CN111771902A - Efficient cyhalothrin nano water aqua and preparation method and application thereof - Google Patents
Efficient cyhalothrin nano water aqua and preparation method and application thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N53/00—Biocides, pest repellants or attractants, or plant growth regulators containing cyclopropane carboxylic acids or derivatives thereof
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- 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
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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
- A01N25/30—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 characterised by the surfactants
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Abstract
The invention belongs to the technical field of pesticides, and discloses a high-efficiency cyhalothrin nano-water agent which is prepared by taking high-efficiency cyhalothrin, a surfactant and water as raw materials, adding no organic solvent and adopting a surfactant micelle solubilization method; wherein, the mass percentage content of the high-efficiency cyhalothrin is 0.5 to 10 percent, the mass percentage content of the surfactant is 5 to 20 percent, and the balance is water. Compared with the conventional pesticide formulation, the nano water agent prepared by adopting the surfactant micelle solubilization method has excellent stability, is still stable after being respectively stored at 0 ℃ for 7 days and at 54 ℃ for 14 days, is not separated out, is convenient to store and has longer shelf life; the nano water aqua has lower production cost, more excellent quick action and persistence, does not have adverse reactions such as phytotoxicity and the like, and is more suitable for unmanned aerial vehicles.
Description
Technical Field
The invention belongs to the technical field of production and processing of pesticides, and particularly relates to a lambda-cyhalothrin nano-water aqua and a preparation method and application thereof.
Background
The Cyhalothrin (Cyhalothrin) can be widely used for controlling pests such as aphids, armyworms, diamondback moths, cabbage caterpillars, oriental tobacco budworms, corn bollworms, pink bollworms, peach plantlets, oriental fruit moths, citrus leaf miners, tea caterpillars, tea loopers, tea leafhoppers and the like on crops such as wheat, rape, vegetables, cotton, fruit trees, tea leaves, tobacco and the like.
The efficient cyhalothrin is insoluble in water, and the pesticide formulations developed by taking the efficient cyhalothrin as a raw material at present mainly comprise missible oil, emulsion in water and the like. However, both missible oil and emulsion in water contain a large amount of organic solvent, and in the using process, the organic solvent not only can cause serious harm to the environment, but also can seriously affect the quality of agricultural products, accelerate the food safety crisis and harm human health.
With the increasing environmental awareness of users and the rapidly growing demand for sanitary medicine, the existing dosage forms of lambda-cyhalothrin cannot meet the use demand. In order to accelerate the popularization and the use of the efficient cyhalothrin product on the premise of safety and environmental protection, it is particularly necessary to develop a novel preparation which is friendly to people and livestock and is convenient for the application of aerial plant protection technologies and equipment such as unmanned aerial vehicles and the like.
Disclosure of Invention
Aiming at the defects of the existing problems, the invention provides a high-efficiency cyhalothrin nano water aqua and a preparation method and application thereof; the invention creatively discovers that a novel nano water aqua is formed by adopting certain surfactants, adopting a surfactant micelle solubilization technology and utilizing the nano micelle formed by the surfactants to bear the water-insoluble pesticide component, namely the high-efficiency cyhalothrin under the condition of not using an organic solvent for solubilizing.
The purpose of the invention can be realized by the following technical scheme:
the efficient cyhalothrin nano-water agent is prepared by taking efficient cyhalothrin, a surfactant and water as raw materials, does not contain any organic solvent and adopting a surfactant micelle solubilization method, wherein the efficient cyhalothrin in the nano-water agent accounts for 0.5-10% by mass, the surfactant accounts for 5-20% by mass and the balance of water
Preferably, the efficient cyhalothrin comprises, by mass, 1-5% of the efficient cyhalothrin, 5-20% of the surfactant and the balance of water.
The surfactant is selected from 1 or more of fatty alcohol-polyoxyethylene ether, alkylphenol formaldehyde resin polyoxyethylene ether, styryl phenol polyoxyethylene ether, tristyryl phenol polyoxyethylene ether phosphate, fatty alcohol-polyoxyethylene ether phosphate, alkylphenol polyoxyethylene ether phosphate, fatty alcohol-polyoxyethylene ether sodium sulfate and fatty acid methyl ester sodium sulfonate.
