Fine glufosinate soluble concentrate and preparation method thereof

By adding Synergen ME adjuvant and isomeric C13 fatty alcohol polyoxyethylene ether MULTISO 13-100 to glufosinate soluble concentrate, and combining the electrostatic repulsion between fatty alcohol polyoxyethylene ether phosphate monoester and carrageenan, the storage stability problem of glufosinate soluble concentrate was solved, resulting in higher efficacy and application effectiveness.

CN121730318APending Publication Date: 2026-03-27QIAOCHANG MODERN AGRI CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-12-05
Publication Date
2026-03-27

AI Technical Summary

Technical Problem

Existing glufosinate-ammonium soluble concentrates are prone to decomposition, precipitation, or crystallization during storage, posing issues with thermal and cold storage stability.

Method used

A stable soluble agent was prepared by combining glufosinate-ammonium, synergist Synergen ME, compound fatty alcohol polyoxyethylene ether phosphate monoester solution, fatty alcohol polyoxyethylene ether, and organosilicon defoamer, by adjusting the pH value and stirring. The synergistic effect of synergist and surfactant is used to improve wettability and permeability, and the electrostatic repulsion between fatty alcohol polyoxyethylene ether phosphate monoester and carrageenan prevents the components from agglomerating or precipitating.

Benefits of technology

It significantly improved the storage stability of glufosinate-ammonium soluble concentrate, enhanced efficacy and application effectiveness, and reduced losses during storage.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a refined glufosinate soluble concentrate and a preparation method thereof, and mainly relates to the technical field of herbicides. The refined glufosinate-ammonium soluble concentrate comprises refined glufosinate-ammonium, a synergist, a compound fatty alcohol-polyoxyethylene ether phosphate monoester solution, fatty alcohol-polyoxyethylene ether, an organic silicon defoaming agent and water, the synergist is a SynergenME auxiliary agent in SynergenTM series products researched and developed by Clarian Company, and it is found that the synergist is also helpful for improving the drug effect of the crude drug of the refined glufosinate-ammonium soluble concentrate. Compared with the prior art, the refined glufosinate-ammonium soluble concentrate prepared by the invention has better dispersity and storage stability, other components in the soluble concentrate are prevented from being agglomerated or precipitated in the storage process, and a uniform dispersion state is kept, so that the storage stability of the whole system of the soluble concentrate is improved; and the pesticide effect of the refined glufosinate-ammonium soluble concentrate can be improved and prolonged in practical application.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of herbicides, in particular to a glufosinate-ammonium soluble liquid and a preparation method thereof. BACKGROUND

[0002] Glufosinate-ammonium is a racemic mixture, which has two enantiomers, L-glufosinate-ammonium and D-glufosinate-ammonium. Glufosinate-ammonium is an L-configuration isomer of glufosinate-ammonium, which is a highly efficient, low-toxicity and safe herbicide. Glufosinate-ammonium has extremely strong herbicidal activity. Compared with glufosinate-ammonium, the application amount per mu of glufosinate-ammonium is only half of that of glufosinate-ammonium, which can greatly reduce the amount of raw materials, improve the economy of the product, effectively reduce the cost of use, and reduce the impact on the environment. Glufosinate-ammonium has good water solubility and structural stability, which is convenient for processing and mixing use. Common dosage forms include water-soluble agents, soluble liquids, emulsions, emulsifiable concentrates, granules, oils and powders.

[0003] The main component of glufosinate-ammonium soluble liquid is glufosinate-ammonium, and the dosage form is soluble liquid. When the glufosinate-ammonium soluble liquid sprays and contacts the surface of weeds, it is conducted inside the leaves of the contacted weeds through the transpiration of plants, and then transferred to other organs and tissues in the body of the weeds by the flow of internal water, so that the weeds cannot normally obtain the required nutrients, resulting in plant death, thereby achieving the effect of weeding. Glufosinate-ammonium soluble liquid is more convenient to use in practical application, which can be directly sprayed on the crops that need to be controlled without the need for secondary dilution or mixing. The drug dosage is less and the drug efficacy is higher. It is easier to store and transport, reducing the cost of packaging and transportation. However, glufosinate-ammonium soluble liquid is easily affected by factors such as temperature, light and humidity, which can cause decomposition, precipitation or crystallization during storage. Therefore, the storage stability needs to be concerned.

