CN111296422A

CN111296422A - Insecticidal composition containing diatomite with special shape and application thereof

Info

Publication number: CN111296422A
Application number: CN202010110384.8A
Authority: CN
Inventors: 刘永山
Original assignee: Guangxi Yicai Agricultural Development Co ltd
Current assignee: Guangxi Yicai Agricultural Development Co ltd
Priority date: 2020-02-24
Filing date: 2020-02-24
Publication date: 2020-06-19

Abstract

The invention relates to the technical field of pesticides, and particularly relates to an insecticidal composition containing diatomite in a special shape and application thereof. The preparation raw materials of the insecticidal composition comprise special-shaped diatomite and an active ingredient, wherein the special-shaped diatomite is saw-toothed, and the active ingredient is buprofezin or dinotefuran. The invention provides an insecticidal composition, which can increase insecticidal effect and insecticidal efficiency through the combined action of diatomite with a special saw-toothed shape and buprofezin or dinotefuran and the like, has obvious control effect on pests such as citrus red spiders, citrus scale insects, frankliniella occidentalis, trialeurodes vaporariorum, liriomyza, prodenia litura, tea lesser leafhopper, tea yellow thrips, tea geometrid, green plant bugs, grape aphids and the like, and is favorable for reducing the loss of the buprofezin or dinotefuran and the like after being washed by rainwater by using the saw-toothed diatomite.

Description

Insecticidal composition containing diatomite with special shape and application thereof

Technical Field

The invention relates to the technical field of pesticides, and particularly relates to an insecticidal composition containing diatomite in a special shape and application thereof.

Background

The physical disinsection by using the diatomite is also a safe and pollution-free method and is widely concerned. The advantages of good insect prevention and killing effect, long protection period, no toxicity to mammals, no environmental pollution and the like are achieved, the development direction of green stored grains is met, and the method is popular with many national pest control experts. The diatomite pesticide is a medicament prepared by processing food-grade diatomite which is specially processed as a main raw material and other raw materials such as a synergist and the like as auxiliary materials. The diatomite is skeleton fossil deposited by the new generation algae plants, and the main component of the diatomite is amorphous SiO 2. However, in China, the diatomite pesticide is in the beginning stage, the dispersion and wettability of the pesticide are poor due to the nature of the diatomite, the insecticidal efficiency is affected, and when the diatomite is used for killing insects, the using amount is increased.

Through the combined action of the chemical active ingredients and the diatomite, the chemical insecticide achieves high insecticidal effect while using less diatomite, which is a research focus, but the chemical insecticide may cause harm to people and livestock, and especially in rainy days, the chemical insecticide enters soil or rivers along with rain wash, which causes pollution to the environment.

Disclosure of Invention

In order to solve the above problems, according to a first aspect of the present invention, there is provided an insecticidal composition comprising specially shaped diatomaceous earth, wherein the specially shaped diatomaceous earth is saw-toothed, and an active ingredient is buprofezin or dinotefuran.

As a preferable technical scheme, the insecticidal composition further comprises a wetting agent, wherein the wetting agent accounts for 6-10 wt% of the total weight of the special-shaped diatomite and the active ingredients.

As a preferable technical scheme of the present invention, the wetting agent is selected from one or more of sodium dodecyl sulfate, sodium alkyl naphthalene sulfonate, fatty alcohol polyglycol ether sulfate, fatty alcohol polyoxyethylene ether carboxylate, alkyl naphthalene sulfonate, fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether carboxylate, nonylphenol polyoxyethylene ether, sorbitan fatty acid ester polyoxyethylene ether, and alkyl naphthalene formaldehyde.

As a preferable technical scheme, the preparation raw materials of the insecticidal composition also comprise a dispersing agent, and the dispersing agent accounts for 6-10 wt% of the total weight of the diatomite with the special shape and the active ingredients.

In a preferred embodiment of the present invention, the dispersant is one or more selected from the group consisting of lignosulfonate, sodium polyacrylate, polycarboxylate, methylenedinaphthalenesulfonate, calcium alkylbenzenesulfonate, amine alkylbenzenesulfonate, sodium methylenedinaphthalenesulfonate formaldehyde condensate, polyoxyethylene polyoxypropylene block copolymer, carboxymethylcellulose, polyvinyl alcohol, polyvinylpyrrolidone, sodium tripolyphosphate, and alkylnaphthalenesulfonate polycondensate.

As a preferable technical scheme, the preparation raw materials of the insecticidal composition further comprise a filler, and the filler accounts for 10-15 wt% of the total weight of the diatomite with the special shape and the active ingredients.

As a preferable technical scheme, the dosage form of the insecticidal composition is wettable powder and/or water dispersible granules.

The invention provides a thiazine ketone pesticide, which is prepared from the raw materials of the thiazine ketone pesticide, wherein the weight ratio of the diatomite with the special shape to the buprofezin is (1: 40) - (100: 1).

The third aspect of the invention provides a dinotefuran insecticide, which is prepared from the raw materials of the dinotefuran insecticide composition, wherein the weight ratio of the diatomite with the special shape to the dinotefuran is (1: 60) - (400: 1).

In a second aspect, the invention provides an application of the insecticidal composition containing the diatomite with the special shape, which is applied to control plant pests.

Compared with the prior art, the invention has the following beneficial effects: the invention provides an insecticidal composition, which can increase insecticidal effect and insecticidal efficiency through the combined action of diatomite with a special saw-toothed shape and buprofezin or dinotefuran and the like, has obvious control effect on pests such as citrus red spiders, citrus scale insects, frankliniella occidentalis, whiteflies, liriomyza sativae, prodenia litura, tea lesser leafhoppers, tea yellow thrips, tea geometrid, green plant bugs, grape aphids and the like, and is favorable for reducing the loss of buprofezin or dinotefuran and the like after being washed by rainwater by using the saw-toothed diatomite; in addition, the applicant is favorable for increasing the wetting and suspending performances of the insecticidal composition by selecting proper auxiliary agents such as a wetting agent, a dispersing agent, a filler and the like, and can be used for various formulations such as wettable powder, water dispersible granules and the like.

Drawings

Fig. 1 is an optical microscope image of a serrated diatomaceous earth Celite 610.

FIG. 2 is an electron microscope image of a sawtooth-shaped diatomaceous earth Celite 610.

Detailed Description

The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.

The term "prepared from …" as used herein is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.

The conjunction "consisting of …" excludes any unspecified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.

When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.

The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. "optional" or "any" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.

Approximating language, as used herein throughout the specification and claims, is intended to modify a quantity, such that the invention is not limited to the specific quantity, but includes portions that are literally received for modification without substantial change in the basic function to which the invention is related. Accordingly, the use of "about" to modify a numerical value means that the invention is not limited to the precise value. In some instances, the approximating language may correspond to the precision of an instrument for measuring the value. In the present description and claims, range limitations may be combined and/or interchanged, including all sub-ranges contained therein if not otherwise stated.

In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.

The present invention is illustrated by the following specific embodiments, but is not limited to the specific examples given below.

The invention provides an insecticidal composition containing specially-shaped diatomite, which is prepared from specially-shaped diatomite and an active ingredient.

In the present invention, the term "composition" means that the components of the composition are packaged in combination or separately and used together when used. That is, in the present invention, the "special-shaped diatomaceous earth and active ingredient" means that the special-shaped diatomaceous earth and active ingredient may be mixed and packaged together and used together at the time of use; also comprises special shape diatomite and active component separately packaged, and mixed at a certain proportion for use.

Special-shaped diatomite

In one embodiment, the specially shaped diatomaceous earth of the present invention is in the shape of a saw tooth.

