High-efficiency haloxyfop-methyl and glufosinate-ammonium microemulsion adjuvant and preparation method and application thereof
By using microemulsion additives with components such as diethanolamide cocoate and amine ether, the problem of poor stability of high-efficiency flupyrimethol and glufosinate microemulsion during storage is solved, and efficient and stable efficacy is achieved.
Patent Information
- Application Number
- CN202310634474.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-05-31
- Publication Date
- 2025-04-18
- Estimated Expiration
- 2043-05-31
AI Technical Summary
The existing high-efficiency flupyrimethol and glufosinate ammonium microemulsions have poor stability during storage, easy to precipitate at low temperatures, easy to turbidity at high temperatures, and high-efficiency flupyrimethol and the high-efficiency flupyrimethol is easy to decompose.
A microemulsion additive is used to combine diethanolamide cocoate and amine ethers with a specific composition of sodium isomer alcohol ether sulfate and sodium fatty alcohol polyoxyethylene ether sulfate to adjust the pH value to improve the stability and efficacy of the microemulsion.
The high and low temperature storage stability of high-efficiency flupiramole and glufosinate microemulsion is significantly improved, the thermal storage decomposition rate of high-efficiency flupiramole and original drug is reduced, and the efficacy is improved.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of pesticides, and in particular relates to a high-efficiency haloxyfop-methyl and glufosinate-ammonium microemulsion adjuvant and a preparation method and application thereof. Background Art
[0002] Herbicides are agents that can kill weeds completely or selectively, and are used to eliminate or inhibit plant growth. Herbicides can be classified according to the mode of action, application site, source of compounds, and other aspects. According to the mode of action, they are divided into selective herbicides and life-threatening herbicides. Selective herbicides have different resistance levels to different types of seedlings. This agent can kill weeds but is harmless to seedlings, such as galactone, trifluralin, promethazine, simazine, and goer herbicide. Life-threatening herbicides are toxic to all plants. As long as they come into contact with the green part, regardless of seedlings or weeds, they will be harmed or killed. They are mainly used before sowing, before germination after sowing, and on the main and secondary roads of the nursery, such as glyphosate. According to the movement of herbicides in the plant body, they are divided into contact herbicides, systemic herbicides, and systemic herbicides and contact herbicides. Contact herbicide: When the agent contacts the weeds, only the part in contact with the agent is killed, playing a local killing role, and cannot be conducted in the plant body, such as herbicide ether and paraquat. Systemic conduction herbicide: After the agent is absorbed by the root system or leaves, bud sheaths or stems, it is conducted into the plant body, causing the plant to die, such as glyphosate and promethazine. Systemic conduction and contact comprehensive herbicide: It has the dual functions of systemic conduction and contact killing, such as herbicide. According to the chemical structure, it is divided into inorganic compound herbicides and organic compound herbicides. Inorganic compound herbicides are composed of natural mineral raw materials and do not contain carbon compounds, such as potassium chlorate and copper sulfate. Organic compound herbicides are mainly synthesized from organic compounds such as benzene, alcohol, fatty acid, organic amine, such as ethers-Gol, triazines-promethazine, substituted ureas-herbicide No. 1, etc. According to the method of use, it can be divided into stem and leaf treatment agents, soil treatment agents, and stem and leaf, soil treatment agents. Stem and leaf treatment agents: dilute the herbicide solution with water and spray it evenly on the plants in fine droplets. The herbicides used in this spraying method are called stem and leaf treatment agents, such as Gaifenon and glyphosate. Soil treatment agents: spray the herbicide evenly on the soil to form a drug layer of a certain thickness. When the young shoots, seedlings and roots of weed seeds are contacted and absorbed, they play a weed-killing role. This kind of herbicide is called soil treatment agent, such as Simazine, Promethazine, Trifluralin, etc., which can be applied by spraying, pouring, or poisoning soil. Stem and leaf, soil treatment agents: They can be used for stem and leaf treatment or soil treatment, such as atrazine.
