CN111616143A - Auxiliary agent for fluorosulfonic water agent and fluorosulfonic water agent prepared by same - Google Patents
Auxiliary agent for fluorosulfonic water agent and fluorosulfonic water agent prepared by same Download PDFInfo
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- CN111616143A CN111616143A CN202010371445.6A CN202010371445A CN111616143A CN 111616143 A CN111616143 A CN 111616143A CN 202010371445 A CN202010371445 A CN 202010371445A CN 111616143 A CN111616143 A CN 111616143A
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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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- 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
-
- 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
- A01N41/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a sulfur atom bound to a hetero atom
- A01N41/02—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a sulfur atom bound to a hetero atom containing a sulfur-to-oxygen double bond
- A01N41/04—Sulfonic acids; Derivatives thereof
- A01N41/06—Sulfonic acid amides
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Dentistry (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses an auxiliary agent for a fluorosulfonic water agent, which comprises the following components in percentage by weight: 10-15% of polyglycerol ether, 20-30% of plant amine polyoxyethylene ether amine oxide, 15-20% of cocamidopropyl amine oxide, 10-15% of alkyl glycoside and the balance of water. The invention also discloses a fluorosulfonic water agent containing the auxiliary agent and a preparation method of the fluorosulfonic water agent. The fluorosulfonate water agent disclosed by the invention has high herbicidal activity, has a good control effect on various weeds in northeast cold regions, greatly reduces the speed of generating drug resistance of the weeds, and improves the herbicidal activity of the fluorosulfonate water agent.
Description
Technical Field
The invention relates to the technical field of pesticides, in particular to an auxiliary agent for a fluorosulfonic water agent and a fluorosulfonic water agent prepared by the same.
Background
Farmland weeds are a type of pest that seriously threatens the growth of crops. Weeds can cause an average loss of 34% of crop yield, which is far more harmful than pests and germs. At present, chemical herbicides are still the most economic and effective means for controlling weed harm in modern agricultural production, but with the long-term use of a large amount of herbicides, various problems such as drug resistance, environmental pollution and the like are brought.
The fomesafen is a herbicide widely applied to soybean fields, has the advantages of wide weed control spectrum, good weeding effect, safety to environment and succeeding crops and the like, and can be used before and after soybean seedlings. Fomesafen, namely 5- (2-chloro-alpha, alpha-trifluoro-p-tolyloxy) -N-methylsulfonyl-2-nitrobenzamide, has the effective component content of 95 percent and is an off-white powdery solid in appearance. It is a post-seedling herbicide with high selectivity for soybean and peanut fields. The fluorine sulphur can be absorbed by the stem leaves and the roots of the weeds, the photosynthesis of the weeds is damaged, the leaves are yellowed or have withered spots, and finally the weeds are withered and die quickly. The soybean root can be degraded quickly after absorbing the fluorine-containing pesticide, and the herbicide has the characteristic of safety to soybean.
However, when the fluorosulfonic acid aqueous solution is used in a drought or cold environment, the chemical solution is likely to be hardly absorbed by the leaf surfaces, and the pharmaceutical effect is deteriorated. Therefore, the fluorosulfonic water agent auxiliary with excellent wettability is developed, and the problem can be effectively solved, so that the drug effect of the fluorosulfonic water agent used in the drought and cold environments is improved.
Disclosure of Invention
The invention mainly aims to overcome the defects of the existing fluorosulfonic water agent and solve the technical problem that the pesticide effect is poor due to the fact that the pesticide liquid is difficult to be fully absorbed on the leaf surfaces when the fluorosulfonic water agent is used in a drought and cold environment, so that an auxiliary agent formula with a good moisturizing effect and the fluorosulfonic water agent prepared by the auxiliary agent formula are provided to improve the pesticide effect when the fluorosulfonic water agent is used.
The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme.
The invention provides an auxiliary agent for a fluorosulfonic water agent, which comprises the following components in percentage by weight: 10-15% of polyglycerol ether, 20-30% of plant amine polyoxyethylene ether amine oxide, 15-20% of cocamidopropyl amine oxide, 10-15% of alkyl glycoside and the balance of water.
The object of the present invention and the technical problems solved thereby can be further achieved by the following technical measures.