The sawtooth-shaped diatomite has a larger specific surface area and a sawtooth-shaped structure, is one of inert powder, is easier to adsorb on the surfaces of pests due to the sawtooth-shaped structure of the sawtooth-shaped diatomite and damages wax layers on the epidermis parts of the pests, so that the water loss in the pests is excessive, and the sawtooth-shaped diatomite has the advantages of good insect prevention and killing effect, long protection period, no toxicity to mammals, no environmental pollution and the like. The saw-toothed diatomite of the present invention can be manufactured or purchased by self, and in a preferred embodiment, the saw-toothed diatomite of the present invention is purchased from Celite610 of yirui stone, france, and the saw-toothed structure thereof can be observed by an optical microscope and an electron microscope, as shown in fig. 1 and fig. 2, and the saw-toothed honeycomb structure of the diatomite can be seen.

Active ingredient

Preferably, the active ingredient of the invention is buprofezin or dinotefuran.

More preferably, the active ingredient of the present invention is buprofezin; furthermore, the weight ratio of the diatomite with the special shape to the buprofezin is (1: 40) - (100: 1).

Buprofezin, also known as "delphacidofol", belongs to the class of insecticides of insect growth regulators. When the pesticide is sprayed on a large area as a farmland pesticide, the direct pollution of soil can be caused, certain pollution is caused to water, and pesticide residues on crops can be caused after long-term use. The insecticidal composition is mainly used for controlling pests of crops such as rice, fruit trees, tea trees, vegetables and the like, and has lasting larvicidal activity on coleoptera, partial homoptera and acarina. Can effectively prevent and treat the rice from the cicada and the plant hopper: cicadae on potato; whitefly family on citrus, cotton and vegetables; lecanidae, pelaginaceae and Lecanidae on citrus. The action mechanism of the insect is mainly to act on the neuroendocrine system of the insect through different medicine receiving parts, interfere the normal activities of the heart side body, the chest gland and the like and present a series of adverse reactions. The adverse reaction is irreversible, so that the pests cannot recover after receiving the drug. The two action modes of the brown rice lice eggs are that egg shells (or egg pores) act on embryo bodies, the formation of each ectoderm meat-trap organ (system) is seriously interfered in the embryo development process, or newly hatched individuals are killed by contacting medicaments, the brown rice lice eggs have special effects on homoptera pests such as plant hoppers, leafhoppers, whiteflies, scale insects and the like, and can inhibit the synthesis of chitin of insects and interfere the metabolism. In a preferred embodiment, the buprofezin of the present invention is purchased from the hoard agrichemical company, continuous cloud port.

Further preferably, the active ingredient of the invention is dinotefuran; furthermore, the weight ratio of the diatomite with the special shape to the dinotefuran is (1: 60) - (400: 1).

Dinotefuran (dinotefuran) is the latest generation of super-nicotinoid insecticides. The chemical structure of the pesticide is quite different from that of the prior nicotine pesticide, the tetrahydrofuran group of the pesticide replaces the prior chloropyridyl and chlorothiazyl, and does not contain halogen elements. Meanwhile, the pesticide is different from nicotine in performance and has a wider insecticidal spectrum, so that the pesticide is called as furanonicotine. Has the characteristics of strong contact toxicity, stomach toxicity and root systemic property, high quick effect, long lasting period of 4-8 weeks (43 days of theoretical lasting effect), wide insecticidal spectrum and the like, has excellent control effect on the pests of the sucking mouth parts, and shows high insecticidal activity at very low dosage. The insecticidal composition is mainly used for preventing and treating 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, diptera, lepidoptera and homoptera pests, and has high efficiency on sanitary pests such as cockroaches, termites, houseflies and the like. However, recent studies have found that the possible contamination of ground water and ground water with neonicotinoid insecticides can present a threat to vertebrates and may have negative effects on human health. In a preferred embodiment, the dinotefuran is purchased from Nanjing Ponno Biotech, Inc.

The applicant finds that when the saw-toothed diatomite with the special shape and active ingredients such as the buprofezin or the dinotefuran act together, the insecticidal effect can be increased, and the insecticidal spectrum can be enlarged, probably because the saw-toothed structure of the diatomite is favorable for the active ingredients to be adsorbed on the surface of the diatomite, when the diatomite destroys epidermal cells of pests, the active ingredients such as the buprofezin or the dinotefuran contact with the pests and even enter the pests to play a role, so that the insecticidal efficiency is increased, and the insecticidal composition has a high control effect on various pests such as citrus red spider, citrus scale insect, frankliniella occidentalis, western flower thrips, whitefly, leaf miner, prodenia litura, tea leafhopper, tea yellow thrips, tea geometrid, green plant bug, grape aphid and the like.

However, the applicant finds that although the zigzag diatomite can reduce the dosage of active ingredients such as buprofezin or dinotefuran, but the buprofezin or dinotefuran has the risk of polluting the environment, especially in rainy days, the buprofezin or dinotefuran can easily cause environmental or human harm as the rainwater enters the soil or rivers, but the applicant has surprisingly found that when the diatomite with a special shape such as the zigzag diatomite is used, the buprofezin or dinotefuran can be reduced to flow into the soil along with the rainwater, the adhesion between the buprofezin or dinotefuran and the plant surface can be increased, which is probably because the zigzag protrusions arranged regularly on the zigzag diatomite have larger surface tension when acting with the rainwater, so that the active ingredients adsorbed at the gaps among the zigzag diatomite protrusions can be reduced to fall into the soil along with the rainwater washing, and the insecticidal sustainable time can be prolonged, the pollution to soil and the like is reduced.

However, due to the influence of the zigzag structure, the special-shaped diatomite has poor suspension property and wettability.

In one embodiment, the raw materials for preparing the insecticidal composition of the present invention further comprise a wetting agent.

Wetting agent

In one embodiment, the wetting agent of the present invention is selected from one or more of sodium dodecyl sulfate, sodium alkyl naphthalene sulfonate, fatty alcohol polyglycol ether sulfate, fatty alcohol polyoxyethylene ether carboxylate, alkyl naphthalene sulfonate, fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether carboxylate, nonylphenol polyoxyethylene ether, sorbitan fatty acid ester polyoxyethylene ether, and alkyl naphthalene formaldehyde.

Preferably, the wetting agent comprises fatty alcohol polyoxyethylene ether carboxylate and alkylphenol polyoxyethylene ether carboxylate, and the weight ratio is (3-5): 1; further, the weight ratio of the fatty alcohol-polyoxyethylene ether carboxylate to the alkylphenol polyoxyethylene ether carboxylate is 4: 1.

fatty alcohol polyoxyethylene ether carboxylates, abbreviated as AEC, are a novel class of anionic surfactants, which are modified from nonionic surfactants, having both anionic and nonionic surfactant characteristics. The modified surfactant has better water solubility, chemical stability, wettability, emulsibility and hard water resistance, strong dispersing power and small irritation to skin, can be used as cosmetics, washing and caring articles, crude oil demulsifiers, sewage treatment agents, softeners, emulsion stabs, antistatic agents and the like, and is a multifunctional green surfactant. The fatty alcohol-polyoxyethylene ether can be prepared by self or purchased, and when purchased, the fatty alcohol-polyoxyethylene ether comprises but is not limited to AEC-15Na (the polymerization degree of polyoxyethylene ether is 15), AEC-9Na (the polymerization degree of polyoxyethylene ether is 9), AEC-7Na (the polymerization degree of polyoxyethylene ether is 7), AEC-6Na (the polymerization degree of polyoxyethylene ether is 6), AEC-5Na (the polymerization degree of polyoxyethylene ether is 5) and AEC-3Na (the polymerization degree of polyoxyethylene ether is 3) of a new catagma Honghou company; further, the fatty alcohol-polyoxyethylene ether carboxylate is AEC-15Na and/or AEC-9 Na.