[0003] High-efficiency fluazifop-p-ethyl is a post-emergence selective herbicide with systemic conduction, safety for the next crop, and high selectivity between gramineous weeds and dicotyledonous crops. It is mainly used to control annual and perennial gramineous weeds in various broad-leaved crop fields such as soybeans, cotton, and peanuts. Glufosinate-ammonium is a broad-spectrum contact herbicide with weak systemic action. Unlike glyphosate, which kills the roots, glufosinate-ammonium kills the leaves first and can be conducted in the xylem of the plant through plant transpiration. Its rapidity is between paraquat and glyphosate. Therefore, mixing high-efficiency fluazifop-p-ethyl and glufosinate-ammonium herbicides can play a synergistic role in improving the broad-spectrum weed control. For example, Chinese patent application CN114617132A discloses a herbicide composition, a herbicide and a preparation method, wherein the herbicide composition is composed of an active ingredient A, an active ingredient B, and a synergist, wherein the active ingredient A is glufosinate or refined glufosinate; the active ingredient B is high-efficiency fluazifop-p-ethyl; the synergist is one or more of peppermint oil, cinnamon, piperine, cyclohexanehexol, dimethyl isosorbide DMI, unsaturated linoleic acid, and sodium pyrrolidone carboxylic acid; specifically, it provides a refined glufosinate synergistic herbicide composition, the dosage form of which is a microemulsion, and the composition comprises, by weight percentage: 17.5% refined glufosinate, 2.5% high-efficiency fluazifop-p-ethyl, 3% dodecylbenzene sulfonate, 12% tristyrylphenol polyoxyethylene ether, 3% ethylene oxide-propylene oxide block copolymer, 6% unsaturated linoleic acid, 3% 150# solvent oil, 2% ethanol, 1.5% glacial acetic acid, 0.1% kason, and water is supplemented to 100%. Although the herbicidal composition has a good weed control effect, due to the presence of a large amount of water in the system, it has poor stability during storage, is easy to precipitate at low temperature storage, is easy to become turbid at high temperature storage, and has the problem of easy decomposition of the high-efficiency halofop-p-ethyl technical. Therefore, it is urgent to develop a high-efficiency halofop-p-ethyl and glufosinate microemulsion that can improve the high and low temperature storage stability of the preparation while ensuring the efficacy, and the high-efficiency halofop-p-ethyl technical in the obtained preparation is not easy to decompose. Summary of the invention
[0004] In view of the deficiencies of the prior art, the object of the present invention is to provide a high-efficiency haloxyfop-methyl and glufosinate-ammonium microemulsion adjuvant and a preparation method and application thereof. The high-efficiency haloxyfop-methyl and glufosinate-ammonium microemulsion adjuvant provided by the present invention is used in the high-efficiency haloxyfop-methyl and glufosinate-ammonium microemulsion, while ensuring the efficacy, not only can the high and low temperature storage stability of the obtained preparation be significantly improved, but also the high-efficiency haloxyfop-methyl original drug in the obtained preparation is not easy to decompose.
[0005] The technical solution of the present invention is:
[0006] A high-efficiency fluazifop-p-ethyl and glufosinate-ammonium microemulsion adjuvant comprises the following raw materials and their weight proportions: 10-15 parts of coconut acid diethanolamide, 5-10 parts of trihydroxyethylamine, 40-50 parts of isomeric alcohol ether sodium sulfate, 5-8 parts of fatty alcohol polyoxyethylene ether sodium sulfate, 5-10 parts of amine ether, 5-7 parts of citric acid and 10-22 parts of water.
[0007] Furthermore, the high-efficiency fluazifop-butyl and glufosinate microemulsion adjuvant comprises the following raw materials and their weight proportions: 10 parts of coconut acid diethanolamide, 8 parts of trihydroxyethylamine, 50 parts of sodium isocyanate sulfate, 5 parts of sodium fatty alcohol polyoxyethylene ether sulfate, 8 parts of amine ether, 7 parts of citric acid, and 12 parts of water.
[0008] Furthermore, the isomeric alcohol ether sodium sulfate includes isomeric tridecanol polyoxyethylene ether sodium sulfate and isomeric decanol polyoxyethylene ether sodium sulfate.