The invention also provides a fluorosulfonic water agent containing the auxiliary agent for fluorosulfonic water agent, and the fluorosulfonic water agent comprises the following components: the pesticide composition comprises fomesafen, sodium hydroxide, an auxiliary agent and water.
The fluorine sulfonic water agent comprises the following components in percentage by weight: fomesafen original drug: sodium hydroxide: auxiliary agent: water =23.5:2.5:10: 64.
The object of the present invention and the technical problem to be solved are also achieved by the following technical means.
The invention also provides a method for preparing the fluorosulfonic water agent, wherein the method comprises the following steps:
(1) preparing plant amine polyoxyethylene ether amine oxide;
(2) mixing the prepared plant amine polyoxyethylene ether amine oxide, polyglycerol ether, cocamidopropyl amine oxide, alkyl glycoside and water, adding into a reaction kettle, and uniformly stirring to obtain an auxiliary agent;
(3) mixing the fomesafen original drug, sodium hydroxide and water, adding the mixture into a reaction kettle to react until the materials are uniform and transparent, then adding the obtained auxiliary agent, and stirring uniformly to obtain the fluorosulfonic water agent.
In the preparation method, the plant amine polyoxyethylene ether amine oxide in the step (1) is prepared by the following steps: adding plant amine into a polymerization reaction kettle, introducing ethylene oxide, adding an alkali catalyst, and carrying out polymerization reaction to obtain an intermediate plant amine ether; then adding plant amine ether into the reaction kettle, slowly adding hydrogen peroxide in batches, and carrying out oxidation reaction to obtain the plant amine polyoxyethylene ether amine oxide.
The preparation method, wherein the plant amine is selected from cocoamine or laurylamine.
The preparation method described above, wherein the polymerization reaction conditions are: the temperature is 130 ℃, and the time is 2 h; the oxidation reaction conditions are as follows: the temperature is 40 ℃ and the time is 6 h.
In the preparation method, the temperature in the reaction kettle in the step (2) is 50 ℃.
The preparation method comprises the step (2) of adding the plant amine polyoxyethylene ether amine oxide, the polyglycerol ether, the cocamidopropyl amine oxide, the alkyl glycoside and the water according to the weight ratio of (20-30): (10-15): (15-20): (10-15): 20-45).
The preparation method described above, wherein the reaction conditions in the step (3) are: the temperature is 50 ℃ and the time is 4 h.
Compared with the prior art, the invention has the obvious advantages and beneficial effects that: the newly prepared fluorine-containing water agent has an assistant formula with a good moisturizing effect, and the pesticide effect of the fluorine-containing water agent in use can be effectively improved. The fluorosulfonate water agent disclosed by the invention has high herbicidal activity, has a good control effect on various weeds in northeast cold regions, greatly reduces the speed of generating drug resistance of the weeds, and improves the herbicidal activity of the fluorosulfonate water agent. The preparation method is simple, easy to operate and convenient for industrial production.
In conclusion, the special auxiliary for the fluorosulfonic water agent and the fluorosulfonic water agent prepared by the special auxiliary can solve the problem that the pesticide effect is poor due to the fact that the pesticide liquid is difficult to be fully absorbed on the leaf surface when the conventional fluorosulfonic water agent is used in a drought and cold environment. The fluorine-containing water aqua has the advantages and practical values, does not have similar design publication or use in similar products, is innovative, has great improvement on method or function, has great technical progress, produces good and practical effects, has multiple efficacies improved compared with the existing fluorine-containing water aqua, is more suitable for practical use, has industrial wide utilization value, and is a novel, advanced and practical new design.
The foregoing is a summary of the present invention, and in order to provide a clear understanding of the technical means of the present invention and to be implemented in accordance with the present specification, the following is a detailed description of the preferred embodiments of the present invention.
Specific embodiments of the present invention are given in detail by the following examples.
Detailed Description
In order to further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description will be given to specific embodiments, methods, features and effects of the adjuvant for fluorosulfonic water solution and fluorosulfonic water solution prepared by the adjuvant according to the present invention.
According to the auxiliary agent for the fluorosulfonic water agent, the auxiliary agent comprises the following components in percentage by weight: 10-15% of polyglycerol ether, 20-30% of plant amine polyoxyethylene ether amine oxide, 15-20% of cocamidopropyl amine oxide, 10-15% of alkyl glycoside and the balance of water.
