CN111213647A

CN111213647A - Novel insecticidal pesticide composition and preparation method thereof

Info

Publication number: CN111213647A
Application number: CN202010114008.6A
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: 2020-06-02

Abstract

The invention relates to the technical field of pesticides, in particular to a novel insecticidal pesticide composition and a preparation method thereof. A novel insecticidal pesticide composition comprises diatomite with a specific structure and a raw pesticide substance as effective components, wherein the mass ratio of the diatomite with the specific structure to the raw pesticide substance is (1: 40) - (300: 1); the active pharmaceutical ingredients are selected from any one of thiodicarb, bendiocarb and ethiprole. The invention provides a novel insecticidal pesticide composition, which is prepared by mixing diatomite and a raw material medicament in a special structure, can achieve the effect of preventing and controlling pests under the using amount of a small amount of raw material medicament, and simultaneously, the developed novel diatomite and the developed complex system of the raw material medicament have higher co-toxicity coefficient, can reduce the selective pressure generated by singly and continuously using the medicament to prevent and control the pests, slow down the development of the drug resistance of the pests, reduce the using amount of the pesticides, reduce the environmental pollution, increase the grain safety, and accord with the national policy of reducing the using amount of fertilizers and pesticides.

Description

Novel insecticidal pesticide composition and preparation method thereof

Technical Field

The invention relates to the technical field of pesticides, in particular to a novel insecticidal pesticide composition.

Background

Thiodicarb is a broad-spectrum, quick-acting insecticide, is effective for various pests of aphid, bollworm, etc., and can be used for crops of grain, cotton, vegetable, tobacco and fruit, etc. The carbofuran has contact poisoning and stomach poisoning effects on pests, is mainly used for controlling sanitary pests such as cockroaches, crickets, ants, bedbugs and the like, and can also be used for controlling soil treatment and underground pests. Ethiprole belongs to a second generation of insecticide acting on GABA, is effective to various chewing and piercing-sucking pests under low consumption, can be used for seed treatment and leaf surface spraying, and has a lasting period of 21-28 days.

Diatomaceous earth is a white soft sedimentary stone that can be easily ground into powder. Low density, porous, rough feeling, and is a fossil of diatom. The common diatomite has insecticidal action, damages the outer wax-like layer of the exoskeleton of insects by physical adsorption, leads the insects to die by dehydration, and can be used as an insecticide, but the insecticidal effect is not obvious, and the common diatomite is often only useful for certain specific insects, so the common diatomite is only used as an adsorbent in pesticides.

However, in the current market, a single medicament is continuously used for preventing and treating pests for a long time, so that the pests are easy to generate drug resistance, and meanwhile, pesticide is applied in a large amount due to the generation of the drug resistance, so that the residual pesticide amount in the environment is increased, hidden dangers are brought to the ecological environment and the grain safety, and the national policy of reducing the using amount of fertilizer and pesticide is not met.

Disclosure of Invention

In order to solve the technical problems, the invention provides a novel insecticidal pesticide composition, which comprises diatomite with a specific structure and a raw pesticide substance as effective components, wherein the mass ratio of the diatomite with the specific structure to the raw pesticide substance is (1: 40) - (300: 1); the active pharmaceutical ingredients are selected from any one of thiodicarb, bendiocarb and ethiprole.

As a preferable technical scheme, the diatomite with the specific structure has a sawtooth-shaped honeycomb structure.

As a preferable technical scheme, the mass ratio of the diatomite with the specific structure to the thiodicarb is (1: 60) - (150: 1).

In a preferable embodiment, the mass ratio of the diatomite with the specific structure to the bendiocarb is (1: 60) - (150: 1).

In a preferable embodiment, the mass ratio of the diatomaceous earth with the specific structure to the ethiprole is (1: 40) - (150: 1).

As a preferable technical scheme, the composition is any one preparation formulation prepared by taking diatomite with a specific structure and original medicine substances as active ingredients and compounding with pesticide auxiliary agents.

As a preferable technical scheme, the pesticide auxiliary agent is selected from one or more of an adsorbent, a dispersing agent, a wetting agent, a tackifier and a synergist.

As a preferable technical scheme, the preparation formulation is any one of missible oil, suspending agent, wettable powder, granules, aqueous solution, poison bait, mother solution and mother powder.

As a preferable technical scheme, the content of the effective components in the composition is 0.001-99.999 wt%.

As a preferable technical scheme, the content of the effective components in the composition is 30-70 wt%.