[0009] Furthermore, the isomeric alcohol ether sodium sulfate is composed of isomeric tridecanol polyoxyethylene ether sodium sulfate and isomeric decanol polyoxyethylene ether sodium sulfate in a mass ratio of 1:4-6.
[0010] Furthermore, the isomeric alcohol ether sodium sulfate is composed of isomeric tridecanol polyoxyethylene ether sodium sulfate and isomeric decanol polyoxyethylene ether sodium sulfate in a mass ratio of 1:5.
[0011] Another object of the present invention is to provide a method for preparing the highly effective haloxyfop-methyl and glufosinate-ammonium microemulsion adjuvant, comprising the following steps:
[0012] Mix sodium fatty alcohol polyoxyethylene ether sulfate and trihydroxyethylamine, stir evenly, then add coconut acid diethanolamide and stir evenly, add sodium isomeric alcohol ether sulfate, amine ether and water and stir evenly, finally add citric acid, adjust the pH, and stir until completely transparent and uniform.
[0013] Another object of the present invention is to provide the use of the high-efficiency haloxyfop-butyl and glufosinate microemulsion adjuvant in the preparation of high-efficiency haloxyfop-butyl and glufosinate microemulsion.
[0014] A high-efficiency haloxyfop-methyl and glufosinate microemulsion comprises the following raw materials and their mass percentages: 3% of high-efficiency haloxyfop-methyl, 19% of glufosinate ammonium, 8% of xylene, 3% of the high-efficiency haloxyfop-methyl and glufosinate microemulsion adjuvant, and 67% of water.
[0015] The preparation method of the high-efficiency haloxyfop-methyl and glufosinate microemulsion is as follows: high-efficiency haloxyfop-methyl and xylene are mixed, stirred until completely dissolved, and then high-efficiency haloxyfop-methyl and glufosinate microemulsion adjuvants, water and glufosinate are added and stirred for 30 minutes until completely transparent.
[0016] Due to the presence of a large amount of water in the microemulsion system, it is poorly stable during storage, and there is a problem that the high-efficiency haloxyfop-p-ethyl original drug is easily decomposed. Therefore, how to emulsify high-efficiency haloxyfop-p-ethyl well, and solubilize it in glufosinate-ammonium, and achieve that low temperature does not precipitate, high temperature is not turbid, and the problem that reduces the high-efficiency haloxyfop-p-ethyl original drug is easily decomposed is the technical difficulty that the high-efficiency haloxyfop-p-ethyl and glufosinate-ammonium microemulsion of the prior art exist. In the present invention, coconut oil diethanolamide and amine ether cooperate with each other, not only can high-efficiency haloxyfop-p-ethyl be well emulsified, but also can greatly improve the compatibility of high-efficiency haloxyfop-p-ethyl and glufosinate-ammonium system, is not easy to precipitate during low temperature storage, and then improves the stability of microemulsion system. Coconut oil diethanolamide and trihydroxyethylamine (trolamine) cooperate with each other, can be well conducted in plant body, improve drug efficacy. The isomeric alcohol ether sodium sulfate and fatty alcohol polyoxyethylene ether sodium sulfate of the specific composition in the present invention cooperate with each other, not only can the emulsified high-efficiency haloxyfop-methyl be dissolved into the glufosinate ammonium liquid preparation, but also make the preparation more transparent and stable, and not prone to turbidity, stratification and precipitation during storage, and have a good stabilizing effect on the active ingredient high-efficiency haloxyfop-methyl, effectively reduce the heat storage decomposition rate of the high-efficiency haloxyfop-methyl original drug in the microemulsion, significantly improve thermal stability, and provide suitable surface tension for the liquid medicine, so that the liquid medicine is wetted and spread on the surface of the target plant and has a large drug retardation amount, thereby improving drug efficacy. The citric acid used in the present invention can adjust the pH of the entire system, so that the system is more stable within a suitable pH range.