[0004] CN114176080A discloses a herbicidal pesticide composition containing triacontanol, wherein the effective components of the herbicidal pesticide composition are compounded by triacontanol and glufosinate-ammonium or glufosinate-ammonium. When triacontanol and glufosinate-ammonium or glufosinate-ammonium are compounded, the mixture shows obvious prevention and control effect on weeds, indicating that triacontanol can enhance the prevention and control effect of glufosinate-ammonium or glufosinate-ammonium on weeds, reduce the application amount of glufosinate-ammonium or glufosinate-ammonium, and reduce the pollution to the environment. Triacontanol is a colorless, odorless, nontoxic and environmentally friendly surfactant. When it is compounded with glufosinate-ammonium or glufosinate-ammonium, the prevention and control effect on weeds can be improved. However, the problem of decomposition, precipitation or crystallization during storage after being made into a soluble liquid has not been solved.

[0005] CN116686825A discloses a quick-acting type of phosphoramidon soluble solution and a preparation method thereof. The quick-acting type of phosphoramidon soluble solution prepared in the invention comprises brassinolide, antibacterial phosphoramidon, florasulam and an auxiliary agent. The antibacterial phosphoramidon is prepared by hydrolysis of antibacterial factors and calcium hydroxide under the catalysis of a chiral catalyst. The antibacterial factors are prepared by complexing ethylenediamine derivatives with potassium ions and then introducing hydroxyl groups. The ethylenediamine derivatives are prepared by connecting 5,5-dimethylhydantoin with formaldehyde. The potassium ions are coordinated, and then hydroxyl groups are introduced to form antibacterial factors with crystal structure, which can not only enhance the antibacterial property and the herbicidal effect, but also enhance the storage stability of the soluble solution. The brassinolide, antibacterial phosphoramidon, florasulam and auxiliary agent are combined, and the florasulam is uniformly dispersed in the soluble solution to further enhance the herbicidal efficiency. The florasulam is uniformly dispersed in the phosphoramidon soluble solution in the invention, which may enhance the storage stability of the soluble solution. However, the storage stability of the phosphoramidon or the phosphoramidon composition in the form of a soluble solution has not been verified by test examples, and the problems of the thermal storage stability and the cold and hot storage stability have not been solved simultaneously. SUMMARY

[0006] In view of the above-mentioned defects of the prior art, the technical problem to be solved by the present application is to improve the thermal storage stability and the cold storage stability of the phosphoramidon soluble solution.

[0007] To achieve the above-mentioned purpose, the present application provides a phosphoramidon soluble solution and a preparation method thereof. The phosphoramidon soluble solution comprises the following components: phosphoramidon, a synergist, a composite fatty alcohol polyoxyethylene ether phosphate monoester solution, a fatty alcohol polyoxyethylene ether, a silicone defoaming agent, water.

[0008] Specifically, the 10wt% phosphoramidon soluble solution comprises the following components by mass fraction: phosphoramidon 10wt%, a synergist 4-6wt%, a composite fatty alcohol polyoxyethylene ether phosphate monoester solution 40-70wt%, a fatty alcohol polyoxyethylene ether 4-8wt%, a silicone defoaming agent 0.05-0.5wt%, water to make up 100wt%.

[0009] Preferably, the 10wt% phosphoramidon soluble solution comprises the following components by mass fraction: phosphoramidon 10wt%, a synergist 5-6wt%, 50-70 wt% of compound fatty alcohol polyoxyethylene ether phosphate monoester solution Fatty alcohol polyoxyethylene ether 7-8 wt% Organosilicon defoamer 0.1-0.3wt% Add water to make up to 100 wt%.

[0010] The synergist is Synergen ME adjuvant; the Synergen ME adjuvant is Synergen from Clariant. TM Synergen ME products are part of a series of adjuvants.

[0011] The fatty alcohol polyoxyethylene ether is an isomeric C13 fatty alcohol polyoxyethylene ether; preferably, it is the isomeric C13 fatty alcohol polyoxyethylene ether MULTISO 13-100 product from Sasol's MULTISO series.

[0012] The silicone defoamer is SAG 1572 defoamer.

[0013] Specifically, the preparation method of the glufosinate-ammonium soluble concentrate is as follows: Weigh out glufosinate, synergist, fatty alcohol polyoxyethylene ether, and organosilicon defoamer and add them to the composite fatty alcohol polyoxyethylene ether phosphate monoester solution. Stir at room temperature for 10-30 minutes, add 10-20wt% hydrochloric acid to adjust the pH to 4.0-8.0, add water to make up to 100%, and continue stirring for 10-20 minutes until clear and transparent. After testing and filling, the glufosinate ammonium salt soluble concentrate is obtained.