According to the fluorosulfonic water agent containing the auxiliary agent for fluorosulfonic water agents, the fluorosulfonic water agent comprises the following components: the pesticide composition comprises fomesafen, sodium hydroxide, an auxiliary agent and water. According to the weight percentage, the fomesafen is prepared from the following raw materials: sodium hydroxide: auxiliary agent: water =23.5:2.5:10: 64.
The method for preparing the fluorosulfonic water agent comprises the following steps: (1) preparing plant amine polyoxyethylene ether amine oxide; (2) mixing the prepared plant amine polyoxyethylene ether amine oxide, polyglycerol ether, cocamidopropyl amine oxide, alkyl glycoside and water, adding into a reaction kettle, and uniformly stirring to obtain an auxiliary agent; (3) mixing the fomesafen original drug, sodium hydroxide and water, adding the mixture into a reaction kettle to react until the materials are uniform and transparent, then adding the obtained auxiliary agent, and stirring uniformly to obtain the fluorosulfonic water agent.
The reaction process of the plant amine polyoxyethylene ether amine oxide in the step (1) comprises the following steps: adding plant amine into a polymerization reaction kettle, introducing ethylene oxide, adding an alkali catalyst, and carrying out polymerization reaction for 2 hours at the temperature of 130 ℃ to obtain an intermediate plant amine ether; adding plant amine ether into a reaction kettle, slowly adding hydrogen peroxide in batches, and stirring for 6 hours at 40 ℃ to obtain the plant amine polyoxyethylene ether amine oxide. The specific reaction scheme is as follows:
wherein R is cocoyl or lauryl, and x + y = 15-20.
In the step (2), the plant amine polyoxyethylene ether amine oxide, the polyglycerol ether, the cocamidopropyl amine oxide, the alkyl glycoside and the water are added according to the weight ratio of (20-30): (10-15): (15-20): (10-15): 20-45). The polymerization conditions were: the temperature is 130 ℃ and the time is 2 h. The oxidation reaction conditions after adding hydrogen peroxide are as follows: the temperature is 40 ℃ and the time is 6 h. The temperature in the reaction kettle was 50 ℃.
The reaction conditions in the reaction kettle in the step (3) are as follows: the temperature is 50 ℃ and the time is 4 h.
The following description will be given with reference to specific examples, in which the respective raw materials are in parts by weight.
Example 1
Preparing cocoamine polyoxyethylene ether amine oxide: adding 193 parts of cocoamine into a polymerization reaction kettle, introducing 660 parts of ethylene oxide, adding an alkali catalyst, and carrying out polymerization reaction for 2 hours at 130 ℃ to obtain an intermediate cocoamine ether; adding cocoanut oil amine ether into a reaction kettle, slowly adding 895 parts of hydrogen peroxide (with the content of 50 percent) in batches, and stirring and reacting for 6 hours at the temperature of 40 ℃ to obtain cocoanut oil amine polyoxyethylene ether amine oxide (15 EO).
Preparing an auxiliary agent: adding 10 parts of polyglycerol ether, 30 parts of cocoamine polyoxyethylene ether amine oxide (15 EO), 20 parts of cocamidopropyl amine oxide, 10 parts of alkyl glycoside and 30 parts of water into a reaction kettle, and uniformly stirring at 50 ℃ to obtain the assistant.
Preparation of 250g/L fluorosulfonic water agent: adding 23.5 parts of fomesafen original drug (with the content of 98%), 2.5 parts of sodium hydroxide and 64 parts of water into a reaction kettle, reacting for 4 hours at 50 ℃ until the materials are uniform and transparent, adding 10 parts of auxiliary agent, and uniformly stirring to obtain the fluorosulfonic water agent.
Example 2
Preparing laurylamine polyoxyethylene ether amine oxide: adding 183 parts of laurylamine into a polymerization reaction kettle, introducing 880 parts of ethylene oxide, adding an alkali catalyst, and carrying out polymerization reaction for 2 hours at 130 ℃ to obtain an intermediate laurylamine ether; adding laurylamine ether into a reaction kettle, slowly adding 1116 parts of hydrogen peroxide (with the content of 50 percent) in batches, and stirring and reacting for 6 hours at the temperature of 40 ℃ to obtain laurylamine polyoxyethylene ether amine oxide (20 EO).
