CN111183985A - Insecticidal composition containing sawtooth-shaped diatomite and azadirachtin and application thereof - Google Patents

Insecticidal composition containing sawtooth-shaped diatomite and azadirachtin and application thereof Download PDF

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CN111183985A
CN111183985A CN202010106726.9A CN202010106726A CN111183985A CN 111183985 A CN111183985 A CN 111183985A CN 202010106726 A CN202010106726 A CN 202010106726A CN 111183985 A CN111183985 A CN 111183985A
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azadirachtin
diatomite
saw
diatomaceous earth
insecticide
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陈瑞明
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Benson Huizhou Biotechnology Co Ltd
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Benson Huizhou Biotechnology Co Ltd
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/08Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01GHORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
    • A01G13/00Protecting plants
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/12Powders or granules
    • A01N25/14Powders or granules wettable
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/30Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests characterised by the surfactants
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/90Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Environmental Sciences (AREA)
  • Dentistry (AREA)
  • Engineering & Computer Science (AREA)
  • Plant Pathology (AREA)
  • Pest Control & Pesticides (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Agronomy & Crop Science (AREA)
  • Toxicology (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention relates to the technical field of pesticides, and particularly relates to an insecticide containing sawtooth-shaped diatomite and azadirachtin and application thereof. The preparation raw materials of the pesticide comprise, by weight, 60-80 parts of active ingredients, 2-6 parts of wetting dispersants and 2-6 parts of carriers; the effective components comprise saw-tooth diatomite and azadirachtin. The applicant provides an insecticide containing sawtooth-shaped diatomite and azadirachtin, which can expand the insecticidal spectrum by compounding diatomite and azadirachtin in a specific shape according to a certain proportion, and has good insecticidal effects on various plant pests, such as citrus red spiders, citrus scale insects, frankliniella occidentalis, whiteflies, liriomyza sativae, prodenia litura, tea leafhoppers, tea yellow thrips, tea geometrid, green plant bugs, grape aphids and the like; and the applicant has found that by selecting an appropriate wetting dispersant, the wettability, suspendability and stability of the insecticide can be improved and the contamination of the air by the drift of the insecticide powder can be suppressed.

Description

Insecticidal composition containing sawtooth-shaped diatomite and azadirachtin and application thereof
Technical Field
The invention relates to the technical field of pesticides, and particularly relates to an insecticidal composition containing sawtooth-shaped diatomite and azadirachtin and application thereof.
Background
China is a big agricultural country, the damage of pests to agricultural production in China is huge, chemical insecticides are mainly used at present, but the pests are easy to generate resistance by using a single chemical insecticide, in order to achieve the effect of pest control, more toxic pesticides have to be used or the usage amount of the pesticides is increased, so that the economic cost is increased, the safety of agricultural products is influenced, and the natural enemies of a large number of pests are killed, so that the pests are rampant. At present, a large number of mixed insecticides are available in the market, but most of the mixed insecticides are chemical pesticides, have high toxicity to people and livestock, and can generate multiple drug resistances after long-time use, thereby further aggravating the difficulty in pest control.
Aiming at the problems of chemical pesticides, non-chemical control is adopted according to a comprehensive pest control strategy, and the method gradually becomes a new direction for grain storage pest control development. The inert powder is an important means for non-chemical prevention and control of the stored grain pests, and the diatomite pesticide is used as one of the inert powders, has the advantages of good insect prevention and control effect, long protection period, no toxicity to mammals, no environmental pollution and the like, accords with the development direction of green stored grains, and is favored by 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 new-generation algae plants, and the main component of the diatomite is amorphous SiO2. However, the diatomite pesticide is in the beginning stage in China at present, and due to the nature of diatomite, the pesticide is poor in dispersion and wettability.
In addition, the biological insecticide is a direction, has the characteristics of convenient material taking, low cost, long control period, high efficiency, economy, safety, no pollution, high compatibility with the environment and the like, azadirachtin is a compound with the strongest activity separated from the neem, belongs to tetracyclic triterpenes, is a worldwide recognized broad-spectrum, high-efficiency, low-toxicity, easily degradable, residue-free insecticide at present, has no drug resistance, has a killing effect on almost all plant pests, and has no pollution to people, livestock and the surrounding environment. The focus of current development is by selecting suitable non-chemical pesticides in place of chemical pesticides.
Disclosure of Invention
In order to solve the above problems, the present invention provides, in a first aspect, an insecticidal composition comprising diatomaceous earth having a saw-toothed shape and azadirachtin.
As a preferable technical scheme of the invention, the weight ratio of the sawtooth-shaped diatomite to the nimbin is 600: 1-1: 60.
the second aspect of the invention provides an insecticide containing sawtooth-shaped diatomite and azadirachtin, which comprises 60-80 parts by weight of an insecticide composition, 2-6 parts by weight of a wetting dispersant and 2-6 parts by weight of a carrier.
As a preferred technical solution of the present invention, the wetting dispersant is one or more selected from the group consisting of sodium salt of maleic acid-acrylic acid copolymer, ethylene oxide-propylene oxide block copolymer, polycarboxylate, alkyl naphthalene sulfonate formal, polyoxyethylene ether, and lignosulfonate.
As a preferable technical scheme of the invention, the wetting dispersant comprises maleic acid-acrylic acid copolymer sodium salt, and the number average molecular weight is 20000-30000.
