An L-glufosinate-ammonium soluble concentrate and its preparation method

Abstract

The present invention relates to the field of agricultural herbicides, and specifically relates to an L - glufosinate - ammonium soluble concentrate and a preparation method thereof. The L - glufosinate - ammonium soluble concentrate, by weight percentage, comprises 5 - 50% of L - glufosinate - ammonium, 2 - 20% of an alkali, 10 - 30% of a surfactant, 1 - 20% of a synergist, 0.1 - 1% of an antifoaming agent, 1 - 10% of a solvent, and the balance being deionized water. The L - glufosinate - ammonium soluble concentrate of the present invention is an agricultural herbicide with good herbicidal effect, simple production process and no environmental pollution.

Description

Technical Field

[0001] The present invention relates to the field of agricultural herbicides, and particularly to an L-glufosinate-ammonium soluble liquid formulation and a preparation method thereof. Background Art

[0002] L-glufosinate-ammonium, also known as glufosinate-ammonium, was initially discovered as the active metabolite of the biopesticide herbicide bilanafos in plants. Its herbicidal activity is twice that of ordinary glufosinate-ammonium, and the application rate per mu is only 50% of that of glufosinate-ammonium. The application costs of the two are basically the same. It is mainly used in orchards, vineyards, non-cultivated land, potato fields, etc. to control annual and perennial dicotyledonous and gramineous weeds, such as Alopecurus myosuroides, Digitaria sanguinalis, Echinochloa crusgalli, Hordeum spontaneum, Lolium multiflorum, Setaria viridis, Setaria glauca, Triticum aestivum, Zea mays, etc., and perennial gramineous weeds and sedges, such as Poa annua, Deschampsia flexuosa, Festuca ovina, etc.

[0003] The active ingredient of L-glufosinate-ammonium is acidic. It is a non-selective herbicide with semi-systemic or weak systemic and no conduction properties, and is not suitable for direct use in agricultural production. Developing and producing L-glufosinate-ammonium will greatly reduce the dosage of the technical material, which is very important for improving product economy, reducing pesticide usage, and alleviating environmental pressure.

[0004] Patents CN105660688A, CN105638724A, and CN107467061A disclose methods for preparing L-glufosinate-ammonium soluble liquid formulations under acidic conditions. At present, no preparation method for a soluble liquid formulation of L-glufosinate-ammonium after salification has been seen. Summary of the Invention

[0005] The purpose of the present invention is to provide an L-glufosinate-ammonium soluble liquid formulation with good herbicidal effect, simple production process, and no environmental pollution, and a preparation method thereof.

[0006] In order to achieve the above purpose, the technical solution of the present invention is as follows:

[0007] An L-glufosinate-ammonium soluble liquid formulation, calculated by weight percentage, contains 5-50% of L-glufosinate-ammonium, 2-20% of alkali, 10-30% of surfactant, 1-20% of synergist, 0.1-1% of defoamer, 1-10% of solvent, and the balance is deionized water.

[0008] Preferably, calculated by weight percentage, it contains 10-20% of L-glufosinate-ammonium, 3-15% of alkali, 15-25% of surfactant, 5-20% of synergist, 0.2-1% of defoamer, 5-10% of solvent, and the balance is deionized water.

[0009] The alkali is selected from one or a combination of several of sodium hydroxide, potassium hydroxide, barium hydroxide, copper hydroxide, potassium carbonate, sodium carbonate, triethanolamine, and ammonia water.

[0010] The surfactant is selected from one or a combination of sulfosuccinate anions, phosphate anions, hyperbranched polyether star polymers, fluorine-modified polyacrylates, modified isomeric alcohol ethers, modified isomeric alcohol alkylene oxide block copolymers, and alkyl glycosides.

[0011] The synergist is selected from one or a combination of potassium chloride, potassium sulfate, potassium nitrate, potassium chlorate, potassium dihydrogen phosphate, potassium polyphosphate, potassium bisulfate, potassium metaaluminate, and potassium alum.

[0012] The defoamer is selected from one or a combination of silicones, C8-C10 fatty alcohols, phosphates, polyethers, C10-C20 saturated fatty acids, and amides.

[0013] The solvent is selected from one or a combination of methanol, ethanol, propylene glycol, propylene glycol methyl ether, ethylene glycol monobutyl ether, and propylene glycol monobutyl ether.

[0014] The preparation method of the L-glufosinate-ammonium soluble concentrate is as follows: according to the above proportions, add the L-glufosinate-ammonium technical material, alkali, and deionized water to a modulation kettle, start stirring, and after the technical material is completely dissolved, add the surfactant, synergist, defoamer, and solvent in proportion respectively. After stirring evenly, the finished product of the L-glufosinate-ammonium soluble concentrate is obtained.