Preferably, the number of the surfactants is 1 to 4.
The efficient cyhalothrin nano-water aqua with good stability and better drug effect is obtained by compounding or singly using the nonionic surfactant, the anionic surfactant and the like and then compounding the effective component cyhalothrin.
Preferably, the efficient cyhalothrin can be independently prepared into a nano water aqua for use, and can also be compounded with other deinsectization mite removal medicaments to be prepared into the nano water aqua for use by selecting a proper surfactant.
The invention also aims to provide a preparation method of the lambda-cyhalothrin nano-water aqua.
Specifically, the preparation method of the lambda-cyhalothrin nano water agent comprises the following steps:
mixing and stirring the efficient cyhalothrin and the surfactant at normal temperature (10-35 ℃) to uniformly disperse the efficient cyhalothrin in the surfactant;
and (2) adding water, and uniformly stirring to form a surfactant micelle solution, namely the efficient cyhalothrin nano-water aqua.
Preferably, in the step (1), the stirring speed is adjusted according to actual conditions, so that the beta-cypermethrin is uniformly dispersed in the surfactant.
Preferably, in the step (1), the stirring speed is 60-100 revolutions per second, the stirring time is generally 0.5h, and the time can be adjusted by a technician so that the efficient cyhalothrin is uniformly dispersed in the surfactant.
Preferably, in the step (2), the stirring speed is adjusted according to actual conditions, so as to form the surfactant micelle solution by uniformly stirring.
Preferably, in the step (2), the stirring speed is 60-100 rpm/s, and the stirring time is 0.5-1 h.
The efficient cyhalothrin nano-water aqua is used for controlling pests such as aphids, armyworms, diamondback moths, cabbage caterpillars, oriental tobacco budworms, corn bollworms, pink bollworms, peach plantlets, oriental fruit moths, citrus leaf miners, tea caterpillars, tea plant hoppers, tea leafhoppers and the like on crops such as wheat, rapes, vegetables, cotton, fruit trees, tea leaves, tobacco and the like.
Different from the conventional pesticide aqueous solution, the active ingredients in the nano aqueous solution are insoluble in water and can not form a true solution, but are coated by nano-scale surfactant micelles and uniformly dispersed in water to form the true solution.
The nano water agent containing the efficient cyhalothrin is transparent and colorless in appearance, and the average particle size of the surfactant micelle is in a nano level; after entering water, the water-soluble polymer can be quickly dissolved with water to form a completely transparent solution, and the dilution stability is qualified.
Compared with the prior art, the invention has the beneficial effects that:
1. the efficient cyhalothrin nano water aqua disclosed by the invention does not contain any organic solvent, is safe and environment-friendly, belongs to an environment-friendly formulation, is suitable for agricultural medication, is suitable for the requirement of sanitary medication, and can be widely applied to the fields of agriculture, families and public health.
2. Because the active ingredients are carried by the nano micelle, the invention can form true solution, the preparation is more stable, the preparation is still stable after being stored at 0 ℃ for 7 days and stored at 54 ℃ for 14 days, the high-efficiency cyhalothrin can not be separated out, the storage is convenient, and the shelf life is longer.
3. The invention is a nanometer preparation product, has extremely small medicine fineness, no particle precipitation and better medicine effect, and is more suitable for the unmanned aerial vehicle pesticide application technology.
4. The nano water aqua has excellent quick action and persistence, and adverse reactions such as phytotoxicity and the like can not occur.
5. The efficient cyhalothrin nano water aqua has the advantages of low production cost, simple preparation process and good economy.
Drawings
FIG. 1 shows the 4.5% aqueous solution of lambda-cyhalothrin prepared in example 8 after standing at low temperature (0 deg.C) for 1-2 days and then heating to room temperature.
FIG. 2 shows the situation of 4.5% of lambda-cyhalothrin aqueous solution prepared in comparative example 4 at room temperature after being placed at low temperature (0 deg.C) for 1-2 days and then heated to room temperature.
Detailed Description
The present invention will be described in further detail with reference to examples. The reagents or instruments used are not indicated by manufacturers, and are regarded as conventional products which can be purchased in the market.
The method for detecting the particle size of the nano water agent comprises the following steps:
the particle size of the surfactant micelle in the pesticide Nano water agent is measured by a Marvens high-sensitivity Nano particle size analyzer Zetasizer Nano S (25 ℃).