As a preferable technical scheme, the wetting dispersant further comprises an ethylene oxide-propylene oxide block copolymer, and the number average molecular weight is 2500-4500.
As a preferable technical scheme of the invention, the weight ratio of the maleic acid-acrylic acid copolymer sodium salt to the ethylene oxide-propylene oxide block copolymer is (2-3): 1.
in a preferred embodiment of the present invention, the carrier is one or more selected from kaolin, white carbon black, magnesium aluminum silicate, anhydrous sodium sulfate, glucose, kaolin, sericite, fructose, and soluble starch.
As a preferable technical scheme, the pesticide has a dosage form selected from one or more of missible oil, wettable powder, water dispersible granules, suspending agents, aqueous emulsion, microemulsion, dispersible oil suspending agents, microcapsule suspending agents and soluble powder.
In a second aspect, the present invention provides a method for preparing the insecticide containing the saw-toothed diatomite and the azadirachtin, which comprises the following steps: mixing and crushing the preparation raw materials of the pesticide except the saw-tooth-shaped diatomite, and then adding the saw-tooth-shaped diatomite for mixing to obtain the pesticide.
In a third aspect, the invention provides an application of the insecticide containing the saw-toothed diatomite and the azadirachtin, which is used for controlling plant pests.
Compared with the prior art, the invention has the following beneficial effects: the applicant provides an insecticide containing sawtooth-shaped diatomite and azadirachtin, which can expand the insecticidal spectrum by compounding diatomite and azadirachtin in a specific shape according to a certain proportion, and has good insecticidal effects on various plant pests, such as citrus red spiders, citrus scale insects, frankliniella occidentalis, whiteflies, liriomyza sativae, prodenia litura, tea leafhoppers, tea yellow thrips, tea geometrid, green plant bugs, grape aphids and the like; and the applicant has found that by selecting an appropriate wetting dispersant, the wettability, suspendability and stability of the insecticide can be improved and the contamination of the air by the drift of the insecticide powder can be suppressed.
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.
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 phrase "containing the diatomite in a zigzag shape and the azadirachtin" means that the diatomite in a zigzag shape and the azadirachtin can be mixed and packaged together and used together when in use; also comprises a package containing the saw-toothed diatomite and the azadirachtin, which are mixed together according to the proportion when in use.
In a first aspect of the invention, there is provided an insecticidal composition comprising diatomaceous earth in a saw-tooth form and azadirachtin, the insecticidal composition comprising diatomaceous earth in a saw-tooth form and azadirachtin.
In a preferred embodiment, the preparation raw materials of the pesticide comprise 70 parts of effective components, 5 parts of wetting and dispersing agents and 5 parts of carriers according to parts by weight.
The second aspect of the invention provides an insecticide containing sawtooth-shaped diatomite and azadirachtin, which comprises 60-80 parts by weight of an insecticide composition, 2-6 parts by weight of a wetting dispersant and 2-6 parts by weight of a carrier.
Active ingredient
The effective component is the insecticidal composition.
In one embodiment, the active ingredients of the present invention comprise saw-tooth diatomaceous earth and azadirachtin.
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.
Azadirachtin is a substance contained in seeds, leaves and barks of neem trees, and is a worldwide recognized pesticide with broad spectrum, high efficiency, low toxicity, easy degradation, no residue and no drug resistance. Azadirachtin belongs to tetracyclic triterpenoids, and the chemical structure of the azadirachtin can be roughly divided into two parts, namely decalin and tricyclic furan, and the azadirachtin contains 16 chiral centers which comprise 7 quaternary carbons, 9 secondary carbons and 16 oxygen atoms. The insecticidal composition has the effect of repelling and killing almost all plant pests, indoor bedbugs, fleas, flies, mosquitoes and the like, and has special effects on preventing and controlling more than 400 agricultural and forestry pests with 10 meshes, storage pests and sanitary pests, particularly the pests of hemiptera lepidoptera, coleoptera and the like. From the chemical structure, the nimbin compounds are very similar to the steroid, steroid and other hormone substances in the insect body, so that the pests are not easy to distinguish whether the nimbin compounds are inherent in the body or imposed outside, and the nimbin compounds can enter the pest body to interfere with the life process of the pests, thereby killing the pests and being not easy to cause the resistance of the pests to the drugs. The structure of the compound is different from that of hormone in vertebrates, so that the compound has no pollution to human, livestock and surrounding environment. The azadirachtin of the present invention may be purchased or self-made, and in a preferred embodiment, is purchased from wuhan woxuan science and technology ltd.
Preferably, the weight ratio of the saw-toothed diatomite to the azadirachtin is 600: 1-1: 60.
applicants found that when the weight ratio of the saw-toothed diatomaceous earth to azadirachtin was controlled to 600: 1-1: the pesticide has good insecticidal effect at 60 hours, and the weight ratio of the serrated diatomite to the nimbin is 600: 1. 300, and (2) 300: 1. 1: 1. 1: 30. 1: 60.
