CN114514927A - Nano pesticide suspoemulsion taking fatty acid starch ester as coating matrix and preparation method thereof - Google Patents

Nano pesticide suspoemulsion taking fatty acid starch ester as coating matrix and preparation method thereof Download PDF

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Publication number
CN114514927A
CN114514927A CN202111665584.0A CN202111665584A CN114514927A CN 114514927 A CN114514927 A CN 114514927A CN 202111665584 A CN202111665584 A CN 202111665584A CN 114514927 A CN114514927 A CN 114514927A
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acid starch
starch ester
fatty acid
pesticide
nano
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崔建国
黄燕敏
陈勇
熊齐鹏
李香荧
胡艳红
江杨
催郭勤
卢瑞
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Guangxi Tianyuan Biochemical Co Ltd
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Guangxi Tianyuan Biochemical Co Ltd
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    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
    • A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • A—HUMAN NECESSITIES
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    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/22—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing ingredients stabilising the active ingredients
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    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/26—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests in coated particulate form
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    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
    • A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
    • A01N43/14—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings
    • A01N43/16—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings with oxygen as the ring hetero atom
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    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
    • A01N43/36—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom five-membered rings
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    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
    • A01N43/40—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
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    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
    • A01N43/56—1,2-Diazoles; Hydrogenated 1,2-diazoles
    • A—HUMAN NECESSITIES
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    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
    • A01N43/647—Triazoles; Hydrogenated triazoles
    • A01N43/653—1,2,4-Triazoles; Hydrogenated 1,2,4-triazoles
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    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
    • A01N43/707—1,2,3- or 1,2,4-triazines; Hydrogenated 1,2,3- or 1,2,4-triazines
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    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
    • A01N43/88—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms six-membered rings with three ring hetero atoms
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    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/90—Biocides, 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
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/02—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having no bond to a nitrogen atom
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    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
    • A01N47/10—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
    • A01N47/24—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof containing the groups, or; Thio analogues thereof
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    • A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
    • A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
    • A01N47/38—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< where at least one nitrogen atom is part of a heterocyclic ring; Thio analogues thereof
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    • A01N51/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds having the sequences of atoms O—N—S, X—O—S, N—N—S, O—N—N or O-halogen, regardless of the number of bonds each atom has and with no atom of these sequences forming part of a heterocyclic ring
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    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
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Abstract

The invention relates to a nano pesticide suspoemulsion taking fatty acid starch ester as a wrapping matrix, which wraps active molecules of pesticide raw materials in the fatty acid starch ester through high-speed emulsification and ultrasonic dispersion to form the nano pesticide suspoemulsion.

Description

Nano pesticide suspoemulsion taking fatty acid starch ester as coating matrix and preparation method thereof
Technical Field
The invention belongs to the technical field of pesticides, and particularly relates to a nano pesticide suspoemulsion taking fatty acid starch ester as a coating matrix and a preparation method thereof.
Background
At present, in addition to accelerating the research and development of novel pesticides with high efficiency and low toxicity, the pesticide effect of the existing pesticides is fully exerted and the pesticide dosage is reduced by improving the dosage form and the formula of the existing pesticides, so that the method is another effective way for the sustainable development of modern agriculture and environmental protection.
Compared with the traditional pesticide preparation, the nano pesticide preparation appearing in recent years is a novel pesticide preparation with good development prospect. The pesticide component in the nano preparation has smaller particle size, higher specific surface area and better blade coverage rate. Meanwhile, as the active ingredients of the pesticide are wrapped by the carrier, the pesticide also has the effects of ultraviolet resistance, decomposition resistance and slow release, can improve the stability of the pesticide, reduce the application amount or the use times of the pesticide, further improve the bioavailability of the pesticide and reduce the influence on the environment ecology. At present, the application of nano pesticide formulations in agriculture is still in the exploration stage, mainly because it is difficult to produce stable nano particles with controlled particle size distribution, and the problems of high preparation cost, storage stability and the like in the preparation process.
Starch is a natural polymer material, and has the characteristics of no toxicity, rich resources, low price, easy processing, easy biodegradation and environmental friendliness, so that the starch is widely concerned by people, and the application of the starch as an encapsulation matrix material of a nano pesticide preparation is a better choice (jerocin J, et al. biodegradable polymer based encapsulation of neem oil emulsion for controlled release of Aza-A [ J ]. Carbohydryls polymers.2012, (90) (1750: (1756)). However, the natural starch has a large number of hydroxyl groups in the structure to show strong hydrophilicity, and most pesticides have poor water solubility, so that the affinity between the starch and pesticide ingredients is poor, and the application of the natural starch as an encapsulating material in controlled-release pesticides is limited. Chemical modification of starch can reduce or eliminate these disadvantages while increasing the hydrophobicity, water resistance of native starch, continuing to maintain its biodegradability (Alissandrates A, et al. biocompatible functional of static [ J ]. Chemical communications.2011,47(2): 683-.
