CN112889824A - Self-emulsifying aqueous emulsion containing acetochlor - Google Patents
Self-emulsifying aqueous emulsion containing acetochlor Download PDFInfo
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- CN112889824A CN112889824A CN202110086796.7A CN202110086796A CN112889824A CN 112889824 A CN112889824 A CN 112889824A CN 202110086796 A CN202110086796 A CN 202110086796A CN 112889824 A CN112889824 A CN 112889824A
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- aqueous emulsion
- acetochlor
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- water
- emulsifier
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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
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/18—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof
- A01N37/26—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof containing the group; Thio analogues thereof
-
- 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
Abstract
The invention relates to an aqueous emulsion containing acetochlor, the average grain diameter of which is 0.4-0.7 mu m; the acetochlor-containing aqueous emulsion comprises the following components in percentage by mass: 20-60% of acetochlor technical product, 3-6% of emulsifier, 2-8% of antifreezing agent and the balance of water; the emulsifier comprises the following components in parts by weight: 0.5-2 parts of polyvinyl alcohol, 1-3 parts of castor oil polyoxyethylene ether and 2-4 parts of calcium dodecyl benzene sulfonate; the emulsion in water provided by the invention does not need high-speed shearing, namely the average particle size formed by automatic emulsification is smaller, and the product stability is improved.
Description
Technical Field
The invention belongs to the field of pesticide preparations, and particularly relates to a self-emulsifying aqueous emulsion containing acetochlor.
Background
The acetochlor series dry land amide herbicide has the characteristics of safety, high efficiency, wide weed control spectrum and the like, can be used for soybeans, corns, peanuts, cotton, rapes, watermelons and the like, generally has a control effect after 10-20 days of application, has a pesticide effect peak period of 30-60 days and has a residual effect period of 70-80 days. Can prevent and kill a series of weeds such as crabgrass, barnyard grass, green bristlegrass, alopecurus, teff, goosegrass, stiff grass, chickweed, pigweed, sparrow tongue grass, purslane and the like.
The traditional acetochlor aqueous emulsion is usually prepared by mixing acetochlor, an emulsifier and a solvent to prepare an oil phase, then dropwise adding the oil phase into a water phase, and then crushing oil drops into 0.5-2 micron emulsion through high-speed shearing.
Chinese patent document CN102885042A (application number: 201210424065.X) discloses an environment-friendly potato field weeding composition, which consists of 30-85 parts by weight of acetochlor, 1-30 parts by weight of soybean oil, 5-20 parts by weight of emulsifier special for acetochlor and 3-30 parts by weight of turpentine; wherein the emulsifier special for acetochlor is prepared from calcium dodecylbenzenesulfonate, phenethylphenol polyoxyethylene ether and castor oil polyoxyethylene ether according to the proportion of (1-3): (1.5-4): (2-8) at normal temperature and pressure.
The invention is different from the patent document CN102885042A in that the invention takes water as a substrate, polyvinyl alcohol as an emulsifier and calcium dodecyl benzene sulfonate and castor oil polyoxyethylene ether are used for synergistic action, the particle size of the prepared emulsion is less than 0.7 micron, and the product stability is good.
Chinese patent document CN101530079A (application number: 200810101927.9) discloses an aqueous emulsion containing acetochlor, which relates to the aqueous emulsion containing 5-70% by weight of acetochlor, 5-40% by weight of organic solvent, 5-30% by weight of emulsifier, 1-8% by weight of antifreeze agent, 0.5-5% by weight of thickener and the balance of water; the organic solvent is selected from methanol, ethanol, toluene, xylene, acetone and cyclohexanone; the emulsifier is fatty alcohol polyoxyethylene ether, castor oil polyoxyethylene ether, fatty acid polyoxyethylene ester, calcium dodecyl benzene sulfonate and the like; the antifreeze is one of glycol, polyethylene glycol, glycerol and urea; the thickening agent in the aqueous emulsion is one of hydroxypropyl cellulose, hydroxyethyl cellulose, xanthan gum, polyethylene glycol, polyvinyl alcohol, propyl cellulose and ethyl cellulose; the preparation process of the water emulsion includes dissolving acetochlor in organic solvent, adding emulsifier, mixing, adding water slowly while stirring, adding antifreezing agent, shearing in shearing machine and adding thickener.
