4.0% of alkylphenol polyoxyethylene polyoxypropylene ether, 1.6% of structure stabilizer fumed silica, 0.8% of organic bentonite, 150# 2.5% of oil solvent oil, 200# 8.0% of solvent oil and methyl oleate added to 100%. The preparation method is the same as example 11.
The quality stability of the dinotefuran and bifenthrin compound preparation products prepared in the above examples and comparative examples is tested.
Wherein, the method for detecting the fineness of the wettable powder is CIPAC MT185, the method for detecting the suspension percentage is CIPAC MT15.1, and the method for detecting the heat storage stability is CIPAC MT 46.3. The suspension rate detection method of the dispersible oil suspending agent is CIPAC MT184, and the heat storage stability detection method is CIPAC MT 46.3.
The detection results of dinotefuran and bifenthrin wettable powder are shown in the following table 2.
TABLE 2 quality of the wettable powder product prepared by compounding dinotefuran and bifenthrin
As can be seen from table 2 above, the suspension percentage of the wettable powder obtained in the embodiment of the present invention can reach over 84%, and the fineness can reach over 99.5%. The quality after hot storage remained stable and was superior to that of comparative example 1. The wettable powders of examples 1 to 5, in which the preferred adjuvant was used, performed better. Dinotefuran in the active ingredient can be dissolved in water, and only bifenthrin and a part of water-insoluble filler need to be dispersed and suspended, so that the suspension rate in each example is higher compared with each other. In the comparative example, the performance of the auxiliary agent is poor, and the proportion of the water-insoluble filler is high, so that the suspension rate and the fineness are poor.
Furthermore, from examples 1 to 5, in the case of selecting the preferred adjuvant, there were also differences in the performance of the resulting wettable powder products when the content of the pharmaceutically active ingredient was varied within the range of 10 to 60%, which indicates that the content of the drug has some influence on the dosage form performance. As can be seen from examples 6-10, in the case of the conventional adjuvant, the performance of the obtained wettable powder is relatively reduced, and the replacement of the adjuvant has no significant effect improvement, which shows that the components and contents of the preferred adjuvant have significant effect of improving the performance of the wettable powder, while the conventional adjuvant does not.
The detection results of the dinotefuran and bifenthrin dispersible oil suspending agent are shown in the following table 3.
TABLE 3 quality of dispersible oil suspension prepared by compounding dinotefuran and bifenthrin
From the above table 3, it can be seen that the suspension percentage of the dispersible oil suspending agent obtained in the embodiment of the present invention can reach more than 80%, the appearance of the dispersible oil suspending agent is uniformly fluid, the suspension percentage after thermal storage is stable, the individual appearance has slight oil separation, the quality requirements are still met, and the suspension percentage is superior to that of the comparative example 1. The dispersible oil suspensions of examples 11-15, in which the preferred adjuvants were used, performed better.
Furthermore, from examples 11 to 15, it can be seen that, in the case of selecting the preferred adjuvant, the dispersible oil suspension products obtained when the content of the pharmaceutically active ingredient is varied within the range of 10 to 40% also have variations in properties, which indicates that the content of the drug has some influence on the properties of the dosage form. It can be seen from examples 16-20 that in the case of the conventional adjuvant, the performance of the resulting dispersible oil suspension concentrate is relatively reduced, and there is no significant effect improvement in replacing the adjuvant, which indicates that the ingredients and contents of the preferred adjuvant provide significant improvements in the performance of the dispersible oil suspension concentrate, while the conventional adjuvant does not.
Dinotefuran and bifenthrin compound field pesticide effect test determination
1. Field test for preventing and controlling soybean aphids
And performing pesticide effect tests on the prevention and treatment of the aphid in the soybean field by the dinotefuran and bifenthrin compound preparation prepared in the embodiment and the comparative example. The experimental arrangement was conducted locally at the Weifang, and the control agents were 20% dinotefuran SG (commercially available) and 40% bifenthrin EC (commercially available).