Alkylphenol polyoxyethylene ether carboxylate, abbreviated as APEC, is obtained by modifying alkylphenol polyoxyethylene ether, contains two hydrophilic groups (anion and nonionic) with different properties, and has the advantages of an anionic surfactant and a nonionic surfactant. High temperature and high salt resistance, and the compounding with sodium heavy alkyl benzene sulfonate and other anionic surfactants can improve the hardness resistance of the latter. The alkylphenol polyoxyethylene ether carboxylate can be prepared by self or purchased, and when purchased, the alkylphenol polyoxyethylene ether carboxylate comprises but is not limited to APEC-4Na (the polymerization degree of polyoxyethylene ether is 4), APEC-6Na (the polymerization degree of polyoxyethylene ether is 6), APEC-10Na (the polymerization degree of polyoxyethylene ether is 10), APEC-15Na (the polymerization degree of polyoxyethylene ether is 15) and APEC-20Na (the polymerization degree of polyoxyethylene ether is 10) of the catapyne new material company Limited; furthermore, the alkylphenol polyoxyethylene ether carboxylate is APEC-4Na and/or APEC-6 Na.

The degree of polymerization is an indicator of the molecular size of the polymer. Based on the number of repeating units, i.e., the average of the number of repeating units contained in the macromolecular chain of the polymer.

More preferably, the polymerization degree of polyoxyethylene ether in the fatty alcohol-polyoxyethylene ether carboxylate is 9-15; further, the polymerization degree of polyoxyethylene ether in the fatty alcohol-polyoxyethylene ether carboxylate is 15.

Further preferably, the polymerization degree of polyoxyethylene ether in the alkylphenol polyoxyethylene ether carboxylate is 4-6; further, the polymerization degree of polyoxyethylene ether in the alkylphenol polyoxyethylene ether carboxylate is 4.

More preferably, the wetting agent accounts for 6-10 wt% of the total weight of the specially-shaped diatomite and the active ingredient; further, the wetting agent of the present invention accounts for 8 wt% of the total weight of the specially shaped diatomaceous earth and the active ingredient.

The applicant has unexpectedly found that by adding fatty alcohol-polyoxyethylene ether carboxylate and alkylphenol polyoxyethylene ether carboxylate with different degrees of polymerization to act together, the increase of suspension performance is promoted, and the wetting and adhesion effects on the plant surface can be increased, so as to further increase the rain wash resistance, which is probably because by using fatty alcohol-polyoxyethylene ether carboxylate with higher degree of polymerization, lipophilic fatty alcohol chain can cover the surface of diatomite, while longer polyoxyethylene ether chain provides higher hydrophilicity, so that the agglomeration and precipitation of diatomite in water are reduced, and hydrophilic and lipophilic arranged fatty alcohol-polyoxyethylene ether carboxylate chain is also beneficial to the improvement of surface tension, so as to increase the wetting ability on the plant surface, but higher polyoxyethylene ether chain is not beneficial to the adhesion and permeation of diatomite and active ingredients on the plant surface, when being washed by rain, but rather the rain erosion resistance is further degraded.

Through a large number of experiments, the applicant finds that if alkylphenol polyoxyethylene ether carboxylate and fatty alcohol polyoxyethylene ether carboxylate with low degree of polymerization are used as wetting agents, when the alkylphenol polyoxyethylene ether carboxylate and the fatty alcohol polyoxyethylene ether carboxylate act together, a conjugated system of alkylphenol and a short polyoxyethylene ether molecular chain are beneficial to acting together with the fatty alcohol polyoxyethylene ether carboxylate while suspension property is not affected, surface tension can be further reduced, and adhesion performance is improved, so that loss of active ingredients, diatomite and the like under rain wash is reduced, and rain wash resistance of the insecticidal composition is improved.

In one embodiment, the raw materials for preparing the pesticidal composition further include a dispersant.

Dispersing agent

In one embodiment, the dispersant of the present invention is selected from one or more of lignosulfonates, sodium polyacrylates, polycarboxylates, methylene bis-naphthalene sulfonates, calcium alkylbenzene sulfonates, amine sulfonates, sodium methylene bis-naphthalene sulfonate formaldehyde condensates, polyoxyethylene polyoxypropylene block copolymers, carboxymethylcellulose, polyvinyl alcohol, polyvinylpyrrolidone, sodium tripolyphosphate, and alkyl naphthalene sulfonate polycondensates.

Preferably, the dispersant of the present invention is a polycarboxylate.

The molecules of the polycarboxylate are of a comb-shaped or dendritic structure artificially formed by molecular design, and a plurality of branched chains (side chains) with certain length and rigidity are connected to the main chain of the molecule. The main chain is also provided with sulfonate or other groups capable of charging the solid particles, and once the main chain is adsorbed on the surface of the solid particles, the branched chains form stereo crossing with the branched chains on the surfaces of other particles, so that the particles are prevented from approaching each other, and the dispersion effect is achieved. This steric hindrance is not weakened by a prolonged period of time, and the dispersing action is more durable. The polycarboxylate is purchased or self-made, and when purchased, the polycarboxylate comprises, but is not limited to, DC01, DC02, DC04 and GY-JZS-B of Beijing Guangyuan agricultural chemical Limited liability company, HMK-D1005 and HMK-D1003 of Moke chemical technology Co., Ltd, Beijing Han, GY-D900, GY-D800, GY-D180, GY-D06, GY-D09 and GY-D07 of Nanjing Jiejun technology Co., Ltd; further, the polycarboxylate of the present invention is HMK-D1005 and/or HMK-D1003; further, the polycarboxylate of the present invention is HMK-D1005.

HMK-D1003 is anionic polymer surfactant with comb structure and obtained by copolymerization of unsaturated monomer. The pesticide composite has a main chain with strong lipophilicity, can effectively adsorb and wrap pesticide particles, and has a good dispersing effect on a raw pesticide with strong hydrophobicity.

HMK-D1005 high molecular polycarboxylate dispersant and micromolecule acrylic copolymer dispersant are compounded, the dispersant is applied to water dispersible granules and wettable powder, can improve the adaptability of different water qualities of formulations, and still has good physical stability in high-hardness water quality.

More preferably, the dispersant accounts for 6-10 wt% of the total weight of the special-shaped diatomite and the active ingredient; further, the dispersant of the present invention accounts for 8 wt% of the total weight of the specially shaped diatomaceous earth and the active ingredient.

Since the special shape of the diatomite used in the present invention has a saw-tooth shape, precipitation and aggregation easily occur in water, by adding a polycarboxylate, especially a polycarboxylate containing a small molecule acrylic copolymer, the comb-shaped strong polar structure of the polycarboxylate is beneficial to strong adsorption with diatomite, and the existence of the micromolecular acrylic copolymer is beneficial to increasing the interaction between the polyoxyethylene ether carboxylate and the macromolecular polycarboxylate to form a cross-network protective film, so that the protective film is prevented from being damaged due to larger difference of molecular weight, polarity and the like of the polyoxyethylene ether carboxylate and the macromolecular polycarboxylate, the thicker double electric layer protective film and the steric hindrance formed by the wetting agent and the dispersing agent are also beneficial to reducing the aggregation among the diatomite and improving the suspension property, and when the strong non-bond acting force acts on the surface of the plant, the strong non-bond acting force is also beneficial to the adsorption with the plant, and the loss during rain wash is reduced.

