CN111171215B - Environment-friendly agricultural dispersant and preparation method thereof - Google Patents
Environment-friendly agricultural dispersant and preparation method thereof Download PDFInfo
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- CN111171215B CN111171215B CN202010115528.9A CN202010115528A CN111171215B CN 111171215 B CN111171215 B CN 111171215B CN 202010115528 A CN202010115528 A CN 202010115528A CN 111171215 B CN111171215 B CN 111171215B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/30—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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F222/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
- C08F222/04—Anhydrides, e.g. cyclic anhydrides
- C08F222/06—Maleic anhydride
- C08F222/08—Maleic anhydride with vinyl aromatic monomers
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Agronomy & Crop Science (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Toxicology (AREA)
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- Wood Science & Technology (AREA)
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Abstract
The invention discloses an environment-friendly agricultural dispersant and a preparation method thereof, belonging to the technical field of agricultural additives. The invention discloses an environment-friendly agricultural dispersant which comprises the following components in parts by weight: 25-70 parts of acrylic monomers, 15-35 parts of styrene, 15-35 parts of allyloxy hydroxypropyl sodium sulfonate, 5-15 parts of an initiator, 15-35 parts of alkali and 100-300 parts of water. The environment-friendly agricultural dispersant disclosed by the invention is simple in synthesis process, environment-friendly and good in dispersing performance.
Description
Technical Field
The invention relates to the technical field of agricultural additives, in particular to an environment-friendly agricultural dispersant and a preparation method thereof.
Background
Currently, pesticide preparations are preparations using water as a carrier, such as aqueous suspension concentrates, water dispersible granules and the like. These pesticide formulations do not leave a dispersant. The polyacrylic acid dispersant has the characteristics of adjustable monomers and molecular weight, and is the most extensive dispersant with the best performance.
However, since water-insoluble monomers such as styrene exist in the polymerization process, the synthesis is generally carried out at home and abroad by using solvents, such as 2700 of Hensmei, T36 of Solvay, and the like, and the process is not environment-friendly.
Therefore, providing an agricultural dispersant for an environmental protection process and a preparation method thereof are problems that need to be solved by those skilled in the art.
Disclosure of Invention
In view of the above, the invention provides an environment-friendly agricultural dispersant and a preparation method thereof, and the agricultural dispersant with environment-friendly process and better dispersibility is obtained.
In order to achieve the purpose, the invention adopts the following technical scheme:
an environment-friendly agricultural dispersant comprises the following components in parts by weight: 25-70 parts of acrylic monomers, 15-35 parts of styrene, 15-35 parts of allyloxy hydroxypropyl sodium sulfonate, 5-15 parts of an initiator, 15-35 parts of alkali and 100-300 parts of water.
Further, the environment-friendly agricultural dispersant comprises the following components in parts by weight: 45-60 parts of acrylic monomers, 18-27 parts of styrene, 18-27 parts of allyloxy hydroxypropyl sodium sulfonate, 10-15 parts of an initiator, 15-35 parts of alkali and 100-300 parts of water.
Further, the weight average relative molecular weight of the agricultural dispersant is 5000-35000.
Further, the acrylic monomer is at least one of acrylic acid, methacrylic acid, maleic anhydride and fumaric acid.
Further, the initiator is at least one of persulfate and hydrogen peroxide water-soluble initiator. When the number of the initiators is more than two, the proportion of the specific substances is not particularly limited, and the specific substances can be mixed according to any proportion.
Further, the alkali is at least one of sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, ammonia water, ethanolamine, diethanolamine and triethanolamine. When the number of the alkali is two or more, the specific ratio of the specific substances is not particularly limited, and the specific substances can be mixed at any ratio.