In a second aspect, the present invention provides a method for preparing a wettable powder containing the pesticidal composition as described above, comprising the steps of: weighing effective components and pesticide adjuvant, and performing high-speed universal pulverization; and adding diatomite with a specific structure, shaking, transferring into a flask, stirring and mixing for 30min by using a stirrer, and fully and uniformly mixing.

In a third aspect, the present invention provides a method for preparing a wettable powder containing the pesticide composition as described above, comprising the steps of: weighing effective components and pesticide adjuvant, and performing high-speed universal pulverization; and adding diatomite with a specific structure into the flask, shaking, transferring the mixture into the flask, stirring and mixing the mixture for 30min by using a stirrer, fully and uniformly mixing the mixture, and then granulating the mixture.

Has the advantages that: the invention provides a novel insecticidal pesticide composition, which is prepared by mixing diatomite and a raw material medicament in a special structure, can achieve the effect of preventing and controlling pests under the using amount of a small amount of raw material medicament, and simultaneously, the developed novel diatomite and the developed complex system of the raw material medicament have higher co-toxicity coefficient, can reduce the selective pressure generated by singly and continuously using the medicament to prevent and control the pests, slow down the development of the drug resistance of the pests, reduce the using amount of the pesticides, reduce the environmental pollution, increase the grain safety, and accord with the national policy of reducing the using amount of fertilizers and pesticides.

Drawings

Fig. 1 is an optical microscope of the diatomite having a specific structure of the saw-toothed honeycomb structure according to the present invention.

FIG. 2 is an electron micrograph of a specific structure diatomaceous earth having a saw-toothed honeycomb structure according to the present invention.

Detailed Description

Unless otherwise indicated, implied from the context, or customary in the art, all parts and percentages herein are by weight and the testing and characterization methods used are synchronized with the filing date of the present application. To the extent that a definition of a particular term disclosed in the prior art is inconsistent with any definitions provided herein, the definition of the term provided herein controls.

The technical features of the technical solutions provided by the present invention are further clearly and completely described below with reference to the specific embodiments, and the scope of protection is not limited thereto.

The words "preferred", "preferably", "more preferred", and the like, in the present invention, refer to embodiments of the invention that may provide certain benefits, under certain circumstances. However, other embodiments may be preferred, under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention. The sources of components not mentioned in the present invention are all commercially available.

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 "diatomaceous earth and raw medicinal materials having specific structures" means: the diatomite with a specific structure and the original medicine substance can be mixed and packaged together and used together when in use; further comprising: the diatomite with a specific structure and the original medicine substances are separately packaged and mixed together according to a proportion when in use.

(diatomaceous earth of specific structure)

The diatomite with the specific structure is diatomite with the specific crystal structure, and the general diatomite contains a small amount of Al besides the main component of silicon dioxide₂O₃、Fe₂O₃CaO, MgO, etc., and organic matter. The diatomite with a specific structure is diatomite with a specific sawtooth-shaped honeycomb structure silicon dioxide content after being purified.

In a preferred embodiment, the specially structured diatomaceous earth has a saw-tooth honeycomb structure.

In a preferred embodiment, the silica with a specific saw-tooth-shaped honeycomb structure can be diatomite with a specific structure under the trade name of Celite610 from the company of viry stones france. As shown in FIGS. 1 and 2, under an optical microscope and an electron microscope, Celite610 can be seen to have a clear saw-toothed honeycomb structure.

The optical micrograph was measured by an OLYMPUS C X31 biomicroscope (16X 40 times, Olympus, Japan); the electron micrographs were determined by conventional methods.

On one hand, the diatomite with the specific structure has a larger specific surface area due to the saw-tooth-shaped honeycomb structure, and is favorable for being better adsorbed on a wax layer on the body surface of the insect, so that the insect body is quickly dehydrated. On the other hand, due to the zigzag honeycomb structure, the composition is beneficial to causing damage to a wax layer on the surface of the insect body, tearing the surface of the insect body, rapidly permeating into the insect body and causing fatal damage to the insect, thereby improving the lethality of the composition.

The synergistic effect of the thiodicarb, the bendiocarb and the ethiprole can be realized by the synergistic effect of the thiodicarb, the bendiocarb and the ethiprole with the participation of pesticide auxiliary agents, the epidermis of an insect is quickly pierced by the diatomite with the structure, the raw pesticide substance can quickly permeate under the driving of the diatomite to cause the respiratory and digestive function disorder of the insect, the control efficiency of the composition on the insect is obviously improved under the synergistic effect of the raw pesticide substance and the diatomite with the specific structure, and the fast acting performance and the lethality are very high.

