CN111165477A - Acetochlor emulsion in water and preparation method thereof - Google Patents

Acetochlor emulsion in water and preparation method thereof Download PDF

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Publication number
CN111165477A
CN111165477A CN202010076445.3A CN202010076445A CN111165477A CN 111165477 A CN111165477 A CN 111165477A CN 202010076445 A CN202010076445 A CN 202010076445A CN 111165477 A CN111165477 A CN 111165477A
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CN
China
Prior art keywords
acetochlor
aqueous emulsion
parts
water
emulsifier
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Pending
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CN202010076445.3A
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Chinese (zh)
Inventor
朱建秀
卢忠利
张宗俭
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BEIJING GRAND AGROCHEM Ltd
Central Research Institute Of China Chemical Science And Technology Co ltd
Original Assignee
BEIJING GRAND AGROCHEM Ltd
Central Research Institute Of China Chemical Science And Technology Co ltd
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Priority to CN202010076445.3A priority Critical patent/CN111165477A/en
Publication of CN111165477A publication Critical patent/CN111165477A/en
Pending legal-status Critical Current

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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, 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
    • A01N25/02Biocides, 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
    • A01N25/04Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N37/00Biocides, 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
    • A01N37/18Biocides, 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
    • A01N37/26Biocides, 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

Abstract

The invention relates to an acetochlor aqueous emulsion and a preparation method thereof, belonging to the technical field of pesticide application. The acetochlor aqueous emulsion comprises the following components in percentage by mass: 5-25% of acetochlor original drug, 3-6% of polymer emulsifier, 1-5% of thickener, 2-8% of antifreeze, 2-10% of solvent and the balance of water; wherein the polymer emulsifier is formed by copolymerizing acrylic monomers and acrylate monomers; the weight ratio of the acrylic monomer to the acrylate monomer is 1-6:1-5, and the weight average relative molecular weight of the macromolecular emulsifier is 10000-50000. The acetochlor aqueous emulsion prepared by the invention has better low-temperature stability and heat storage stability, good preparation efficacy and stable system.