Further, a preparation method of the environment-friendly agricultural dispersant comprises the following specific steps:
(1) pouring an initiator into a certain amount of water to prepare an initiator solution with the concentration of 30-40 percent;
(2) adding the residual amount of water into the reaction kettle, sequentially adding allyloxy hydroxypropyl sodium sulfonate, acrylic monomers and styrene according to weight, and starting stirring at the stirring speed of 500-;
(3) sealing, and heating to 85-100 deg.C;
(4) dripping initiator solution for 0.5-3 h;
(5) after the dropwise addition is finished, continuously keeping the temperature and stirring for 1-4 h;
(6) cooling, adding alkali for neutralization, and keeping the temperature at 50-70 ℃;
(7) cooling to room temperature, and discharging;
(8) spray drying, and packaging.
According to the technical scheme, compared with the prior art, the invention discloses and provides the environment-friendly agricultural dispersant and the preparation method thereof, the solvent is not used in the preparation process of the agricultural dispersant, the reaction is carried out in water, the process synthesis is simple, and the environment is protected; the invention enables the reaction to be smoothly carried out by controlling reaction conditions such as stirring speed, temperature and the like; the obtained agricultural dispersant has better dispersing performance.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the present invention, the materials and reagents used are not specifically described, and are commercially available.
Example 1
An environment-friendly agricultural dispersant comprises the following components in parts by weight: 66 parts of methacrylic acid, 16 parts of styrene, 17 parts of allyloxy hydroxypropyl sodium sulfonate, 5 parts of ammonium persulfate, 31 parts of sodium hydroxide and 300 parts of water.
The preparation method of the environment-friendly agricultural dispersant comprises the following specific steps:
(1) pouring 5g of ammonium persulfate into 7.5g of water to prepare a 40% initiator solution;
(2) 292.5g of water is added into a reaction kettle, 17g of allyloxy hydroxypropyl sodium sulfonate, 66g of methacrylic acid and 16g of styrene are sequentially added, stirring is started, and the stirring speed is 800 revolutions per minute;
(3) sealing, and heating to 85 ℃;
(4) dripping an initiator solution for 0.5 h;
(5) after the dropwise addition, continuously keeping the temperature and stirring for 1 h;
(6) cooling, adding sodium hydroxide for neutralization, and keeping the temperature at 50 ℃;
(7) cooling to room temperature, and discharging;
(8) spray drying, and packaging.
Example 2
An environment-friendly agricultural dispersant comprises the following components in parts by weight: 61 parts of maleic anhydride, 19 parts of styrene, 19.5 parts of allyloxy hydroxypropyl sodium sulfonate, 15 parts of ammonium persulfate, 29 parts of ammonia water and 250 parts of water.
The preparation method of the environment-friendly agricultural dispersant comprises the following specific steps:
(1) pouring 15g of ammonium persulfate into 29g of water to prepare 34% of initiator solution;
(2) adding 221g of water into a reaction kettle, sequentially adding 19.5g of allyloxy hydroxypropyl sodium sulfonate, 61g of maleic anhydride and 19g of styrene according to weight, and starting stirring at the stirring speed of 500 revolutions per minute;
(3) sealing, and heating to 95 ℃;
(4) dropping an initiator solution for 3 hours;
(5) after the dropwise addition, continuously keeping the temperature and stirring for 1 h;
(6) cooling, adding ammonia water for neutralization, and keeping the temperature at 70 ℃;
(7) cooling to room temperature, and discharging;
(8) spray drying, and packaging.
Example 3
An environment-friendly agricultural dispersant comprises the following components in parts by weight: 44 parts of acrylic acid, 27 parts of styrene, 28 parts of allyloxy hydroxypropyl sodium sulfonate, 10 parts of sodium persulfate, 21 parts of sodium carbonate and 200 parts of water.
The preparation method of the environment-friendly agricultural dispersant comprises the following specific steps:
(1) pouring 10g of sodium persulfate into 23g of water to prepare 30% of initiator solution;
(2) 177g of water is added into a reaction kettle, then 28g of allyloxy hydroxypropyl sodium sulfonate, 44g of acrylic acid and 27g of styrene are sequentially added according to the weight, and stirring is started, wherein the stirring speed is 1000 r/min;
(3) sealing, and heating to 100 ℃;
(4) dropping an initiator solution for 2 hours;
(5) after the dropwise addition, continuously keeping the temperature and stirring for 2 hours;
(6) cooling, adding sodium carbonate for neutralization, and keeping the temperature at 60 ℃;
(7) cooling to room temperature, and discharging;
(8) spray drying, and packaging.