(thiodicarb)

The Thiodicarb (Thiodicarb) is a broad-spectrum and quick-acting insecticide, is effective to various pests such as aphids, cotton bollworms and the like, and can be used for crops such as grains, cotton, vegetables, tobacco, fruits and the like. The insecticidal activity is similar to that of methomyl, and the toxicity is lower than that of methomyl. Belongs to carbamyl oxime pesticide, and is a cholinesterase inhibitor. The spray of stem and leaf and the treatment of seed for many crops have certain contact killing and stomach poisoning effects.

In a preferred embodiment, the mass ratio of the diatomaceous earth with the specific structure to the thiodicarb is (1: 60) - (150: 1).

In a preferred embodiment, the mass ratio of the diatomite with the specific structure to the thiodicarb is (1: 60) - (50: 1).

In a preferred embodiment, the mass ratio of the diatomaceous earth with a specific structure to thiodicarb is (1: 50) - (40: 1).

In some preferred embodiments: the mass ratio of the diatomite and the thiodicarb with the specific structure can be 1:50, 1:49, 1:48, 1:47, 1:46, 1:45, 1:44, 1:42, 1:41, 1:40, 1:39, 1:38, 1:37, 1:36, 1:35, 1:34, 1:33, 1:32, 1:31, 1:30, 1:29, 1:28, 1:27, 1:26, 1:25, 1:24, 1:22, 1:21, 1:20, 1:19, 1:18, 1:17, 1:16, 1:15, 1:14, 1:13, 1:12, 1:11, 1:10, 1:9, 1:8, 1:7, 1:6, 1:5, 1:4, 1:3, 1:2, 1:1, 1:5, 1:4, 1:9, 1:8, 1:7, 1:6, 1: 5:4, 1: 3:4, 1:2, 1:1, 1:6, 12:1, 13:1, 14:1, 15:1, 16:1, 17:1, 18:1, 19:1, 20:1, 21:1, 22:1, 23:1, 24:1, 25:1, 26:1, 27:1, 28:1, 29:1, 30:1, 31:1, 32:1, 33:1, 34:1, 35:1, 36:1, 37:1, 38:1, 39:1, 40:1, 2:3, 3:2, 2:5, 5:2, 3:4, 4:3, 5:2, 2:5, 5:3, 3:5, 5:4, 4: 5.

(bendiocarb)

The bendiocarb and the pesticide are pure white solids, and have melting points of 128-130 ℃. The solubility in water is 0.04g/L, and the product is easily dissolved in acetone and dimethyl sulfoxide. The carbamate pesticide is prepared by reacting 2, 2-dimethyl-4-hydroxy-1, 3-dioxane formed by pyrogallic acid and 2, 2-dimethoxypropane with methyl isocyanate. The carbofuran has contact poisoning and stomach poisoning effects on pests, is mainly used for controlling sanitary pests such as cockroaches, crickets, ants, bedbugs and the like, and can also be used for controlling soil treatment and underground pests.

In a preferred embodiment, the mass ratio of the diatomite with the specific structure to the bendiocarb is (1: 60) - (150: 1).

In a preferred embodiment, the mass ratio of the diatomite with the specific structure to the bendiocarb is (1: 60) - (100: 1).

In a preferred embodiment, the mass ratio of the diatomite with the specific structure to the bendiocarb is (1: 50) - (40: 1).

In some preferred embodiments: the mass ratio of the diatomite and the bendiocarb with the specific structure can be 1:50, 1:49, 1:48, 1:47, 1:46, 1:45, 1:44, 1:42, 1:41, 1:40, 1:39, 1:38, 1:37, 1:36, 1:35, 1:34, 1:33, 1:32, 1:31, 1:30, 1:29, 1:28, 1:27, 1:26, 1:25, 1:24, 1:22, 1:21, 1:20, 1:19, 1:18, 1:17, 1:16, 1:15, 1:14, 1:13, 1:12, 1:11, 1:10, 1:9, 1:8, 1:7, 1:6, 1:5, 1:4, 1:3, 1:2, 1:1, 1:5, 1:4, 1:9, 1:8, 1:7, 1:6, 1: 5:4, 1: 3:4, 1:2, 1:1, 1:1, 1:6, 12:1, 13:1, 14:1, 15:1, 16:1, 17:1, 18:1, 19:1, 20:1, 21:1, 22:1, 23:1, 24:1, 25:1, 26:1, 27:1, 28:1, 29:1, 30:1, 31:1, 32:1, 33:1, 34:1, 35:1, 36:1, 37:1, 38:1, 39:1, 40:1, 2:3, 3:2, 2:5, 5:2, 3:4, 4:3, 5:2, 2:5, 5:3, 3:5, 5:4, 4: 5.