The fatty acid starch ester is modified starch and is generated by reacting fatty acid, acid anhydride or fatty acid chloride with starch. The long-chain hydrocarbon modified natural starch is introduced through esterification reaction, so that the hydrophobic property of the starch is obviously enhanced, and the compatibility of the starch and a hydrophobic substance is further improved. Fatty acid starch esters have been widely used in the fields of food, textile, cosmetics, biodegradable materials and medicine (king red, et al, long-chain fatty acid starch ester synthesis and application research progress, chemical industry progress, 2006, 25(7), 760-764). However, the application of fatty acid starch esters in the field of pesticides is rarely reported.
The invention patent CN201310610629.3 reports the application of starch as a pesticide filler; the invention patent 'a preparation method and application of fatty acid starch ester (CN 200810124497)' introduces the application of fatty acid starch ester in food; the invention patent CN201410752445.5 reports a method for preparing starch-derived film-forming pesticide adjuvant by using starch or modified starch; wang S et al prepared a polyvinyl alcohol-starch ester composite membrane for embedding 2, 4-dichlorophenoxyacetic acid, and the resulting composite membrane had good drug-releasing and biodegradation properties (Wang S, et al preparation of a biodegradable poly (vinyl alcohol) -stage composite membrane and its application in pharmaceutical controlled release [ J ]. Journal of Applied Polymer science.2017,134(28): 45051.).
Aiming at the problems in the prior art, the invention utilizes fatty acid starch ester with rich sources as a basic wrapping material, researches and develops a nano-particle pesticide preparation product which has simple preparation method, high drug loading capacity, low cost and good photolysis resistance and slow release performance, and has good market application prospect.
Disclosure of Invention
In order to solve the problems, the invention provides a nano pesticide suspoemulsion taking fatty acid starch ester as a wrapping matrix, which wraps active molecules of pesticide raw materials in the fatty acid starch ester through high-speed emulsification and ultrasonic dispersion to form the nano pesticide suspoemulsion. The suspending agent has good photolysis resistance and oxidation resistance, good slow release performance, high insecticidal lethality rate, long insecticidal duration, simple preparation method, easy implementation, small equipment investment and no three wastes in the production process, and can be suitable for preparing different pesticide nano preparations.
In order to achieve the purpose, the scheme provided by the invention is as follows:
a nano pesticide suspoemulsion taking fatty acid starch ester as a coating matrix is prepared by coating active molecules of a pesticide raw material in the fatty acid starch ester by using the fatty acid starch ester as the coating matrix through a high-speed emulsification and ultrasonic dispersion method, and then adding a dispersing agent for ultrasonic dispersion again to obtain the nano pesticide suspoemulsion taking the fatty acid starch ester as the coating matrix.
The fatty acid starch ester is one or more of starch acetate, starch propionate, starch butyrate, starch valerate, starch caproate, starch heptanoate, starch caprylate, starch caprate, starch laurate, fatty acid starch ester with sixteen carbon atoms and fatty acid starch ester with eighteen carbon atoms.
Specifically, the pesticide raw material is one or more of indoxacarb, abamectin, emamectin benzoate, chlorantraniliprole, cyhalothrin, high-efficiency cypermethrin, thiamethoxam, dinotefuran, nitenpyram, pymetrozine, buprofezin, fipronil, chlorfenapyr, tolfenpyrad, kasugamycin, tebuconazole, azoxystrobin, difenoconazole, thifluzamide, epoxiconazole, hexaconazole, pyraclostrobin, tricyclazole, Dufulin, pyraclostrobin, boscalid, cyprodinil and prochloraz.
Specifically, the preparation method of the nano pesticide suspoemulsion taking the fatty acid starch ester as the coating matrix comprises the following steps:
(1) weighing fatty acid starch ester, pesticide raw material, organic solvent, surfactant, water and dispersant according to the raw material proportion for later use;
(2) adding fatty acid starch ester into an organic solvent, and ultrasonically stirring at the temperature of 60-90 ℃ until the fatty acid starch ester is dissolved to obtain a solution 1;
(3) adding the original pesticide into an organic solvent, and dissolving the original pesticide by high-speed stirring or ultrasonic treatment at room temperature to obtain a solution 2;
(4) adding a surfactant into water, stirring at a high speed for dispersing to obtain a solution 3 containing the surfactant, then respectively and quickly adding the solution 1 and the solution 2 into the solution 3 under high-speed stirring, and continuously stirring at a high speed for 20-40 min to obtain a suspension emulsion;
(5) carrying out ultrasonic dispersion on the suspension emulsion obtained in the step (4) at the low temperature of 0-10 ℃ for 20-40 min to obtain a nano suspension emulsion;
(6) and (4) adding a dispersing agent accounting for 0.5-6 wt% of the nano suspoemulsion obtained in the step (5), and continuing to perform ultrasonic dispersion for 20-40 min to obtain the nano pesticide suspoemulsion taking the fatty acid starch ester as a coating matrix.