[0015] Due to the implementation of the above technical solutions, the present invention has the following advantages compared with the prior art: the preparation of the present invention makes up for the defects of the existing L-glufosinate-ammonium preparation, such as high cost, poor efficacy, and poor weeding effect; secondly, by adding alkali in the system to make the technical material into a salt, and at the same time adding a synergist to further change the systemic absorption and conductivity of the technical material, thereby significantly improving the weeding effect; and the production process is simple, the operation is convenient, no heating is required, and it can be produced at room temperature. Detailed implementation mode

[0016] The following specific examples are used to further illustrate the present invention in detail, but the present invention is by no means limited to these examples. Methods well known to those skilled in the art are all included in the scope of the present invention. Percentages in the formula are all by weight. The active ingredient is added according to the dose after being converted to 100% purity (content 90-95%) prepared according to the records of the prior art. The proportions of each component are in weight percentages, and all other raw materials are commercially available products.

[0017] Example 1 5% L-glufosinate-ammonium soluble concentrate

[0018] (1) L-glufosinate-ammonium 5%, ammonia water 5%, modified isomeric alcohol ether 10%, defoamer SAG630 0.5%, ethylene glycol monobutyl ether 3%, and the balance is deionized water (made up to 100%).

[0019] (2) 5% L-Glyphosate, 5% ammonia water, 10% modified isomeric alcohol ether, 10% potassium dihydrogen phosphate, 0.5% defoamer SAG630, 3% ethylene glycol monobutyl ether, and the balance is deionized water (made up to 100%)

[0020] Example 2: 5% L-Glyphosate Soluble Concentrate

[0021] (1) 5% L-Glyphosate, 5% ammonia water, 8% fluorine-modified polyacrylate, 4% phosphate ester anions, 0.5% defoamer SAG630, 3% ethylene glycol monobutyl ether, and the balance is deionized water (made up to 100%).

[0022] (2) 5% L-Glyphosate, 5% ammonia water, 8% fluorine-modified polyacrylate, 4% phosphate ester anions, 10% potassium metaaluminate, 0.5% defoamer SAG630, 3% ethylene glycol monobutyl ether, and the balance is deionized water (made up to 100%).

[0023] Example 3: 10% L-Glyphosate Soluble Concentrate

[0024] (1) 10% L-Glyphosate, 10% sodium carbonate, 5% copper hydroxide, 15% hyperbranched polyether star polymer, 0.5% defoamer SAG630, 5% ethylene glycol monobutyl ether, and the balance is deionized water (made up to 100%).

[0025] (2) 10% L-Glyphosate, 10% sodium carbonate, 5% copper hydroxide, 15% hyperbranched polyether star polymer, 10% potassium chloride, 0.5% defoamer SAG630, 5% ethylene glycol monobutyl ether, and the balance is deionized water (made up to 100%).

[0026] Example 4: 10% L-Glyphosate Soluble Concentrate

[0027] (1) 10% L-Glyphosate, 15% sodium carbonate, 10% modified isomeric alcohol alkylene oxide block copolymer, 0.5% defoamer SAG630, 5% ethanol, and the balance is deionized water (made up to 100%).

[0028] (2) 10% L-Glyphosate, 15% sodium carbonate, 10% modified isomeric alcohol alkylene oxide block copolymer, 10% potassium alum, 0.5% defoamer SAG630, 5% ethanol, and the balance is deionized water (made up to 100%).

[0029] Example 5: 15% L-Glyphosate Soluble Concentrate

[0030] (1) 15% L-Glyphosate, 5% sodium hydroxide, 15% modified isomeric alcohol alkylene oxide block copolymer, 5% alkyl polyglycoside, 0.5% defoamer SAG630, 5% propylene glycol monomethyl ether, and the balance is deionized water (made up to 100%).

[0031] (2) 15% L-Glyphosate, 5% Sodium hydroxide, 15% Modified isomeric alcohol alkylene oxide block copolymer, 5% Alkyl polyglycoside, 10% Potassium chlorate, 0.5% Defoamer SAG630, 5% Propylene glycol methyl ether, balance deionized water (made up to 100%)

[0032] Example 6: 20% L-Glyphosate soluble concentrate

[0033] (1) 20% L-Glyphosate, 7% Sodium hydroxide, 15% Modified isomeric alcohol alkylene oxide block copolymer, 10% Alkyl polyglycoside, 0.5% Defoamer SAG630, 10% Propylene glycol butyl ether, balance deionized water (made up to 100%).