Description

Acetochlor emulsion in water and preparation method thereof
Technical Field
The invention relates to the technical field of pesticide application, and particularly provides an acetochlor aqueous emulsion and a preparation method thereof.
Background
Acetochlor is an excellent herbicide for dry land, has the characteristics of high activity, good pesticide effect and the like, and is widely applied in China. However, the traditional acetochlor emulsifiable concentrate needs a large amount of organic solvent, is easy to cause human body harm and environmental pollution during production and application, and is easy to cause phenomena of crop phytotoxicity and the like. The water emulsion is used to replace missible oil, and the defects are overcome to a certain extent.
The aqueous emulsion is a relatively stable suspension system formed by uniformly dispersing raw medicines which are not dissolved in water by adding a proper preparation, namely, the aqueous suspension agent with the oil phase as a dispersed phase and the water as a continuous phase. Compared with missible oil, the emulsion has more advantages in manufacturing, using safety, cost, transportation and packaging. Contains no or only a small amount of organic solvent, has high flash point and no risk of ignition and explosion. Cheap water is used as a matrix, the dosage of the emulsifier is equivalent to that of missible oil, and the cost is reduced in different ranges; the requirements for packaging containers are also far less demanding than emulsifiable concentrates, which already compete with emulsifiable concentrates in terms of price. When the pesticide is sprayed, the particle size of fog drops is larger than that of missible oil, so that the drifting of effective components and the pollution to the environment can be reduced. Although aqueous emulsions have many advantages, the difficulty of preparation is increased accordingly. Since the aqueous emulsion is in a thermodynamically unstable state, it must be formed into a uniform emulsion state by a specific external force and be stable. Therefore, the key point of preparing the acetochlor aqueous emulsion is to solve the problem of system instability.
Disclosure of Invention
In order to solve the problems of unstable system of the acetochlor aqueous emulsion in the prior art and the like, the invention provides the acetochlor aqueous emulsion and the preparation method thereof.
In order to solve the technical problems, the invention provides the following technical scheme:
on one hand, the invention provides an acetochlor aqueous emulsion which comprises the following components in percentage by mass: 5-25% of acetochlor original drug, 3-6% of polymer emulsifier, 1-5% of thickener, 2-8% of antifreeze, 2-10% of solvent and the balance of water;
wherein the polymer emulsifier is formed by copolymerizing acrylic monomers and acrylate monomers; the weight ratio of the acrylic monomer to the acrylate monomer is 1-6:1-5, and the weight average relative molecular weight of the macromolecular emulsifier is 10000-50000.
Further, the polymer emulsifier is prepared from the following components in parts by weight: 10-70 parts of acrylic monomer, 5-50 parts of acrylate monomer, 20-100 parts of alcohol, 10-40 parts of initiator, 1-40 parts of alkali and 50-200 parts of water.
Preferably, the acrylic monomer is acrylic acid and/or methacrylic acid; the acrylate monomer is one or two of acrylate with carbon number of 5-18 alcohol and methacrylate with carbon number of 5-18 alcohol.
Preferably, the alcohol is propanol and/or isopropanol; the alkali is one or more of sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate and ammonia water; the initiator is persulfate.
Further, the polymer emulsifier is prepared by the following steps:
step 1: adding deionized water and alcohols into a reaction kettle, uniformly stirring, and heating to 65-90 ℃;
step 2: simultaneously dripping acrylic monomers, acrylic ester monomers and an initiator solution into the solution, finishing dripping within 0.5-2.5 hours, and reacting for 1-6 hours under the condition of heat preservation;
and step 3: and (3) stirring the solution obtained in the step (2), cooling to room temperature, adjusting the pH to 6.0-8.0 by using alkali, and discharging to obtain the catalyst.
An emulsifier is a substance used to prepare an emulsion and impart it with a minimum degree of stability, and is an essential component. The polymer emulsifier generally refers to a polymer compound having a surface active function with a relative molecular mass of more than several thousands. They can be strongly adsorbed at the interface between the continuous and dispersed phases, they can either reduce the interfacial tension or they can form electrostatic or steric barriers between the droplets. In addition, their solvating properties may in turn increase the thickness of the effective adsorbent layer, increase interfacial viscosity, and create other factors contributing to good stability of the emulsion system.
Preferably, the thickener is magnesium aluminum silicate and/or xanthan gum.
Preferably, the antifreeze is one or more of ethylene glycol, urea and propylene glycol.
Preferably, the solvent is methyl oleate and/or fatty acid methyl esters.
On the other hand, the invention also provides a preparation method of the acetochlor aqueous emulsion, which comprises the following steps:
