CN110973152A - High-efficiency cypermethrin nano water aqua and preparation method and application thereof - Google Patents
High-efficiency cypermethrin 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
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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
- A01N25/02—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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- 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
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- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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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
- A01N25/30—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 cypermethrin nano-water agent which takes high-efficiency cypermethrin, a surfactant and water as raw materials, does not contain any organic solvent, and is prepared by adopting a surfactant micelle solubilization method; wherein, the weight percentage content of the beta-cypermethrin in the nano water agent is 0.5-5%, the weight percentage content of the surfactant is 5-25%, and the balance is water. Compared with the conventional pesticide formulation, the nano water agent prepared by adopting the surfactant micelle solubilization technology has excellent stability, is still stable after being respectively stored at 0 ℃ for 7 days and at 54 ℃ for 14 days, is convenient to store and has longer shelf life, and the beta-cypermethrin is not precipitated; 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 novel beta-cypermethrin preparation and a preparation method and application thereof.
Background
Beta cypermethrin, chemical name 2, 2-dimethyl-3- (2, 2-dichlorovinyl) cyclopropane carboxylic acid- α -cyano- (3-phenoxy) benzyl ester, molecular formula C22H19CL2NO3. The high-efficiency cypermethrin is a broad-spectrum pesticide and has high insecticidal activity on a plurality of pests. Can be applied to crops such as various fruit trees, various vegetables, grain, cotton, oil-tea trees and the like and various forests. The pesticide has good killing effect on a plurality of pests such as oriental tobacco budworms, cotton bollworms, plutella xylostella, beet armyworms, prodenia litura, tea geometrids, pink bollworms, aphids, liriomyza, beetles, stinkbugs, psyllids, thrips, carpophagus, leaf rollers, caterpillars, moths, stinging moths, citrus leaf miners, ceroplastes and the like.
The beta-cypermethrin is difficult to dissolve in water, and the solubility of the beta-cypermethrin in water is 93.4 mu g/L at 25 ℃; the pesticide formulations developed by taking the beta-cypermethrin 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; the use of organic solvent is reduced, and the development of aqueous dosage forms is a necessary way for the development of the high-efficiency cypermethrin dosage forms.
With the increasing environmental awareness of users and the rapidly growing demand for sanitary medicine, the existing dosage forms of beta-cypermethrin can not meet the use requirements. In order to accelerate the popularization and the application of the high-efficiency cypermethrin product on the premise of safety and environmental protection, the development of a novel preparation which is friendly to people, livestock and environment and is convenient for the application of aerial plant protection technologies and equipment such as unmanned aerial vehicles is particularly necessary.
Disclosure of Invention
The invention provides a high-efficiency cypermethrin nano water aqua, a preparation method and application thereof aiming at the existing technical problems; the application adopts a surfactant micelle solubilization technology, and utilizes a nano-scale micelle solution formed by the surfactant to bear pesticide component beta-cypermethrin which is insoluble in water under the condition of no organic solvent for assisting in dissolution, so as to form a novel nano water aqua. 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 wrapped by the nano-scale surfactant micelle and uniformly dispersed in water to form the true solution.
The purpose of the invention can be realized by the following technical scheme:
the beta-cypermethrin nano water agent is prepared by taking beta-cypermethrin, a surfactant and water as raw materials, does not contain any organic solvent and is prepared by adopting a surfactant micelle solubilization technology; wherein, the weight percentage content of the beta-cypermethrin in the nano water agent is 0.5-5%, the weight percentage content of the surfactant is 5-25%, and the balance is water.
Preferably, the beta-cypermethrin is 1-4.5% by mass, the surfactant is 5-20% by mass, and the balance is water.