the applicant finds that the insecticidal effect of the insecticide can be increased by adding the saw-toothed diatomite and the azadirachtin for compounding, probably because the saw-toothed diatomite has large specific surface area and special structure, which is favorable for adsorbing the azadirachtin and greatly increasing the adsorption on the surface of pests, thereby causing dehydration of the pests and increasing the utilization rate of the insecticide, in addition, because the special shape of the diatomite is also favorable for tearing the epidermis of the pests and promoting the diatomite to carry the azadirachtin into the pests, wherein the azadirachtin is very similar to hormones such as steroids of the pests, and the azadirachtin entering the pests can interfere the life process of the pests, thereby killing the pests, and because the physical insecticidal effect of the saw-toothed diatomite and the similarity of the azadirachtin and the hormones of the pests, the insecticide resistance to the diatomite and the azadirachtin is not easy to generate, the pesticide has the advantages that the pesticide can increase the effectiveness and the persistence of the pesticide, has good effects on citrus red spiders, citrus scale insects, frankliniella occidentalis, trialeurodes vaporariorum, liriomyza sativae, prodenia litura, tea leafhopper, tea yellow thrips, tea geometrid, lygus lucorum and grape aphids, and in addition, as the difference between the hormone structures of azadirachtin and vertebrates is great, and the harmlessness of the sawtooth-shaped diatomite per se, the good safety of the pesticide can be ensured. However, applicants have unexpectedly found that due to the greater surface tension of the saw-tooth structure, the wetting and dispersion of diatomaceous earth is poor.
Wetting and dispersing agent
The wetting dispersant is an assistant for improving the dispersion efficiency, rheological property and the like of the solid powder.
In one embodiment, the wetting and dispersing agent of the present invention is selected from one or more of maleic acid-acrylic acid copolymer sodium salt, ethylene oxide-propylene oxide block copolymer, polycarboxylate, alkyl naphthalene sulfonate formal, polyoxyethylene ether, and lignosulfonate.
Preferably, the wetting and dispersing agent of the present invention comprises a maleic acid-acrylic acid copolymer sodium salt.
The maleic acid-acrylic acid copolymer sodium salt is the sodium salt of a polymer obtained by copolymerizing maleic acid and acrylic acid, is free of phosphorus, toxicity and pollution, has excellent chelating and dispersing capabilities, and has the number average molecular weight of thousands to tens of thousands. The maleic acid-acrylic acid copolymer sodium salt of the present invention is either self-made or purchased, and when purchased, includes, but is not limited to, basf's CP5 (number average molecular weight of 70000), CP88 (number average molecular weight of 3000), fu mei s PMAS-90 (number average molecular weight of 20000 to 30000).
More preferably, the number average molecular weight of the maleic acid-acrylic acid copolymer sodium salt is 20000-30000; further, the sodium salt of the maleic acid-acrylic acid copolymer is PMAS-90.
The number average molecular weight is the sum of the relative atomic masses of the atoms in the formula, and is the number average molecular weight according to the present invention, as measured according to methods well known in the art.
Further preferably, the wetting and dispersing agent of the present invention further comprises an ethylene oxide-propylene oxide block copolymer.
The ethylene oxide-propylene oxide block copolymer is a block copolymer formed by copolymerizing ethylene oxide and propylene oxide, and the surface activity of the block copolymer can be changed in a large range along with the difference of the sequence, the length and the content of the block in a molecular chain. The ethylene oxide-propylene oxide of the present invention may be purchased or manufactured by oneself, and when purchased, includes, but is not limited to, basf RFE 1720 (number average molecular weight of 2150), RFE 1740 (number average molecular weight of 2650), RFE2035 (number average molecular weight of 4100), RFE 2520 (number average molecular weight of 3100), RFE 2525 (number average molecular weight of 2000), RFE 3110 (number average molecular weight of 3500). In a preferred embodiment, the ethylene oxide-propylene oxide block copolymer of the present invention is RFE 1740 and/or RFE 2035.
More preferably, the number average molecular weight of the ethylene oxide-propylene oxide block copolymer is 2500-4500; furthermore, the number average molecular weight of the ethylene oxide-propylene oxide block copolymer is 4000-4500.
In a preferred embodiment, the weight ratio of the sodium salt of the maleic acid-acrylic acid copolymer and the ethylene oxide-propylene oxide block copolymer is (2-3): 1; further, the weight ratio of the maleic acid-acrylic acid copolymer sodium salt and the ethylene oxide-propylene oxide block copolymer is 2.5: 1.
the applicant found that when maleic acid-acrylic acid copolymer sodium salt and ethylene oxide-propylene oxide block copolymer are added as wetting agent, the wetting and stability of the diatomaceous earth and azadirachtin of the present invention can be increased, and the suspensibility in water can be increased, probably because, by using maleic acid-acrylic acid copolymer with high number average molecular weight and diatomaceous earth and azadirachtin, because the strong carboxyl of the maleic acid-acrylic acid copolymer sodium salt and the diatomaceous earth and azadirachtin produce strong adsorption, it is beneficial to cover a protective film with viscoelasticity on the surface, so that in aqueous solution, especially hard water, part of the maleic acid-acrylic acid copolymer can react with metal ions such as calcium ions, the influence of calcium ions and the like on the pesticide can be avoided, and the high number average molecular weight of maleic acid-acrylic acid and the action of negative charge, the aggregation of diatomite and azadirachtin is reduced, the suspension rate is increased, and when the sodium salt of the maleic acid-acrylic acid copolymer is acted on the surface of the plant, the surface tension can be reduced, the adsorption on the surface of the plant such as leaf surface is increased, and the wetting property is increased. However, when the number average molecular weight of the sodium salt of the maleic acid-acrylic acid copolymer is too large, the amount of adsorption of diatomaceous earth, azadirachtin, etc. may be too large, which may affect the fineness of the pesticide.