Specifically, the water is deionized water or distilled water.
Preferably, the surfactant is one or a combination of a nonionic surfactant, an amine salt type cationic surfactant or an ionic surfactant; the nonionic surfactant comprises: tween, span, BY-125, lecithin, alkylphenol polyoxyethylene ether, high-carbon fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ester, castor oil polyoxyethylene ether, polyoxyethylene alkylamine, sorbitan ester, sucrose ester, polyoxyethylene alkylolamide, styrylphenol polyoxyethylene ether and polyether; the ionic surfactant comprises: anionic polyacrylamide, sodium alkyl benzene sulfonate, alkyl sulfate ester salt and alkyl phosphate ester salt.
Preferably, the organic solvent is one or more of dichloromethane, ethyl acetate, sec-butyl acetate, isobutyl acetate, N-butyl acetate, cyclohexanone, benzyl butyl phthalate, diethyl phthalate, dimethyl phthalate, diethylene glycol butyl ether, diethylene glycol ethyl ether, diethylene glycol methyl ether, tetrahydrofuran, N-hexane, cyclohexanone, xylene, dupont DBE, solvay Green25, solvay ADMA810, polacrlean, RPDE, dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide, acetamide, decanamide, tert-butyl methyl ether, isopropyl ether, paraffin oil, naphtha, solvent oil and vegetable oil.
Preferably, the dispersing agent is one or more of sodium alginate, chitin, gum arabic, xanthan gum, methylcellulose, sodium carboxymethylcellulose, hydroxyethyl cellulose, hydroxypropyl starch ether, isomeric alcohol ether, hydroxypropyl distarch phosphate, acetylated distarch phosphate, NS-500LQ, J-601, Darun DSV, SP-SC29, gelatin, soybean protein glue, agar, polyacrylamide, polyvinyl alcohol, polyvinylpyrrolidone, polyethylene oxide, polyacrylate copolymer emulsion and the like.
Preferably, the raw materials are in the following proportion: the pesticide composition comprises fatty acid starch ester, pesticide raw materials, a surfactant and a dispersing agent according to a mass ratio of 1-10: 1-30: 0.1 to-5: 0.1 to 6.
Preferably, the high-speed stirring rotating speed is 800-11000 r/min.
Preferably, the ultrasonic dispersion parameters are: ultrasonic liquid flow rate is 0.1-1.0 m3H; the ultrasonic power is 3-15 kW; the primary ultrasonic circulation time is 10-60 min.
Preferably, the adding amount of the organic solvent in the step (2) and the step (3) is 5-60% of the weight of the preparation; the adding amount of the water in the step (4) is 20-70% of the total weight of the suspending agent.
In the preparation method, long-chain aliphatic hydrocarbon in fatty acid starch ester is combined with hydrophobic pesticide active molecules in aqueous solution to form spherical nanoparticles, and the spherical nanoparticles are wrapped inside the particles, while free hydroxyl in the starch ester is positioned outside the particles and is combined with water molecules or hydrophilic emulsifying agents to form a stable nano suspoemulsion preparation. The invention is mainly suitable for hydrophobic pesticide molecules, and is also suitable for some hydrophilic pesticides with smaller water solubility.
The invention has the following beneficial effects:
1. the invention adopts the mode that natural macromolecular fatty acid starch ester wraps pesticide molecules to wrap the pesticide molecules in the nano particles to form nano pesticide particles, then the dispersing agent is added to stabilize the preparation, and the nano pesticide suspoemulsion taking the fatty acid starch ester as the wrapping matrix is prepared.
2. The nano pesticide suspoemulsion disclosed by the invention has the advantages that the raw materials such as pesticide raw materials, fatty acid starch ester, a surfactant and a dispersing agent are strictly controlled in proportion, and the preparation method is strictly controlled, so that the prepared nano pesticide suspoemulsion has a good slow-release effect, has good photolysis resistance and oxidation resistance, can fully exert the pesticide effect after being applied, further reduces the pesticide dosage, and is favorable for promoting the sustainable development of modern agriculture and environmental protection.
3. The invention directly encapsulates pesticide molecules through fatty acid starch ester, has wide application range and can be used for hydrophobic pesticide raw drug molecules of different types or some hydrophilic pesticides with smaller water solubility; the main solvent is water, so the price is low; the fatty acid starch ester used as the wrapping base material is harmless in natural environment, relatively environment-friendly and environment-friendly.