(ethiprole)

The Ethiprole is an insecticide and acaricide discovered by Ronapplanck and developed by Bayer company, belongs to a second generation insecticide acting on GABA, is effective to various chewing and piercing-sucking pests under low consumption, can be used for seed treatment and leaf surface spraying, and has a lasting period of 21-28 days. (mainly used for preventing and controlling thrips, stinkbug, weevil, beet armyworm, aphid, plant hopper, locust and the like, and also shows activity to some whitefly (especially has strong activity to the extremely difficult-to-control rice pest rice green stink bug).

In a preferred embodiment, the mass ratio of the diatomite with the specific structure to the ethiprole is (1: 40) - (150: 1).

In a preferred embodiment, the mass ratio of the diatomite with the specific structure to the ethiprole is (1: 40) - (100: 1).

In a preferred embodiment, the mass ratio of the diatomite with the specific structure to the ethiprole is (1: 40) - (50: 1).

In some preferred embodiments: the mass ratio of the diatomite and the ethiprole with the specific structure can be 1:40, 1:39, 1:38, 1:37, 1:36, 1:35, 1:34, 1:33, 1:32, 1:31, 1:30, 1:29, 1:28, 1:27, 1:26, 1:25, 1:24, 1:22, 1:21, 1:20, 1:19, 1:18, 1:17, 1:16, 1:15, 1:14, 1:13, 1:12, 1:11, 1:10, 1:9, 1:8, 1:7, 1:6, 1:5, 1:4, 1:3, 1:2, 1:1, 2:1, 3:1, 4:1, 5:1, 6:1, 7:1, 8:1, 9:1, 10:1, 11:1, 12:1, 1: 13:1, 1:1, 1:1, 22:1, 23:1, 24:1, 25:1, 26:1, 27:1, 28:1, 29:1, 30:1, 31:1, 32:1, 33:1, 34:1, 35:1, 36:1, 37:1, 38:1, 39:1, 40:1, 41:1, 42:1, 43:1, 44:1, 45:1, 46:1, 47:1, 48:1, 49:1, 50:1, 2:3, 3:2, 2:5, 5:2, 3:4, 4:3, 5:2, 2:5, 5:3, 3:5, 5:4, 4: 5.

In some embodiments, other active ingredients of pesticides may be added in appropriate amounts in addition to the preferred active ingredients of the present invention (diatomaceous earth of specific structure and thiodicarb/bendiocarb/ethiprole), and the present invention is not particularly limited to the other active ingredients of pesticides and may be insecticides, bactericides, herbicides, and the like, which are conventionally added in the art.

As the kind of the conventional insecticide, bactericide, herbicide, specifically, the following may be mentioned.

(insecticides)

BT, CVMP, CVP, CYAP, DDVP, DEP, MEP, MIPC, NAC, PHC, acetamiprid, acephate, oxazaphos, imidacloprid, ethofenprox, clothianidin, chlorthion, cyhalothrin, silafluofen, wireworm, plegia, pleocidin, diazinon, thiamethoxam, thiodicarb, tebufenozide, teflubenzuron, tralomethrin, bifenthrin, pyridaphenthion, fenobucarb, ブルウエルア & ロウカルア, prothiofos, permethrin microcapsules, permethrin, monosulfuron, methomyl, monocrotophos, flupropathrin, fipronil, fluazuron, flufenoxuron, lufenuron, flubencarb, tefluthrin, transfluthrin and the like.

(Bactericide)

TPN, azoxystrobin, iprodione, isoprothiolane, iminoctadine, imazalil, clomazole, carboxin, captan, kresoxim-methyl, dicyclopentenyl, cyproconazole, simeconazole, sulfur hydrate, thiuram, thiophanate-methyl, thifluzamide, tetraconazole, tebuconazole, triadimefon, tolclofos-methyl, triflumizole, triforine, tolclofos-methyl, validamycin A, bitertanol, hydroxyisoxazole, clomeprop, fenarimol, ferimzone, flutolanil, procymidone, propamocarb hydrochloride, propiconazole, benomyl, pencycuron, fosetyl-aluminum, polyoxin D zinc salt, foamectin, mike, milbemycin, metalaxyl, mefenoxamine, organo-copper and the like.