[0034] (2) 20% L-Glyphosate, 7% Sodium hydroxide, 15% Modified isomeric alcohol alkylene oxide block copolymer, 10% Alkyl polyglycoside, 10% Potassium bisulfate, 0.5% Defoamer SAG630, 10% Propylene glycol butyl ether, balance deionized water (made up to 100%).

[0035] Example 7: 20% L-Glyphosate soluble concentrate

[0036] (1) 20% L-Glyphosate, 7% Sodium hydroxide, 5% Modified isomeric alcohol ether, 15% Alkyl polyglycoside, 0.5% Defoamer SAG6300.5, 10% Propylene glycol methyl ether, balance deionized water (made up to 100%).

[0037] (2) 20% L-Glyphosate, 7% Sodium hydroxide, 5% Modified isomeric alcohol ether, 15% Alkyl polyglycoside, 10% Potassium dihydrogen phosphate, 0.5% Defoamer SAG630, 10% Propylene glycol methyl ether, balance deionized water (made up to 100%).

[0038] Example 8: 20% L-Glyphosate soluble concentrate

[0039] (1) 20% L-Glyphosate, 7% Sodium hydroxide, 15% Modified isomeric alcohol ether, 10% Alkyl polyglycoside, 3% Sulfosuccinate anion, 0.5% Defoamer SAG630, 10% Propylene glycol methyl ether, balance deionized water (made up to 100%).

[0040] (2) 20% L-Glyphosate, 7% Sodium hydroxide, 15% Modified isomeric alcohol ether, 10% Alkyl polyglycoside, 3% Sulfosuccinate anion, 10% Potassium nitrate, 0.5% Defoamer SAG630, 10% Propylene glycol methyl ether, balance deionized water (made up to 100%).

[0041] Example 9: 25% L-Glyphosate soluble concentrate

[0042] (1) 25% L - glufosinate - ammonium, 9% sodium hydroxide, 10% modified isomeric alcohol ether, 5% alkyl polyglycoside, 5% sulfosuccinate anion, 0.5% defoamer SAG630, 10% propylene glycol methyl ether, balance deionized water (made up to 100%).

[0043] (2) 25% L - glufosinate - ammonium, 9% sodium hydroxide, 10% modified isomeric alcohol ether, 5% alkyl polyglycoside, 5% sulfosuccinate anion, 15% potassium polyphosphate, 0.5% defoamer SAG630, 10% propylene glycol methyl ether, balance deionized water (made up to 100%).

[0044] The preparation process of the L - glufosinate - ammonium soluble concentrate in each of the above - mentioned examples is as follows: Add the L - glufosinate - ammonium technical, alkali, and deionized water into a modulation kettle in proportion, start stirring. After the technical is completely dissolved, filter to remove the water - insoluble inorganic salts and impurities. Then, add surfactants, synergists, defoamers, and solvents in proportion in sequence. After stirring evenly, the finished product of the L - glufosinate - ammonium soluble concentrate is obtained.

[0045] If all substances are added to the modulation kettle and stirred to dissolve the materials according to the existing preparation method, the viscosity of the preparation will be too high and the fluidity will be reduced due to the addition of surfactants, thus prolonging the filtration time and causing difficulties in the subsequent filtration process. The extension of the production time of the product is not conducive to industrial production; therefore, the specific order described above needs to be adopted to achieve the optimal effect.

[0046] Perform heat storage (14 d, 54 °C ± 2 °C) and cold storage (7 d, 0 °C ± 2 °C) tests and physical and chemical property detections on (1) and (2) in Examples 1 - 9, the control sample (10% glufosinate - ammonium soluble concentrate (Jingbaoshida, produced by BASF)) and the technical (L - glufosinate - ammonium). The test results are shown in Table 1.

[0047] Table 1. Results of heat and cold storage experiments of samples

[0048]

[0049]

[0050] As can be seen from Table 1, in Examples 1-9, on the premise that other conditions are the same, the addition of potassium-containing compounds not only significantly improves the thermal storage decomposition rate of the active ingredient in the preparation, but also significantly reduces the surface tension and contact angle of the preparation. The lower the value of the thermal storage decomposition rate, the better the chemical stability of the active ingredient under the complex storage and transportation conditions during the shelf life. The lower the values of the surface tension and contact angle, the better the liquid medicine can adhere to and spread on the leaf surface of weeds, and the larger the contact area with weeds, which helps to improve the drug efficacy and utilization rate of the active ingredient. The technical effects brought by the addition of potassium-containing compounds in terms of the stability of the active ingredient, surface tension and contact angle are unpredictable. Through analysis and speculation, it is possible that the addition of potassium-containing compounds reduces the intermolecular interaction force of the liquid, thereby reducing the surface tension and contact angle. The results of field trials show that the drug efficacy of the samples prepared according to this scheme is better than that of the control agent, and the synergistic effect is obvious.