[0017] The preparation technology of pesticide microemulsion is high and difficult. Microemulsion adjuvant is a prerequisite for preparing microemulsion. The use of microemulsion adjuvant for the preparation of microemulsion is unpredictable, and a large amount of creative work is required to prepare a microemulsion that meets the requirements. In the present invention, each component cooperates with each other, each component is indispensable, and the dosage of each component is very important. Only under the condition of the formula composition and dosage range of the present invention can the technical effect of the present invention be achieved.
[0018] Compared with the prior art, the present invention has the following advantages:
[0019] (1) The high-efficiency haloxyfop-butyl and glufosinate microemulsion adjuvant provided by the present invention can well emulsify the high-efficiency haloxyfop-butyl and solubilize it into glufosinate, and can achieve the goal of not precipitating at low temperatures and not turning white at high temperatures, thereby significantly improving the high and low temperature storage stability of the high-efficiency haloxyfop-butyl and glufosinate microemulsion.
[0020] (2) The results of the heat storage stability test show that the high-efficiency haloxyfop-butyl and glufosinate microemulsions using the microemulsion adjuvant of the present invention have good heat storage stability, and the decomposition rate of high-efficiency haloxyfop-butyl in the microemulsion is very low.
[0021] (3) The results of the efficacy experiment show that the application of the microemulsion adjuvant with a specific composition of the present invention in the high-efficiency halpyr-methyl and glufosinate microemulsions can also improve the efficacy. DETAILED DESCRIPTION
[0022] The present invention is further illustrated below through the description of specific implementation modes, but this is not a limitation of the present invention. Those skilled in the art can make various modifications or improvements based on the basic idea of the present invention, but as long as they do not deviate from the basic idea of the present invention, they are all within the scope of the present invention.
[0023] The raw materials used in the present invention are all commercially available unless otherwise specified. For example, coconut oil diethanolamide is coconut oil diethanolamide 6501, which can be purchased from Guangzhou Yeshi Chemical Co., Ltd.; fatty alcohol polyoxyethylene ether sodium sulfate (AES) can be purchased from Zanyu Technology Group Co., Ltd.; amine ether is fatty amine polyoxyethylene ether, specification AC-1205, which can be purchased from Jiangsu Haian Petrochemical Plant.
[0024] Example 1: A highly effective haloxyfop-butyl and glufosinate microemulsion adjuvant
[0025] The high-efficiency flupyrazole and glufosinate microemulsion adjuvant comprises the following raw materials and their weight proportions: 10 parts of coconut acid diethanolamide, 8 parts of trihydroxyethylamine, 50 parts of isomeric alcohol ether sodium sulfate, 5 parts of fatty alcohol polyoxyethylene ether sodium sulfate, 8 parts of amine ether, 7 parts of citric acid, and 12 parts of water; the isomeric alcohol ether sodium sulfate is composed of isomeric tridecanol polyoxyethylene ether sodium sulfate and isomeric decanol polyoxyethylene ether sodium sulfate in a weight ratio of 1:5.
[0026] The preparation method of the high-efficiency haloxyfop-methyl and glufosinate-ammonium microemulsion adjuvant comprises the following steps:
[0027] Mix sodium fatty alcohol polyoxyethylene ether sulfate and trihydroxyethylamine, stir evenly, then add coconut acid diethanolamide and stir evenly, add sodium isomeric alcohol ether sulfate, amine ether and water and stir evenly, finally add citric acid, adjust the pH, and stir until completely transparent and uniform.
[0028] Example 2: A highly effective haloxyfop-butyl and glufosinate microemulsion adjuvant
[0029] The high-efficiency flupyrazole and glufosinate microemulsion adjuvant comprises the following raw materials and their weight proportions: 10 parts of coconut acid diethanolamide, 5 parts of trihydroxyethylamine, 40 parts of isomeric alcohol ether sodium sulfate, 8 parts of fatty alcohol polyoxyethylene ether sodium sulfate, 10 parts of amine ether, 5 parts of citric acid, and 22 parts of water; the isomeric alcohol ether sodium sulfate is composed of isomeric tridecanol polyoxyethylene ether sodium sulfate and isomeric decanol polyoxyethylene ether sodium sulfate in a weight ratio of 1:4.
[0030] The preparation method of the highly effective haloxyfop-butyl and glufosinate-ammonium microemulsion adjuvant is similar to that in Example 1.