[0014] The preparation method of the composite fatty alcohol polyoxyethylene ether phosphate monoester solution is as follows, in parts by weight: Add 0.2-0.4 parts of hydroxymethyl cellulose to 40-50 parts of water and stir at room temperature for 10-20 minutes. Add 5-6 parts of fatty alcohol polyoxyethylene ether phosphate monoester and stir at 10000-12000 r / min for 10-30 minutes to obtain a dispersion. Add 1-2 parts of carrageenan to 10-20 parts of water, heat to 60-80℃ and stir for 1-2 hours until completely dissolved to obtain a carrageenan aqueous solution. Then add the carrageenan aqueous solution to the dispersion and stir at room temperature for 0.5-1 hour to obtain the composite fatty alcohol polyoxyethylene ether phosphate monoester solution.

[0015] The testing standards are as follows: glufosinate mass fraction of 10±1.0wt%, glufosinate ammonium salt mass fraction of 10.9±1.0wt%, ammonium ion mass fraction ≥0.9wt%, L-enantiomer ratio ≥96%, pH range of 4.0-8.0, qualified dilution stability (20 times), persistent foaming property (foam volume after 1 minute) ≤60, and appearance meeting the requirements.

[0016] SynergenME, developed by Clariant, is part of the Synergen™ series. It is safe and biodegradable, containing various surfactants that provide optimal retention and coverage on leaves. The added ingredients cause leaf texture swelling, allowing for effective penetration of glufosinate-ammonium technical. When added to the glufosinate-ammonium soluble concentrate of this invention and applied to weeds, it ensures more complete wetting and facilitates easier penetration of the active ingredient into the weed plant, fully utilizing the potential of the active substance and minimizing wind-induced droplet drift, thus reducing losses and ultimately improving the efficacy and application effectiveness of the glufosinate-ammonium soluble concentrate. The fatty alcohol polyoxyethylene ether is selected from Sasol's MULTISO series, specifically the isomeric C13 fatty alcohol polyoxyethylene ether MULTISO13-100 product. This nonionic surfactant possesses excellent surface activity, reducing the surface tension of the liquid, making it easier to spread and wet the weed plant surface, and prolonging the efficacy. In the practical application of glufosinate-ammonium soluble concentrate, it can improve wetting and penetration.

[0017] Fatty alcohol polyoxyethylene ether phosphate monoester is a novel surfactant with both nonionic and anionic properties. It also exhibits good thermal stability, good stability in acidic, alkaline, and electrolyte environments, and is not prone to stratification or precipitation. Furthermore, it demonstrates high compatibility and synergistic effects with various surfactants. Carrageenan, an charged polysaccharide extracted from red algae, possesses excellent stability and heat resistance. When dissolved in hot water, it forms a cross-linked network through intermolecular forces, suspending itself in the system. It forms an electrostatic repulsion with fatty alcohol polyoxyethylene ether phosphate monoester, resulting in a composite coexisting solution. This composite fatty alcohol polyoxyethylene ether phosphate monoester solution is then used to prepare glufosinate-ammonium soluble concentrate. Utilizing its repulsion, it prevents the aggregation or precipitation of other components in the soluble concentrate during storage, maintaining a uniform dispersion state and thus improving the overall storage stability of the soluble concentrate system.

[0018] The beneficial effects of this invention are: 1. Compared with the prior art, the glufosinate soluble agent of the present invention incorporates a special synergist, SynergenME, which is a product of the Synergen™ series developed by Clariant. It has been found that this synergist also helps to improve the efficacy of the glufosinate soluble agent. Furthermore, the combined effect of various surfactants contained in SynergenME can provide optimal retention and coverage on the leaves. The added ingredients cause the leaf surface texture to swell, allowing the glufosinate technical grade to effectively penetrate into the weed plants, fully utilize the potential of the active substances, and ultimately improve the efficacy and application effectiveness of the glufosinate soluble agent. 2. Compared with the prior art, the glufosinate soluble agent of the present invention contains a fatty alcohol polyoxyethylene ether, which is the isomer C13 fatty alcohol polyoxyethylene ether MULTISO13-100 product of Sasol's MULTISO series. It is a nonionic surfactant with good surface activity. By reducing the surface tension of the liquid, it makes the liquid easier to spread and wet the surface of weed plants and prolongs the efficacy. In the practical application of glufosinate soluble agent, it can play a role in improving wettability and penetration. 3. Compared with the prior art, the styrax ammonium phosphate soluble agent of the present invention combines fatty alcohol polyoxyethylene ether phosphate monoester with natural polysaccharide carrageenan. By utilizing the respective properties of the two and the effect of electrostatic repulsion, a composite solution with high dispersibility, good thermal stability, and good stability in acid, alkali and electrolyte environments is prepared. This prevents other components in the soluble agent from agglomerating or precipitating during storage, maintaining a uniform dispersion state, thereby improving the storage stability of the entire soluble agent system. Detailed Implementation