4. The nano pesticide suspoemulsion has the advantages that the particle size range of nano particles is 100-200 nm, the slow release performance is good, the release rate in 50% methanol water for 40h is only 40%, and the release rate of a control group reaches 60%; and the photolysis resistance is good, the decomposition rate at 48 hours is 58%, and the decomposition rate is improved by more than 50% compared with that of the common pesticide (the decomposition rate at 48 hours is over 90%).
5. The nano pesticide suspoemulsion has good insecticidal effect and long insecticidal lasting period, and 3% of indoxacarb nano pesticide suspoemulsion is taken as an example, the insecticidal mortality rate of 1 day after application can reach more than 98%, the insecticidal mortality rate of 7 days after application can also reach about 72%, and the insecticidal mortality rate of 14 days after application can also be kept about 58%; the insecticidal lethality of the 3% ordinary indoxacarb suspending agent in the control group is lower than 50% after 10 days of application.
6. The nano pesticide suspoemulsion taking the fatty acid starch ester as the wrapping matrix also has the advantages of simple preparation method, easy implementation, small equipment investment, no three wastes in the production process and the like.
Drawings
Fig. 1 is a TEM image of the nano indoxacarb suspoemulsion of example 1.
Fig. 2 is a particle size distribution diagram of the nano-indoxacarb suspoemulsion of example 1.
FIG. 3 is a graph comparing the release kinetics curves of the indoxacarb cumulative release rate versus time for example 1 and the control group.
FIG. 4 is a graph comparing the UV resistance of example 1 with that of the control group.
FIG. 5 is a graph comparing the insecticidal lethality of example 1 to control groups against prodenia litura.
FIG. 6 is a graph comparing the pesticidal efficacy of example 1 and a control group against prodenia litura.
Detailed Description
The invention is further described with reference to the following examples:
example 1
The preparation method of the 3% indoxacarb nano pesticide suspending agent with the starch stearate as the coating matrix comprises the following steps:
(1) weighing 0.6kg of starch stearate, 3.8kg of indoxacarb (the content is more than 98 percent), 55L of butyl acetate, 1.5kg of surfactant BY-125, 60L of deionized water and 1.0kg of dispersant EI-40 according to the proportion of the raw materials for later use;
(2) adding starch stearate into 30L butyl acetate, and ultrasonically stirring at 80 ℃ for 10min until the starch stearate is dissolved to obtain a solution 1;
(3) adding indoxacarb into 25L of butyl acetate, and dissolving the indoxacarb by ultrasonic treatment at room temperature to obtain a solution 2;
(4) adding a surfactant BY-125 into deionized water, stirring at a high speed for dispersion to obtain a solution 3 containing the surfactant, then respectively and quickly adding the solution 1 and the solution 2 into the solution 3 under high-speed stirring, and continuously stirring at a high speed for 30min to obtain a suspension emulsion;
(5) carrying out ultrasonic dispersion on the suspension emulsion obtained in the step 4 at the low temperature of 2 ℃ to obtain nano suspension emulsion;
(6) and (3) adding 1.0kg of dispersant EI-40 into the nano suspoemulsion obtained in the step (5), and then carrying out ultrasonic dispersion for 30min again to obtain the 3% indoxacarb nano pesticide suspoemulsion taking starch stearate as a coating matrix.
Example 2
The preparation method of the 3.5 percent avermectin nano pesticide suspending agent taking palmitic acid starch ester as a coating matrix comprises the following steps:
(1) weighing 0.7kg of palmitic acid starch ester, 5.3kg of abamectin (the content is more than 80 percent), 35L of butyl acetate, 15L of decanamide, 2.0kg of surfactant BY-125, 65L of deionized water and 1.5kg of dispersant Darun DSV according to the proportion of the raw materials for standby;
(2) adding the palmitic acid starch ester into 10L of butyl acetate and 15L of decanamide, and ultrasonically stirring at the temperature of 80 ℃ for 10min until the palmitic acid starch ester is dissolved to obtain a solution 1;
(3) adding abamectin into 25L of butyl acetate, and stirring at a high speed at room temperature to dissolve the abamectin to obtain a solution 2;
(4) adding surfactant Tween-80 into deionized water, stirring at high speed for dispersing to obtain solution 3 containing surfactant, rapidly adding solution 1 and solution 2 into solution 3 under high speed stirring, and continuously stirring at high speed for 30min to obtain suspension;
(5) carrying out ultrasonic dispersion on the suspension emulsion obtained in the step 4 at a low temperature of 5 ℃ to obtain nano suspension emulsion;
(6) and (3) adding 1.5kg of dispersing agent into the nano-suspension emulsion obtained in the step (5) to achieve DSV, and then performing ultrasonic dispersion for 30min to obtain the 3.5% avermectin nano-pesticide suspension emulsion taking the starch palmitate as a coating matrix.