(1) uniformly mixing an acetochlor technical product, a high-molecular emulsifier and a solvent to obtain an oil phase;
(2) uniformly mixing a thickening agent, an antifreezing agent and water to obtain a water phase;
(3) dropwise adding the oil phase in the step (1) into the water phase in the step (2), and uniformly mixing by using a high-speed shearing machine;
(4) the mixed liquid is placed on a rotary stirrer to be stirred for 15min, and the grain diameter D50 is detected to be less than 5 micrometers, then the material can be discharged.
Compared with the prior art, the invention has the following beneficial effects:
the high molecular emulsifier has a large molecular weight and a long oleophylic chain, and can well wrap an oil phase, so that the stability of the prepared emulsion in water is greatly improved. The acetochlor aqueous emulsion prepared by the invention has the advantages of good appearance fluidity, low-temperature stability, heat storage stability and the like which meet the standards of the aqueous emulsion, good preparation effect and stable system.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved by the present invention clearer, the following detailed description is given with reference to specific embodiments.
The reagents and the like used in the present invention are all commercially available products, as specifically described.
The invention provides an acetochlor aqueous emulsion and a preparation method thereof, and the specific embodiment is as follows.
Example 1
An acetochlor aqueous emulsion comprises the following components in percentage by mass: 17.65% of acetochlor with the content of 93.5%, 5.5% of high-molecular emulsifier, 1% of xanthan gum, 7% of glycol, 9% of methyl oleate and the balance of water.
The preparation process of the polymer emulsifier is as follows: adding 100 parts of water and 50 parts of propanol into a reaction kettle, and heating while stirring; when the temperature of the solution in the reaction kettle is raised to 85 ℃, 15 parts of acrylic acid, 20 parts of isooctyl acrylate and 30 parts of initiator ammonium persulfate solution are dripped, the dripping is finished within 1.5 hours, and then the reaction is carried out for 2 hours under heat preservation; after the reaction is finished, the temperature is reduced to room temperature while stirring, and the pH is adjusted to 7.2 by using a sodium hydroxide solution.
The preparation method of the acetochlor aqueous emulsion comprises the following steps:
(1) uniformly mixing an acetochlor technical product, a high-molecular emulsifier and a solvent to obtain an oil phase;
(2) uniformly mixing a thickening agent, an antifreezing agent and water to obtain a water phase;
(3) dropwise adding the oil phase in the step (1) into the water phase in the step (2), and uniformly mixing by using a high-speed shearing machine;
(4) the mixed liquid is placed on a rotary stirrer to be stirred for 15min, and the grain diameter D50 is detected to be less than 5 micrometers, then the material can be discharged.
Example 2
An acetochlor aqueous emulsion comprises the following components in percentage by mass: 5.5% of acetochlor with the content of 93.5%, 3% of high molecular emulsifier, 5% of magnesium aluminum silicate, 1% of glycol, 1% of propylene glycol, 2% of fatty acid methyl ester and the balance of water, and the rest is the same as the step of example 1.
Example 3
An acetochlor aqueous emulsion comprises the following components in percentage by mass: 26.5% of acetochlor with the content of 93.5%, 6% of high molecular emulsifier, 2% of magnesium aluminum silicate, 1% of xanthan gum, 4% of ethylene glycol, 4% of propylene glycol, 5% of fatty acid methyl ester, 5% of methyl oleate and the balance of water, and the rest is the same as example 1.
Example 4
An acetochlor aqueous emulsion comprises the following components in percentage by mass: 93.5% of acetochlor 17.65%, 5.5% of high-molecular emulsifier, 1% of xanthan gum, 3% of glycol and the balance of water. The rest is the same as in example 1.
Example 5
The preparation process of the polymer emulsifier is as follows: adding 100 parts of water and 50 parts of isopropanol into a reaction kettle, and heating while stirring; when the temperature of the solution in the reaction kettle is raised to 80 ℃, 20 parts of acrylic acid, 15 parts of isooctyl acrylate and 30 parts of initiator ammonium persulfate solution are dripped, the dripping is finished within 0.5 hour, and then the reaction is carried out for 2 hours under heat preservation; and (3) after the heat preservation reaction is finished, stirring and cooling to room temperature, and adjusting the pH to 7.2 by using a sodium hydroxide solution to obtain the polymer emulsifier.
The remaining conditions were the same as in example 1.
Example 6
The preparation process of the polymer emulsifier is as follows: adding 100 parts of water and 50 parts of alcohols into a reaction kettle, and heating while stirring; when the temperature of the solution in the reaction kettle is raised to 70 ℃, 10 parts of acrylic acid, 20 parts of isooctyl acrylate and 30 parts of initiator ammonium persulfate solution are dripped, the dripping is finished within 1.5 hours, and then the reaction is carried out for 2 hours under heat preservation; and (3) after the heat preservation reaction is finished, stirring and cooling to room temperature, and adjusting the pH to 7.2 by using a sodium hydroxide solution to obtain the polymer emulsifier.