When the pesticide is applied, 25 soybean fields are selected for testing at the early stage of aphid outbreak, wherein one soybean field is selected as a blank control area, the control area is clear water spray without spraying a pesticide, and the other test fields are pesticide treatment areas and are sprayed with different preparations. The application method comprises the following steps: the preparation dosage per hectare is mixed with 150kg of water to prepare liquid medicine, and the liquid medicine is evenly sprayed according to the conversion of the liquid medicine amount in the residential area. The weather is good during the test period, and the daily average temperature is 20-26.0 ℃. No rain is produced on the day of application, and no rain is produced 15 days after application.
Investigation method
Investigating population base before applying pesticide, investigating live insect quantity in 3 rd, 7 th and 14 th days after pesticide application, calculating, correcting and preventing effect, and observing the safety of the test pesticide on crops.
Drug effect calculation method
In the experimental process, the composition of the invention has no adverse effect on soybean in the range of experimental application, and the control results on soybean field aphids are shown in table 4:
TABLE 4 field efficacy test results of treatment agents for controlling soybean aphids
As can be seen from Table 4, after the dinotefuran and the bifenthrin are compounded, soybean aphids can be effectively controlled, and the control effect is superior to that of a control medicament and is also superior to that of a comparative example. The control effect of the embodiment using the preferable auxiliary agent and the preferable proportion is more than 80 percent in other embodiments, and the control effect on soybean aphids is more than 14 days after the pesticide is applied.
2. Cabbage caterpillar control field experiment
And performing pesticide effect tests on the prevention and treatment of the aphid in the soybean field by the dinotefuran and bifenthrin compound preparation prepared in the embodiment and the comparative example. The experiment was conducted in the sunlight, and the control agent was 20% dinotefuran SG (commercially available) and 40% bifenthrin EC (commercially available).
When the pesticide is applied, 25 cabbage fields are selected for testing at the initial stage of the full-fleshed cabbage caterpillars, wherein one cabbage field is selected as a blank control area, the control area is sprayed with clear water without spraying a pesticide, and the other test fields are pesticide treatment areas and sprayed with different preparations. The application method comprises the following steps: the preparation dosage per hectare is mixed with 150kg of water to prepare liquid medicine, and the liquid medicine is evenly sprayed according to the conversion of the liquid medicine amount in the residential area. The weather is good during the test period, and the daily average temperature is 20-26.0 ℃. No rain is produced on the day of application, and no rain is produced 15 days after application.
Investigation method
Investigating population base before applying pesticide, investigating live insect quantity in 3 rd, 7 th and 14 th days after pesticide application, calculating, correcting and preventing effect, and observing the safety of the test pesticide on crops.
Drug effect calculation method
In the experimental process, the composition of the invention has no adverse effect on cabbage in the application range of the experiment, and the control results on cabbage caterpillar are shown in table 5:
TABLE 5 field efficacy test results of treatment agents for cabbage field cabbage caterpillar control
As can be seen from Table 5, after the dinotefuran and the bifenthrin are compounded, cabbage field cabbage caterpillar can be effectively controlled, and the control effect is superior to that of a control medicament and is also superior to that of a comparative example. The control effect on cabbage caterpillar is more than 80% 14 days after the pesticide is applied, the control effect of the embodiment using the preferred auxiliary agent and the preferred proportion is better than that of other embodiments, and the control effect can be more than 90%.