[0019] The parameters of the specific chemical substances used in the examples are from the following sources: Glufosinate: purity 97wt%, manufacturer is Wuhan Pushida Biotechnology Co., Ltd., product number 20221205.

[0020] Carrageenan: purity 99wt%, manufacturer: Shandong Fengtai Biotechnology Co., Ltd., model: FT11.

[0021] Synergen ME adjuvant is from Clariant's Synergen. TM A series of additives, model number Synergen ME.

[0022] The isomeric C13 fatty alcohol polyoxyethylene ether MULTISO 13-100 is from Sasol's MULTISO series products, model number MULTISO 13-100.

[0023] Fatty alcohol polyoxyethylene ether phosphate monoester: Brand: Chenrun Chemical, Model: ODP.

[0024] SAG 1572 defoamer: Brand is Momentive Advanced Materials Inc., USA, model is SAG 1572.

[0025] Example 1 A method for preparing a 10wt% glufosinate-ammonium soluble concentrate is as follows: Weigh 100g glufosinate, 60g Synergen ME adjuvant, 80g isomeric C13 fatty alcohol polyoxyethylene ether MULTISO 13-100, and 2g SAG 1572 defoamer and add them to 700g of water. Stir at room temperature for 30 minutes, add 10wt% hydrochloric acid to adjust the pH to 7.5, add water to make up to 1000g, and continue stirring for 15 minutes until clear and transparent. After testing and filling, the soluble form of glufosinate ammonium salt is obtained.

[0026] The testing standards are as follows: glufosinate mass fraction of 10wt%, glufosinate ammonium salt mass fraction of 10.9wt%, ammonium ion mass fraction ≥0.9wt%, L-enantiomer ratio ≥96%, pH of 7.5, qualified dilution stability (20 times), persistent foaming property (foam amount after 1 minute) ≤60, and appearance meeting the requirements.

[0027] Example 2 A method for preparing a 10wt% glufosinate-ammonium soluble concentrate is as follows: 60g of fatty alcohol polyoxyethylene ether phosphate monoester was added to 650g of water and stirred at 10000r / min for 20 minutes to obtain a dispersion, which is the fatty alcohol polyoxyethylene ether phosphate monoester solution. 100g of glufosinate, 60g of Synergen ME adjuvant, and 2g of SAG 1572 defoamer were weighed and added to 700g of fatty alcohol polyoxyethylene ether phosphate monoester solution. The mixture was stirred at room temperature for 30 minutes, and 10wt% hydrochloric acid was added to adjust the pH to 7.5. Water was added to make up to 1000g, and stirring was continued for 15 minutes until clear and transparent. After testing and filling, the glufosinate ammonium salt soluble concentrate was obtained.

[0028] The testing standards are as follows: glufosinate mass fraction of 10wt%, glufosinate ammonium salt mass fraction of 10.9wt%, ammonium ion mass fraction ≥0.9wt%, L-enantiomer ratio ≥96%, pH of 7.5, qualified dilution stability (20 times), persistent foaming property (foam amount after 1 minute) ≤60, and appearance meeting the requirements.

[0029] Example 3 A method for preparing a 10wt% glufosinate-ammonium soluble concentrate is as follows: Add 60g of fatty alcohol polyoxyethylene ether phosphate monoester to 650g of water and stir at 10000r / min for 20 minutes to obtain a dispersion, which is the fatty alcohol polyoxyethylene ether phosphate monoester solution. Weigh 100g of glufosinate, 60g of Synergen ME adjuvant, 80g of isomeric C13 fatty alcohol polyoxyethylene ether MULTISO 13-100, and 2g of SAG 1572 defoamer and add them to 700g of fatty alcohol polyoxyethylene ether phosphate monoester solution. Stir at room temperature for 30 minutes, add 10wt% hydrochloric acid to adjust the pH to 7.5, add water to make up to 1000g, and continue stirring for 15 minutes until clear and transparent. After testing and filling, the glufosinate ammonium salt soluble concentrate is obtained.