In one embodiment, the raw materials for preparing the insecticidal composition according to the invention further comprise a filler.

Filler material

In one embodiment, the filler of the present invention is selected from one or more of kaolin, white carbon, magnesium aluminum silicate, anhydrous sodium sulfate, glucose, china clay, sericite, fructose, and soluble starch.

Preferably, the filler is white carbon black; further, the white carbon black is modified white carbon black.

The white carbon black is white powdery X-ray amorphous silicic acid and silicate, and mainly refers to precipitated silica, fumed silica and superfine silica gel. White carbon black is a porous substance, and the composition of the white carbon black can be represented by SiO2 & nH2O, wherein nH2O exists in the form of surface hydroxyl. High-temperature resistance, non-combustion, tastelessness, odorless and good electrical insulation. The white carbon black can be purchased or manufactured by self, and in a preferred embodiment, the white carbon black is purchased from one or more of Wake HDKV15, HDK N20, HDK T30, HDK T40, HDK H15, HDK H20, HDK H17, HDK H18, HDK H30 and HDK H2000; in a more preferred embodiment, the white carbon black of the present invention is obtained from HDK V15 (specific surface area 150 m)²(g), HDK N20 (specific surface area 200 m)²/g), HDK T30 (specific surface area 300 m)²/g), HDK T40 (specific surface area 400 m)²One or more of the following components/g).

More preferably, the modifier of the modified white carbon black is polyether modified polysiloxane.

The polyether modified polysiloxane is generally formed by graft copolymerization of polyether and polydimethylsiloxane, contains a hydrophilic polyether chain segment and a hydrophobic polysiloxane chain segment in a molecular structure, is an organosilicon surfactant with unique performance, can be purchased or manufactured by self, and comprises but is not limited to BD-3077 (the viscosity at 25 ℃ is 20-40 cps), BD3055 (the viscosity at 25 ℃ is 800-1200 cps), BD3056 (the viscosity at 25 ℃ is 1000-1500 cps) and BD3071 (the viscosity at 25 ℃ is 30-60 cps) of Nanjing Jiezui technology Limited; further, the polyether modified polysiloxane is BD-3077 and/or BD 3071.

Viscosity represents the fluid's own resistance to flow and can be measured according to methods well known in the art.

Further preferably, the viscosity of the polyether modified polysiloxane is 20-60 cps at 25 ℃; furthermore, the viscosity of the polyether modified polysiloxane is 20-40 cps at 25 ℃.

More preferably, in the modified white carbon black of the present invention, the weight ratio of the modifier to the white carbon black is 1: (0.1 to 0.3); further, in the modified white carbon black of the invention, the weight ratio of the modifier to the white carbon black is 1: 0.2.

the preparation method of the modified white carbon black is a method well known in the field. In a preferred embodiment, the preparation method of the modified white carbon black comprises the following steps: and mixing the polyether modified silicone oil and the white carbon black at the temperature of 30-40 ℃, and drying to obtain the modified white carbon black.

In a preferred embodiment, the filler of the invention accounts for 10-15 wt% of the total weight of the special-shaped diatomite and the active ingredient; further, the filler of the present invention accounts for 12 wt% of the total weight of the specially shaped diatomaceous earth and the active ingredient.

The applicant has unexpectedly found that when modified white carbon black of which the modifier is polyether modified polysiloxane is used as the modifier, the wettability can be further increased, but the rain wash resistance can be affected, probably because the polysiloxane adsorbed on the surface of the white carbon black reduces the surface tension and simultaneously facilitates the wetting of the insecticidal composition of the invention by rain, and the applicant has unexpectedly found that the suspension property and the adhesion property to the plant surface can be effectively increased by adding polycarboxylate as a dispersant and the combined action of modified diatomite, and the improvement of the hot press stability can be facilitated when the dosage form is water dispersible granules. This is probably because when the insecticidal composition is dissolved in water, the multi-comb carboxyl structure acts on the surface of the diatomaceous earth and also acts on the surface of the white carbon black, and due to the combined action of the large van der waals force and other acting forces of the small-molecular acrylic copolymer in the polycarboxylate and the high-molecular polycarboxylate, the adhesion of the modified white carbon black to plants is increased without affecting the wettability of the polysiloxane, so that the influence of the modified white carbon black on the rain wash resistance is prevented.

In addition, the applicant has unexpectedly found that when the modified white carbon black is used, it is advantageous to increase the hot-pressing stability, which may be because in the mixing process, the components such as polyether modified polysiloxane on the surface of the white carbon black and the adsorbed wetting agent are uniformly mixed with the white carbon black and the diatomite, so that the prepared wettable powder particles are tightly adhered together, the increase of voids caused by the saw-tooth-shaped protrusions of the diatomite is reduced, the hot-pressing stability is increased, and the damage of the saw-tooth-shaped shape of the diatomite due to external forces such as mutual collision and the like in the transportation process is reduced. In addition, the applicants have found that when too much alkylphenol ethoxylate carboxylate is used compared to fatty alcohol ethoxylate carboxylate, or too much modifier is used in the modified white carbon black, the rain wash performance is also affected, probably because the wetting performance on the plant surface is greater than the adhesion performance.

In one embodiment, the formulation of the insecticidal composition of the present invention is selected from one or more of emulsifiable solution, wettable powder, water dispersible granules, suspending agent, aqueous emulsion, microemulsion, dispersible oil suspending agent, microcapsule suspending agent and soluble powder; furthermore, the dosage form of the insecticidal composition is wettable powder and/or water dispersible granules.

The preparation raw materials of the insecticidal composition can also comprise conventional auxiliary materials or carriers in pesticide preparations, including but not limited to any one or more of thickening agent, antifreezing agent, stabilizing agent, preservative, disintegrating agent, binder or defoaming agent; for example, the thickener may be selected from any one or more of xanthan gum, carboxymethyl cellulose, sodium polyacrylate, magnesium aluminium silicate, fumed silica or attapulgite; the antifreezing agent can be selected from any one or a mixture of more than one of ethylene glycol, propylene glycol, glycerol-diethyl ether diglycol or methyl propylene diglycol according to any proportion; the stabilizer can be selected from any one or more of 2, 6-di-tert-butyl-4-methylphenol (BHT), citric acid or Butyl Hydroxy Anisole (BHA); the preservative can be sodium benzoate; the disintegrating agent can be selected from one or more of urea, bentonite, montmorillonite or sodium alginate; the binder can be selected from one or more of gelatin, arabic gum, xanthan gum, sodium tripolyphosphate, phenolic resin or polyvinylpyrrolidone; the defoaming agent can be defoaming agent such as organosilicon.

In one embodiment, the preparation raw materials of the insecticidal composition of which the dosage form is water dispersible granules further comprise a disintegrating agent and a binding agent; furthermore, the disintegrating agent accounts for 0.1-3 wt% of the total weight of the special-shaped diatomite and the active ingredient, and the binder accounts for 0.1-3 wt% of the total weight of the special-shaped diatomite and the active ingredient.

The preparation method of the insecticidal composition with the dosage form of wettable powder or water dispersible granules is a method well known in the field; in one embodiment, the preparation method of the wettable powder of the invention comprises the following steps: mixing and crushing the active ingredients, the wetting agent, the dispersing agent and the filler, adding diatomite with a special shape, mixing and sieving to obtain the wettable powder; in one embodiment, the preparation method of the water dispersible granule comprises the following steps: mixing and crushing the active ingredients, the wetting agent, the dispersing agent, the filler, the binder and the disintegrating agent, adding the sawtooth-shaped diatomite, kneading, granulating, drying and screening to obtain the water dispersible granule.