The invention is different from the CN101530079A patent in that polyvinyl alcohol is used as an emulsifier, not used as a thickener, the key is that the polyvinyl alcohol is put into a water phase in advance, and is cooperated with calcium dodecyl benzene sulfonate and castor oil polyoxyethylene ether to play a good emulsification effect, the polyvinyl alcohol can be automatically emulsified into 0.7 micron emulsion by simple stirring without shearing, and the CN101530079A patent polyvinyl alcohol is added as the thickener after being prepared, and needs high shearing, and has large energy consumption and low efficiency.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a self-emulsifying aqueous emulsion containing acetochlor.
The invention aims to develop a method which can automatically emulsify to form a homogeneous stable emulsion without shearing and adding a thickening agent, and the technology can effectively reduce the equipment investment cost, improve the production efficiency and improve the product stability.
The technical scheme of the invention is as follows:
an aqueous emulsion containing acetochlor, which has an average particle size of 0.4-0.7 mu m.
According to the invention, the preferable aqueous emulsion containing acetochlor comprises the following components in percentage by mass: 20-60% of acetochlor technical product, 3-6% of emulsifier, 2-8% of antifreezing agent and the balance of water;
the emulsifier comprises the following components in parts by weight: 0.5-2 parts of polyvinyl alcohol, 1-3 parts of castor oil polyoxyethylene ether and 2-4 parts of calcium dodecyl benzene sulfonate.
According to the invention, in the preferable aqueous emulsion, the antifreezing agent is one or more of ethylene glycol, polyethylene glycol, glycerol and urea.
According to the invention, the preferable aqueous emulsion containing acetochlor comprises the following components in percentage by mass: 30% of acetochlor technical product, 4.5% of emulsifier, 4% of antifreezing agent and the balance of water;
the emulsifier comprises the following components in parts by weight: 0.5 part of polyvinyl alcohol, 2 parts of castor oil polyoxyethylene ether and 2 parts of calcium dodecyl benzene sulfonate;
the antifreezing agent is glycerol.
According to the invention, the water in the aqueous emulsion is preferably deionized water and/or distilled water.
The preparation method of the aqueous emulsion comprises the following steps:
(1) according to the corresponding weight parts, acetochlor, castor oil polyoxyethylene ether and calcium dodecyl benzene sulfonate are uniformly mixed to prepare an oil phase;
(2) uniformly mixing polyvinyl alcohol in corresponding weight parts, an antifreezing agent in corresponding amount and water to prepare a water phase;
(3) and (3) adding the oil phase prepared in the step (1) into the water phase prepared in the step (2), and stirring to prepare the acetochlor aqueous emulsion.
According to the invention, the stirring condition in the step (3) is preferably 30-80r/min and the stirring time is preferably 10-40 min.
The aqueous emulsion containing acetochlor is used as herbicide.
The application method of the acetochlor-containing aqueous emulsion comprises the following steps:
diluting with water by 800 times and 1500 times, spraying before weed germination, and spraying the diluted pesticide liquid 45-60kg per mu.
The technical scheme of the invention has the beneficial effects
1. The acetochlor emulsion in water has the average grain size of 0.4-0.7 micron, smaller grain size, raised product stability and no delamination.
2. Compared with the existing preparation process of the aqueous emulsion, the preparation process of the aqueous emulsion of acetochlor can be automatically emulsified to form a homogeneous stable emulsion without high-speed shearing, and the technology can effectively reduce the equipment investment cost, improve the production efficiency and improve the product stability.
3. The acetochlor aqueous emulsion has no unpleasant toxic odor, has small irritation to eyes, reduces the pollution to the environment, and greatly improves the safety of production, storage, transportation and users.