[0031] Example 3: A highly effective haloxyfop-butyl and glufosinate microemulsion adjuvant
[0032] The high-efficiency flupyrazole and glufosinate microemulsion adjuvant comprises the following raw materials and their weight proportions: 15 parts of coconut acid diethanolamide, 10 parts of trihydroxyethylamine, 50 parts of isomeric alcohol ether sodium sulfate, 5 parts of fatty alcohol polyoxyethylene ether sodium sulfate, 5 parts of amine ether, 5 parts of citric acid, and 10 parts of water; the isomeric alcohol ether sodium sulfate is composed of isomeric tridecanol polyoxyethylene ether sodium sulfate and isomeric decanol polyoxyethylene ether sodium sulfate in a weight ratio of 1:6.
[0033] The preparation method of the highly effective haloxyfop-butyl and glufosinate-ammonium microemulsion adjuvant is similar to that in Example 1.
[0034] Example 4: A highly effective haloxyfop-butyl and glufosinate microemulsion
[0035] The high-efficiency haloxyfop-methyl and glufosinate microemulsion comprises the following raw materials and their mass percentages: 3% of high-efficiency haloxyfop-methyl, 19% of glufosinate ammonium, 8% of xylene, 3% of the high-efficiency haloxyfop-methyl and glufosinate microemulsion adjuvant prepared in Example 1, and 67% of water.
[0036] The preparation method of the high-efficiency haloxyfop-methyl and glufosinate-ammonium microemulsion is:
[0037] Mix high-efficiency haloxyfop-butyl and xylene, stir until completely dissolved, then add high-efficiency haloxyfop-butyl and glufosinate microemulsion adjuvant, water and glufosinate ammonium and stir for 30 minutes until completely transparent.
[0038] Example 5: A highly effective haloxyfop-butyl and glufosinate microemulsion
[0039] The high-efficiency haloxyfop-methyl and glufosinate microemulsion comprises the following raw materials and their mass percentages: 3% of high-efficiency haloxyfop-methyl, 19% of glufosinate, 8% of xylene, 3% of the high-efficiency haloxyfop-methyl and glufosinate microemulsion adjuvant prepared in Example 2, and 67% of water.
[0040] The preparation method of the high-efficiency fluazifop-ethyl and glufosinate-ammonium microemulsion is similar to that of Example 4.
[0041] Example 6: A highly effective haloxyfop-butyl and glufosinate microemulsion
[0042] The high-efficiency haloxyfop-methyl and glufosinate microemulsion comprises the following raw materials and their mass percentages: 3% of high-efficiency haloxyfop-methyl, 19% of glufosinate ammonium, 8% of xylene, 3% of the high-efficiency haloxyfop-methyl and glufosinate microemulsion adjuvant prepared in Example 3, and 67% of water.
[0043] The preparation method of the high-efficiency fluazifop-ethyl and glufosinate-ammonium microemulsion is similar to that of Example 4.
[0044] Comparative Example 1: A highly effective haloxyfop-butyl and glufosinate microemulsion adjuvant
[0045] The high-efficiency flupyrazole and glufosinate microemulsion adjuvant comprises the following raw materials and their weight proportions: 10 parts of coconut acid diethanolamide, 8 parts of trihydroxyethylamine, 50 parts of isomeric alcohol ether sodium sulfate, 5 parts of fatty alcohol polyoxyethylene ether sodium sulfate, 8 parts of amine ether, 7 parts of citric acid, and 12 parts of water; the isomeric alcohol ether sodium sulfate is composed of isomeric tridecanol polyoxyethylene ether sodium sulfate and isomeric decanol polyoxyethylene ether sodium sulfate in a weight ratio of 5:1.
[0046] The preparation method of the highly effective haloxyfop-butyl and glufosinate-ammonium microemulsion adjuvant is similar to that in Example 1.
[0047] The difference from Example 1 is that the isomeric alcohol ether sodium sulfate is composed of isomeric tridecanol polyoxyethylene ether sodium sulfate and isomeric decanol polyoxyethylene ether sodium sulfate in a mass ratio of 5:1.