However, the applicant found that the wetting property is still poor and the storage stability is not good when the sodium salt of the maleic acid-acrylic acid copolymer is used alone, which may be caused by the partial attraction due to the larger polarity and charge action of the sodium salt of the maleic acid-acrylic acid copolymer, and the applicant found that when the ethylene oxide-propylene oxide copolymer with the proper number average molecular weight is added and the weight ratio of the ethylene oxide-propylene oxide copolymer to the sodium salt of the maleic acid-acrylic acid copolymer is controlled, due to the low polarity of the ethylene oxide-propylene oxide, the long chain part is inserted into the protective film formed by the sodium salt of the maleic acid-acrylic acid copolymer, but most of the ethylene oxide-propylene oxide long chain is positioned on the surface of the protective film, and the flexible ethylene oxide-propylene oxide long chain is also beneficial to promote the wetting property on the surface of the plant and reduce the entanglement and mutual attraction of the divided chains, the storage stability is increased.
Carrier
In one embodiment, the carrier of the present invention is selected from one or more of kaolin, white carbon black, magnesium aluminum silicate, anhydrous sodium sulfate, glucose, china clay, sericite, fructose, and soluble starch.
Preferably, the carrier of the present invention is sericite.
Sericite is one of mica, which belongs to silicate minerals having a layered structure. Sericite has wide application, and can be used in rubber, plastic, coating, paint, ceramic, heat insulation, cosmetics, pigment, paper making, metallurgy and other industries. Is a natural fine-grained muscovite, is silicate with a layered structure, can be split into extremely thin sheets, the thickness of the sheets can reach less than 1 mu m (theoretically, the sheets can be cut into 0.001 mu m), and the diameter-thickness ratio is large; the wear resistance and the abrasion resistance are good; heat-resistant insulation; is difficult to dissolve in acid-base solution; the chemical property is stable. In addition, the chemical composition and structure of sericite are similar to those of kaolin, and the sericite also has certain characteristics of clay minerals, namely good dispersion and suspension properties in an aqueous medium and an organic solvent, white and fine particles, viscosity and the like. Therefore, sericite combines many characteristics of mica minerals and clay minerals. The sericite of the invention has the diameter-thickness ratio of more than 80, and can be purchased or made by oneself. In a preferred embodiment, the sericite of the present invention is purchased from tita sericite mining ltd, Chuzhou.
The aspect ratio is a numerical ratio of the diameter and thickness of the material, and is determined by testing according to methods well known in the art.
More preferably, the sericite is modified sericite, and the raw materials for preparing the modified sericite comprise polyether modified silicone oil and sericite in a weight ratio of (0.05-0.2): 1; further, the weight ratio of the polyether modified silicone oil to the sericite is 0.1: 1.
the polyether modified silicone oil is an organosilicon nonionic surfactant with unique performance, which is prepared by graft copolymerization of polyether and dimethyl siloxane. The polyether modified silicone oil can be purchased or self-made, and when purchased, the polyether modified silicone oil comprises but is not limited to H-204 (viscosity of 1000-3500 mPa.s at 25 ℃) of Jiujiang phenanthrene blue high-new material Co., Ltd, DM-2041EB (viscosity of 500-1500 mPa.s at 25 ℃) of Qingdao Meisbe organic silicon Co., Ltd, and EW-116 (viscosity of 30-70 mPa.s at 25 ℃) of Daohui chemical.
Further preferably, the viscosity of the polyether modified silicone oil is 30-70 mPa.s at 25 ℃; further, the polyether modified silicone oil provided by the invention is EW-116.
The preparation method of the modified sericite according to the invention is a method well known in the art. In a preferred embodiment, the preparation method of the modified sericite according to the invention comprises the following steps: and mixing the polyether modified silicone oil and the sericite at 30-40 ℃, and drying to obtain the modified sericite.
The applicant has unexpectedly found that when sericite, particularly modified sericite having polyether-modified silicone oil as a modifier, is added, wetting, suspension and storage stability of an insecticide can be further promoted and air pollution by insecticide powder scattering can be reduced, which is probably because, by adding modified sericite, sericite automatically forms parallel arrangement due to the high aspect ratio of sericite when an aqueous solution of an insecticide contacts the surface of a plant, and the surface of sericite is promoted to be rapidly wetted by the insecticide under the action of polyether-modified silicone oil and wetting agent on the surface of sericite, saw-toothed diatomaceous earth and azadirachtin, thereby further increasing wetting performance, and because the lamellar stacking arrangement of sericite in water and the interaction of polyether-modified silicone oil and wetting agent on the surface of sericite facilitate the formation of a spatial three-dimensional structure in water, the precipitation of the insecticide is reduced, the suspension rate is increased, and when the insecticide is used, such as the insecticide is easily poured out from storage, the flexible long chains on the sericite and the adsorption performance of the sericite are beneficial to reducing the powder dispersion, so that the air pollution is reduced. And the applicant finds that when the viscosity of the polyether modified silicone oil in the raw material for preparing the modified sericite is too large, namely the molecular chain is too long, the modified sericite is easy to bond, and the wetting, the dispersion and the storage stability of the pesticide are influenced.