Detailed Description
The technical solution of the present invention is further described with reference to the following examples, but the scope of the present invention is not limited thereto. Reagents and medicines involved in the examples are all common commercial products unless otherwise specified; the experimental procedures referred to in the examples are those conventional in the art unless otherwise specified.
Sources of materials
Acetochlor, available from Shandong Shengbang Green-field chemical Co., Ltd;
phenethylphenol polyoxyethylene ether: purchased from south kyo taihua chemical ltd;
fatty alcohol polyoxyethylene ether: purchased from south kyo taihua chemical ltd;
polyvinyl alcohol: purchased from shanxi three-dimensional chemical limited;
castor oil polyoxyethylene ether: purchased from south kyo taihua chemical ltd;
calcium dodecylbenzenesulfonate: purchased from south kyo taihua chemical ltd;
the glycerol, the glycol and the polyethylene glycol are all common commercial products.
Example 1
An aqueous emulsion containing acetochlor comprises the following components in percentage by mass:
the preparation method of the self-emulsifying aqueous emulsion of the acetochlor is used for preparing 1000 g of 30 percent aqueous emulsion of the acetochlor in percentage by mass, and comprises the following steps:
(1) in a 1000ml beaker, 333.3 g of acetochlor original drug (with the content of 90 percent) is firstly added, and then 20 g of castor oil polyoxyethylene ether and 20 g of calcium dodecyl benzene sulfonate are added, and an oil phase is obtained after uniform stirring;
(2) in another 2000ml beaker, 5 g of polyvinyl alcohol, 40 g of glycerol and 581.7 g of distilled water were stirred uniformly to obtain an aqueous phase;
(3) and (3) adding the oil phase obtained in the step (1) into the water phase obtained in the step (2), and stirring at the speed of 60r/min for 12min to form the stable 30% acetochlor aqueous emulsion by automatic emulsification.
Example 2
An aqueous emulsion containing acetochlor comprises the following components in percentage by mass:
the preparation method of the self-emulsifying aqueous emulsion of the acetochlor is used for preparing 1000 g of 40 percent aqueous emulsion of the acetochlor by mass percent, and comprises the following steps:
(1) in a 1000ml beaker, firstly adding 444.5 g of acetochlor original drug (with the content of 90 percent), then adding 25 g of castor oil polyoxyethylene ether and 25 g of calcium dodecyl benzene sulfonate, and uniformly mixing to obtain an oil phase;
(2) in another 2000ml beaker, 8 grams of polyvinyl alcohol, 50 grams of ethylene glycol and 447.5 grams of distilled water solvent were mixed well to obtain an aqueous phase;
(3) and (3) adding the oil phase obtained in the step (1) into the water phase obtained in the step (2), and stirring at the speed of 50r/min for 20min to form the stable 40% acetochlor aqueous emulsion by automatic emulsification.
Example 3
An aqueous emulsion containing acetochlor comprises the following components in percentage by mass:
the preparation method of the self-emulsifying aqueous emulsion of the acetochlor is used for preparing 1000 g of 50 percent aqueous emulsion of the acetochlor in percentage by mass, and comprises the following steps:
(1) in a 1000ml beaker, firstly adding 555.6 g of acetochlor original drug (with the content of 90 percent), then adding 30 g of castor oil polyoxyethylene ether and 20 g of calcium dodecyl benzene sulfonate, and uniformly mixing to obtain an oil phase;
(2) in another 2000ml beaker, 15 g polyvinyl alcohol, 40 g polyethylene glycol and 339.4 g deionized water solvent were mixed uniformly to obtain a water phase;
(3) and (3) adding the oil phase obtained in the step (1) into the water phase obtained in the step (2), and stirring at the speed of 70r/min for 15min to automatically emulsify to form the stable 50% acetochlor aqueous emulsion.
Comparative example 1
The other points are the same as those of the embodiment 1,
an aqueous emulsion containing acetochlor comprises the following components in percentage by mass:
comparative example 2
The other points are the same as those of the embodiment 1,
comparative example 3
The other points are the same as those of the embodiment 1,
comparative example 4
The other points are the same as those of the embodiment 1,
the distilled water is complemented to 100 percent.