[0048] Comparative Example 2: A highly effective haloxyfop-butyl and glufosinate microemulsion adjuvant
[0049] The high-efficiency flupyrazole and glufosinate microemulsion adjuvant comprises the following raw materials and their weight proportions: 10 parts of coconut acid diethanolamide, 8 parts of trihydroxyethylamine, 50 parts of isomeric alcohol ether sodium sulfate, 5 parts of fatty alcohol polyoxyethylene ether sodium sulfate, 8 parts of amine ether, 7 parts of citric acid, and 12 parts of water; the isomeric alcohol ether sodium sulfate is isomeric decanol polyoxyethylene ether sodium sulfate.
[0050] The preparation method of the highly effective haloxyfop-butyl and glufosinate-ammonium microemulsion adjuvant is similar to that in Example 1.
[0051] The difference from Example 1 is that the isomeric alcohol ether sodium sulfate is isomeric deca-alcohol polyoxyethylene ether sodium sulfate. Comparative Example 3: A highly effective halpyrazole and glufosinate microemulsion adjuvant
[0052] The high-efficiency flupyrazole and glufosinate microemulsion adjuvant includes the following raw materials and their mass fractions: 10 parts of tristyrylphenol polyoxyethylene ether (Nongru 600), 8 parts of trihydroxyethylamine, 50 parts of isomeric alcohol ether sodium sulfate, 5 parts of fatty alcohol polyoxyethylene ether sodium sulfate, 8 parts of amine ether, 7 parts of citric acid, and 12 parts of water; the isomeric alcohol ether sodium sulfate is composed of isomeric tridecanol polyoxyethylene ether sodium sulfate and isomeric decanol polyoxyethylene ether sodium sulfate in a mass ratio of 1:5.
[0053] The preparation method of the highly effective haloxyfop-butyl and glufosinate-ammonium microemulsion adjuvant is similar to that in Example 1.
[0054] The difference from Example 1 is that coconut oil diethanolamide is replaced by tristyrylphenol polyoxyethylene ether (Nongru 600).
[0055] Comparative Example 4: A highly effective haloxyfop-butyl and glufosinate microemulsion
[0056] The high-efficiency haloxyfop-methyl and glufosinate microemulsion comprises the following raw materials and their mass percentages: 3% of high-efficiency haloxyfop-methyl, 19% of glufosinate ammonium, 8% of xylene, 3% of the high-efficiency haloxyfop-methyl and glufosinate microemulsion adjuvant prepared in comparative example 1, and 67% of water.
[0057] The preparation method of the high-efficiency fluazifop-ethyl and glufosinate-ammonium microemulsion is similar to that of Example 4.
[0058] Comparative Example 5: A highly effective haloxyfop-butyl and glufosinate microemulsion
[0059] The high-efficiency haloxyfop-methyl and glufosinate microemulsion comprises the following raw materials and their mass percentages: 3% of high-efficiency haloxyfop-methyl, 19% of glufosinate ammonium, 8% of xylene, 3% of the high-efficiency haloxyfop-methyl and glufosinate microemulsion adjuvant prepared in comparative example 2, and 67% of water.
[0060] The preparation method of the high-efficiency fluazifop-ethyl and glufosinate-ammonium microemulsion is similar to that of Example 4.
[0061] Comparative Example 6: A highly effective haloxyfop-butyl and glufosinate microemulsion
[0062] The high-efficiency haloxyfop-methyl and glufosinate microemulsion comprises the following raw materials and their mass percentages: 3% of high-efficiency haloxyfop-methyl, 19% of glufosinate ammonium, 8% of xylene, 3% of the high-efficiency haloxyfop-methyl and glufosinate microemulsion adjuvant prepared in comparative example 3, and 67% of water.
[0063] The preparation method of the high-efficiency fluazifop-ethyl and glufosinate-ammonium microemulsion is similar to that of Example 4.
[0064] Test Example 1: Stability Test
[0065] 1.1. Test samples: microemulsions obtained in Example 4, Example 5, Example 6, Comparative Example 4, Comparative Example 5, and Comparative Example 6.