The applicants have unexpectedly found that the reduction of fly-away of the insecticide powder by modified sericite is enhanced when maleic acid-acrylic acid sodium salt and ethylene oxide-propylene oxide are added as wetting agents, probably because the polyether modified silicone oil long chains on the surface of sericite can attract the maleic acid-acrylic acid sodium salt protective film on the surface of diatomaceous earth and azadirachtin during pouring of the insecticide, and the flexible ethylene oxide-propylene oxide long chains and the silicone oil long chains interact with each other, thereby promoting the co-downward movement during powder pouring and reducing fly-away to the surroundings. When the amount of ethylene oxide-propylene oxide is excessive relative to the amount of the commercially available sodium acrylate, the ethylene oxide-propylene oxide enters the interior of the protective film, and the protective film structure is broken to a certain extent, and the inhibition effect on powder dispersion is reduced.
The preparation raw materials of the pesticide 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 pesticide of the invention has a dosage form selected from one or more of missible oil, wettable powder, water dispersible granule, suspending agent, aqueous emulsion, microemulsion, dispersible oil suspending agent, microcapsule suspending agent and soluble powder; furthermore, the pesticide of the invention is in the form of wettable powder.
In a second aspect, the present invention provides a method for preparing the insecticide containing the saw-toothed diatomite and the azadirachtin as described above, comprising the steps of: mixing and crushing the preparation raw materials of the pesticide except the saw-tooth-shaped diatomite, and then adding the saw-tooth-shaped diatomite for mixing to obtain the pesticide.
The preparation method of the pesticide containing the saw-toothed diatomite and the azadirachtin is a preparation method well known in the field, and for reference, the preparation method of the pesticide composition comprises the following steps: and mixing and crushing the ethylene oxide-propylene oxide block copolymer and a carrier, adding azadirachtin and maleic acid-acrylic acid copolymer sodium salt, mixing and crushing, adding sawtooth-shaped diatomite, and mixing to obtain the wettable powder.
In a third aspect, the present invention provides the use of a pesticide comprising diatomaceous earth and azadirachtin as described above for combating plant pests.
The insecticide provided by the invention can improve the effect of preventing plant pests by compounding the sawtooth-shaped diatomite and the azadirachtin, and particularly has good effects on citrus red spiders, citrus scale insects, frankliniella occidentalis, whiteflies, liriomyza sativae, prodenia litura, tea leafhoppers, tea yellow thrips, tea geometrid, lygus lucorum and grape aphids.
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.
Example 1
The embodiment provides an insecticide containing saw-toothed diatomite and azadirachtin, which is prepared from 70 parts of active ingredients, 5 parts of wetting and dispersing agents and 5 parts of carriers in parts by weight; the effective component comprises saw-toothed diatomite; the wetting dispersant comprises maleic acid-acrylic acid copolymer sodium salt and ethylene oxide-propylene oxide block copolymer, and the weight ratio is 2.5: 1; the carrier is modified sericite.
The diatomaceous earth in saw-tooth form was purchased from Celite610 of the garnets, france.
The maleic acid-acrylic acid copolymer sodium salt is PMAS-90.
The ethylene oxide-propylene oxide block copolymer is RFE 2035.
The preparation raw materials of the modified sericite comprise polyether modified silicone oil and sericite, wherein the weight ratio of the polyether modified silicone oil to the sericite is 0.1: 1, the polyether modified silicone oil is EW-116, and the sericite is purchased from the treasure sericite mining company, Inc. of Chuzhou; the preparation method of the modified sericite comprises the following steps: and mixing the polyether modified silicone oil and the sericite at 35 ℃, and drying to obtain the modified sericite.
This example also provides a method of preparing the above insecticide comprising diatomaceous earth in saw tooth form and azadirachtin, comprising the steps of: mixing and crushing the preparation raw materials of the pesticide except the saw-tooth-shaped diatomite, and then adding the saw-tooth-shaped diatomite for mixing to obtain the pesticide.
Example 2
The embodiment provides an insecticide containing saw-toothed diatomite and azadirachtin, which is prepared from 70 parts of active ingredients, 5 parts of wetting and dispersing agents and 5 parts of carriers in parts by weight; the effective component comprises azadirachtin; the wetting dispersant comprises maleic acid-acrylic acid copolymer sodium salt and ethylene oxide-propylene oxide block copolymer, and the weight ratio is 2.5: 1; the carrier is modified sericite.
The azadirachtin is purchased from Wuhan Wooxuan science and technology Co.
The maleic acid-acrylic acid copolymer sodium salt is PMAS-90.
The ethylene oxide-propylene oxide block copolymer is RFE 2035.
The preparation raw materials of the modified sericite comprise polyether modified silicone oil and sericite, wherein the weight ratio of the polyether modified silicone oil to the sericite is 0.1: 1, the polyether modified silicone oil is EW-116, and the sericite is purchased from the treasure sericite mining company, Inc. of Chuzhou; the preparation method of the modified sericite comprises the following steps: and mixing the polyether modified silicone oil and the sericite at 35 ℃, and drying to obtain the modified sericite.
This example also provides a method of preparing the above insecticide comprising diatomaceous earth in saw tooth form and azadirachtin, comprising the steps of: mixing and crushing preparation raw materials of the pesticide to obtain the pesticide.