[0030] The testing standards are as follows: glufosinate mass fraction of 10wt%, glufosinate ammonium salt mass fraction of 10.9wt%, ammonium ion mass fraction ≥0.9wt%, L-enantiomer ratio ≥96%, pH of 7.5, qualified dilution stability (20 times), persistent foaming property (foam amount after 1 minute) ≤60, and appearance meeting the requirements.

[0031] Example 4 A method for preparing a 10wt% glufosinate-ammonium soluble concentrate is as follows: Weigh 100g of glufosinate, 60g of Synergen ME adjuvant, 80g of isomeric C13 fatty alcohol polyoxyethylene ether MULTISO 13-100, and 2g of SAG 1572 defoamer, and add them to 700g of composite fatty alcohol polyoxyethylene ether phosphate monoester solution. Stir at room temperature for 30 minutes, add 10wt% hydrochloric acid to adjust the pH to 7.5, add water to make up to 1000g, and continue stirring for 15 minutes until clear and transparent. After testing and filling, the glufosinate ammonium salt soluble concentrate is obtained.

[0032] The testing standards are as follows: glufosinate mass fraction of 10wt%, glufosinate ammonium salt mass fraction of 10.9wt%, ammonium ion mass fraction ≥0.9wt%, L-enantiomer ratio ≥96%, pH of 7.5, qualified dilution stability (20 times), persistent foaming property (foam amount after 1 minute) ≤60, and appearance meeting the requirements.

[0033] The preparation method of the composite fatty alcohol polyoxyethylene ether phosphate monoester solution is as follows: Add 4g of hydroxymethyl cellulose to 500g of water and stir at room temperature for 20 minutes. Add 60g of fatty alcohol polyoxyethylene ether phosphate monoester and stir at 10000r / min for 20 minutes to obtain a dispersion. Add 20g of carrageenan to 150g of water, heat to 80℃ and stir for 1 hour until completely dissolved to obtain a carrageenan aqueous solution. Then add the carrageenan aqueous solution to the dispersion and stir at room temperature for 1 hour to obtain the composite fatty alcohol polyoxyethylene ether phosphate monoester solution.

[0034] Example 5 A method for preparing a 10wt% glufosinate-ammonium soluble concentrate is as follows: Weigh 100g of glufosinate, 80g of isomeric C13 fatty alcohol polyoxyethylene ether MULTISO 13-100, and 2g of SAG 1572 defoamer and add them to 700g of composite fatty alcohol polyoxyethylene ether phosphate monoester solution. Stir at room temperature for 30 minutes, add 10wt% hydrochloric acid to adjust the pH to 7.5, add water to make up to 1000g, and continue stirring for 15 minutes until clear and transparent. After testing and filling, the glufosinate ammonium salt soluble concentrate is obtained.

[0035] The testing standards are as follows: glufosinate mass fraction of 10wt%, glufosinate ammonium salt mass fraction of 10.9wt%, ammonium ion mass fraction ≥0.9wt%, L-enantiomer ratio ≥96%, pH of 7.5, qualified dilution stability (20 times), persistent foaming property (foam amount after 1 minute) ≤60, and appearance meeting the requirements.

[0036] The preparation method of the composite fatty alcohol polyoxyethylene ether phosphate monoester solution is as follows: Add 4g of hydroxymethyl cellulose to 500g of water and stir at room temperature for 20 minutes. Add 60g of fatty alcohol polyoxyethylene ether phosphate monoester and stir at 10000r / min for 20 minutes to obtain a dispersion. Add 20g of carrageenan to 150g of water, heat to 80℃ and stir for 1 hour until completely dissolved to obtain a carrageenan aqueous solution. Then add the carrageenan aqueous solution to the dispersion and stir at room temperature for 1 hour to obtain the composite fatty alcohol polyoxyethylene ether phosphate monoester solution.