Example 4
An environment-friendly agricultural dispersant comprises the following components in parts by weight: 28 parts of acrylic acid, 34 parts of styrene, 35 parts of allyloxy hydroxypropyl sodium sulfonate, 15 parts of potassium persulfate, 15 parts of sodium hydroxide and 200 parts of water.
The preparation method of the environment-friendly agricultural dispersant comprises the following specific steps:
(1) pouring 15g of potassium persulfate into 22.5g of water to prepare a 40% initiator solution;
(2) 177.5g of water is added into a reaction kettle, 35g of allyloxy hydroxypropyl sodium sulfonate, 28g of acrylic acid and 34g of styrene are sequentially added according to the weight, and stirring is started at the stirring speed of 1000 revolutions per minute;
(3) sealing, and heating to 100 ℃;
(4) dropping an initiator solution for 1 h;
(5) after the dropwise addition, continuously keeping the temperature and stirring for 3 hours;
(6) cooling, adding sodium hydroxide for neutralization, and keeping the temperature at 60 ℃;
(7) cooling to room temperature, and discharging;
(8) spray drying, and packaging.
Example 5
An environment-friendly agricultural dispersant comprises the following components in parts by weight: 55 parts of methacrylic acid, 22 parts of styrene, 23 parts of allyloxy hydroxypropyl sodium sulfonate, 10 parts of ammonium persulfate, 26 parts of sodium hydroxide and 200 parts of water.
The preparation method of the environment-friendly agricultural dispersant comprises the following specific steps:
(1) pouring 10g of ammonium persulfate into 20g of ammonium persulfate to prepare a 33.3 percent initiator solution;
(2) adding 180g of water into a reaction kettle, sequentially adding 23g of allyloxy hydroxypropyl sodium sulfonate, 55g of methacrylic acid and 22g of styrene, and starting stirring at the stirring speed of 700 revolutions per minute;
(3) sealing, and heating to 100 ℃;
(4) dropping an initiator solution for 1 h;
(5) after the dropwise addition is finished, the temperature is kept and stirring is continued for 4 hours;
(6) cooling, adding sodium hydroxide for neutralization, and keeping the temperature at 60 ℃;
(7) cooling to room temperature, and discharging;
(8) spray drying, and packaging.
Comparative example 1
Specific composition of the agricultural dispersant referring to example 5, the only difference is that sodium allyloxy hydroxypropyl sulfonate is replaced with an equal amount of methacrylic acid. The preparation method is the same as example 5.
Comparative example 2
Specific composition of agricultural dispersant referring to example 5, the preparation method is the same as example 5 except that the stirring speed of step (2) is changed from 700 rpm to 400 rpm.
Comparative example 3
Specific composition of agricultural dispersant referring to example 5, the preparation method is the same as example 5 except that the stirring speed of step (2) is changed from 700 rpm to 200 rpm.
Comparative example 4
Specific composition of agricultural dispersant referring to example 5, the preparation method is the same as example 5 except that the temperature of step (3) is raised to 100 ℃ and is changed to 80 ℃.
Comparative example 5
Specific composition of agricultural dispersant referring to example 5, the preparation method is the same as example 5 except that the temperature of step (3) is raised to 100 ℃ and is changed to 70 ℃.
The following performance tests were carried out on the agricultural dispersants prepared in examples 1 to 5 and comparative examples 1 to 5:
(1) reaction conditions
Since styrene was insoluble in water, unreacted styrene was extracted by extraction, and the conversion of the reaction (mass of added styrene-mass of unreacted styrene)/mass of added styrene was measured, and the results are shown in table 1.