Example 3
The embodiment provides an insecticide containing saw-toothed diatomite and azadirachtin, which is prepared from 70 parts of active ingredients, 5 parts of wetting and dispersing agents and 5 parts of carriers in parts by weight; the active ingredients comprise saw-tooth diatomite and azadirachtin in a weight ratio of 600: 1; the wetting dispersant comprises maleic acid-acrylic acid copolymer sodium salt and ethylene oxide-propylene oxide block copolymer, and the weight ratio is 2.5: 1; the carrier is modified sericite.
The diatomaceous earth in saw-tooth form was purchased from Celite610 of the garnets, france.
The azadirachtin is purchased from Wuhan Wooxuan science and technology Co.
The maleic acid-acrylic acid copolymer sodium salt is PMAS-90.
The ethylene oxide-propylene oxide block copolymer is RFE 2035.
The preparation raw materials of the modified sericite comprise polyether modified silicone oil and sericite, wherein the weight ratio of the polyether modified silicone oil to the sericite is 0.1: 1, the polyether modified silicone oil is EW-116, and the sericite is purchased from the treasure sericite mining company, Inc. of Chuzhou; the preparation method of the modified sericite comprises the following steps: and mixing the polyether modified silicone oil and the sericite at 35 ℃, and drying to obtain the modified sericite.
This example also provides a method of preparing the above insecticide comprising diatomaceous earth in saw tooth form and azadirachtin, comprising the steps of: mixing and crushing the preparation raw materials of the pesticide except the saw-tooth-shaped diatomite, and then adding the saw-tooth-shaped diatomite for mixing to obtain the pesticide.
Example 4
The embodiment of the present invention is similar to that of embodiment 3, except that the active ingredients include saw-tooth diatomaceous earth and azadirachtin in a weight ratio of 300: 1.
this example also provides a method of preparing the above insecticide containing diatomaceous earth and azadirachtin in a similar manner to example 3.
Example 5
The present example provides an insecticide containing saw-toothed diatomaceous earth and azadirachtin, which is similar to example 3, except that the active ingredients include saw-toothed diatomaceous earth and azadirachtin in a weight ratio of 1: 1.
this example also provides a method of preparing the above insecticide containing diatomaceous earth and azadirachtin in a similar manner to example 3.
Example 6
The present example provides an insecticide containing saw-toothed diatomaceous earth and azadirachtin, which is similar to example 3, except that the active ingredients include saw-toothed diatomaceous earth and azadirachtin in a weight ratio of 1: 30.
this example also provides a method of preparing the above insecticide containing diatomaceous earth and azadirachtin in a similar manner to example 3.
Example 7
The present example provides an insecticide containing saw-toothed diatomaceous earth and azadirachtin, which is similar to example 3, except that the active ingredients include saw-toothed diatomaceous earth and azadirachtin in a weight ratio of 1: 60.
this example also provides a method of preparing the above insecticide containing diatomaceous earth and azadirachtin in a similar manner to example 3.
Example 8
This example provides an insecticide containing diatomaceous earth and azadirachtin in zigzag form, and is similar to example 4, except that the weight ratio of the sodium salt of maleic acid-acrylic acid copolymer to the ethylene oxide-propylene oxide block copolymer is 10: 1.
this example also provides a method of preparing the above insecticide containing diatomaceous earth and azadirachtin in a similar manner to example 3.
Example 9
This example provides an insecticide containing diatomaceous earth and azadirachtin in zigzag form, and is similar to example 4, except that the sodium salt of maleic acid-acrylic acid copolymer is basf's CP 5.
This example also provides a method of preparing the above insecticide containing diatomaceous earth and azadirachtin in a similar manner to example 3.
Example 10
This example provides an insecticide containing diatomaceous earth and azadirachtin in zigzag form, and is similar to example 4, except that the sodium salt of maleic acid-acrylic acid copolymer is basf's CP 88.
This example also provides a method of preparing the above insecticide containing diatomaceous earth and azadirachtin in a similar manner to example 3.
Example 11
This example provides an insecticide containing diatomaceous earth in zigzag form and azadirachtin in a similar manner to example 4, except that the ethylene oxide-propylene oxide block copolymer is RFE 1740.
This example also provides a method of preparing the above insecticide containing diatomaceous earth and azadirachtin in a similar manner to example 3.
Example 12
This example provides an insecticide containing diatomaceous earth and azadirachtin in saw-tooth form, and is similar to example 4, except that the weight ratio of the sodium salt of maleic acid-acrylic acid copolymer to the ethylene oxide-propylene oxide block copolymer is 1: 1.
this example also provides a method of preparing the above insecticide containing diatomaceous earth and azadirachtin in a similar manner to example 3.
Example 13
This example provides an insecticide containing diatomaceous earth in saw-tooth form and azadirachtin, which is similar to example 4, except that the carrier is sericite, which is available from sericite mining ltd, pagoda, Chuzhou.
This example also provides a method of preparing the above insecticide containing diatomaceous earth and azadirachtin in a similar manner to example 3.
Example 14
The present example provides an insecticide containing saw-toothed diatomaceous earth and azadirachtin, and is similar to example 4, except that the weight ratio of the polyether modified silicone oil to sericite is 0.4: 1.
this example also provides a method of preparing the above insecticide containing diatomaceous earth and azadirachtin in a similar manner to example 3.
Example 15
This example provides an insecticide containing saw-toothed diatomaceous earth and azadirachtin, and is similar to example 4, except that the polyether-modified silicone oil is DM-2041 EB.