The remaining conditions were the same as in example 1.
Example 7
The preparation process of the polymer emulsifier is as follows: adding 200 parts of water and 20 parts of alcohols into a reaction kettle, and heating while stirring; when the temperature of the solution in the reaction kettle is raised to 90 ℃, dropwise adding 30 parts of methacrylic acid, 5 parts of isooctyl methacrylate and 30 parts of initiator ammonium persulfate solution, finishing dropwise adding within 0.5 hour, and then carrying out heat preservation reaction for 6 hours; and (3) after the heat preservation reaction is finished, stirring and cooling to room temperature, and adjusting the pH to 8 by using a sodium hydroxide solution to obtain the polymer emulsifier.
The remaining conditions were the same as in example 1.
Example 8
The preparation process of the polymer emulsifier is as follows: adding 50 parts of water and 100 parts of alcohols into a reaction kettle, and heating while stirring; when the temperature of the solution in the reaction kettle is increased to 65 ℃, 70 parts of acrylic acid, 50 parts of isooctyl acrylate and 30 parts of initiator ammonium persulfate solution are dripped, the dripping is finished within 2.5 hours, and then the reaction is carried out for 4 hours under heat preservation; and (3) after the heat preservation reaction is finished, stirring and cooling to room temperature, and adjusting the pH to 6 by using a sodium hydroxide solution to obtain the polymer emulsifier.
The remaining conditions were the same as in example 1.
To further illustrate the beneficial effects of the aqueous acetochlor emulsion of the present invention, the following comparative examples were constructed only in example 5 for reasons of space.
Comparative example 1
The polymer emulsifier was replaced with the same amount of fatty alcohol-polyoxyethylene ether, and the rest of the conditions were the same as in example 5.
Comparative example 2
The remaining conditions were the same as in example 5 except that 5.5% of the polymeric emulsifier was replaced with 2% of castor oil polyoxyethylene ether and 3.5% of fatty acid polyoxyethylene ester.
Comparative example 3
The same conditions as in example 5 were used except that the 5.5% polymer emulsifier was prepared by replacing the alcohol with an equivalent amount of ammonium allyloxy nonylphenoxypropanol polyoxyethylene ether sulfate.
Comparative example 4
The same procedure as in example 5 was repeated except that isooctyl acrylate was replaced with methyl acrylate in the preparation of 5.5% polymer emulsifier.
Comparative example 5
The same procedure as in example 5 was repeated except that isooctyl acrylate was replaced with behenyl acrylate in the preparation of 5.5% polymer emulsifier.
Comparative example 6
The methyl oleate was replaced with an equal amount of methanol and the other conditions were the same as in example 5.
Comparative example 7
The amount of methyl oleate was changed to 15% and the amount of water was reduced accordingly, and the other conditions were the same as in example 5.
The acetochlor aqueous emulsions prepared in the above examples 1 to 8 and comparative examples 1 to 7 were tested for their properties, as follows, and the results are shown in Table 1.
TABLE 1
As can be seen from the table above, the application enables the prepared acetochlor aqueous emulsion to have excellent heat storage stability and low temperature stability by adding the polymer emulsifier and the specific solvent for matching use and specifically limiting the dosage of each substance.
The herbicidal properties of the acetochlor aqueous emulsions prepared in the above examples 1 to 8 and comparative examples 1 to 7 were tested, and the specific tests are as follows.
The acetochlor aqueous emulsion is used for preventing and killing weeds in soybean fields: spraying the pesticide in soybean field one day before sowing, and mixing the pesticide above the soil (1-4 cm soil layer). The aqueous emulsions of examples 1 to 8 and comparative examples 1 to 7 and the commercial aqueous emulsion of acetochlor are used for carrying out pesticide effect experiments on weeds in soybean fields. The fresh weight control effect of the test 30 days after the administration is shown in Table 2.
TABLE 2 results of field experiments for controlling weeds in soybean fields
As shown in the table, the acetochlor aqueous emulsion prepared by the invention has better control effect on weeds in soybean fields, especially large crabgrass, black nightshade and goosegrass. Compared with the commercial acetochlor aqueous emulsion, the fresh weight control effect of the large crabgrass is improved by 11.2 percent, the fresh weight control effect of the black nightshade is improved by 6.8 percent, and the fresh weight control effect of the eleusine indica is improved by 10.3 percent; compared with comparative examples 1-7, the acetochlor aqueous emulsion prepared by the method has greatly improved control effect on weeds in soybean fields.
In conclusion, the acetochlor aqueous emulsion with better heat storage and low-temperature stability is obtained by selecting the macromolecular emulsifier with larger molecular weight and matching with the substances such as solvent and the like, and has better control effect on weeds in soybean fields.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (9)

