CN110999902A - Nanometer water agent containing prochloraz and processing method thereof - Google Patents
Nanometer water agent containing prochloraz and processing method thereof Download PDFInfo
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- CN110999902A CN110999902A CN201911109339.4A CN201911109339A CN110999902A CN 110999902 A CN110999902 A CN 110999902A CN 201911109339 A CN201911109339 A CN 201911109339A CN 110999902 A CN110999902 A CN 110999902A
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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
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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
- 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
Abstract
The invention belongs to the technical field of pesticides, and discloses a nano water agent containing prochloraz, which contains 0.5-10% of prochloraz by mass, 5-25% of surfactant by mass and the balance of water, and does not contain any organic solvent, and the nano water agent is prepared by adopting a surfactant micelle solubilization technology, has excellent stability compared with the conventional pesticide formulation, is still stable after being respectively stored at 0 ℃ for 7 days and 54 ℃ for 14 days, cannot precipitate chlorpyrifos, 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 novel preparation containing prochloraz-nano water aqua and a processing method thereof.
Background
Prochloraz (Prochloraz) is a broad-spectrum bactericide with the molecular formula: c15H16Cl3N3O2The chemical name is: N-propyl-N- [2- (2,4, 6-trichlorophenoxy) ethyl]-imidazole-1-carboxamide. The prochloraz has obvious control effect on diseases of various crops caused by ascomycetes and adelomycetes, and can also be mixed with most of bactericides, insecticides and herbicides to achieve better control effect. It has therapeutic and eradicating effects on various diseases of field crops, fruits and vegetables, turf and ornamental plants.
Prochloraz is insoluble in water and has a solubility of only 5.5mg/L in water at 25 ℃. The pesticide formulations developed by taking prochloraz as a raw material at present mainly comprise missible oil, an aqueous emulsion and the like, and both the missible oil and the aqueous emulsion contain a large amount of organic solvents. In the using process, the organic solvent not only causes serious harm to the environment, but also seriously affects the quality of agricultural products, accelerates the food safety crisis and harms human health.
With the increasing environmental awareness of users and the rapidly growing demand for sanitary medicine, the existing dosage forms of prochloraz cannot meet the use requirements. In order to accelerate the popularization and use of prochloraz products on the premise of safety and environmental protection, it is particularly necessary to develop a novel preparation which is friendly to human 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 technical problems, the inventor screens out a specific surfactant, and utilizes the surfactant to form a micelle with an average particle size of nanometer under the condition of no organic solvent for assisting dissolution, wherein the micelle is used for bearing a pesticide ingredient prochloraz which is difficult to dissolve in water, so as to realize water aqua formulation and form a novel pesticide nano water aqua.
The purpose of the invention is realized by the following technical scheme:
a nanometer aqueous solution containing prochloraz, only regard technical, surfactant active and water of prochloraz as raw materials, adopt the solubilization technology of surfactant micelle to make, the nanometer aqueous solution does not contain any organic solvent; wherein the mass percent of the active ingredient prochloraz is 0.5-25%, the mass percent of the surfactant is 3-25%, and the balance is water.
Preferably, in the nano water agent, the mass percentage of the prochloraz is 1-10%, the mass percentage of the surfactant is 3-25%, and the balance is water.
The surfactant is selected from 1 or more of fatty alcohol-polyoxyethylene ether, alkylphenol formaldehyde resin polyoxyethylene ether, styryl phenol polyoxyethylene ether, fatty alcohol-polyoxyethylene ether phosphate, tristyryl phenol polyoxyethylene ether phosphate, sodium fatty acid methyl ester sulfonate, sodium alcohol ether succinic acid monoester sulfonate and sorbitan fatty acid ester polyoxyethylene ether.
The invention also aims to provide a preparation method of the nano water aqua containing the prochloraz.
Specifically, the preparation method of the prochloraz-containing nano water agent comprises the following steps:
mixing prochloraz active compound and surfactant at normal temperature (10-35 ℃), and stirring to uniformly disperse prochloraz in the surfactant;
and (2) adding water, and uniformly stirring to form a surfactant micelle solution, namely the prochloraz nano-water solution.