[0037] Example 6 A method for preparing a 10wt% glufosinate-ammonium soluble concentrate is as follows: Add 60g of fatty alcohol polyoxyethylene ether phosphate monoester to 650g of water and stir at 10000r / min for 20 minutes to obtain a dispersion, which is the fatty alcohol polyoxyethylene ether phosphate monoester solution. Weigh 100g of glufosinate, 80g of isomeric C13 fatty alcohol polyoxyethylene ether MULTISO 13-100, and 2g of SAG 1572 defoamer and add them to 700g of fatty alcohol polyoxyethylene ether phosphate monoester solution. Stir at room temperature for 30 minutes, add 10wt% hydrochloric acid to adjust the pH to 7.5, add water to make up to 1000g, and continue stirring for 15 minutes until clear and transparent. After testing and filling, the glufosinate ammonium salt soluble concentrate is obtained.

[0038] The testing standards are as follows: glufosinate mass fraction of 10wt%, glufosinate ammonium salt mass fraction of 10.9wt%, ammonium ion mass fraction ≥0.9wt%, L-enantiomer ratio ≥96%, pH of 7.5, qualified dilution stability (20 times), persistent foaming property (foam amount after 1 minute) ≤60, and appearance meeting the requirements.

[0039] Comparative Example 1 A method for preparing a 10wt% glufosinate-ammonium soluble concentrate is as follows: Weigh 100g glufosinate and 2g SAG 1572 defoamer and add them to 700g of water. Stir at room temperature for 30 minutes, add 10wt% hydrochloric acid to adjust the pH to 7.5, add water to make up to 1000g, and continue stirring for 15 minutes until clear and transparent. After testing and filling, the soluble form of glufosinate ammonium salt is obtained.

[0040] The testing standards are as follows: glufosinate mass fraction of 10wt%, glufosinate ammonium salt mass fraction of 10.9wt%, ammonium ion mass fraction ≥0.9wt%, L-enantiomer ratio ≥96%, pH of 7.5, qualified dilution stability (20 times), persistent foaming property (foam amount after 1 minute) ≤60, and appearance meeting the requirements.

[0041] Test Example 1 thermal storage stability test The 10 wt% glufosinate-ammonium soluble concentrate obtained by the methods of Examples 1-6 and Comparative Example 1 of this invention was subjected to stability tests. The test procedures were based on the thermal storage stability test in the national standard GB / T 43172-2023 "Glufosinate-ammonium". The test data are shown in Table 1.

[0042] 1000g of 10wt% glufosinate-ammonium soluble concentrate sample was evenly distributed into four sealed glass bottles and stored in a constant temperature chamber at 54℃ for 14 days. After storage, the bottles were removed, placed in a desiccator, and cooled to room temperature. The mass fraction of glufosinate-ammonium, the active ingredient in the glufosinate-ammonium soluble concentrate, was determined within 24 hours. Before the test, the mass fraction of glufosinate-ammonium, the active ingredient in each soluble concentrate, was 10.0wt%. The change rate was calculated as (mass fraction of glufosinate-ammonium after the thermal storage stability test / initial mass fraction of glufosinate-ammonium) × 100%.

[0043] Table 1 Results of thermal storage stability test

[0044] As can be seen from the comparison of Test Example 1, the 10wt% glufosinate-ammonium soluble concentrate in Comparative Example 1 has low thermal storage stability. Examples 1, 2, 5 and 6 all have certain thermal stability. Among them, the effective component mass fraction in the thermal storage stability test of Examples 3-4 is not less than 95% of that before storage, and Example 4 has better stability.

[0045] Test Example 2 Low temperature stability test The 10 wt% glufosinate-ammonium soluble concentrate obtained by the methods of Examples 1-6 and Comparative Example 1 of this invention was subjected to stability tests. The test procedures were based on the low-temperature stability test in the national standard GB / T 43172-2023 "Glufosinate-ammonium". The test data are shown in Table 2.

[0046] Transfer 100g of the sample into a centrifuge tube and cool it to 0℃ in a refrigerator. Keep the centrifuge tube and its contents at 0℃ for 1 hour, stirring every 15 minutes for 15 seconds each time. Check and record whether any solid or oily substances are precipitated. Return the centrifuge tube to the refrigerator and continue to place it at 0℃ for 7 days. After 7 days, remove the centrifuge tube, let it stand at room temperature for 3 hours, and centrifuge for 15 minutes (the relative centrifugal force at the top of the tube is 500g, where g is the acceleration due to gravity). Record the volume of the precipitate at the bottom of the tube (accurate to 0.05mL).