The surfactant is selected from any 1 or more of tristyrylphenol polyoxyethylene ether phosphate, alcohol ether succinic acid monoester sodium sulfonate, styrylphenol polyoxyethylene ether, fatty alcohol-polyoxyethylene ether phosphate, alkylphenol polyoxyethylene ether phosphate, fatty alcohol-polyoxyethylene ether, sorbitan fatty acid ester polyoxyethylene ether and alkylphenol formaldehyde resin polyoxyethylene ether, and the preferable number is 1-4.
The invention also aims to provide a preparation method of the beta-cypermethrin nano water aqua.
Specifically, the preparation method of the beta-cypermethrin nano water agent comprises the following steps:
mixing and stirring the beta-cypermethrin and the surfactant at normal temperature (10-35 ℃) to uniformly disperse the beta-cypermethrin in the surfactant;
and (2) adding water, and uniformly stirring to form a surfactant micelle solution, namely the high-efficiency cypermethrin nano water aqua.
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 beta-cypermethrin is uniformly dispersed in the surfactant.
Preferably, in the step (2), the stirring speed is 60-100 rpm/s, and the stirring time is 0.5-1 h.
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 a true solution.
The beta-cypermethrin nano water agent is light yellow transparent liquid, and the average grain diameter of a 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 beta-cypermethrin nano water aqua 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 and still stable after being stored at 0 ℃ for 7 days and at 54 ℃ for 14 days, the beta-cypermethrin 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 high-efficiency cypermethrin nano water agent has low production cost, simple processing technology and very good economy.
Drawings
FIG. 1 shows the 2.5% aqueous solution of beta-cypermethrin prepared in example 4 after being left at low temperature (0 ℃) for 1-2 days and then heated to normal temperature.
FIG. 2 shows the state of 2.5% aqueous solution of beta-cypermethrin prepared in comparative example 3 at room temperature after being placed at low temperature (0 ℃) 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 cypermethrin (calculated by effective components, the same below) and 70g of fatty alcohol-polyoxyethylene ether phosphate, mixing, stirring for 0.5h at the rotating speed of 90 revolutions per second, adding 940g of water under the stirring state, and continuously stirring for 1h to obtain the 1% efficient cypermethrin nano-water aqua.
The nano water agent in the embodiment is light yellow transparent liquid, the viscosity is 85mPa.s, and the average particle size is 13.0 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 beta-cypermethrin nano water agent is prepared.
The nano water agent of the embodiment is light yellow transparent liquid, the viscosity is 100mPa.s, and the average particle size is 16.5 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 3
The preparation method is the same as that of the example 1, and the 2 percent beta-cypermethrin nano water agent is prepared.
The nano water agent of the embodiment is light yellow transparent liquid, the viscosity is 92mPa.s, and the average particle size is 18.0 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 beta-cypermethrin nano water agent is prepared.
The nano water agent of the embodiment is light yellow transparent liquid, the viscosity is 88mPa.s, and the average particle size is 22.5 nm.
The nano water agent can be quickly dissolved with water after being put into 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 beta-cypermethrin nano water aqua is prepared.
The nano water agent of the embodiment is light yellow transparent liquid, the viscosity is 75mPa.s, and the average particle size is 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 6
The preparation method is the same as that of the example 1, and the 3.5 percent beta-cypermethrin nano water agent is prepared.
The nano water agent of the embodiment is light yellow transparent liquid, the viscosity is 77mPa.s, and the average particle size is 18.5 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 beta-cypermethrin nano water agent is prepared.
The nano water agent of the embodiment is light yellow transparent liquid, the viscosity is 78mPa.s, and the average particle size is 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 8
The preparation method is the same as that of the example 1, and the 4.5 percent beta-cypermethrin nano water agent is prepared.
The nano water agent of the embodiment is light yellow transparent liquid, the viscosity is 85mPa.s, and the average particle size is 21.3 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.
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 formulations of comparative examples 1-4
The preparation method is the same as example 1.
In comparative examples 1 and 2, the beta-cypermethrin was still not completely dissolved in water with the addition of the adjuvant, and a satisfactory aqueous solution could not be formed.