The invention provides a thiazine ketone insecticide, which is prepared from the above insecticidal composition, wherein the weight ratio of the diatomite with the special shape to the buprofezin is (1: 40) - (100: 1).

According to a third aspect of the invention, the dinotefuran insecticide is prepared from the insecticidal composition, and the weight ratio of the special-shaped diatomite to the dinotefuran is (1: 60) - (400: 1).

In a fourth aspect, the present invention provides the use of the pesticidal composition comprising diatomaceous earth of a specific shape as described above for controlling plant pests.

Examples

The present invention will be specifically described below by way of examples. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention.

A: special shapes of diatomaceous earth Celite610 and buprofezin

B: special-shaped diatomite Celite610 and dinotefuran insecticide

C1: wetting agent

The wetting agent is fatty alcohol polyoxyethylene ether carboxylate, AEC-15Na purchased from Zibohong New materials Co.

C2: wetting agent

The wetting agent is fatty alcohol polyoxyethylene ether carboxylate, AEC-3Na available from Zibohong New materials Co.

C3: wetting agent

The wetting agent is alkylphenol polyoxyethylene ether carboxylate, APEC-6Na purchased from Zibohong new materials Co.

C4: wetting agent

The wetting agent is alkylphenol polyoxyethylene ether carboxylate, APEC-15Na purchased from Zibohong new materials Co.

C5: wetting agent

The wetting agent is fatty alcohol polyoxyethylene ether carboxylate, AEC-9Na purchased from Zibohong New materials Co.

C6: wetting agent

The wetting agent is alkylphenol polyoxyethylene ether carboxylate, APEC-4Na purchased from Zibohong New materials Co.

D1: dispersing agent

The dispersant was a polycarboxylate available from HMK-D1005, Moke chemical technologies, Inc., Beijing Han.

D2: dispersing agent

The dispersant is a polycarboxylate available from HMK-D1003 of Moke chemical technology, Inc., Beijing Han.

E1: filler material

The filler was white carbon black, available from wacker HDK T30.

E2: filler material

The filler is modified white carbon black, and the preparation method of the modified white carbon black comprises the following steps: mixing the polyether modified silicone oil and the white carbon black at 35 ℃, and drying to obtain modified white carbon black; the weight ratio of the polyether modified silicone oil to the white carbon black is 0.2: 1. the white carbon black is purchased from HDK T30 of watt; the polyether modified silicone oil is purchased from BD-3077 of Jirun technologies, Inc. of Nanjing.

E3: filler material

The filler is modified white carbon black, and the preparation method of the modified white carbon black comprises the following steps: mixing the polyether modified silicone oil and the white carbon black at 35 ℃, and drying to obtain modified white carbon black; the weight ratio of the polyether modified silicone oil to the white carbon black is 0.6: 1. the white carbon black is purchased from HDK T30 of watt; the polyether modified silicone oil is purchased from BD-3077 of Jirun technologies, Inc. of Nanjing.

E4: filler material

The filler is modified white carbon black, and the preparation method of the modified white carbon black comprises the following steps: mixing the polyether modified silicone oil and the white carbon black at 35 ℃, and drying to obtain modified white carbon black; the weight ratio of the polyether modified silicone oil to the white carbon black is 0.2: 1. the white carbon black is purchased from HDK T30 of watt; the polyether modified silicone oil is purchased from BD3055 of Jirun technologies, Inc. of Nanjing.

E5: filler material

The filler is modified white carbon black, and the preparation method of the modified white carbon black comprises the following steps: mixing the polyether modified silicone oil and the white carbon black at 35 ℃, and drying to obtain modified white carbon black; the weight ratio of the polyether modified silicone oil to the white carbon black is 0.2: 1. the white carbon black is purchased from HDK N20 of Wake; the polyether modified silicone oil is purchased from BD-3071 of Jirun technologies, Inc. of Nanjing.

TABLE 1

Examples	A	C1	C2	C3	C4	D1	D2	E1	E2	E3	E4
												1	100	6.4	1.6		8			12
2	100	6.4		1.6		8			12
												3	100	6.4	1.6		8			12
4	100	6.4		1.6		8			12
												5	100	6.4	1.6		8			12
6	100	6.4		1.6		8			12
												7	100	6.4	1.6		8		12
8	100	8				8		12
												9	100	4	4		8		12
10	100		6.4	1.6		8		12
												11	100	6.4		1.6	8		12
12	100	6.4		1.6			8	12
												13	100	6.4	1.6			8		12
14	100	6.4		1.6		8				12
												15	100	6.4	1.6		8				12

Examples 1 to 15 provide a thiazine ketone insecticide in the form of a wettable powder, the formulation of which is shown in table 1, the formulation amounts being in parts by weight; the preparation method of the wettable powder comprises the following steps: and mixing and crushing the buprofezin, the wetting agent, the dispersing agent and the filler, adding diatomite with a special shape, mixing and sieving to obtain the wettable powder. The weight ratios of the special-shaped diatomaceous earth Celite610 and buprofezin in examples 1 to 15 are shown in table 2.

TABLE 2 weight ratio of diatomaceous earth Celite610 and buprofezin in specific shapes

Examples	Weight ratio of	Examples	Weight ratio of	Examples	Weight ratio of
						1	0：1	6	1：40	11	1：1
2	100：1	7	1：1	12	1：1
						3	50：1	8	1：1	13	1：1
4	1：1	9	1：1	14	1：1
						5	1：20	10	1：1	15	1：1

The embodiment 1-15 also provides a thiazine ketone insecticide in a water dispersible granule dosage form, wherein the preparation raw materials of the insecticide comprise the preparation raw materials shown in table 1, and the insecticide also comprises a disintegrating agent and a binder; the disintegrating agent accounts for 2 wt% of the total weight of the sawtooth-shaped diatomite, and the binder accounts for 3 wt% of the total weight of the sawtooth-shaped diatomite; the disintegrating agent is ammonium sulfate, and the binder is Arabic gum, which is purchased from Hebei Pengyu biotechnology Limited; the preparation method of the water dispersible granule comprises the following steps: mixing and crushing buprofezin, a wetting agent, a dispersing agent, a filler, a binder and a disintegrating agent, adding sawtooth-shaped diatomite, kneading, granulating, drying and screening to obtain the water dispersible granule.

TABLE 3

Examples	B	C5	C6	D1	E5
						16	100	6.4	1.6	8	12
17	100	6.4	1.6	8	12
						18	100	6.4	1.6	8	12
19	100	6.4	1.6	8	12
						20	100	6.4	1.6	8	12
21	100	6.4	1.6	8	12

Examples 16 to 21 provide dinotefuran insecticides in the form of wettable powders, the formulation of which is shown in table 3, the formulation amounts being in parts by weight; the preparation method of the wettable powder comprises the following steps: mixing and crushing dinotefuran, a wetting agent, a dispersing agent and a filler, adding diatomite with a special shape, mixing and sieving to obtain the wettable powder. The weight ratios of the special-shaped diatomaceous earth Celite610 and dinotefuran in examples 1-15 are shown in table 4.