Preferably, in the step (1), the stirring speed is 60-100 r/s, and the stirring time is about 0.5h to uniformly disperse the prochloraz 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.
Compared with 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 the nano-scale surfactant micelle and uniformly dispersed in water to form the true solution. The prochloraz-containing nano water agent is light yellow transparent liquid, can be quickly dissolved with water after being put into water to form completely transparent solution, is qualified in dilution stability, and is more suitable for the unmanned aerial vehicle pesticide application technology.
The nano water aqua containing the prochloraz can be widely applied to prevention and treatment of various fungal diseases such as rice blast, wheat sheath blight and pepper anthracnose on field crops, fruits, vegetables, turf and ornamental plants, has excellent quick-acting performance compared with the existing emulsifiable concentrate, is more convenient for attachment, spreading and penetration on a target due to the existence of the prochloraz in the nano water aqua as nano particles, is more resistant to rain wash, has excellent persistence, has the prevention effect remarkably higher than that of the prochloraz emulsifiable concentrate with the same period by 25 percent under the premise of the same application amount, and has more excellent pesticide effect.
The invention discloses a method for detecting the particle size of a nano water agent, which 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 ℃).
Compared with the prior art, the invention has the beneficial effects that:
1. the prochloraz nano water aqua disclosed by the invention does not contain any organic solvent, is safe and environment-friendly, belongs to an environment-friendly dosage form, is suitable for agricultural medication, meets the requirement of sanitary medication, and can be widely applied to the fields of agriculture, families and public health.
2. The invention has the advantages of low production cost, simple processing technology and good economy.
3. The active ingredients in the invention are carried by the nano micelle, so that a true solution can be formed, the preparation is more stable, the preparation is still stable after being stored at 0 ℃ for 7 days and at 54 ℃ for 14 days, the prochloraz cannot be separated out, the storage is convenient, and the shelf life is longer.
4. The invention is a nanometer preparation product, has extremely small medicine fineness, no particle precipitation and better medicine effect.
Drawings
FIG. 1 shows the 6% prochloraz water-base nano-agent prepared in example 6 after standing at low temperature (0 deg.C) for 1-2 days and then heating to room temperature.
FIG. 2 shows the 6% prochloraz water 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 invention is further illustrated by the following examples, without limiting the scope of the invention:
example 1
The preparation method comprises the following steps: weighing 10g of prochloraz original drug (calculated by the ingredients, the same below), 80g of styrylphenol polyoxyethylene ether and 20g of alkylphenol formaldehyde resin polyoxyethylene ether according to the dosage, mixing the three, stirring for 0.5h at the rotating speed of 100 revolutions per second, adding 890g of water in the stirring state, and continuously stirring for 1h to obtain the 1% prochloraz nano-aqueous solution.
The nano water agent of the embodiment has yellowish and transparent appearance, viscosity of 105 mPas and average particle size of 12.0 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 nano water agent of the embodiment has no precipitation phenomenon after being stored at 0 ℃ for 7 days and at 54 ℃ for 14 days respectively, and is still stable.
Example 2
The preparation method is the same as that of the example 1, and 2 percent of prochloraz nano water aqua is prepared.
The nano water aqua of the embodiment has transparent and colorless appearance, viscosity of 86mPa · s and average particle size of 14.7 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 nano water agent of the embodiment has no precipitation phenomenon after being stored at 0 ℃ for 7 days and at 54 ℃ for 14 days respectively, and is still stable.
Example 3
The preparation method is the same as the example 1, and the 3 percent prochloraz nano water aqua is prepared.
The nano water agent of the embodiment has yellowish and transparent appearance, viscosity of 95mPa & s and average particle size of 17.8 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 nano water agent of the embodiment has no precipitation phenomenon after being stored at 0 ℃ for 7 days and at 54 ℃ for 14 days respectively, and is still stable.
Example 4
The preparation method is the same as the example 1, and 4 percent of prochloraz nano water aqua is prepared.