Comparative examples 3 and 4 were able to prepare aqueous solutions at normal temperature (10-35 ℃), but when the aqueous solutions were placed at low temperature (below 0 ℃), the cypermethrin base compound would be continuously precipitated and would not recover after warming, indicating that acceptable aqueous solutions of cypermethrin could not be prepared using surfactants other than the surfactant of the present invention or the conventional aqueous solutions other than the surfactant composition.
Comparing the 2.5% beta-cypermethrin nano-water agent of the example 4 with the 2.5% beta-cypermethrin water agent of the comparative example, referring to fig. 1 and 2, fig. 1 is a state that the 2.5% beta-cypermethrin nano-water agent prepared in the example 4 is placed at a low temperature (0 ℃) for 1-2 days and then heated to a normal temperature; FIG. 2 shows the state of 2.5% aqueous solution of beta-cypermethrin prepared in comparative example 3 at room temperature after being placed at low temperature (0 ℃) 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, and the solution of the comparative example is turbid and has a foaming phenomenon.
Example 9 comparison of biological Activity
The first field pesticide effect test:
reagent to be tested: the aqueous solutions of beta-cypermethrin of examples 1 to 8.
Control agents: 4.5% of high-efficiency cypermethrin emulsifiable concentrate (sold on the market).
Control target: cotton bollworm.
The test method comprises the following steps: the normal interplantation amount (effective component) of the high-efficiency cypermethrin 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 beta-cypermethrin nano water aqua shows excellent quick-acting property and lasting effect on the prevention and treatment of cotton bollworms, 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 (2) field efficacy test II:
reagent to be tested: the aqueous solutions of beta-cypermethrin of examples 1 to 8.
Control agents: 4.5% of high-efficiency cypermethrin emulsifiable concentrate (sold on the market).
Control target: cotton aphids.
The test method comprises the following steps:
adopting the dosage (effective component) of the high-efficiency cypermethrin in the normal field, setting three times of repetition of dosage treatment, repeatedly adopting random block arrangement, and setting the area of each repetition to be 20m2Conventional spraying is carried out by using a knapsack sprayer, the number of aphid larvae is investigated 1 day, 3 days, 7 days, 15 days, 30 days, 45 days and 60 days after treatment, and the method and the data statistical analysis are carried out according to GB/T17980.75-2004 relevant standards.
TABLE 3 field test Effect of Cotton aphids
As can be seen from the table above, the beta-cypermethrin nano water aqua shows excellent quick-acting property and lasting property in the prevention and treatment of cotton aphids, and the lasting period is as long as 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: 8 high-efficiency cypermethrin nano-water agents in the embodiments 1 to 8.
Control agents: 4.5% of high-efficiency cypermethrin emulsifiable concentrate (sold on the market).
Control target: cabbage borer.
The test method comprises the following steps:
adopts the normal field dosage of the beta-cypermethrin (includingEffective component), the dose treatment was set up in three replicates, the replicates were arranged in random blocks, each replicate setting an area of 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 high-efficiency cypermethrin nano-water aqua shows excellent quick-acting property and lasting effect on the prevention and treatment of the cabbage borer, 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 beta-cypermethrin nano water agent is characterized in that the nano water agent is prepared by taking beta-cypermethrin, a surfactant and water as raw materials and adopting a surfactant micelle solubilization method; wherein, the weight percentage content of the high-efficiency cypermethrin in the nano water agent is 0.5-5%, the weight percentage content of the surfactant is 5-25%, and the balance is water.
2. The beta-cypermethrin nano water aqua according to claim 1, which is characterized in that the content of the beta-cypermethrin is 1-4.5% by mass.