Examples of effects
The main reference indexes for preparing the aqueous emulsion prepared in the above examples 1 to 3 and comparative examples 1 to 4 are shown in Table 1; the results of the measured index data are shown in Table 2.
The particle size is measured by a laser particle size distribution instrument, the content of effective components is detected by a liquid chromatograph, and the emulsion stability is GB/T1603-2001; the thermal storage stability was carried out in accordance with GB/T19136-2003 and the cold storage stability was carried out in accordance with GB/T19137-2003.
TABLE 1
| Detecting items | Reference index |
| Effective component content% | Theoretical content. + -. 2.5 |
| Average particle diameter, μm | ≤10 |
| Emulsion stability | Qualified |
| Stability in Heat storage | Qualified |
| Stability in Cold storage | Qualified |
| Centrifugal test (4000 rotating for 2 hours) | The layering rate is less than 5 percent |
| Cold and hot alternation test (first 7 days at-18 ℃ C. and then 7 days at 54 ℃ C.) | Homogeneous emulsions |
TABLE 2
As can be seen from the experimental data in Table 2, the acetochlor aqueous emulsion of the invention has the average particle size of 0.4-0.7 μm compared with the comparative example; the components of the acetochlor aqueous emulsion provided by the invention generate a certain synergistic effect, high-speed shearing is not required, namely the acetochlor aqueous emulsion prepared by automatic emulsification has smaller particle size, the product stability is improved, no layering is generated, no oil drop is separated out, and the stability of a centrifugal test and a cold-hot alternation test is particularly superior.
Application example
The acetochlor aqueous emulsion prepared in the examples 1-2 and the comparative examples 1-4 is used for controlling weeds in soybean fields: spraying in soybean field one day before sowing, wherein 13.5 g of acetochlor active ingredient is used per mu, and the treatment concentration is 1000-fold 1333 times; the acetochlor aqueous emulsion prepared in the examples and the comparative examples 1-4 is adopted to carry out the drug effect experiment on weeds in soybean fields, water is used as a blank control, and the fresh weight control effect is investigated 30 days after the application.
The fresh weight control effect calculation method comprises the following steps: fresh weight control effect (fresh weight of weeds in blank control zone-fresh weight of weeds in treated zone)/fresh weight of weeds in blank control zone 100%
TABLE 3 table of the results of the field efficacy test
The data in Table 3 show that the acetochlor aqueous emulsion has smaller particle size, can be better dispersed and spread, is more favorable for absorbing weeds, has obvious herbicidal effect compared with the acetochlor aqueous emulsion prepared in a comparative ratio, and particularly has better herbicidal effect on large crabgrass and eleusine indica.
In conclusion, the components of the acetochlor aqueous emulsion provided by the invention generate a certain synergistic effect, high-speed shearing is not needed, namely the acetochlor aqueous emulsion prepared by automatic emulsification has smaller particle size, the product stability is improved, no layering is generated, no oil drop is separated out, and particularly the stability of a centrifugal test and a cold-hot alternation test is more advantageous; the acetochlor aqueous emulsion has more obvious effect of preventing and controlling weeds; and the preparation method is more convenient, has low energy consumption and small equipment investment, and is beneficial to market popularization and application.
Claims (9)
1. An aqueous emulsion containing acetochlor is characterized in that the average particle size of the aqueous emulsion is 0.4-0.7 mu m.
2. The aqueous emulsion of claim 1, characterized in that the aqueous emulsion comprises the following components in percentage by mass: 20-60% of acetochlor technical product, 3-6% of emulsifier, 2-8% of antifreezing agent and the balance of water;
the emulsifier comprises the following components in parts by weight: 0.5-2 parts of polyvinyl alcohol, 1-3 parts of castor oil polyoxyethylene ether and 2-4 parts of calcium dodecyl benzene sulfonate.