[0066] 1.2 Test methods:
[0067] 1.2.1 Cold storage stability test:
[0068] 100 mL of the microemulsions obtained in Example 4, Example 5, Example 6, and Comparative Example 6 were respectively transferred into centrifuge tubes and stored at -5°C for 7 days. After 7 days, the centrifuge tubes were taken out and allowed to stand at room temperature for a period of time to observe whether the microemulsions had precipitation and crystallization, and whether there was stratification. The microemulsions were allowed to stand at room temperature for 3 hours, and centrifuged for 15 minutes, and the volume of the precipitate at the bottom of the tube was recorded.
[0069] 1.2.2. Hot storage stability test:
[0070] 30 mL of the microemulsion obtained in Example 4, Example 5, Example 6, Comparative Example 4, and Comparative Example 5 were respectively placed in an ampoule, sealed, and the sealed ampoule was placed in a metal container, and the metal container was kept at a constant temperature of 54° C. for 14 days, then taken out and observed for turbidity and stratification. The content of high-efficiency halpyrazole in the test samples before and after the heat storage stability test was determined by high performance liquid chromatography.
[0071] 1.3. Test results: The cold storage stability test results are shown in Table 1, and the hot storage stability test results are shown in Table 2.
[0072] Table 1: Cold storage stability test results
[0073]
[0074] As can be seen from Table 1, after the cold storage stability test, the high-efficiency halpyrazole and glufosinate microemulsions obtained in Examples 4-6 of the present invention can still remain clear and transparent, without precipitation, crystallization, stratification, and separation, while the high-efficiency halpyrazole and glufosinate microemulsions obtained in Comparative Example 6 have crystallization after the cold storage stability test, and the volume of the separation is as high as 0.2 mL. It can be seen that the high-efficiency halpyrazole and glufosinate microemulsions obtained in the present invention have good cold storage stability, and are not easy to precipitate or crystallize at low temperature cold storage.
[0075] Table 2: Hot storage stability test results
[0076]
[0077] As can be seen from Table 2, after the heat storage stability test, the high-efficiency halpyrazole and glufosinate microemulsions obtained in Examples 4-6 of the present invention can still remain clear and transparent, without turbidity or stratification, and the decomposition rate is as low as 0.432%, while the high-efficiency halpyrazole and glufosinate microemulsions obtained in Comparative Examples 4 and 5 become turbid after the heat storage stability test, and the decomposition rates of high-efficiency halpyrazole in the test samples are 1.196% and 1.639%, respectively. It can be seen that the high-efficiency halpyrazole and glufosinate microemulsions obtained in the present invention have good heat storage stability, are not easy to become turbid, and the high-efficiency halpyrazole decomposition rate in the microemulsion is low.
[0078] Test Example 2: Efficacy Test
[0079] 2.1. Test samples: microemulsions obtained in Example 4, Comparative Example 4, Comparative Example 5 and Comparative Example 6.
[0080] 2.2 Biological target: Eleutherodactylus truncatula
[0081] 2.3 Test methods:
[0082] Select several plastic pots with a diameter of 25 cm, add moist sterilized soil, the organic matter content in the soil is 160%, and the pH value is 6.7. Use the bottom infiltration irrigation method to make the soil completely moist, take mature and full goosegrass seeds, evenly sow the goosegrass seeds on the soil surface, cover with 1 cm of soil, and move into the greenhouse for conventional cultivation after sowing. The culture conditions are: temperature is 25℃, relative humidity is 60%-80%, light: dark is 14h:10h, intensity is 2000Lux, and water is replenished by bottom infiltration irrigation of pots. Thinning is carried out at the 1-2 leaf stage, and the seedlings are determined when the goosegrass is in the 3-4 leaf stage. The seedlings with relatively consistent growth size and density are retained, and 15 plants are left in each pot. The pesticide spray treatment is carried out at the 6-7 leaf stage, and each treatment is repeated 4 times, and spraying water is set as a blank control. 21 days after treatment, the aboveground weeds are harvested and weighed. Control effect (%) = (fresh weight of control weeds - fresh weight of treated weeds) / fresh weight of control weeds × 100.