Claims (8)
1. An insecticidal composition characterized by: the active ingredients of the medicine are dinotefuran and bifenthrin, the mass ratio of the dinotefuran to the bifenthrin is 1-20:1, and the preparation is dispersible oil suspending agent or wettable powder;
when the preparation form is dispersible oil suspending agent, the dispersible oil suspending agent consists of the following components in percentage by weight: 10-40% of a medicinal active ingredient, 2-5% of a dispersing agent, 15.0-25.0% of an emulsifying agent, 1-5% of a structure stabilizing agent and the balance of an oil solvent, wherein the dispersing agent is formed by mixing sodium alkyl naphthalene sulfonate formaldehyde condensate and ammonium polycarboxylate according to the mass ratio of 1:2-4, the emulsifying agent is formed by mixing calcium dodecyl benzene sulfonate, polyoxyethylene lauryl ether and polyoxyethylene castor oil according to the mass ratio of 3-5:1-2:1, the structure stabilizing agent is formed by mixing white carbon black and organic bentonite according to the mass ratio of 1-2:1, and the oil solvent is a mixture of solvent oil No. 150, solvent oil No. 200 and methyl oleate;
when the dosage form is wettable powder, the wettable powder comprises the following components in percentage by weight: 10-60% of medicinal active ingredients, 2.0-6.0% of a dispersing agent, 2.0-4.0% of a wetting agent, 5.0-10.0% of an anti-caking agent and the balance of a filler, wherein the dispersing agent is prepared by mixing sodium alkyl polyoxyethylene ether sulfate and sodium naphthalene sulfonate formaldehyde condensate according to the mass ratio of 1.0-1.5:1.0, the wetting agent is prepared by mixing sodium diisobutylnaphthalenesulfonate and sodium dodecyl sulfonate according to the mass ratio of 1.0-1.5:1.0, the anti-caking agent is white carbon black, and the filler is a mixture of kaolin and anhydrous sodium sulfate.
2. The insecticidal composition as claimed in claim 1, wherein: the mass ratio of the dinotefuran to the bifenthrin is 1-10: 1.
3. The insecticidal composition as claimed in claim 1, wherein: the mass ratio of the dinotefuran to the bifenthrin is 1-5: 1.
4. The insecticidal composition as claimed in claim 1, wherein: the mass ratio of the dinotefuran to the bifenthrin is 4: 1.
5. The insecticidal composition as claimed in claim 1, wherein: when the preparation form is dispersible oil suspending agent, the dispersible oil suspending agent consists of the following components in percentage by weight: 10-40% of active pharmaceutical ingredients, 2.5-3.5% of dispersing agents, 21.0-25.0% of emulsifying agents, 2.0-2.5% of structure stabilizing agents and the balance of oil solvents;
when the dosage form is wettable powder, the wettable powder comprises the following components in percentage by weight: 10-60% of active ingredients of the medicine, 2.5% of dispersing agent, 2.5% of wetting agent, 7.0% of anti-caking agent and the balance of filler.
6. The insecticidal composition as claimed in claim 1, wherein: when the preparation form is dispersible oil suspending agent, the dispersible oil suspending agent consists of the following components in percentage by weight: 20-30% of active ingredients of the medicine, 3.0-3.5% of dispersing agent, 21.0-25.0% of emulsifying agent, 2.0-2.5% of structure stabilizer and the balance of oil solvent;
when the dosage form is wettable powder, the wettable powder comprises the following components in percentage by weight: 45-55% of active pharmaceutical ingredients, 2.5% of dispersing agent, 2.5% of wetting agent, 7.0% of anti-caking agent and the balance of filler.
7. Use of the pesticidal composition of any one of claims 1-6 for controlling pests on food crops, vegetables or fruit trees, said pests being hemipteran, lepidopteran or homopteran pests.
8. Use according to claim 7, characterized in that: the insect pest is aphid, stinkbug, whitefly or cabbage caterpillar.
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| CN114631539A (en) * | 2020-12-15 | 2022-06-17 | 江苏扬农化工股份有限公司 | Low-content insecticidal nano preparation applied to household environment flowers and preparation method thereof |
| CN113558068A (en) * | 2021-07-26 | 2021-10-29 | 中诚国联（河南）生物科技有限公司 | Preparation method and application of pesticide-fertilizer granules containing dinotefuran and bifenthrin |
| CN115104620B (en) * | 2021-08-13 | 2023-08-11 | 山东恒利达生物科技有限公司 | Furannicotine insecticidal composition and application thereof |
| CN113841704A (en) * | 2021-10-28 | 2021-12-28 | 河北沃德丰药业有限公司 | Nanometer dry suspending agent of pymetrozine and dinotefuran and preparation method thereof |
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