Example 1
The preparation method comprises the following steps: weighing 10g of raw efficient cyhalothrin (calculated by effective components, the same below) and 60g of fatty alcohol-polyoxyethylene ether, mixing the raw efficient cyhalothrin and the fatty alcohol-polyoxyethylene ether, stirring the mixture for 0.5h at the rotating speed of 100 revolutions per second, adding 930g of water under the stirring state, and continuously stirring the mixture for 1h to obtain the 1% efficient cyhalothrin nano-water aqua.
The nano water agent of the embodiment has transparent and colorless appearance, viscosity of 82mPa.s and average particle size of 224 nm. The nano water agent can be quickly dissolved with water after entering water to form a completely transparent solution, and the dilution stability is qualified.
The preparation has no precipitation phenomenon after cold storage at 0 deg.C for 7 days and hot storage at 54 deg.C for 14 days, and is stable.
Example 2
The preparation method is the same as that of the example 1, and the 1.5 percent efficient cyhalothrin nano-water agent is prepared.
The nano water agent of the embodiment has transparent and colorless appearance, viscosity of 100mPa.s and average particle size of 21.1 nm. The nano water agent can be quickly dissolved with water after entering water to form a completely transparent solution, and the dilution stability is qualified.
The preparation has no precipitation phenomenon after cold storage at 0 deg.C for 7 days and hot storage at 54 deg.C for 14 days, and is stable.
Example 3
The preparation method is the same as that of the example 1, and the efficient cyhalothrin nano water agent is prepared.
The nano water agent of the embodiment has transparent and colorless appearance, the viscosity of 95mPa.s and the average particle size of 18.4 nm. The nano water agent can be quickly dissolved with water after entering water to form a completely transparent solution, and the dilution stability is qualified.
The preparation has no precipitation phenomenon after cold storage at 0 deg.C for 7 days and hot storage at 54 deg.C for 14 days, and is stable.
Example 4
The preparation method is the same as that of the example 1, and the 2.5 percent efficient cyhalothrin nano-water agent is prepared.
The nano water agent of the embodiment has transparent and colorless appearance, viscosity of 102mPa.s and average particle size of 15.8 nm. The nano water agent can be quickly dissolved with water after entering water to form a completely transparent solution, and the dilution stability is qualified.
The preparation has no precipitation phenomenon after cold storage at 0 deg.C for 7 days and hot storage at 54 deg.C for 14 days, and is stable.
Example 5
The preparation method is the same as that of the example 1, and the 3 percent efficient cyhalothrin nano-water agent is prepared.
The nano water agent of the embodiment has transparent and colorless appearance, the viscosity of 78mPa.s and the average particle size of 22.3 nm. The nano water agent can be quickly dissolved with water after entering water to form a completely transparent solution, and the dilution stability is qualified.
The preparation has no precipitation phenomenon after cold storage at 0 deg.C for 7 days and hot storage at 54 deg.C for 14 days, and is stable.
Example 6
The preparation method is the same as that of the example 1, and the 3.5 percent efficient cyhalothrin nano-water agent is prepared.
The nano water agent of the embodiment has transparent and colorless appearance, viscosity of 89mPa.s and average particle size of 19.5 nm. The nano water agent can be quickly dissolved with water after entering water to form a completely transparent solution, and the dilution stability is qualified.
The preparation has no precipitation phenomenon after cold storage at 0 deg.C for 7 days and hot storage at 54 deg.C for 14 days, and is stable.
Example 7
The preparation method is the same as that of the example 1, and the 4 percent efficient cyhalothrin nano-water agent is prepared.
The nano water aqua of the embodiment has transparent and colorless appearance, the viscosity of 86mPa.s and the average particle size of 24.5 nm. The nano water agent can be quickly dissolved with water after entering water to form a completely transparent solution, and the dilution stability is qualified.
The preparation has no precipitation phenomenon after cold storage at 0 deg.C for 7 days and hot storage at 54 deg.C for 14 days, and is stable.
Example 8
The preparation method is the same as that of the example 1, and 4.5 percent of high-efficiency cyhalothrin nano-water agent is prepared.