3. The aqueous emulsion of claim 2, wherein the anti-freezing agent is one or more of ethylene glycol, polyethylene glycol, glycerol, and urea.
4. The aqueous emulsion of claim 3, characterized in that the aqueous emulsion comprises the following components in percentage by mass: 30% of acetochlor technical product, 4.5% of emulsifier, 4% of antifreezing agent and the balance of water;
the emulsifier comprises the following components in parts by weight: 0.5 part of polyvinyl alcohol, 2 parts of castor oil polyoxyethylene ether and 2 parts of calcium dodecyl benzene sulfonate;
the antifreezing agent is glycerol.
5. The aqueous emulsion of any one of claims 1 to 4, wherein the water in the aqueous emulsion is deionized and/or distilled water.
6. The process for preparing the aqueous emulsion of any one of claims 1 to 4, comprising the steps of:
(1) according to the corresponding weight parts, acetochlor, castor oil polyoxyethylene ether and calcium dodecyl benzene sulfonate are uniformly mixed to prepare an oil phase;
(2) uniformly mixing polyvinyl alcohol in corresponding weight parts, an antifreezing agent in corresponding amount and water to prepare a water phase;
(3) and (3) adding the oil phase prepared in the step (1) into the water phase prepared in the step (2), and stirring to prepare the acetochlor aqueous emulsion.
7. The method according to claim 6, wherein the stirring in the step (3) is carried out at 30 to 80r/min for 10 to 40 min.
8. Use of the aqueous emulsions of any of claims 1 to 4 as herbicides.
9. The use of the aqueous emulsion of any one of claims 1 to 4, characterized in that it comprises the following steps:
diluting with water by 800 times and 1500 times, spraying before weed germination, and spraying the diluted pesticide liquid 45-60kg per mu.
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| CN202110086796.7A CN112889824B (en) | 2021-01-22 | 2021-01-22 | Self-emulsifying aqueous emulsion containing acetochlor |
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| CN202110086796.7A CN112889824B (en) | 2021-01-22 | 2021-01-22 | Self-emulsifying aqueous emulsion containing acetochlor |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1395831A (en) * | 2002-08-14 | 2003-02-12 | 江苏省农药研究所 | Amide-type herbiciding aqueous emulsion and its preparing process |
| CN101530079A (en) * | 2008-03-14 | 2009-09-16 | 北京绿色农华植保科技有限责任公司 | Aqueous emulsion containing acetochlor |
| CN107136079A (en) * | 2017-05-12 | 2017-09-08 | 扬州大学 | A kind of aqueous cyhalofop-butyl emulsion and preparation method thereof |
| CN111165477A (en) * | 2020-01-23 | 2020-05-19 | 中化化工科学技术研究总院有限公司 | Acetochlor emulsion in water and preparation method thereof |
-
2021
- 2021-01-22 CN CN202110086796.7A patent/CN112889824B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1395831A (en) * | 2002-08-14 | 2003-02-12 | 江苏省农药研究所 | Amide-type herbiciding aqueous emulsion and its preparing process |
| CN101530079A (en) * | 2008-03-14 | 2009-09-16 | 北京绿色农华植保科技有限责任公司 | Aqueous emulsion containing acetochlor |
| CN107136079A (en) * | 2017-05-12 | 2017-09-08 | 扬州大学 | A kind of aqueous cyhalofop-butyl emulsion and preparation method thereof |
| CN111165477A (en) * | 2020-01-23 | 2020-05-19 | 中化化工科学技术研究总院有限公司 | Acetochlor emulsion in water and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 刘步林等: "《农药剂型加工技术》", 31 October 1998 * |
| 裘炳毅等: "《现代化妆品科学与技术 上》", 30 March 2016 * |
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Denomination of invention: A self-emulsifying water emulsion containing acetochlor Effective date of registration: 20230914 Granted publication date: 20220524 Pledgee: Bank of Beijing Co.,Ltd. Jinan Branch Pledgor: JINAN TIANBANG CHEMICAL Co.,Ltd. Registration number: Y2023980056643 |
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