3. The cypermethrin nano-water aqua according to claim 1, wherein the surfactant is selected from any 1-4 of tristyrylphenol polyoxyethylene ether phosphate, alcohol ether succinic acid monoester sodium sulfonate, styrylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether phosphate, alkylphenol polyoxyethylene ether phosphate, fatty alcohol polyoxyethylene ether, sorbitan fatty acid ester polyoxyethylene ether and alkylphenol formaldehyde resin polyoxyethylene ether.
4. The preparation method of the beta-cypermethrin nano water aqua of claim 1 is characterized in that the beta-cypermethrin is mixed with a surfactant, water is added, and the mixture is stirred to form a surfactant micelle solution, namely the beta-cypermethrin nano water aqua.
5. The preparation method of the beta-cypermethrin nano water aqua according to claim 4, which is characterized by comprising the following steps:
mixing and stirring the beta-cypermethrin and the surfactant at normal temperature to uniformly disperse the beta-cypermethrin in the surfactant;
and (2) adding water, and uniformly stirring to form a surfactant micelle solution, namely the high-efficiency cypermethrin nano water aqua.
6. The preparation method of the beta-cypermethrin nano water aqua according to claim 5, wherein in the step (1) and the step (2), the stirring speed is 60-100 revolutions per second.
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| PCT/CN2020/085763 WO2021093271A1 (en) | 2019-11-12 | 2020-04-21 | Beta cypermethrin nano aqueous agent, preparation method therefor and use thereof |
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Cited By (6)
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| WO2021093268A1 (en) * | 2019-11-12 | 2021-05-20 | 南京华洲药业有限公司 | High-efficiency cyhalothrin nano aqueous solution, preparation method therefor and application thereof |
| WO2021093270A1 (en) * | 2019-11-13 | 2021-05-20 | 南京华洲药业有限公司 | Compound insecticidal and acaricidal nano aqueous formulation containing fenpropathrin and emamectin benzoate, and use thereof |
| WO2021093267A1 (en) * | 2019-11-12 | 2021-05-20 | 南京华洲药业有限公司 | Composite insecticidal and acaricidal nano-aqueous agent containing fenpropathrin and chlorpyrifos, and preparation method therefor and use thereof |
| WO2021093271A1 (en) * | 2019-11-12 | 2021-05-20 | 南京华洲药业有限公司 | Beta cypermethrin nano aqueous agent, preparation method therefor and use thereof |
| WO2021093266A1 (en) * | 2019-11-11 | 2021-05-20 | 南京华洲药业有限公司 | Compound insecticidal and acaricidal nano aqueous formulation containing lambda-cyhalothrin and emamectin benzoate, and use thereof |
| WO2021093269A1 (en) * | 2019-11-13 | 2021-05-20 | 南京华洲药业有限公司 | Nano aqueous agent comprising prochloraz and processing method therefor |
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| WO2021093266A1 (en) * | 2019-11-11 | 2021-05-20 | 南京华洲药业有限公司 | Compound insecticidal and acaricidal nano aqueous formulation containing lambda-cyhalothrin and emamectin benzoate, and use thereof |
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| WO2021093267A1 (en) * | 2019-11-12 | 2021-05-20 | 南京华洲药业有限公司 | Composite insecticidal and acaricidal nano-aqueous agent containing fenpropathrin and chlorpyrifos, and preparation method therefor and use thereof |
| WO2021093271A1 (en) * | 2019-11-12 | 2021-05-20 | 南京华洲药业有限公司 | Beta cypermethrin nano aqueous agent, preparation method therefor and use thereof |
| WO2021093270A1 (en) * | 2019-11-13 | 2021-05-20 | 南京华洲药业有限公司 | Compound insecticidal and acaricidal nano aqueous formulation containing fenpropathrin and emamectin benzoate, and use thereof |
| WO2021093269A1 (en) * | 2019-11-13 | 2021-05-20 | 南京华洲药业有限公司 | Nano aqueous agent comprising prochloraz and processing method therefor |
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| WO2021093271A1 (en) | 2021-05-20 |
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