The nano water agent of the embodiment has yellowish and transparent appearance, viscosity of 78 mPas 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 nano water agent of the embodiment has no precipitation phenomenon after being stored at 0 ℃ for 7 days and at 54 ℃ for 14 days respectively, and is still stable.
Example 5
The preparation method is the same as that of the example 1, and 5 percent of prochloraz nano water aqua is prepared.
The nano water agent of the embodiment has yellowish and transparent appearance, viscosity of 80 mPas and average particle size of 21.7 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 nano water agent of the embodiment has no precipitation phenomenon after being stored at 0 ℃ for 7 days and at 54 ℃ for 14 days respectively, and is still stable.
Example 6
The preparation method is the same as the example 1, and 6 percent of prochloraz nano water aqua is prepared.
The nano water agent of the embodiment has yellowish and transparent appearance, viscosity of 76mPa & s and average particle size of 23.6 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 nano water agent of the embodiment has no precipitation phenomenon after being stored at 0 ℃ for 7 days and at 54 ℃ for 14 days respectively, and is still stable. Referring to fig. 1, after the 6% prochloraz nano water agent is placed at 0 ℃ for 1-2 days and then heated to normal temperature, the appearance is still yellowish and transparent without precipitates.
Example 7
The preparation method is the same as that of the example 1, and the 7 percent prochloraz nano water aqua is prepared.
The nano water agent of the embodiment has yellowish and transparent appearance, viscosity of 78mPa · s and average particle size of 24.1 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 nano water agent of the embodiment has no precipitation phenomenon after being stored at 0 ℃ for 7 days and at 54 ℃ for 14 days respectively, and is still stable.
Example 8
The preparation method is the same as the example 1, and 9 percent of prochloraz nano water aqua is prepared.
The nano water agent of the embodiment has yellowish and transparent appearance, viscosity of 67 mPas and average particle size of 23.7 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 nano water agent of the embodiment has no precipitation phenomenon after being stored at 0 ℃ for 7 days and at 54 ℃ for 14 days respectively, and is still stable.
Example 9
The preparation method is the same as that of the example 1, and the 10 percent prochloraz nano water aqua is prepared.
The nano water agent of the embodiment has yellowish and transparent appearance, viscosity of 80mPa & 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 nano water agent of the embodiment has no precipitation phenomenon after being stored at 0 ℃ for 7 days and at 54 ℃ for 14 days respectively, and is still stable.
Comparative examples 1 to 4
The preparation experiment of the aqueous solution is carried out by adopting a conventional auxiliary agent (wetting agent), and the specific formula is shown in table 1.
TABLE 1 formulations of comparative examples 1 to 4
The raw materials are weighed according to the formulas of the comparative example 1 and the comparative example 2, and the preparation method of the example 1 is adopted, so that the prochloraz can not be completely dissolved in water under the condition of adding the auxiliary agent, and a qualified aqueous solution can not be formed. According to the formulas of the comparative example 3 and the comparative example 4, the raw materials are weighed, the preparation method of the example 1 is adopted, the aqueous solution can be prepared at normal temperature (10-35 ℃), but when the aqueous solution is placed at low temperature (below 0 ℃), prochloraz is continuously separated out, and the prochloraz cannot be recovered after the temperature is raised (see figure 2). It is demonstrated that the surfactant used by the conventional water aqua besides the surfactant of the invention can not be used for preparing qualified prochloraz nano water aqua.
Example 11 comparison of biological Activity
The first field pesticide effect test:
reagent to be tested: examples 1-9 the prochloraz water aqua nanoparticles prepared in example 1.
Control agents: 25% prochloraz emulsifiable concentrate (commercially available).
Control target: rice blast of rice.
The test method comprises the following steps:
1. and (3) test treatment: the test agent dosage is respectively set with three treatment concentrations according to different components, and the contrast agent is a pesticide single-agent 25% prochloraz emulsifiable concentrate and a blank clear water test.