Preparing an auxiliary agent: adding 15 parts of polyglycerol ether, 20 parts of laurylamine polyoxyethylene ether amine oxide (20 EO), 15 parts of cocamidopropyl amine oxide, 15 parts of alkyl glycoside and 35 parts of water into a reaction kettle, and uniformly stirring at 50 ℃ to obtain the assistant.
Preparation of 250g/L fluorosulfonic water agent: adding 23.5 parts of fomesafen original drug (with the content of 98%), 2.5 parts of sodium hydroxide and 64 parts of water into a reaction kettle, reacting for 4 hours at 50 ℃ until the materials are uniform and transparent, adding 10 parts of auxiliary agent, and uniformly stirring to obtain the fluorosulfonic water agent.
Example 3
Preparing laurylamine polyoxyethylene ether amine oxide: adding 183 parts of laurylamine into a polymerization reaction kettle, introducing 792 parts of ethylene oxide, adding an alkali catalyst, and carrying out polymerization reaction for 2 hours at 130 ℃ to obtain an intermediate laurylamine ether; adding laurylamine ether into a reaction kettle, slowly adding 1024 parts of hydrogen peroxide (the content of 50 percent) in batches, and stirring and reacting for 6 hours at the temperature of 40 ℃ to obtain laurylamine polyoxyethylene ether amine oxide (18 EO).
Preparing an auxiliary agent: 12 parts of polyglycerol ether, 25 parts of laurylamine polyoxyethylene ether amine oxide (15 EO), 18 parts of cocamidopropyl amine oxide, 12 parts of alkyl glycoside and 33 parts of water are added into a reaction kettle and stirred uniformly at 50 ℃ to obtain the assistant.
Preparation of 250g/L fluorosulfonic water agent: adding 23.5 parts of fomesafen original drug (with the content of 98%), 2.5 parts of sodium hydroxide and 64 parts of water into a reaction kettle, reacting for 4 hours at 50 ℃ until the materials are uniform and transparent, adding 10 parts of auxiliary agent, and uniformly stirring to obtain the fluorosulfonic water agent.
Comparative example 1
Preparation of 250g/L fluorosulfonic water agent: adding 23.5 parts of fomesafen original drug (with the content of 98%), 2.5 parts of sodium hydroxide and 64 parts of water into a reaction kettle, reacting for 4 hours at 50 ℃ until the materials are uniform and transparent, adding 10 parts of commercial auxiliary agent I, and stirring uniformly to obtain the fluorosulfonic water agent.
Comparative example 2
Preparation of 250g/L fluorosulfonic water agent: adding 23.5 parts of fomesafen original drug (with the content of 98%), 2.5 parts of sodium hydroxide and 64 parts of water into a reaction kettle, reacting for 4 hours at 50 ℃ until the materials are uniform and transparent, adding 10 parts of commercial auxiliary agent II, and stirring uniformly to obtain the fluorosulfonic water agent.
Test example 1 measurement of wetting power of fluorosulfonic water agent
Test subjects: the fluorosulfonic water agents obtained in examples 1 to 3 and the fluorosulfonic water agents obtained in comparative examples 1 to 2.
The test method comprises the following steps: contact angle method: clean weeds are poured into three leaves, flat parts are selected, small blocks are cut, the flat parts are placed on a glass slide and then placed into a sample groove, a micro-sampler is used for sucking the fluorosulfonic water agent prepared in the examples 1-3 and the fluorosulfonic water agent prepared in the comparative examples 1-2 respectively, 2 microliters of liquid drops are dripped onto the leaves, contact angles of the fluorosulfonic water agent and the fluorosulfonic water agent are observed after 30 seconds, and the results are shown in table 1.
TABLE 1 contact angle test values for various fluorosulfonic water agents
From the results in table 1, it can be seen that the auxiliary agents prepared in examples 1 to 3 used in fluorosulfonic water solutions can significantly reduce the contact angle value of fluorosulfonic water solutions on the leaf surface compared to commercially available fluorosulfonic auxiliary agents (comparative examples 1 and 2), and the auxiliary agents of examples 1 to 3 used in fluorosulfonic water solutions can have excellent wetting effects.
Test example 2 efficacy test of fluorine-containing sulfonic acid solutions (see "test criteria for efficacy in agricultural chemical field")
Test formulations: the fluorosulfonic water agents obtained in examples 1 to 3 and the fluorosulfonic water agents obtained in comparative examples 1 to 2.