Example 3
The preparation method of the 5% chlorantraniliprole nano pesticide suspending agent taking palmitic acid starch ester as a coating matrix comprises the following steps:
(1) weighing 0.8kg of starch laurate, 6.3kg of chlorantraniliprole (the content is 95 percent), 20L of butyl acetate, 10L of decanamide, 25L of acetamide, 1.8kg of surfactant Tween-60, 60L of deionized water and 1.2kg of dispersing agent NS-500LQ according to the proportion of the raw materials for later use;
(2) adding starch laurate into 20L of butyl acetate and 10L of capramide, and ultrasonically stirring at the temperature of 80 ℃ for 20min until the starch palmitate is dissolved to obtain a solution 1;
(3) adding chlorantraniliprole into 25 liters of acetamide, and stirring at a high speed at room temperature to dissolve the chlorantraniliprole to obtain a solution 2;
(4) adding a surfactant Tween-60 into deionized water, stirring at a high speed for dispersing to obtain a solution 3 containing the surfactant, then respectively and quickly adding the solution 1 and the solution 2 into the solution 3 under high-speed stirring, and continuously stirring at a high speed for 20min to obtain a suspension emulsion;
(5) carrying out ultrasonic dispersion on the suspension emulsion obtained in the step 4 at a low temperature of 3 ℃ to obtain nano suspension emulsion;
(6) and (3) adding 1.2kg of dispersing agent NS-500LQ into the nano suspoemulsion obtained in the step (5), and then performing ultrasonic dispersion for 30min again to obtain the 5% chlorantraniliprole nano pesticide suspoemulsion taking the fatty acid starch ester as the coating matrix.
Example 4
The preparation method of the 3% cyhalothrin nano pesticide suspending agent taking the starch decanoate as the wrapping matrix comprises the following steps:
(1) weighing 0.6kg of decanoic acid starch ester, 3.8kg of cyhalothrin (content 98%), 30L of acetamide, 25L of butyl acetate, 2.5kg of surfactant span-60, 60L of deionized water and 1.5kg of dispersant J-601 according to the proportion of the raw materials for later use;
(2) adding decanoic acid starch ester into 30L acetamide, and ultrasonically stirring at 80 ℃ for 10min until the decanoic acid starch ester is dissolved to obtain a solution 1;
(3) adding cyhalothrin into 25L of butyl acetate, and stirring at high speed at room temperature to dissolve the cyhalothrin to obtain a solution 2;
(4) adding a surfactant span-60 into deionized water, stirring at a high speed for dispersion to obtain a solution 3 containing the surfactant, then respectively and quickly adding the solution 1 and the solution 2 into the solution 3 under high-speed stirring, and continuously stirring at a high speed for 20min to obtain a suspension emulsion;
(5) carrying out ultrasonic dispersion on the suspension emulsion obtained in the step (4) at the low temperature of 10 ℃ to obtain nano suspension emulsion;
(6) and (3) adding 1.5kg of dispersant J-601 into the nano suspoemulsion obtained in the step (5), and then performing ultrasonic dispersion for 30min to obtain the 3% lambda-cyhalothrin nano pesticide suspoemulsion taking the starch decanoate as a coating matrix.
Example 5
The 5.7 percent emamectin benzoate nano pesticide suspending agent taking palmitic acid starch ester as a coating matrix is prepared by the following steps:
(1) weighing 1.0kg of palmitic acid starch ester, 9.9kg of emamectin benzoate (content of 70%), 40L of sec-butyl acetate, 10L of acetamide, 1.5kg of surfactant Tween-80, 60L of distilled water and 1.5kg of dispersant isomeric alcohol ether-1305 according to the proportion of the raw materials for later use;
(2) adding the palmitic acid starch ester into 10L of sec-butyl acetate and 10L of acetamide, and ultrasonically stirring at the temperature of 80 ℃ for 20min until the palmitic acid starch ester is dissolved to obtain a solution 1;
(3) adding emamectin benzoate into 30L sec-butyl acetate, and stirring at high speed at room temperature to dissolve the emamectin benzoate to obtain a solution 2;
(4) adding surfactant Tween-80 into distilled water, stirring at high speed for dispersing to obtain solution 3 containing surfactant, rapidly adding solution 1 and solution 2 into solution 3 under high speed stirring, and continuously stirring at high speed for 30min to obtain suspension;
(5) carrying out ultrasonic dispersion on the suspension emulsion obtained in the step 4 at a low temperature of 4 ℃ to obtain nano suspension emulsion;
(6) adding 1.5kg of dispersant isomeric alcohol ether-1305 into the nano suspoemulsion obtained in the step (5), and then performing ultrasonic dispersion for 30min again to obtain the 5.7% emamectin benzoate nano pesticide suspoemulsion taking the starch palmitate as a coating matrix.