2. The test method comprises the following steps: each cell area is 66.7m2Repeating the steps for 3 times; the pesticide effect method for investigation before pesticide application and investigation after prevention and treatment comprises the following steps: randomly sampling 5 spots (5 m per spot) in the test treatment area2) Grading the disease condition according to the relevant standards of the national field test, and calculating the prevention effect.
3. The results of the tests are given in the following table:
table 2 field test effects of the formulations of the examples of the present invention on prevention and treatment of Pyricularia oryzae
As can be seen from the table above, the prochloraz nanometer water aqua has excellent quick-acting property and lasting effect on the prevention and treatment of rice blast, and the lasting effect 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 (2) field efficacy test II:
reagent to be tested: examples 1-9 the prochloraz water aqua nanoparticles prepared in example 1.
Control agents: 25% prochloraz emulsifiable concentrate (commercially available).
Control target: anthracnose of hot pepper.
The test method comprises the following steps:
1. and (3) test treatment: the test agent dosage is respectively set with three treatment concentrations according to different components, and the contrast agent is a pesticide single-agent 25% prochloraz emulsifiable concentrate and a blank clear water test.
2. The test method comprises the following steps: each cell area is 66.7m2Repeating the steps for 3 times; the pesticide effect method for investigation before pesticide application and investigation after prevention and treatment comprises the following steps: randomly sampling 5 spots (5 m per spot) in the test treatment area2) Grading the disease condition according to the relevant standards of the national field test, and calculating the prevention effect.
3. The results of the tests are given in the following table:
TABLE 3 field test Effect of the formulations of the examples of the present invention on controlling Pepper anthracnose
As can be seen from the table above, the prochloraz nano-water aqua has excellent quick action and persistence on the prevention and treatment of pepper anthracnose, and the persistence 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.
Claims (6)
1. A nanometer aqueous solution containing prochloraz, characterized by that the nanometer aqueous solution takes prochloraz original medicine, surfactant active and water as raw materials, adopt the solubilized technology of surfactant micelle to make; wherein, the mass percentage of the prochloraz is 0.5-25%, the mass percentage of the surfactant is 3-25%, and the balance is water.
2. The nano water aqua containing prochloraz according to claim 1, wherein the mass percent of the prochloraz is 1-10%, the mass percent of the surfactant is 3-25%, and the balance is water.
3. The prochloraz-containing nano-water aqua of claim 1, wherein the surfactant is selected from the group consisting of 1 or more of fatty alcohol-polyoxyethylene ether, alkylphenol formaldehyde resin polyoxyethylene ether, styrylphenol polyoxyethylene ether, fatty alcohol-polyoxyethylene ether phosphate, tristyrylphenol polyoxyethylene ether phosphate, sodium fatty acid methyl ester sulfonate, sodium alcohol ether succinate monoester sulfonate, and sorbitan fatty acid ester polyoxyethylene ether.
4. The method for processing the nano water aqua containing prochloraz of claim 1, wherein the prochloraz is mixed with the surfactant, and then the mixture is added with water and stirred to form a surfactant micelle solution, thus obtaining the nano water aqua containing prochloraz.
5. The processing method of the prochloraz-containing nano water aqua according to claim 4, characterized by comprising the following steps:
mixing prochloraz active compound and surfactant at normal temperature, and stirring to uniformly disperse the prochloraz in the surfactant;
and (2) adding water, and uniformly stirring to form a surfactant micelle solution, namely the prochloraz nano-water solution.
6. The method for processing the prochloraz-containing nano water aqua according to claim 4, wherein in the step (1), the stirring speed is 60-100 r/s; in the step (2), the stirring speed is 60-100 rpm/s.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911109339.4A CN110999902A (en) | 2019-11-13 | 2019-11-13 | Nanometer water agent containing prochloraz and processing method thereof |
| PCT/CN2020/085622 WO2021093269A1 (en) | 2019-11-13 | 2020-04-20 | Nano aqueous agent comprising prochloraz and processing method therefor |
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| CN201911109339.4A CN110999902A (en) | 2019-11-13 | 2019-11-13 | Nanometer water agent containing prochloraz and processing method thereof |
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Cited By (5)
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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 |
| 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 |
| 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 |
| 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 |
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