(herbicides)

2,4-PA, CAT, MCP, isopropylamine salt, MDBA, SAP, asulam, glufosinate, alachlor, isoxaben, imazaquin, pyrazosulfuron, ethoxysulfuron, oxadiargyl, metamitron, oryzalin, pyraclonil, tolfen-zachlor, xanthomonas campestris, cyanazine, cyclosulfamuron, dithiopyr, cyclosulfamuron, cinosulfuron, cinmethylin, dimethenamid, triaziflam, triclopyr, trifloxysulfuron sodium, epinapropamide, halosulfuron, bifenox, pyributicarb, butafosinate, butafenin, propafen, penoxsulam, florasulam, trifluofen, pendimethalin, 2-methyl-4-chloropropionate calcium salt, metsulfuron, cyclam, fluroxypyr, thiazopyr and the like.

In addition, in the pesticidal composition of the present invention, an additive effect or a significant synergistic effect can be obtained by using the active ingredients (diatomaceous earth of a specific structure and thiodicarb/bendiocarb/ethiprole) in combination with other pesticidal adjuvants.

In some embodiments, the composition is any dosage form prepared by compounding diatomite with a specific structure and a raw drug substance as active ingredients and a pesticide auxiliary agent.

In some embodiments, the pesticide adjuvant is selected from one or more of an adsorbent, a dispersant, a wetting agent, a viscosifier, and a synergist.

In a preferred embodiment, the content of the effective component in the composition is 0.001 to 99.999 wt%.

In a preferred embodiment, the content of the effective component in the composition is 30 to 70 wt%.

In a preferred embodiment, the content of the effective component in the composition is 40 to 60 wt%.

For example, as the pesticide adjuvant, specifically, the following dispersants can be mentioned.

(dispersing agent)

The dispersant of the present invention is an acrylic polymer. The molecular weight of the dispersant is generally larger, and the dispersant is more effective than a micromolecular dispersant.

In some embodiments, the dispersant is a sulfonate, polycarboxylate, such dispersant may preferably be KY-R01, KY-F02, both available from Jiangsu Keyuan science and technology, Inc.

In some embodiments, the dispersant is an acrylic polymer; and the preferred acrylic polymer is comb graft polymer KY-F01, available from Jiangsu Kaiyuan technology Co.

In some embodiments, the dispersant may be SOPA-270, TSPE-S, both available from Jiangsu Keyuan technology, Inc.

KY-F01 is a high molecular surfactant with comb-shaped structure characteristics formed by graft copolymerization of a long chain with a strong lipophilic skeleton and hydrophilic anionic low molecules, and the original drug is difficult to wet due to strong hydrophobicity, so the invention is based on the adsorption of diatomite with a specific structure and the hydrophobic drugs; the inventor has the surprise that when KY-F01 and the original drug are adopted to act, the wetting time can be effectively reduced, and the comb-shaped structure of KY-F01 can be matched with the diatomite with the specific structure to be well adsorbed on the surface of the diatomite, and the hydrophobic original drug is tightly coated by KY-F01 after being adsorbed by the diatomite with the specific structure, so that the wetting time is obviously reduced.

In the research, the inventor unexpectedly finds that when a proper amount of polyoxyethylene ether sulfonate dispersant is compounded in the raw drug system, the suspension rate is obviously improved, for example, the dispersant can be SOPA-270 and TSPE-S, and probably both the SOPA-270 and the TSPE-S contain aromatic rings and aliphatic hydrophobic groups, and the oxygen content of the dispersant and the aromatic rings and aliphatic hydrophobic groups is high, the hydrophobic effect with thiodicarb/bendiocarb/ethiprole is strong, so that the binding force with the raw drug is improved, therefore, the whole particle surface is provided with a plurality of anchoring points, KY-F01 forms multi-point anchoring through the action of dipolar force, and the dispersed medium has enough space stability and electrostatic stability, and finally, the invention is obtained as KY-F01: SOPA-270/TSPE-S ═ 6: (3-4) is most preferable.

In the present invention, in addition to the above-mentioned essential components, other agricultural chemical adjuvants such as an extender, a component stabilizer, a physical property improving agent, etc. which are conventionally used may be added in an appropriate amount as required.