Test subjects: the main weeds in the field comprise green bristlegrass herb, goosegrass herb, barnyard grass, wild oat and the like.
The test method comprises the following steps: the drug effect test selects the area in northeast, the local air temperature is 0-5 ℃, 6 treatments (including blank control group) are set in the experiment, the experiment is repeated for 4 times, 24 areas are totally, the area of each area is 15 square meters, the random block arrangement, the drug application method and the water consumption (liter/hectare): spraying stem leaves, wherein the water consumption is 450 liters per hectare, (the blank group is only sprayed with clean water with the corresponding spraying amount).
And (4) determining the result: 4 spots are randomly selected from each plot, 1/4 square meters are investigated from each spot, and the weed control effect is investigated 30 days after the application of the herbicide, and the results are shown in table 2.
TABLE 2 Total fresh weight control of weeds 30 days after treatment with different fluorosulfonic water agents
As can be seen from the results in table 2, the fluorosulfonic water solutions prepared in examples 1 to 3 of the present invention have significantly improved total weed fresh weight control effect compared to the fluorosulfonic water solutions of comparative examples 1 and 2. Especially in northeast cold areas, has better control effect on various weeds.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. The auxiliary agent for the fluorosulfonic water agent comprises the following components in percentage by weight: 10-15% of polyglycerol ether, 20-30% of plant amine polyoxyethylene ether amine oxide, 15-20% of cocamidopropyl amine oxide, 10-15% of alkyl glycoside and the balance of water.
2. An aqueous fluorosulfonic agent comprising the auxiliary for an aqueous fluorosulfonic agent of claim 1, comprising the following components: the pesticide composition comprises fomesafen, sodium hydroxide, an auxiliary agent and water.
3. The fluorosulfonic water agent of claim 3, wherein the fluorosulfonic water agent comprises the following components in percentage by weight: fomesafen original drug: sodium hydroxide: auxiliary agent: water =23.5:2.5:10: 64.
4. A process for preparing an aqueous fluorosulfonic agent of claim 2 or 3, wherein the process comprises the steps of:
(1) preparing plant amine polyoxyethylene ether amine oxide;
(2) mixing the prepared plant amine polyoxyethylene ether amine oxide, polyglycerol ether, cocamidopropyl amine oxide, alkyl glycoside and water, adding into a reaction kettle, and uniformly stirring to obtain an auxiliary agent;
(3) mixing the fomesafen original drug, sodium hydroxide and water, adding the mixture into a reaction kettle to react until the materials are uniform and transparent, then adding the obtained auxiliary agent, and stirring uniformly to obtain the fluorosulfonic water agent.
5. The preparation method according to claim 4, wherein the plant amine polyoxyethylene ether amine oxide in the step (1) is prepared by the following steps: adding plant amine into a polymerization reaction kettle, introducing ethylene oxide, adding an alkali catalyst, and carrying out polymerization reaction to obtain an intermediate plant amine ether; then adding plant amine ether into the reaction kettle, slowly adding hydrogen peroxide in batches, and carrying out oxidation reaction to obtain the plant amine polyoxyethylene ether amine oxide.
6. The method according to claim 5, wherein the plant amine is selected from cocoamine or laurylamine.
7. The production method according to claim 5, wherein the polymerization reaction conditions are: the temperature is 130 ℃, and the time is 2 h; the oxidation reaction conditions are as follows: the temperature is 40 ℃ and the time is 6 h.
8. The production method according to claim 4, wherein the temperature in the reaction tank in the step (2) is 50 ℃.
9. The preparation method according to claim 4, wherein the plant amine polyoxyethylene ether amine oxide, the polyglyceryl ether, the cocamidopropyl amine oxide, the alkyl glycoside and the water are added in the amount of (20-30): 10-15): 15-20: (10-15): 20-45) by weight in the step (2).
10. The production method according to claim 4, wherein the reaction conditions in the step (3) are: the temperature is 50 ℃ and the time is 4 h.
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| DE69812370T2 (en) * | 1997-08-27 | 2004-02-12 | Syngenta Ltd., Guildford | AGRICULTURAL COMPOSITION |
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2020
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| DE69812370T2 (en) * | 1997-08-27 | 2004-02-12 | Syngenta Ltd., Guildford | AGRICULTURAL COMPOSITION |
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Application publication date: 20200904 |