Examples 6-15 were prepared according to the preparation of example 1, according to the raw material formulation (in weight percent) in table 1 below.
Table 1 examples 6-15 starting materials
Figure BDA0003448220210000071
Figure BDA0003448220210000081
Examples 16-29 were prepared according to the preparation of example 4, according to the raw material formulations in table 2 below.
Table 2 examples 16-29 starting materials
Figure BDA0003448220210000082
The following tests were carried out on the nano-pesticide suspoemulsion prepared in example 1:
morphological characterization of nano pesticide suspoemulsion taking fatty acid starch ester as wrapping matrix
Taking the 3% indoxacarb nano pesticide suspoemulsion prepared in example 1 as a sample, microscopic morphology observation is carried out on the nano-particle indoxacarb suspoemulsion by adopting a transmission electron microscope and a particle size analyzer, and the result is shown in figure 1 and figure 2.
As can be seen from fig. 1 and 2, the nanoparticle suspoemulsion of the present invention has a nanoparticle size of about 100-200 nm, is spherical, and has a relatively smooth outer surface, and belongs to a nanoparticle suspoemulsion preparation.
Second, component release test of nano pesticide suspoemulsion taking fatty acid starch ester as wrapping matrix
The 3% indoxacarb nano pesticide suspoemulsion obtained in example 1 was subjected to a component release test, and a control group was set to be a 3% ordinary indoxacarb suspension.
1g of the 3% indoxacarb nano pesticide suspoemulsion and 3% of the common indoxacarb suspending agent in example 1 are weighed respectively, placed in dialysis bags respectively, added with a plurality of small glass beads, fastened by ropes at two ends and placed in a 100mL open bottle. Then 100mL of 50% methanol-water mixed solvent (pH 7) was added to the flask, and three samples were run in parallel and placed in a shaker at a preset temperature (T25 ℃ C.) (rotation speed 180 r/min). Sampling for 2h for the first time, then sampling once every 12h, replacing fresh solvent after each sampling, and putting back to the shaking table for releasing again. The indoxacarb concentration in the solution of the release liquid is analyzed through high pressure liquid chromatography, the cumulative release rate is calculated, and a release kinetics curve of the indoxacarb cumulative release rate-time is made according to the cumulative release rate and the time, and is shown in figure 3.
As can be seen from the comparison of FIG. 3, the% indoxacarb nano pesticide suspoemulsion of the embodiment 1 of the invention has good slow release performance. In 50% methanol water, the release rate of the nano pesticide suspending emulsion is only 40% in 40h, the release rate of the contrast group reaches 60%, the release rate of the contrast group reaches 80% in 80h, and the release rate of the invention reaches about 80% in 140h, which shows that the nano pesticide suspending emulsion has good slow release performance.
Third, the nano pesticide suspoemulsion taking fatty acid starch ester as the wrapping matrix resists the photolysis test
The 3% indoxacarb nano pesticide suspension emulsion obtained in example 1 was subjected to an anti-photolysis test, a control group was set to be 3% ordinary indoxacarb suspension, and a 45W ultraviolet lamp was used to simulate sunlight irradiation on the preparation.
FIG. 4 is a graph comparing the UV resistance of example 1 with that of the control group. As can be seen from FIG. 4, at 12h, the conventional indoxacarb suspension had decomposed by 70%, and its 48-hour decomposition rate exceeded 90%. The indoxacarb nano pesticide suspoemulsion of the embodiment 1 has the decomposition rate of only 48% at 12 hours and the decomposition rate of only 58% at 48 hours, which is far less than that of the control group. The indoxacarb nano pesticide suspoemulsion provided by the invention has excellent photolysis resistance, and the photolysis resistance is improved by more than 50%. The improvement of the photolysis resistance of the pesticide molecules also means the increase of the insecticidal persistence of the pesticide molecules.
Fourth, insecticidal lethality test of nano pesticide suspoemulsion taking fatty acid starch ester as wrapping matrix
The insecticidal lethality test was performed on the 3% indoxacarb nano pesticide suspoemulsion obtained in example 1, and a control group was set to be 3% ordinary indoxacarb suspension.
1) Insecticidal lethality tests of indoxacarb nano pesticide suspoemulsions at different dilution concentrations: the indoxacarb suspensions of example 1 and the control group were diluted to 6.3ppm, 12.5ppm, 25ppm, 50ppm, 100ppm, 200ppm, respectively, and tested for insecticidal lethality against prodenia litura at the middle and late 3-year old, respectively, for 48 hours after application.