This example also provides a method of preparing the above insecticide containing diatomaceous earth and azadirachtin in a similar manner to example 3.
Evaluation of Performance
1. And (3) combined virulence determination: taking the insecticide containing the serrated diatomaceous earth and azadirachtin provided in the embodiment 1-7 as a reagent to be tested, performing combined toxicity determination on citrus red spiders, citrus scale insects, frankliniella occidentalis, whiteflies, liriomyza sativae, prodenia litura, tea leafhoppers, tea yellow thrips, tea geometrid, lygus lucorum and grape aphids, wherein the specific test method is as follows:
(1) combined toxicity determination of compounded zigzag diatomite and azadirachtin 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
Figure BDA0002388710510000141
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
Figure BDA0002388710510000151
The results are shown in Table 1.
TABLE 1 toxicity test results of blending of saw-toothed diatomaceous earth and azadirachtin against citrus red spider
Figure BDA0002388710510000152
(2) Combined toxicity determination of sawtooth-shaped diatomite and azadirachtin compound pairing citrus scale insect
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.
After 72d, checking the death condition of the test insects by using a dissecting mirror, and recording, wherein the death judgment standard of the test insects is fresh and alive, and the test insects are regarded as live insects in yellow or light yellow; the dead insects are considered to be dead insects if the body of the insects is shriveled and the color is dark.
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. The specific method is shown in (1), and the results are shown in Table 2.
TABLE 2 toxicity test results of Chinella diatomite and azadirachtin in combination with Setaria aurantiaca (Cekularella)
Figure BDA0002388710510000153
Figure BDA0002388710510000161
(3) Combined toxicity determination of Frankliniella occidentalis by compounding sawtooth-shaped diatomite and azadirachtin
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.
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. The specific method is shown in (1), and the results are shown in Table 3.
TABLE 3 toxicity test results of mixing of saw-toothed diatomaceous earth and azadirachtin on Frankliniella occidentalis
Figure BDA0002388710510000162
(4) Combined toxicity determination of saw-tooth-shaped diatomite and azadirachtin compounded on 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.
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. The specific method is shown in (1), and the results are shown in Table 4.
TABLE 4 toxicity test results of mixing of saw-toothed diatomaceous earth and azadirachtin against Bemisia alba
Figure BDA0002388710510000171
(5) Combined toxicity determination of composite pair of sawtooth-shaped diatomite and azadirachtin on 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. The specific method is shown in (1), and the results are shown in Table 5.
TABLE 5 toxicity test results of the mixture of saw-toothed diatomaceous earth and azadirachtin against Liriomyza sativae
Figure BDA0002388710510000181
(6) Combined toxicity determination of prodenia litura by compounding sawtooth-shaped diatomite and azadirachtin
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 (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.
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. The specific method is shown in (1), and the results are shown in Table 6.
TABLE 6 toxicity test results of Twill spodoptera litura after mixing of saw-toothed diatomaceous earth and azadirachtin
Figure BDA0002388710510000182
Figure BDA0002388710510000191
(7) Combined toxicity determination of compounded zigzag diatomite and azadirachtin on 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 sample is placed in an observation chamber.
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.
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. The specific method is shown in (1), and the results are shown in Table 7.
TABLE 7 toxicity test results of mixing of saw-toothed diatomaceous earth and azadirachtin on tea leafhopper
Figure BDA0002388710510000192
(8) Combined toxicity determination of compounding of saw-toothed diatomite and azadirachtin on 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.
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. The specific method is shown in (1), and the results are shown in Table 8.
TABLE 8 toxicity test results of mixing of saw-toothed diatomaceous earth and azadirachtin on tea leaf thrips
Figure BDA0002388710510000201
(9) Combined toxicity determination of sawtooth-shaped diatomite and azadirachtin compounding 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 (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.
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. The specific method is shown in (1), and the results are shown in Table 9.
TABLE 9 toxicity test results of mixing of saw-toothed diatomaceous earth and azadirachtin on tea geometrid
Figure BDA0002388710510000202
Figure BDA0002388710510000211
(10) Combined toxicity determination of crenellated diatomite and azadirachtin compound paired 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.
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. The specific method is shown in (1), and the results are shown in Table 10.
TABLE 10 toxicity test results of Apolygus lucorum mixed with diatomaceous earth and azadirachtin
Figure BDA0002388710510000212
(11) Combined toxicity determination of zigzag diatomite and azadirachtin compound pair 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 (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. The specific method is shown in (1), and the results are shown in Table 11.
TABLE 11 toxicity test results of combining saw-toothed diatomaceous earth and azadirachtin on grape aphid
Figure BDA0002388710510000221
2. Suspension percentage: the suspension rates of the insecticides containing serrated diatomaceous earth and azadirachtin provided in the examples were determined by the GB/T14825-one 2006 method and rated according to the suspension rates, wherein the suspension rate in the 1-grade was 85% or more, the suspension rate in the 2-grade was 80% or more and less than 85%, the suspension rate in the 3-grade was 70% or more and less than 80%, the suspension rate in the 4-grade was 60% or more and less than 70%, and the suspension rate in the 5-grade was less than 60%, and the results are shown in Table 12.