TABLE 4 weight ratio of special shape diatomaceous earth Celite610 and dinotefuran

Examples	Weight ratio of	Examples	Weight ratio of	Examples	Weight ratio of
						16	0：1	18	200：1	20	1：30
17	400：1	19	1：1	21	1：60

Embodiments 16 to 21 also provide a dinotefuran insecticide in the form of water dispersible granules, wherein the preparation raw materials of the insecticide include the preparation raw materials described in table 1, and the insecticide further includes a disintegrant and a binder; the disintegrating agent accounts for 3 wt% of the total weight of the sawtooth-shaped diatomite, and the binder accounts for 3 wt% of the total weight of the sawtooth-shaped diatomite; the disintegrating agent is urea, and the binder is Arabic gum, which is purchased from Hebei Pengyu biotechnology limited; the preparation method of the water dispersible granule comprises the following steps: mixing and crushing dinotefuran, a wetting agent, a dispersing agent, a filler, a binder and a disintegrating agent, adding saw-toothed diatomite, kneading, granulating, drying and screening to obtain the water dispersible granule.

Evaluation of Performance

1. And (3) combined virulence determination: the method for combined toxicity determination of citrus red spiders, citrus scale insects, frankliniella occidentalis, trialeurodes vaporariorum, liriomyza sativae, prodenia litura, tea lesser leafhopper, tea thrips flavivis, tea geometrid, green plant bugs and grape aphids by using the dinotefuran insecticide provided in examples 16-21 as a reagent to be tested is as follows:

(1) and (3) measuring the combined toxicity of the diatomite with the special shape and the dinotefuran on citrus red spiders.

Referring to the method in NY/T1154.13-2008 standard, a leaf spray method was used. Cleaning and wiping the smooth citrus leaves with the same size, sticking the citrus leaves onto wet sponge with the leaf surfaces facing upwards, enclosing the leaves with wet small cotton slivers to prevent test mites from escaping, putting the wet sponge into a culture dish with the diameter of 9cm, adding water into the culture dish, and slightly lowering the water level to be lower than the height of the sponge. Inoculating indoor cultured nymphs to leaves, each leaf having no less than 30 heads. Placing the culture dish on a bottom plate of a Potter spraying tower for spraying, wherein the spraying amount is 1mL, taking out the culture dish after the liquid medicine is settled for 1min, and transferring the culture dish to a breeding condition for breeding. Each treatment was repeated 4 times and a blank control was run.

After 48h, the death of the test insects was examined under a dissecting mirror and recorded. The judgment standard of the death of the test insects is as follows: death was counted as no response when the test insects were gently touched by tweezers.

The co-toxicity coefficient (CTC) of each mixed combination is determined by a Sun & Johnson (1960) co-toxicity coefficient method (CTC) according to a raw test standard method NY/T1154.7-2006. Generally, a co-toxicity coefficient greater than 120 indicates a synergistic effect, less than 80 indicates an antagonistic effect, and between 80 and 120 indicates an additive effect. The co-toxicity coefficient is calculated as follows

The Theoretical Toxicity Index (TTI) of the mixture is the toxicity index of the agent A x the percent (%) of the agent A + the toxicity index of the agent B x the percent (%) of the agent B

The results are shown below.

TABLE 5 toxicity test results of blending diatomaceous earth and dinotefuran with special shape to citrus red spider

(2) And (3) determining the combined toxicity of the special-shaped diatomite and dinotefuran compounded on the citrus scale insects.

The method in NY/T1154.6-2006 is referred to, and the insect-soaking method is adopted. Dipping the trimmed citrus leaves with citrus arrowhead scales in a test solution for 10 seconds, taking out the citrus leaves, absorbing redundant liquid medicine around the leaves and the insects by using filter paper, putting the citrus leaves and the insects into a culture dish (with the diameter of 90mm) filled with moisturizing filter paper, wrapping petioles by using wet cotton balls for moisturizing, repeating the steps for 4 times per concentration, covering the dish cover after the treatment is finished, and placing the dish cover in an observation room for culturing. And (5) after 72 days, checking the death condition of the test insects, and obtaining a virulence determination result by using a co-virulence factor method.

TABLE 6 toxicity test results of Pachylomyces citri (Lecania) Lepidium with special shape by mixing diatomaceous earth and dinotefuran

(3) And (3) determining the combined toxicity of the specially-shaped diatomite and the dinotefuran on the Frankliniella occidentalis.

According to the standard method NY/T1154.14-2008 of biological measurement, a leaf-soaking dish method is adopted. Beating the blades into leaf disks by a puncher with the diameter of 18mm, soaking the leaf disks in a test reagent solution for 10 seconds, putting the leaf disks into a culture dish (with the diameter of 90mm) padded with moisturizing filter paper, putting 5 leaf disks into each dish, naturally drying, then selecting the western flower thrips into the culture dish, sealing the mouth of the dish by a preservative film, pricking some small holes on the film by a needle for ventilation, repeating the treatment for 4 times, finishing the treatment, and placing the dish in an observation room for culture. And (5) after 72 days, checking the death condition of the test insects, and obtaining a virulence determination result by using a co-virulence factor method.

TABLE 7 toxicity test results of blending diatomaceous earth and dinotefuran with special shape to Frankliniella occidentalis

(4) And (3) measuring the combined toxicity of the specially-shaped diatomite and the dinotefuran on the trialeurodes vaporariorum.

Referring to the method in NY/T1154.14-2008 standard, the leaf soaking method is adopted. After dissolving agar (1%) by heating, 20mL to 200mL of the solution was taken out of a beaker and condensed at room temperature for use. Soaking the leaves in a test solution for 10 seconds, taking out, naturally drying, sticking the leaves on the surface of the solidified agar solution, wrapping petioles with wet cotton balls, putting 3-4 leaves in each beaker, inoculating adult trialeurodes vaporariorum, covering 15 heads of each beaker with a preservative film, pricking small holes on the film with needles for ventilation, repeating the treatment for 4 times, and placing the beaker in an observation room for cultivation after the treatment. And (5) after 72 days, checking the death condition of the test insects, and obtaining a virulence determination result by using a co-virulence factor method.

TABLE 8 toxicity test results of blending diatomaceous earth and dinotefuran with special shapes against Bemisia alba

(5) And (3) determining the combined toxicity of the special-shaped diatomite and dinotefuran compound to the liriomyza sativae.

Referring to the method in NY/T1154.13-2008 standard, spraying method is adopted. Transplanting potted cowpea pest-free seedlings into pest-raising cages, inoculating a certain amount of mated adult liriomyza huidonii, taking out bean seedlings with liriomyza huidonii eggs after 6h, placing the bean seedlings in another pest-raising cage, continuously raising the bean seedlings to 2-year larvae (ensuring that each disc contains no less than 80 larvae of 2-year larvae), then carrying out spraying treatment, naturally air drying, and transferring the bean seedlings to an artificial climate box for continuous raising. Each treatment was repeated 4 times and a blank control was run. And (3) cutting bean seedlings from roots at the later stage of 3-year-old larvae, moisturizing the tail ends by using soaked cotton balls, putting the bean seedlings into plastic basins in an artificial climate box, pupating the bean seedlings, and counting the quantity of pupae in each dish.

The co-toxicity coefficient calculation method was the same as (1), and the results are shown below.

TABLE 9 toxicity test results of Paecilomyces lanuginosa mixed with diatomaceous earth and dinotefuran

(6) And (3) determining the combined toxicity of the special-shaped diatomite and dinotefuran compounded on prodenia litura.

Referring to the method in NY/T1154.14-2008 standard, the leaf-dipping dish method is adopted. Beat the cabbage leaf into the leaf dish with the hole puncher of diameter 18mm, dip the leaf dish in the liquid of testing medicine for 10 seconds after, put into the culture dish (diameter 90mm) that has filled with the filter paper that moisturizes, 6 leaf dishes are put into to every dish, wait to dry the back naturally, select again and starve 4h twill noctuid 3 age larva to the culture dish in, every dish is not less than 10, 4 times are repeated, the processing finishes, covers the ware lid, arranges the indoor culture of observation in. And (5) after 72 days, checking the death condition of the test insects, and obtaining a virulence determination result by using a co-virulence factor method.