FIG. 5 is a graph comparing the insecticidal lethality of example 1 to control groups against prodenia litura.
As can be seen from FIG. 5, there was not much difference in insecticidal toxicity between them. At concentrations of 25 and 50ppm, the insecticidal effect of the common indoxacarb suspending agent IN-SC is better than that of a nano preparation, while at 100 and 12.5ppm, the toxic effect of the nano preparation is stronger, and at 200ppm and 6.3ppm, the insecticidal effects of the nano preparation and the nano preparation are equivalent.
2) The insecticidal validity period of the indoxacarb nano pesticide suspoemulsion is determined:
FIG. 6 is a graph comparing the pesticidal efficacy of example 1 and a control group against prodenia litura.
As can be seen from fig. 6, the insecticidal lethality of the 3% indoxacarb nano pesticide suspoemulsion of example 1 was higher than that of the control group in the test period of 14 days. The insecticidal lethality of both the two is kept at about 80% on the 4 th day; after 7 days, the insecticidal efficiency of the control group is obviously reduced, the insecticidal lethality rate is reduced to about 60%, and the insecticidal lethality rate of example 1 can be kept to about 72%. On day 10, the insecticidal mortality of the control group decreased to about 50%, while the insecticidal mortality of example 1 remained about 60%. By day 14, the insecticidal efficiency of the control group is obviously reduced, and is only about 45%, while the insecticidal mortality of example 1 is kept about 58%. Therefore, the indoxacarb nano pesticide suspoemulsion in the embodiment 1 of the invention has better insecticidal effect in the same time and longer insecticidal lasting period.
The nano pesticide suspoemulsions of examples 2-15 were then subjected to photolysis resistance and insecticidal lethality tests. The statistical results are shown in table 3.
TABLE 3 statistical results of examples 1-15 (concentration 100ppm, prodenia litura)
Figure BDA0003448220210000101
Figure BDA0003448220210000111
As can be seen from Table 3, the nano pesticide suspensions of examples 1-15 all have excellent slow release performance, photolysis resistance and high insecticidal lethality.
The nano pesticide suspoemulsions of examples 16-29 were tested for bactericidal performance. The test method and the calculation method refer to GB/T17980.33-2000 pesticide field pesticide effect test criterion (I) that the bactericide prevents and treats the pepper anthracnose, and the area of each cell is 30m2And repeating the treatment for 4 times, treating with clear water as blank control, spraying at the early stage of disease onset, and applying at interval of 7d for the second time. The disease incidence and control effect were calculated by examining the disease incidence in units of plants from the investigation results before the first dose, 7 days after the second dose, and 14 days after the second dose, respectively. The statistical results are shown in table 4.
TABLE 4 statistical results of examples 16-29 (concentration 100ppm, anthracnose of pepper)
Figure BDA0003448220210000112
As can be seen from Table 4, the nano pesticide suspending agents in the embodiments 16 to 29 of the application have excellent bactericidal performance, and the control effects of controlling the pepper anthracnose at 7d and 14d after the second pesticide are still kept at a high level.
Although the embodiments of the present invention have been described with reference to the accompanying drawings, it is not intended to limit the scope of the invention, and it should be understood by those skilled in the art that various modifications and changes may be made without creative efforts based on the technical solutions of the present invention.

Claims (9)

1. A nano pesticide suspoemulsion taking fatty acid starch ester as a coating matrix is characterized in that: coating active molecules of a pesticide raw material in the fatty acid starch ester by using the fatty acid starch ester as a coating matrix through a high-speed emulsification and ultrasonic dispersion method, and then adding a dispersing agent for ultrasonic dispersion again to obtain the nano pesticide suspoemulsion taking the fatty acid starch ester as the coating matrix;
the fatty acid starch ester is one or more of acetic acid starch ester, propionic acid starch ester, butyric acid starch ester, valeric acid starch ester, caproic acid starch ester, enanthic acid starch ester, caprylic acid starch ester, capric acid starch ester, lauric acid starch ester, sixteen carbon fatty acid starch ester and eighteen carbon fatty acid starch ester.
2. The nano pesticide suspoemulsion taking fatty acid starch ester as a coating matrix according to claim 1 is characterized in that: the pesticide raw material is one or more of indoxacarb, abamectin, emamectin benzoate, chlorantraniliprole, cyhalothrin, lambda-cyhalothrin, thiamethoxam, dinotefuran, nitenpyram, pymetrozine, buprofezin, fipronil, chlorfenapyr, tolfenpyrad, kasugamycin, tebuconazole, azoxystrobin, difenoconazole, thifluzamide, epoxiconazole, hexaconazole, pyraclostrobin, tricyclazole, Dufulin, pyraclostrobin, boscalid, cyprodinil and prochloraz.