[0047] Table 2 Low Temperature Stability Test Results

[0048] As can be seen from the comparison of Test Example 2, the 10wt% glufosinate-ammonium soluble concentrate in Comparative Example 1 has low low-temperature stability, and the low-temperature stability of Examples 1-2 is also relatively weak. Examples 3-6, after being stored at 0℃ for 7 days, showed that the volume of the precipitate at the bottom of the tube after centrifugation did not exceed 0.4mL, all of which have a certain degree of low-temperature resistance. Among them, Example 4 has better low-temperature stability.

Claims

1. A soluble form of glufosinate-ammonium, characterized in that, Includes the following components: Glufosinate, Synergists Complex fatty alcohol polyoxyethylene ether phosphate monoester solution Fatty alcohol polyoxyethylene ether, Organosilicon defoamer water.

2. The glufosinate-ammonium soluble concentrate as described in claim 1, characterized in that, The 10wt% glufosinate-ammonium soluble concentrate comprises the following components by mass fraction: 10wt% glufosinate Synergist 4-6wt% 40-70 wt% of compound fatty alcohol polyoxyethylene ether phosphate monoester solution Fatty alcohol polyoxyethylene ether 4-8 wt% Organosilicon defoamer 0.05-0.5wt%, Add water to make up to 100 wt%.

3. The glufosinate-ammonium soluble concentrate as described in claim 2, characterized in that, The 10wt% glufosinate-ammonium soluble concentrate comprises the following components by mass fraction: 10wt% glufosinate Synergist 5-6wt% 50-70 wt% of compound fatty alcohol polyoxyethylene ether phosphate monoester solution Fatty alcohol polyoxyethylene ether 7-8 wt% Organosilicon defoamer 0.1-0.3wt% Add water to make up to 100 wt%.

4. The glufosinate-ammonium soluble concentrate as described in claim 3, characterized in that, The synergist is Synergen ME adjuvant.

5. The glufosinate-ammonium soluble concentrate as described in claim 4, characterized in that, The Synergen ME adjuvant is Synergen from Clariant. TM Synergen ME products are part of a series of adjuvants.

6. The glufosinate-ammonium soluble concentrate according to claim 3, characterized in that, The fatty alcohol polyoxyethylene ether is an isomer of C13 fatty alcohol polyoxyethylene ether.

7. The glufosinate-ammonium soluble concentrate according to claim 6, characterized in that, The isomeric C13 fatty alcohol polyoxyethylene ether is Sasol's MULTISO 13-100 product from the MULTISO series.

8. A method for preparing the glufosinate-ammonium soluble concentrate according to any one of claims 1-7, characterized in that, The preparation method is as follows: Weigh out glufosinate, synergist, fatty alcohol polyoxyethylene ether, and organosilicon defoamer and add them to the composite fatty alcohol polyoxyethylene ether phosphate monoester solution. Stir at room temperature for 10-30 minutes, add 10-20wt% hydrochloric acid to adjust the pH to 4.0-8.0, add water to make up to 100%, and continue stirring for 10-20 minutes until clear and transparent. After testing and filling, the glufosinate ammonium salt soluble concentrate is obtained.

9. The method for preparing glufosinate-ammonium soluble concentrate as described in claim 8, characterized in that, The preparation method is as follows, in parts by weight: Add 0.2-0.4 parts of hydroxymethyl cellulose to 40-50 parts of water and stir at room temperature for 10-20 minutes. Add 5-6 parts of fatty alcohol polyoxyethylene ether phosphate monoester and stir at 10000-12000 r / min for 10-30 minutes to obtain a dispersion. Add 1-2 parts of carrageenan to 10-20 parts of water, heat to 60-80℃ and stir for 1-2 hours until completely dissolved to obtain a carrageenan aqueous solution. Then add the carrageenan aqueous solution to the dispersion and stir at room temperature for 0.5-1 hour to obtain the composite fatty alcohol polyoxyethylene ether phosphate monoester solution.

10. The method for preparing glufosinate-ammonium soluble concentrate as described in claim 8, characterized in that, The testing standards are as follows: glufosinate mass fraction of 10±1.0wt%, glufosinate ammonium salt mass fraction of 10.9±1.0wt%, ammonium ion mass fraction ≥0.9wt%, L-enantiomer ratio ≥96%, pH range of 4.0-8.0, qualified dilution stability (20 times), persistent foaming property (foam volume after 1 minute) ≤60, and appearance meeting the requirements.