TABLE 1 reaction of dispersants of examples and comparative examples
As can be seen from the results in Table 1, the environmentally friendly agricultural dispersants of examples 1-5 of the present invention have stable synthesis process and high conversion rate. In the invention, one component is replaced or the preparation conditions are changed, the monomer conversion rate is low, the appearance of the auxiliary agent is poor, and a large amount of residual monomer exists.
(2) Molecular weight measurement
The molecular weight was measured by GPC using sodium polyacrylate as a standard, and the solution was used for comparative example, and the results are shown in Table 2.
TABLE 2 molecular weight and distribution index of dispersants of examples and comparative examples
The molecular weight is less than 5000, the dispersion effect cannot be achieved, the molecular weight is more than 35000, and the particles cannot be adsorbed on the surfaces rapidly due to the molecular weight. As can be seen from the results in Table 2, the molecular weights of the environmentally friendly agricultural dispersants added in the examples 1-5 of the present invention are within 5000-. One component in the invention is replaced or the preparation condition is changed, the molecular weight does not meet the dispersion requirement, the distribution coefficient is more than 2, and the molecular weight of the dispersant is not concentrated.
(3) Dispersion Performance test
Corn starch, light calcium carbonate and kaolin are common fillers in pesticide preparations, and the dosage is large, and the dispersing suspension performance of the dispersing agent is tested by using the filler. Test methods reference GB/T14825-2006 (method 2), with results in Table 3.
TABLE 3 Dispersion Performance of dispersants of examples and comparative examples
As can be seen from the detection data in Table 3, the environment-friendly agricultural dispersant provided by the invention has good suspension performance on corn starch, light calcium carbonate and kaolin. By replacing one component in the invention or changing the preparation conditions, the dispersion performance of the prepared dispersant is greatly reduced.
The results show that the environment-friendly agricultural dispersant prepared by the invention has the characteristics of complete reaction, simple process and good dispersing performance.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (4)
1. The environment-friendly agricultural dispersant is characterized by comprising the following components in parts by weight: 25-70 parts of acrylic monomers, 15-35 parts of styrene, 15-35 parts of allyloxy hydroxypropyl sodium sulfonate, 5-15 parts of an initiator, 15-35 parts of alkali and 100-300 parts of water;
the acrylic monomer is at least one of acrylic acid, methacrylic acid, maleic anhydride and fumaric acid;
the weight average relative molecular weight of the agricultural dispersant is 5000-35000;
the preparation method of the environment-friendly agricultural dispersant comprises the following steps:
(1) pouring an initiator into a certain amount of water to prepare an initiator solution with the concentration of 30-40 percent;
(2) adding the residual amount of water into the reaction kettle, sequentially adding allyloxy hydroxypropyl sodium sulfonate, acrylic monomers and styrene according to weight, and starting stirring at the stirring speed of 500-;
(3) sealing, and heating to 85-100 deg.C;
(4) dripping initiator solution for 0.5-3 h;
(5) after the dropwise addition is finished, continuously keeping the temperature and stirring for 1-4 h;
(6) cooling, adding alkali for neutralization, and keeping the temperature at 50-70 ℃;
(7) cooling to room temperature, and discharging;
(8) spray drying, and packaging.
2. The environment-friendly agricultural dispersant as claimed in claim 1, which is characterized by comprising the following components in parts by weight: 45-60 parts of acrylic monomers, 18-27 parts of styrene, 18-27 parts of allyloxy hydroxypropyl sodium sulfonate, 10-15 parts of an initiator, 15-35 parts of alkali and 100-300 parts of water.
3. The environment-friendly agricultural dispersant according to claim 1 or 2, wherein the initiator is at least one of persulfate and hydrogen peroxide water-soluble initiator.
4. The environment-friendly agricultural dispersant according to claim 1 or 2, wherein the base is at least one of sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, ammonia water, ethanolamine, diethanolamine, and triethanolamine.
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