[0083] 2.4. The test results are shown in Table 3.
[0084] Table 3: Control effect of microemulsion on goosegrass
[0085] Group Control effect (%) Example 4 94.5 Comparative Example 4 88.2 Comparative Example 5 86.7 Comparative Example 6 85.9
[0086] As can be seen from Table 3, the control effect of the high-efficiency halpyr-methyl and glufosinate microemulsion obtained in Example 4 of the present invention on goosegrass is as high as 94.5%, while the control effects of the high-efficiency halpyr-methyl and glufosinate microemulsions obtained in Comparative Examples 4, 5 and 6 on goosegrass are only 88.2%, 86.7% and 85.9%, respectively. It can be seen that the application of the microemulsion adjuvant of the specific composition of the present invention to the high-efficiency halpyr-methyl and glufosinate microemulsion can improve the efficacy.
[0087] Those skilled in the art should understand that the above embodiments are merely illustrative of the principles and effects of the present invention, and are not intended to limit the present invention. Anyone familiar with the technology may modify or change the above embodiments without violating the spirit and scope of the present invention. Therefore, all equivalent modifications or changes made by those with ordinary knowledge in the art without departing from the spirit and technical ideas disclosed by the present invention should still be covered by the claims of the present invention.
Claims
1. A highly effective haloxyfop-butyl and glufosinate microemulsion adjuvant, characterized in that: The invention comprises the following raw materials and their weight proportions: 10-15 parts of coconut oil diethanolamide, 5-10 parts of trihydroxyethylamine, 40-50 parts of sodium isomeric alcohol ether sulfate, 5-8 parts of sodium fatty alcohol polyoxyethylene ether sulfate, 5-10 parts of amine ether, 5-7 parts of citric acid and 10-22 parts of water; The isomeric alcohol ether sodium sulfate is composed of isomeric tridecanol polyoxyethylene ether sodium sulfate and isomeric decanol polyoxyethylene ether sodium sulfate in a mass ratio of 1:
5.
2. The high-efficiency haloxyfop-butyl and glufosinate-ammonium microemulsion adjuvant according to claim 1, characterized in that: The invention comprises the following raw materials and their weight proportions: 10 parts of coconut oil diethanolamide, 8 parts of trihydroxyethylamine, 50 parts of isomeric alcohol ether sodium sulfate, 5 parts of fatty alcohol polyoxyethylene ether sodium sulfate, 8 parts of amine ether, 7 parts of citric acid and 12 parts of water.
3. The method for preparing the high-efficiency haloxyfop-butyl and glufosinate-ammonium microemulsion adjuvant according to claim 1 or 2, characterized in that: The following steps are involved: Mix sodium fatty alcohol polyoxyethylene ether sulfate and trihydroxyethylamine, stir evenly, then add coconut acid diethanolamide and stir evenly, add sodium isomeric alcohol ether sulfate, amine ether and water and stir evenly, finally add citric acid, adjust the pH, and stir until completely transparent and uniform.
4. Use of the high-efficiency haloxyfop-butyl and glufosinate-ammonium microemulsion adjuvant as claimed in claim 1 or 2 in the preparation of high-efficiency haloxyfop-butyl and glufosinate-ammonium microemulsion.
5. A highly effective haloxyfop-butyl and glufosinate-ammonium microemulsion, characterized in that: The invention comprises the following raw materials and their mass percentages: 3% of high-efficiency haloxyfop-methyl, 19% of glufosinate-ammonium, 8% of xylene, 3% of the high-efficiency haloxyfop-methyl and glufosinate-ammonium microemulsion adjuvant according to claim 1 or 2, and 67% of water.
6. The method for preparing the high-efficiency haloxyfop-ethyl and glufosinate-ammonium microemulsion according to claim 5, characterized in that: The steps are as follows: High-efficiency haloxyfop-methyl and xylene are mixed, stirred until completely dissolved, and then the high-efficiency haloxyfop-methyl and glufosinate microemulsion adjuvant, water and glufosinate are added and stirred for 30 minutes until completely transparent.
Citation Information
Patent Citations
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