TABLE 10 toxicity test results of Spodoptera litura obtained by mixing diatomaceous earth and dinotefuran in special shapes

(7) And (3) determining the combined toxicity of the diatomite with the special shape and the dinotefuran on the tea leafhoppers.

Referring to the method in NY/T1154.11-2008 standard, the dipping method is adopted. Selecting 3 fresh tea tree sprouts, soaking in a test liquid for 30 seconds, taking out, naturally drying, wrapping the base parts of the sprouts with wet absorbent cotton to preserve moisture, sealing absorbent cotton balls with a preservative film, and placing in a glass test tube (phi 200 x 30mm) with 4 times of repetition per concentration. Then, 3-year-old nymphs of tea lesser leafhoppers subjected to ether mild anesthesia treatment are inoculated into a brush pen, 15 +/-2 heads of each tube are used, and the mouth of each tube is sealed by white gauze. After the treatment, the test insects are placed in an observation room, the death condition of the test insects is checked after 72 days, and a toxicity measurement result is obtained by using a co-toxicity coefficient method.

TABLE 11 toxicity test results of blends of diatomaceous earth and dinotefuran with special shapes against tea leafhopper

(8) And (3) determining the combined toxicity of the special-shaped diatomite and dinotefuran on the tea leaf thrips.

According to the standard method NY/T1154.14-2008 of biological measurement, a leaf dipping method is adopted. Selecting fresh 3 tea tree sprout shoots with a certain amount of tea thrips (no less than 20) and soaking in the test liquid medicine for 10 seconds, taking out and naturally drying, wrapping the base parts of the sprout shoots with wet absorbent cotton to preserve moisture, sealing the absorbent cotton balls with a preservative film, and placing in a glass test tube (phi 200 x 30mm) for 4 times of repetition at each concentration. The mouth of the test tube is sealed by a preservative film, and the small holes are punched for ventilation. After the treatment, the sample is placed in an observation chamber. And (5) after 72 days, checking the death condition of the test insects, and obtaining a virulence determination result by using a co-virulence factor method.

TABLE 12 toxicity test results of blend of diatomaceous earth and dinotefuran with special shape on tea leaf thrips

(9) And (3) measuring the combined toxicity of the special-shaped diatomite and the dinotefuran compounded on tea geometrid.

Referring to the method in NY/T1154.14-2008 standard, the leaf soaking method is adopted. Selecting 3 fresh tea tree sprouts, soaking in the test liquid medicine for 30 seconds, taking out, naturally drying, wrapping the bases of the sprouts with wet absorbent cotton to preserve moisture, sealing absorbent cotton balls with a preservative film, and placing in a can bottle, wherein the concentration is repeated for 4 times. Then inoculating 2-year-old nymphs of tea geometrid with consistent size and liveness and health into a brush pen, wherein 15 +/-2 heads of each pot are sealed by white gauze. After the treatment, the sample is placed in an observation chamber. And (5) after 72 days, checking the death condition of the test insects, and obtaining a virulence determination result by using a co-virulence factor method.

TABLE 13 toxicity test results of blending of diatomaceous earth and dinotefuran with special shapes to tea geometrid

(10) And (3) carrying out combined toxicity determination on the green plant bug by compounding the diatomite with the special shape and the dinotefuran.

Referring to the method in NY/T1154.11-2008 standard, a leaf spray method was used. The method comprises the steps of disinfecting, cleaning and airing fresh kidney beans by adopting an immersion method, cutting the kidney beans into 2-3 cm segments, immersing the kidney beans in liquid medicines with different concentrations for 30 seconds, airing the kidney beans under natural conditions, and then putting the kidney beans into transparent plastic boxes (6 cm in diameter and 7cm in height) with smooth air, wherein each box has two sections. Healthy and consistent 3-year-old nymphs of lygus lucorum were inoculated, 15 or so per box, repeated 4 times, and a blank control was set. And putting the plastic box into a light incubator for culturing. And after 48h, the death condition of the test insects in each box is checked, the bodies of the lygus lucorum are lightly touched by the brush tips, and the death judgment standard of the test insects is that no response is calculated when the tweezers lightly touch the test insects. The co-toxicity coefficient calculation method was the same as (1), and the results are shown below.

TABLE 14 toxicity test results of Apolygus lucorum with specific shape of diatomaceous earth mixed with dinotefuran

(11) And (3) measuring the combined toxicity of the special-shaped diatomite and dinotefuran on grape aphids.

The method in NY/T1154.6-2006 is referred to, and the insect-soaking method is adopted. Cutting leaves with a certain amount of grape aphids, soaking in the liquid medicine to be tested for 10 seconds, taking out, absorbing the liquid medicine around the insect body with absorbent filter paper, placing in a culture dish padded with moisturizing filter paper, moisturizing with a wet cotton ball, and covering the culture dish with wet gauze. Each 30 aphids were treated, 4 replicates and a blank treatment without drug (including solvent and emulsifier used) was used. After the treatment, the cells were transferred to an observation room for cultivation. And (3) detecting the death condition of the test insects after 48h, and recording, wherein the judgment standard of the death of the test insects is as follows: the aphids were lightly touched with a writing brush, and the body was judged dead. The co-toxicity coefficient calculation method was the same as (1), and the results are shown below.

TABLE 15 toxicity test results of blend of diatomaceous earth and dinotefuran with special shape on grape aphid

2. And (3) combined virulence determination: the thiazine ketone insecticides of examples 1-6 were used to perform combined virulence determination on icerya citrus scale, thrips occidentalis, whitefly, tea lesser leafhopper, tea yellow thrips, green plant bug and grape aphid, and the specific test methods are as shown above, wherein the combined virulence test results are shown in the following table.

(1) And (3) measuring the combined toxicity of the specially-shaped diatomite and the buprofezin on the citrus scale insects.

TABLE 16 toxicity test results of the combination of diatomaceous earth and buprofezin with special shape to Cuckoo oranges (arrowhead scale)

(2) And (3) measuring the combined toxicity of the specially-shaped diatomite and the buprofezin on Frankliniella occidentalis.

TABLE 17 toxicity test results of blending diatomaceous earth and buprofezin with special shapes to Frankliniella occidentalis

(3) And (3) measuring the combined toxicity of the specially-shaped diatomite and the buprofezin on the trialeurodes vaporariorum.

TABLE 18 toxicity test results of blending diatomaceous earth and buprofezin with special shapes to trialeurodes vaporariorum

(4) And (3) determining the combined toxicity of the special-shaped diatomite and the buprofezin on the tea leafhopper. TABLE 19 toxicity test results of blending of special-shaped diatomaceous earth and buprofezin on tea leafhoppers

(5) And (3) measuring the combined toxicity of the special-shaped diatomite and the buprofezin on the tea leaf thrips tabaci.

TABLE 20 toxicity test results of blend of diatomaceous earth and buprofezin with special shapes on tea leaf thrips

(6) And (3) carrying out combined toxicity determination on the green plant bug compounded by the diatomite with the special shape and the buprofezin.

TABLE 21 toxicity test results of Apolygus lucorum mixed by diatomaceous earth and buprofezin in special shapes

(7) And (3) measuring the combined toxicity of the specially-shaped diatomite and the buprofezin on the grape aphids.