As such a pesticide adjuvant, either solid or liquid; examples of the inorganic fine powder include, but are not limited to, fine mineral powders such as white carbon, clays, calcium carbonate, bentonite, talc, diatomaceous earth, calcium stearate, and colloidal silica, organic or inorganic acid salts such as ammonium sulfate, ammonium hydrogen carbonate, ammonium nitrate, ammonium chloride, potassium chloride, sodium sulfate, magnesium sulfate, sodium citrate, sodium carbonate, and sodium hydrogen carbonate, organic acids such as citric acid and succinic acid, sugars such as sucrose, lactose, and xanthan gum, and water-soluble fine powders such as urea.

In some embodiments, the formulation of the pesticidal composition of the present invention is selected from any one of emulsifiable concentrate, suspension, wettable powder, granule, aqueous agent, poison bait, mother liquor, mother powder.

Among them, wettable powder (wetteapowder) can be produced by air pulverization using a jet mill; the water dispersible powder (Waterdispersablegranule) can be produced by adding water to the wettable powder, kneading, extruding, drying, and granulating.

In a third aspect, the present invention provides a method for preparing a water dispersible powder comprising the pesticidal composition as described above, comprising the steps of: weighing effective components and pesticide adjuvant, and performing high-speed universal pulverization; and adding diatomite with a specific structure into the flask, shaking, transferring the mixture into the flask, stirring and mixing the mixture for 30min by using a stirrer, fully and uniformly mixing the mixture, and then granulating the mixture.

In order to avoid destroying the structure of the Celite610, in the preparation process, mechanical pulverization is not used after the Celite610 is added, but stirring and mixing are carried out; the high-speed universal crushing is carried out by adopting a DTF-50 high-speed universal crusher (Shanghai Xinnuo instruments and equipment Co., Ltd.), and the stirring after adding the diatomite with the specific structure is carried out by adopting a RW20IKA digital display stirrer (Germany IKA group).

In the invention, when the original drug substance in the pesticide composition is any one of thiodicarb, bendiocarb and ethiprole, the pesticide composition can be prepared into wettable powder after being prepared; in addition, when the original drug substance in the pesticide composition is thiodicarb, the thiodicarb can be prepared into water dispersible powder, and the two dosage forms can be diluted with water and the like and applied to plants, water surfaces or soil. In addition, the preparation can also be used in combination with other bactericides, herbicides, insecticides, fertilizers, soil conditioners, and the like.

The fourth aspect of the invention provides application of the pesticide composition preparation in preventing and controlling liriomyza sativae, prodenia litura, tea geometrid, frankliniella occidentalis, tea thrips flavivis, trialeurodes vaporariorum, tea lesser leafhopper, green plant bug and grape aphid.

The present invention is described in detail below with reference to examples, which are provided for the purpose of further illustration only and are not to be construed as limiting the scope of the present invention, and the insubstantial modifications and adaptations thereof by those skilled in the art based on the teachings of the present invention will still fall within the scope of the present invention.

Example 1

Example 1 diatomaceous earth Celite610 with a particular structure replicates the combined virulence of different pests with different bulk drug substances;

diatomaceous earth, Celite610, a specific structure, gareli, france.

Pests: leaf miner, prodenia litura, tea geometrid, frankliniella occidentalis, tea yellow thrips, trialeurodes vaporariorum, tea lesser leafhopper, lygus lucorum and grape aphid.

Wherein, the diatomite Celite610 with a specific structure is abbreviated as: t;

when the active compound substance is thiodicarb, the thiodicarb is abbreviated as follows: a;

when the active compound is bendiocarb, the thiodicarb is abbreviated as follows: a;

when the raw material medicine is ethiprole, the thiodicarb is abbreviated as follows: a;

t: A ═ (100: 1) indicates that the mass ratio of T to A is 100: 1;

t: A ═ (50: 1) indicates that the mass ratio of T to A is 50: 1;

t: A ═ (1: 1) indicates that the mass ratio of T to A is 1: 1;

t: A ═ (1: 20) indicates that the mass ratio of T to A is 1: 20;

t: A ═ (1: 30) indicates that the mass ratio of T to A is 1: 30;

t: A ═ (1: 40) indicates that the mass ratio of T to A is 1: 40;

t: A (1: 60) means that the mass ratio of T to A is 1: 60.