The nano water agent of the embodiment has transparent and colorless appearance, the viscosity of 92mPa.s and the average particle size of 18.7 nm. The nano water agent can be quickly dissolved with water after entering water to form a completely transparent solution, and the dilution stability is qualified.
The preparation has no precipitation phenomenon after cold storage at 0 deg.C for 7 days and hot storage at 54 deg.C for 14 days, and is stable.
Example 9
The preparation method is the same as that of the example 1, and 5 percent of high-efficiency cyhalothrin nano-water agent is prepared.
The nano water agent of the embodiment has transparent and colorless appearance, viscosity of 102mPa.s and average particle size of 20.4 nm. The nano water agent can be quickly dissolved with water after entering water to form a completely transparent solution, and the dilution stability is qualified.
The preparation has no precipitation phenomenon after cold storage at 0 deg.C for 7 days and hot storage at 54 deg.C for 14 days, and is stable.
Comparative examples 1 to 4
The preparation experiment of the aqueous solution is carried out by adopting the auxiliary agent (wetting agent) adopted on the existing aqueous solution, and the specific formula is shown in table 1.
TABLE 1 COMPARATIVE EXAMPLE 1-COMPARATIVE EXAMPLE 4 FORMULATIONS
The preparation method is the same as example 1.
According to comparative examples 1 and 2, the lambda-cyhalothrin still cannot be completely dissolved in water with the addition of the auxiliary agent, and an acceptable aqueous solution cannot be formed.
According to the formulas of comparative example 3 and comparative example 4, the aqueous solution can be prepared at normal temperature (10-35 ℃), but when the aqueous solution is placed at low temperature (below 0 ℃), lambda-cyhalothrin is precipitated and cannot be recovered after heating. It is demonstrated that the qualified lambda-cyhalothrin nano-water agent cannot be prepared by using the surfactant which is not used in the conventional water agent except the surfactant or the surfactant composition in the invention.
Comparing the 4.5% beta-cypermethrin nano-water agent of the example 8 with the 4.5% beta-cypermethrin water agent of the comparative example, referring to fig. 1 and 2, fig. 1 is a state that the 4.5% beta-cyhalothrin nano-water agent prepared in the example 8 is placed at a low temperature (0 ℃) for 1-2 days and then heated to a normal temperature; FIG. 2 shows the situation of 4.5% of lambda-cyhalothrin aqueous solution prepared in comparative example 4 at room temperature after being placed at low temperature (0 deg.C) for 1-2 days and then heated to room temperature. As can be seen from the figure, the beta-cypermethrin nano water aqua of the application is still stable after being placed for 1-2 days, the solution is clear and transparent, while the solution of the comparative example becomes turbid and viscous, and the beta-cyhalothrin is separated out.
Example 10 comparison of biological Activity
The first field pesticide effect test:
reagent to be tested: the aqueous solution formulations of lambda-cyhalothrin of examples 1 to 9.
Control agents: 2.5% lambda-cyhalothrin emulsifiable concentrate (commercially available).
Control target: cotton bollworm. The test method comprises the following steps: the usage amount (effective component) of the high-efficiency cyhalothrin in normal field is adopted, the test cells are arranged in random block groups, and the setting area of each cell is 667m2And spraying by adopting an unmanned aerial vehicle, wherein the drug loading is 10L. Setting the flying height of 1.5m, the spraying width of 4.1m, the flying speed of 5m/s and the spraying amount of mixed water of 0.9L/mu, investigating the quantity of bollworm larvae in 1 day, 3 days, 7 days, 15 days, 30 days, 45 days and 60 days after treatment, and carrying out statistical analysis on the method and data according to the related standard GB/T17980.5-2000.
TABLE 2 field test Effect of Cotton bollworms
As can be seen from the table above, the efficient cyhalothrin nano water aqua shows excellent quick action and persistence on the prevention and treatment of cotton bollworms, and the persistence period is more than one month. In the test process, no adverse reactions such as phytotoxicity and the like are found, and the method has practical popularization and application values.
And (2) field efficacy test II:
reagent to be tested: 9 high-efficiency cyhalothrin nano-water agents in the embodiments 1 to 9.
Control agents: 2.5% lambda-cyhalothrin emulsifiable concentrate (commercially available).