3. A method for preparing the nano pesticide suspoemulsion taking fatty acid starch ester as the wrapping matrix according to claim 1 or 2, which is characterized by comprising the following steps:
(1) weighing fatty acid starch ester, pesticide raw material, organic solvent, surfactant, deionized water and dispersant according to the raw material proportion for later use;
(2) adding fatty acid starch ester into an organic solvent, and ultrasonically stirring at the temperature of 60-90 ℃ until the fatty acid starch ester is dissolved to obtain a solution 1;
(3) adding the original pesticide into an organic solvent, and dissolving the original pesticide by high-speed stirring or ultrasonic treatment at room temperature to obtain a solution 2;
(4) adding a surfactant into deionized water, stirring at a high speed for dispersing to obtain a solution 3 containing the surfactant, then respectively and quickly adding the solution 1 and the solution 2 into the solution 3 under high-speed stirring, and continuously stirring at a high speed for 20-40 min to obtain a suspension emulsion;
(5) carrying out ultrasonic dispersion on the suspension emulsion obtained in the step (4) at the low temperature of 0-10 ℃ for 20-40 min to obtain a nano suspension emulsion;
(6) and (4) adding a dispersing agent accounting for 0.5-6 wt% of the nano suspoemulsion obtained in the step (5), and continuing to perform ultrasonic dispersion for 20-40 min to obtain the nano pesticide suspoemulsion taking the fatty acid starch ester as a coating matrix.
4. The method for preparing the nano pesticide suspoemulsion taking fatty acid starch ester as the coating matrix according to claim 3 is characterized in that: the surfactant is one or combination of a plurality of nonionic surfactants, amine salt cationic surfactants or ionic surfactants; the nonionic surfactant comprises: tween, span, BY-125, lecithin, alkylphenol polyoxyethylene ether, high-carbon fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ester, castor oil polyoxyethylene ether, polyoxyethylene alkylamine, sorbitan ester, sucrose ester, polyoxyethylene alkylolamide, styrylphenol polyoxyethylene ether and polyether; the ionic surfactant comprises: anionic polyacrylamide, sodium alkyl benzene sulfonate, alkyl sulfate ester salt and alkyl phosphate ester salt.
5. The method for preparing the nano pesticide suspoemulsion taking fatty acid starch ester as the coating matrix according to claim 3 is characterized in that: the organic solvent is one or a mixture of more of dichloromethane, ethyl acetate, sec-butyl acetate, isobutyl acetate, N-butyl acetate, cyclohexanone, benzylbutyl phthalate, diethyl phthalate, dimethyl phthalate, diethylene glycol butyl ether, diethylene glycol ethyl ether, diethylene glycol methyl ether, tetrahydrofuran, N-hexane, cyclohexanone, xylene, DuPont DBE, Sorvey Green25, Sorvey ADMA810, POLARCLEAN, RPDE, dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide, acetamide, decanamide, tert-butyl methyl ether, isopropyl ether, paraffin oil, naphtha, solvent oil and vegetable oil.
6. The method for preparing the nano pesticide suspoemulsion taking fatty acid starch ester as the coating matrix according to claim 3 is characterized in that: the dispersing agent is one or a mixture of more of sodium alginate, chitin, gum arabic, xanthan gum, methylcellulose, sodium carboxymethylcellulose, hydroxyethyl cellulose, hydroxypropyl starch ether, isomeric alcohol ether, hydroxypropyl distarch phosphate, acetylated distarch phosphate, NS-500LQ, J-601, Darun DSV, SP-SC29, gelatin, soybean protein glue, agar, polyacrylamide, polyvinyl alcohol, polyvinylpyrrolidone, polyethylene oxide and polyacrylate copolymer emulsion.
7. The method for preparing the nano pesticide suspoemulsion taking fatty acid starch ester as the coating matrix according to claim 3 is characterized in that: the raw materials are in proportion as follows: the pesticide composition comprises fatty acid starch ester, pesticide raw materials, a surfactant and a dispersing agent according to a mass ratio of 1-10: 1-30: 0.1-5: 0.1 to 6.
8. The method for preparing the nano pesticide suspoemulsion taking fatty acid starch ester as the coating matrix according to claim 3 is characterized in that: the high-speed stirring rotating speed is 800-11000 r/min.
9. The method for preparing the nano pesticide suspoemulsion taking fatty acid starch ester as the coating matrix according to claim 3 is characterized in that: the ultrasonic dispersion parameters are as follows: ultrasonic liquid flow rate is 0.1-1.0 m3H; the ultrasonic power is 3-15 kW; the ultrasonic once circulation time is 10-60 min.
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