TABLE 22 toxicity test results of blending special-shaped diatomaceous earth and buprofezin to grape aphid

Referring to the method in NY/T1154.14-2008 standard, the thiazine ketone insecticide and dinotefuran insecticide provided in examples 1, 4, 6, 8, 13, 14, 16 and 19 were dissolved by heating agar (1%) solution by the leaf dipping method, and then the solution was taken out of a 20mL to 200mL beaker and condensed at room temperature for use. Soaking the leaves in a test solution for 10 seconds, taking out, naturally drying the leaves, washing the leaves for 1 hour at the water drop rate of 3 drops/second to simulate rainfall, after drying, sticking the leaves on the surface of the solidified agar solution, wrapping petioles with wet cotton balls, putting 3-4 leaves in each beaker, inoculating adult bemisia alba, wherein the number of the adult bemisia alba is about 15 per beaker, sealing the opening of the beaker with a preservative film, puncturing a small hole with a needle on the film for ventilation, repeating the treatment for 4 times, culturing the beaker in an observation room after the treatment is finished, checking the death condition of the test insects after 72 hours, and recording the death condition of the test insects, wherein the thiazine ketone insecticide provided in example 1 is found to be remarkably reduced compared with the death quantity of the test insects without simulating rainfall, while the death quantity of the test insects in example 4 is reduced compared with the death quantity of the test insects without simulating rainfall, and in addition, the death quantities of the test insects in examples 7, 9 and example 4 are compared, the number of test insect deaths of example 13, example 14 and example 4 was found by ranking from high to low as example 4> example 7> example 9, example 4> example 13> example 14; in addition, when the dinotefuran insecticide provided in examples 16 and 19 is compared with the number of test insect deaths of examples 16 and 19 without simulated rainfall, the number of test insect deaths of example 16 after simulated rainfall is greatly reduced compared with the number of test insect deaths without simulated rainfall, while the number of test insect deaths of example 19 is reduced compared with the number of test insect deaths without simulated rainfall.

3. Suspension percentage: the suspension rates of the thiazine ketone insecticide and dinotefuran insecticide in the form of wettable powder provided in the examples were determined by the method of GB/T14825-.

4. Wettability: the wetting time of the thiazine ketone insecticide and the dinotefuran insecticide in the wettable powder preparation provided by the embodiment is measured, and is rated as 1-5 according to the wetting time, wherein the wetting time of 5 is more than 120s, the wetting time of 4 is more than 80s and less than or equal to 120s, and the wetting time of 3 is more than 60s and less than or equal to 80 s; the wetting times for grade 2 were greater than 40s and less than or equal to 60s, and for grade 1 were less than or equal to 40s, the results are shown in Table 23.

5. And (3) hot-pressing stability: the thiazine ketone insecticide and dinotefuran insecticide in the formulation of water dispersible granules provided in example were extruded at a pressure of 60g/cm3 and placed in an oven at 50 ℃, and the state of the water dispersible granules after 24 hours was observed and rated, wherein grade 1 was no caking and caking, grade 2 was slightly caking and no caking, grade 3 was age-increased and no caking, grade 4 was significant caking and slightly caking, grade 5 was significant caking, and the results are shown in table 23.

TABLE 23 Performance characterization test

Examples	Suspension property	Wettability	Stability of hot pressing
				4	Level 1	Level 1	Level 1
7	Stage 2	Grade 3	Grade 3
				8	Stage 2	4 stage
9	Grade 3	Stage 2
				10	4 stage	Grade 3
11	Stage 2	4 stage
				12	4 stage	Grade 3
13	Grade 3	Level 1	Stage 2
				14		Level 1	Grade 3
15		Stage 2	Grade 5
				19	Level 1	Level 1	Level 1

From the test results shown in tables 5-22, the insecticidal composition provided by the invention is compounded by the special-shaped diatomite and the buprofezin or dinotefuran, and can play a synergistic effect when the weight ratio of the special-shaped diatomite to the buprofezin is (1: 40) - (100: 1) or the weight ratio of the special-shaped diatomite to the dinotefuran is (1: 60) - (400: 1), so that the insecticidal composition has good insecticidal effects on various pests such as citrus red spider, citrus scale insect, frankliniella occidentalis, aleyrodida vaporis, lirioides pulvinosa, liriomyza sativae, prodenia litura, tea lesser leafhopper, tea yellow thrips, tea looper, green plant bug and grape aphid, can be prepared into various dosage forms such as wettable powder, water dispersible granules and the like, and meets the standards of suspension property, wettability, hot-pressing stability and the like; further, the applicant found that when diatomaceous earth of a specific shape is added, the entry of active ingredients such as buprofezin or dinotefuran into soil or rivers with rainwater can be reduced to reduce environmental pollution, and when the applicant performed a rainfall simulation experiment, it was found through the experiments of examples 4, 6, 8, 13, 14, 16 and 19 that when the wettability is too large, the falling of the active ingredients with rainwater is rather promoted, and it is necessary to balance the wetting and adhesion of the composition to the plant surface.

The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.

Claims

1. The insecticidal composition is characterized in that raw materials for preparing the insecticidal composition comprise special-shaped diatomite and an active ingredient, wherein the special-shaped diatomite is saw-toothed, and the active ingredient is buprofezin or dinotefuran.

2. The special-shaped diatomite-containing insecticidal composition according to claim 1, wherein the insecticidal composition further comprises a wetting agent, and the wetting agent accounts for 6-10 wt% of the total weight of the special-shaped diatomite and the active ingredient.

3. The special-shaped diatomite-containing insecticidal composition according to claim 2, wherein the wetting agent is one or more selected from the group consisting of sodium lauryl sulfate, sodium alkylnaphthalene sulfonate, fatty alcohol polyglycol ether sulfate, fatty alcohol polyoxyethylene ether carboxylate, alkylnaphthalene sulfonate, fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether carboxylate, nonylphenol polyoxyethylene ether, sorbitan fatty acid ester polyoxyethylene ether, and alkylnaphthalene formaldehyde.

4. The special-shaped diatomite-containing insecticidal composition according to claim 2, wherein a raw material for preparing the insecticidal composition further comprises a dispersing agent, and the dispersing agent accounts for 6-10 wt% of the total weight of the special-shaped diatomite and the active ingredient.

5. The insecticidal composition according to claim 4, wherein said dispersing agent is selected from one or more of lignosulfonate, sodium polyacrylate, polycarboxylate, methylenedinaphthalene sulfonate, calcium alkylbenzene sulfonate salt, amine alkylbenzene sulfonate salt, sodium methylenedinaphthalene sulfonate formaldehyde condensate, polyoxyethylene polyoxypropylene block copolymer, carboxymethyl cellulose, polyvinyl alcohol, polyvinyl pyrrolidone, sodium tripolyphosphate, and alkyl naphthalene sulfonate polycondensate.

6. The special-shaped diatomite-containing insecticidal composition according to claim 1, wherein a preparation raw material of the insecticidal composition further comprises a filler, and the filler accounts for 10-15 wt% of the total weight of the special-shaped diatomite and the active ingredient.

7. The special-shaped diatomite-containing insecticidal composition according to any one of claims 1 to 6, wherein the dosage form of the insecticidal composition is wettable powder and/or water dispersible granules.

8. A thiazine ketone insecticide is characterized in that a preparation raw material of the thiazine ketone insecticide comprises the insecticidal composition of any one of claims 1 to 9, and the weight ratio of the diatomite with the special shape to the buprofezin is (1: 40) - (100: 1).

9. A dinotefuran insecticide, which is characterized in that a preparation raw material of the dinotefuran insecticide comprises the insecticidal composition of any one of claims 1 to 7, and the weight ratio of the special-shaped diatomite to the dinotefuran is (1: 60) - (400: 1).

10. The use of the insecticidal composition according to any one of claims 1 to 7, characterized in that it is used for controlling plant pests.