Control target: wheat aphids.
The test method comprises the following steps: adopting the dosage (effective component) of the lambda-cyhalothrin in normal field, setting three times of repetition of dosage treatment, repeatedly adopting random block arrangement, and setting the area of each repetition to be 20m2Spraying with knapsack sprayer, investigating aphid larva number 1 day, 3 days, 7 days, 15 days, 30 days, 45 days and 60 days after treatment, and analyzing method and data according to GB/T17980.79-2004 standardThe process is carried out.
TABLE 3 field test Effect of wheat aphids
As can be seen from the table above, the efficient cyhalothrin nano-water agent shows excellent quick-acting property and lasting property in the prevention and treatment of wheat aphids, and the lasting period is more than one month. In the test process, no adverse reactions such as phytotoxicity and the like are found, and the method has practical popularization and application values.
And (3) field efficacy test:
reagent to be tested: 9 high-efficiency cyhalothrin nano-water agents in the embodiments 1 to 9.
Control agents: 2.5% lambda-cyhalothrin emulsifiable concentrate (commercially available).
Control target: cabbage borer.
The test method comprises the following steps: adopting the dosage (effective component) of the lambda-cyhalothrin in normal field, setting three times of repetition of dosage treatment, repeatedly adopting random block arrangement, and setting the area of each repetition to be 20m2And carrying out conventional spraying by using a knapsack sprayer, investigating the quantity of the larvae of the cabbage moth after 1 day, 3 days, 7 days, 15 days, 30 days, 45 days and 60 days after treatment respectively, and carrying out the method and data statistical analysis according to GB/T17980.14-2000 relevant standards.
TABLE 4 field test Effect of the vegetable borer
As can be seen from the above table, the efficient cyhalothrin nano-water aqua shows excellent quick-acting property and lasting effect on the prevention and treatment of the cabbage caterpillar, and the lasting period is more than one month. In the test process, no adverse reactions such as phytotoxicity and the like are found, and the method has practical popularization and application values.
The protection of the present invention is not limited to the above embodiments. Variations and advantages that may occur to those skilled in the art may be incorporated into the invention without departing from the spirit and scope of the inventive concept and the scope of the appended claims is intended to be protected.
Claims (6)
1. The efficient cyhalothrin nano-water agent is characterized in that the nano-water agent is prepared by taking efficient cyhalothrin, a surfactant and water as raw materials and adopting a surfactant micelle solubilization method; wherein the nano water agent contains 0.5-10% of efficient cyhalothrin, 5-20% of surfactant and the balance of water.
2. The lambda-cyhalothrin nano-water aqua according to claim 1, which is characterized in that the content of the lambda-cyhalothrin is 1-5% by mass.
3. The lambda-cyhalothrin nano-water aqua according to claim 1, wherein the surfactant is selected from any 1 or more of fatty alcohol polyoxyethylene ether, alkylphenol formaldehyde resin polyoxyethylene ether, styrylphenol polyoxyethylene ether, tristyrylphenol polyoxyethylene ether phosphate, fatty alcohol polyoxyethylene ether phosphate, alkylphenol polyoxyethylene ether phosphate and sodium fatty acid methyl ester sulfonate.
4. The preparation method of the lambda-cyhalothrin nano-water aqua according to claim 1, which is characterized in that the lambda-cyhalothrin is mixed with a surfactant, water is added, and the mixture is stirred to form a surfactant micelle solution, namely the lambda-cyhalothrin nano-water aqua.
5. The preparation method of lambda-cyhalothrin nano-water aqua according to claim 4, which is characterized by comprising the following steps:
mixing and stirring the efficient cyhalothrin and the surfactant at normal temperature to uniformly disperse the efficient cyhalothrin in the surfactant;
and (2) adding water, and continuously and uniformly stirring to form a surfactant micelle solution, namely the nano water agent containing the efficient cyhalothrin.
6. The method for preparing lambda-cyhalothrin nano water aqua according to claim 5, characterized in that in the step (1) and the step (2), the stirring speed is 60-100 revolutions per second.
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| PCT/CN2020/085561 WO2021093268A1 (en) | 2019-11-12 | 2020-04-20 | High-efficiency cyhalothrin nano aqueous solution, preparation method therefor and application thereof |
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