3. Wettability: the wetting time of the insecticide containing the serrated diatomite and the azadirachtin provided by the embodiment is determined according to a GB/T5451-2001 method, and is rated as 1-5 grade according to the wetting time, wherein the wetting time of 5 grade is more than 120s, the wetting time of 4 grade is more than 100s and less than or equal to 120s, and the wetting time of 3 grade is more than 80s and less than or equal to 100 s; the wetting times for the 2-stage were greater than 60s and less than or equal to 80s, and the wetting times for the 1-stage were less than or equal to 60s, the results are shown in Table 12.
4. Heat storage stability: the insecticides containing diatomaceous earth and azadirachtin in saw-tooth form as provided in examples were evaluated for heat storage stability by the method of GB/T19136-2003 and rated according to the powder state after heat storage, wherein grade 1 was no caking and caking, grade 2 was slightly caking and no caking, grade 3 was age-increasing and no caking, grade 4 was significant caking and slightly caking, grade 5 was significant caking, and the results are shown in Table 12.
Table 12 characterization of properties test
Examples Suspension rate Wetting time Stability in Heat storage
1 Level 1 Level 1 Level 1
8 Stage 2 4 stage Grade 3
9 Stage 2 Stage 2
10 4 stage Grade 3
11 Level 1 Stage 2 Stage 2
12 Grade 3 Stage 2 Grade 3
13 Grade 3 Grade 3 4 stage
14 Stage 2 Stage 2 Grade 3
15 Grade 5 Grade 5 Grade 5
The test results in tables 1 to 11 show that the insecticide containing the sawtooth-shaped diatomite and the azadirachtin is prepared by compounding the sawtooth-shaped diatomite and the azadirachtin according to the weight ratio of 600: 1-1: 60 has synergistic effect on killing insects, and has good insecticidal effect on various plant pests, such as citrus red spider, citrus scale insect, frankliniella occidentalis, trialeurodes vaporariorum, liriomyza, prodenia litura, tea leafhopper, tea yellow thrips, tea looper, green plant bug, grape aphid and the like; in addition, as can be seen from table 12, by selecting appropriate wetting dispersants and carriers, the suspension, wetting and heat storage stability of the insecticide can be increased, and the formulation provided in example 4 is an insecticide in the form of wettable powder, by using modified sericite, better fluidity is achieved compared with unmodified sericite in example 8, and the problem of powder drift of the insecticide is improved well, and by using maleic acid-acrylic acid copolymer sodium salt and ethylene oxide-propylene oxide block copolymer as the wetting dispersant to compound in example 4, the effect of improving the powder drift of the modified sericite can be further promoted, but the applicant also found that the effect of improving the powder drift of the powder of the modified sericite is poor compared with example 4 when the ratio of the two wetting dispersants in example 11 and example 8 is not appropriate; in addition, the applicant found that when the amount or viscosity of the polyether modified silicone oil in the modified sericite in example 14 and example 15 was not proper, the obtained insecticide had poor fluidity.
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 (10)

1. An insecticidal composition containing saw-toothed diatomite and azadirachtin, which is characterized by comprising the saw-toothed diatomite and the azadirachtin.
2. The insecticidal composition according to claim 1, wherein the weight ratio of the diatomaceous earth with saw tooth shape to the nimbin is 600: 1-1: 60.
3. an insecticide, characterized in that the raw materials for its preparation comprise, by weight, 60-80 parts of the insecticidal composition of claim 1, 2-6 parts of wetting dispersant and 2-6 parts of carrier.
4. A saw-tooth diatomaceous earth and azadirachtin-containing pesticide as claimed in claim 3, wherein said wetting dispersant is selected from one or more of maleic acid-acrylic acid copolymer sodium salt, ethylene oxide-propylene oxide block copolymer, polycarboxylate, alkyl naphthalene sulfonate formal, polyoxyethylene ether, lignosulfonate.
5. The insecticide containing serrated diatomaceous earth and azadirachtin as claimed in claim 4, wherein the wetting dispersant comprises a sodium salt of maleic acid-acrylic acid copolymer, and the number average molecular weight is 20000 to 30000.
6. The insecticide containing serrated diatomaceous earth and azadirachtin as claimed in claim 5, wherein the wetting dispersant further comprises an ethylene oxide-propylene oxide block copolymer having a number average molecular weight of 2500 to 4500.
7. The insecticide containing serrated diatomaceous earth and azadirachtin as claimed in claim 6, wherein the weight ratio of the maleic acid-acrylic acid copolymer sodium salt to the ethylene oxide-propylene oxide block copolymer is (2-3): 1.
8. the insecticide containing diatomaceous earth and azadirachtin according to any one of claims 3 to 6, wherein the carrier is one or more selected from kaolin, white carbon, magnesium aluminum silicate, anhydrous sodium sulfate, glucose, china clay, sericite, fructose, and soluble starch.
9. The saw-toothed diatomite and azadirachtin-containing pesticide as claimed in claim 3, wherein the pesticide is in a dosage form selected from one or more of emulsifiable concentrate, wettable powder, water dispersible granules, suspending agents, aqueous emulsion, microemulsion, dispersible oil suspending agents, microcapsule suspending agents and soluble powder.
10. Use of the insecticidal composition according to claim 1 or 2, comprising diatomaceous earth and azadirachtin in a saw-tooth form for controlling plant pests.
CN202010106726.9A 2020-02-21 2020-02-21 Insecticidal composition containing sawtooth-shaped diatomite and azadirachtin and application thereof Withdrawn CN111183985A (en)

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Application publication date: 20200522