(1) Co-toxicity coefficient (CTC) screening: combined virulence assay for Celite610 and thiodicarb against 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 (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

TABLE 1 toxicity test results of mixing Celite610 and thiodicarb against spodoptera litura

(2) Co-toxicity coefficient (CTC) screening: and (3) determining the combined toxicity of the Celite610 and the thiodicarb compound to the 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, after soaking the leaf dish in the liquid of testing medicine for 10 seconds, 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 air naturally the back, 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, cover the dish lid, arrange the indoor culture of observation, the fresh no medicine leaf dish of circumstances interpolation during.

And 5d, detecting the death condition of the test insects, and recording, wherein the death judgment standard of the test insects is that no response is calculated when the tweezers lightly contact the test insects.

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.

TABLE 2 toxicity test results of Celite610 and thiodicarb mixture against spodoptera litura

(3) Co-toxicity coefficient (CTC) screening: and (3) determining the combined toxicity of the Celite610 and thiodicarb compounded on tea leaf 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.

Table 3 toxicity test results of Celite610 and thiodicarb mixed on tea geometrid

(4) Co-toxicity coefficient (CTC) screening: and (3) testing the combined toxicity of the Celite610 and the bendiocarb 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 (4) after 72h, checking and recording the death condition of the test insects, wherein the death judgment standard of the test insects is that the test insects are dead as the result of no response when the pointed writing brush is lightly contacted with the test insects.

TABLE 4 toxicity test results of Celite610 and bendiocarb mixture on Frankliniella occidentalis

(5) Co-toxicity coefficient (CTC) screening: combined virulence determination of Celite610 and oxacloprid for liriomyza sativae.

TABLE 5 toxicity test results of Celite610 and bendiocarb mixed pairing of Liriomyza sativae

(6) Co-toxicity coefficient (CTC) screening: and (3) testing the combined toxicity of the Celite610 and the bendiocarb 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 after 72h, examining the death condition of the test insects under a dissecting mirror, and recording, wherein the death judgment standard of the test insects is that the test insects die because the test insects are not reacted when the pointed writing brush is lightly contacted with the test insects.

TABLE 6 toxicity test results of mixture of Celite610 and bendiocarb on tea leaf thrips

(7) Co-toxicity coefficient (CTC) screening: and (3) testing the combined toxicity of the Celite610 and the ethiprole on the Frankliniella occidentalis.

TABLE 7 toxicity test results of Celite610 and ethiprole mixed on Frankliniella occidentalis

(8) Co-toxicity coefficient (CTC) screening: and (3) testing the combined toxicity of the Celite610 and the ethiprole 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 (4) after 72h, detecting the death condition of the test insects, and recording, wherein the death judgment standard of the test insects is that no response is calculated when the tweezers lightly contact the test insects.

TABLE 8 toxicity test results of Celite610 and ethiprole mixed against Bemisia alba

(9) Co-toxicity coefficient (CTC) screening: celite610 and ethiprole were combined with a virulence determination of Liriomyza punctata.

TABLE 9 toxicity test results of Celite610 and ethiprole mixed Papyriproxyfen

(10) Co-toxicity coefficient (CTC) screening: and (3) testing the combined toxicity of the Celite610 and the ethiprole on the 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.

TABLE 10 toxicity test results of mixing Celite610 with ethiprole against spodoptera litura

(11) Co-toxicity coefficient (CTC) screening: and (3) determining the combined toxicity of the Celite610 and the ethiprole on the tea leafhopper.

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 sample is placed in an observation chamber.

TABLE 11 toxicity test results of Celite610 and ethiprole mixed on tea leafhopper

(12) Co-toxicity coefficient (CTC) screening: and (3) testing the combined toxicity of the Celite610 and the ethiprole on the tea leaf thrips.

TABLE 12 toxicity test results of blend of Celite610 and ethiprole on tea leaf thrips

(13) Co-toxicity coefficient (CTC) screening: and (3) determining the combined toxicity of the Celite610 and the ethiprole on tea geometrid by compounding.

TABLE 13 toxicity test results of Celite610 and ethiprole mixed for tea leaf geometrid

(14) Co-toxicity coefficient (CTC) screening: and (3) testing the combined toxicity of the Celite610 and the ethiprole on the green plant bug.

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.

TABLE 14 toxicity assay results for apolygus lucorum by compounding Celite610 with ethiprole

(15) Co-toxicity coefficient (CTC) screening: and (3) testing the combined toxicity of the Celite610 and the ethiprole on the grape aphid.

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.