[0051] Field control of weeds test examples

[0052] Test name: Field test of 20% glufosinate-ammonium soluble concentrate for controlling weeds. Test agent: Example 7(2), control agent (10% glufosinate-ammonium soluble concentrate)

[0053] Test site:

[0054] Mujia Tun, Taiping Town, Wuming District, Nanning City, Guangxi

[0055] Weed species:

[0056] Mainly broad-leaved weeds, including Alternanthera philoxeroides, Amaranthus tricolor, Mimosa pudica, Eclipta prostrata, Portulaca oleracea, Ageratum conyzoides, Bidens pilosa, Commelina communis, Bryophyte, Emilia sonchifolia, Artemisia, Basella alba, Bidens pilosa (dominant population), Alternanthera philoxeroides, Commelina communis, Scoparia dulcis, Polygonum perfoliatum, Pueraria lobata, Smilax china, Ageratum conyzoides, etc.; Gramineous weeds mainly include Digitaria sanguinalis and Eleusine indica.

[0057] Table 2. Field test results of glufosinate-ammonium soluble concentrate for controlling weeds in non-cultivated land

[0058]

[0059] The above-mentioned recorded dosage is calculated based on the added amount of L-glufosinate-ammonium in the preparation.

[0060] As can be seen from the above table, when the application rate of 20% glufosinate-ammonium soluble concentrate is between 300 g a.i. / hm 2 ~600 g a.i. / hm 2 the visual control effect at 15 days and the plant number control effect at 15 days are both above 90%, which is better than the control agent.

[0061] The above embodiments are only used to illustrate the technical concept and features of the present invention. The purpose is to enable those skilled in the art to understand the content of the present invention and implement it accordingly. It is not intended to limit the protection scope of the present invention. Any modifications made according to the technical features of the present invention should fall within the protection scope of the present invention. The content not described in detail in this specification belongs to the prior art well-known to those skilled in the art.

Claims

1. A soluble liquid formulation of L - glufosinate, characterized in that: For the L - glufosinate - ammonium soluble concentrate, by weight percentage, it contains 5 - 50% of L - glufosinate - ammonium, 2 - 20% of base, 10 - 30% of surfactant, 1 - 20% of synergist, 0.1 - 1% of defoamer, 1 - 10% of solvent, and the balance is deionized water; The synergist is selected from one or a combination of several of potassium chloride, potassium sulfate, potassium nitrate, potassium chlorate, potassium dihydrogen phosphate, potassium polyphosphate, potassium bisulfate, potassium metaaluminate, and potassium alum.

2. The soluble liquid formulation of L - glufosinate according to claim 1, characterized in that, By weight percentage, it contains 10 - 20% of L - glufosinate - ammonium, 3 - 15% of base, 15 - 25% of surfactant, 5 - 20% of synergist, 0.2 - 1% of defoamer, 5 - 10% of solvent, and the balance is deionized water.

3. The soluble liquid formulation of L - glufosinate according to claim 1, characterized in that, The base is selected from one or a combination of several of sodium hydroxide, potassium hydroxide, barium hydroxide, copper hydroxide, potassium carbonate, sodium carbonate, triethanolamine, and ammonia water.

4. The soluble liquid formulation of L - glufosinate according to claim 1, characterized in that, The surfactant is selected from one or a combination of several of sulfosuccinate anions, phosphate anions, hyperbranched polyether star polymers, fluorine - modified polyacrylates, modified isomeric alcohol ethers, modified isomeric alcohol alkylene oxide block copolymers, and alkyl glycosides.

5. The soluble liquid formulation of L - glufosinate according to claim 1, characterized in that, The defoamer is selected from one or a combination of several of silicone - based, C8 - 10 fatty alcohols, phosphate esters, polyethers, C10 - 20 saturated fatty acids and amides.

6. The soluble liquid formulation of L - glufosinate according to claim 1, characterized in that, The solvent is selected from one or a combination of several of methanol, ethanol, propylene glycol, propylene glycol methyl ether, ethylene glycol butyl ether, and propylene glycol butyl ether.

7. The preparation method of the soluble liquid formulation of L - glufosinate according to claim 1, characterized in that, According to the above ratios, add the L - glufosinate - ammonium technical, base, and deionized water into a modulation kettle, start stirring. After the technical is completely dissolved, add the surfactant, synergist, defoamer, and solvent respectively according to the ratios. After stirring evenly, the finished product of the L - glufosinate - ammonium soluble concentrate is obtained.

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