1. The acetochlor aqueous emulsion is characterized by comprising the following components in percentage by mass: 5-25% of acetochlor original drug, 3-6% of polymer emulsifier, 1-5% of thickener, 2-8% of antifreeze, 2-10% of solvent and the balance of water;
wherein the polymer emulsifier is formed by copolymerizing acrylic monomers and acrylate monomers; the weight ratio of the acrylic monomer to the acrylate monomer is 1-6:1-5, and the weight average relative molecular weight of the macromolecular emulsifier is 10000-50000.
2. The acetochlor aqueous emulsion of claim 1, wherein the polymeric emulsifier is prepared from the following components in parts by weight: 10-70 parts of acrylic monomer, 5-50 parts of acrylate monomer, 20-100 parts of alcohol, 10-40 parts of initiator, 1-40 parts of alkali and 50-200 parts of water.
3. The acetochlor aqueous emulsion of claim 2, wherein the acrylic monomer is acrylic acid and/or methacrylic acid; the acrylate monomer is one or two of acrylate with carbon number of 5-18 alcohol and methacrylate with carbon number of 5-18 alcohol.
4. The acetochlor aqueous emulsion of claim 3, wherein the alcohols are propanol and/or isopropanol; the alkali is one or more of sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate and ammonia water; the initiator is persulfate.
5. The acetochlor aqueous emulsion of claim 4, wherein the polymeric emulsifier is prepared by the following steps:
step 1: adding deionized water and alcohols into a reaction kettle, uniformly stirring, and heating to 65-90 ℃;
step 2: simultaneously dripping acrylic monomers, acrylic ester monomers and an initiator solution into the solution, finishing dripping within 0.5-2.5 hours, and reacting for 1-6 hours under the condition of heat preservation;
and step 3: and (3) stirring the solution obtained in the step (2), cooling to room temperature, adjusting the pH to 6.0-8.0 by using alkali, and discharging to obtain the catalyst.
6. The acetochlor aqueous emulsion of claim 1, wherein the thickener is magnesium aluminum silicate and/or xanthan gum.
7. The acetochlor aqueous emulsion of claim 1, wherein the antifreezing agent is one or more of ethylene glycol, urea and propylene glycol.
8. The acetochlor aqueous emulsion of claim 1, characterized in that the solvent is methyl oleate and/or fatty acid methyl esters.
9. The process for preparing an acetochlor aqueous emulsion as claimed in any one of claims 1 to 8, which comprises the following steps:
(1) uniformly mixing an acetochlor technical product, a high-molecular emulsifier and a solvent to obtain an oil phase;
(2) uniformly mixing a thickening agent, an antifreezing agent and water to obtain a water phase;
(3) dropwise adding the oil phase in the step (1) into the water phase in the step (2), and uniformly mixing by using a high-speed shearing machine;
(4) the mixed liquid is placed on a rotary stirrer to be stirred for 15min, and the grain diameter D50 is detected to be less than 5 micrometers, then the material can be discharged.
CN202010076445.3A 2020-01-23 2020-01-23 Acetochlor emulsion in water and preparation method thereof Pending CN111165477A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112889824A (en) * 2021-01-22 2021-06-04 济南天邦化工有限公司 Self-emulsifying aqueous emulsion containing acetochlor

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Publication number Priority date Publication date Assignee Title
CN112889824A (en) * 2021-01-22 2021-06-04 济南天邦化工有限公司 Self-emulsifying aqueous emulsion containing acetochlor

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