TABLE 15 toxicity test results of mixture of Celite610 and ethiprole on grape aphid

Examples 2 to 16

Examples 2 to 16 provide a novel pesticidal composition comprising, in mass percent, 25% of diatomaceous earth having a specific structure, 25% of a raw material, a dispersant, and white carbon black to make up to 100%.

Wherein, the diatomite with the specific structure is Celite610 of the France Yirui stone company; the dispersants are of different kinds; white carbon black was purchased from taida chemical technology ltd;

according to the designed formula, the dispersing agent, the white carbon black and the original drug substance are subjected to high-speed universal grinding, so that the dispersing agent, the white carbon black and the original drug substance can be uniformly mixed with each other, and the fineness is reduced; then adding the Celite610, and in order to avoid destroying the structure of the Celite610, mechanical crushing is not used; then shaking, transferring into a flask after 10min, stirring and mixing for 30min by using a stirrer, and fully and uniformly mixing to obtain the wettable powder.

(1) Determination of the wetting time: the wettable powder is poured from a prescribed height into a beaker containing a prescribed amount of standard hard water, and the time to complete wetting is measured according to the method of GB/T5451-2001.

(2) Measurement of suspension percentage: measured according to the method of GB/T14825-2006, a sample to be measured is prepared into suspension by using standard hard water. Under the specified conditions, after standing in a measuring cylinder, measuring the mass fraction of the effective components in the suspension at the bottom of one tenth of the measuring cylinder, and calculating the suspension rate.

TABLE 16 wetting time, suspension percentage of different dispersants

In the above table, the amount refers to the total amount of the dispersant, and when the dispersant is a single substance, the amount is the amount of the substance itself, and when the dispersant is a complex of multiple substances, the amount is the total amount of the complex mixture; a represents that a raw material medicine substance is ethiprole, b represents that the raw material medicine substance is bendiocarb, c represents that the raw material medicine substance is thiodicarb, d represents that the raw material medicine substance is ethiprole, and Celite610 is replaced by common silicon dioxide with the particle size of 5-7 mu m; KY-F01 abbreviation F01; KY-R01 abbreviation R01; SOPA-270 abbreviation SO; TSPE-S abbreviated TP; k12 was purchased from the national drug group; GY-D06 was purchased from Guangyi agricultural chemistry, Inc. of Beijing.

It can be seen that the wetting time of the product is reduced to some extent by adding different types of wetting agents, wherein the most significant dispersant is F01: SO 3:2, SO KY-F01: SOPA-270/TSPE-S ═ 6: (3-4) as the dispersant of the system, the wetting time can be less than 60s, and the suspension percentage is more than 80%.

Claims

1. A novel insecticidal pesticide composition is characterized by comprising diatomite with a specific structure and a raw pesticide substance as effective components, wherein the mass ratio of the diatomite with the specific structure to the raw pesticide substance is (1: 40) - (300: 1); the active pharmaceutical ingredients are selected from any one of thiodicarb, bendiocarb and ethiprole.

2. A novel pesticidal and pesticidal composition according to claim 1, wherein the diatomaceous earth of specific structure has a zigzag honeycomb structure.

3. A novel pesticidal pesticide composition according to claim 2, wherein the mass ratio of the specific-structure diatomaceous earth to thiodicarb is (1: 60) to (150: 1).

4. A novel pesticidal and pesticidal composition according to claim 2, wherein the mass ratio of the specific-structure diatomaceous earth to bendiocarb is (1: 60) to (150: 1).

5. A novel pesticidal and pesticidal composition according to claim 2, wherein the mass ratio of the specific-structure diatomaceous earth to ethiprole is (1: 40) to (150: 1).

6. A novel pesticidal and pesticidal composition according to any one of claims 1 to 5, which is in any form of a formulation comprising a specific-structure diatomaceous earth and a raw material substance as active ingredients, and a pesticidal auxiliary.

7. A novel pesticidal and pesticidal composition according to claim 6, wherein the pesticidal adjuvant is selected from one or more of an adsorbent, a dispersant, a wetting agent, a tackifier and a synergist.

8. A novel pesticidal and pesticidal composition according to claim 6, wherein the formulation is any one selected from the group consisting of emulsifiable concentrate, suspension concentrate, wettable powder, dust, granule, aqueous agent, poison bait, mother liquor and mother powder.

9. A novel pesticidal composition according to claim 6, wherein the content of the active ingredient in the composition is 0.001 to 99.999% by weight.

10. A novel pesticidal composition according to claim 9, wherein the active ingredient is contained in the composition in an amount of 30 to 70 wt%.