Synthesis method of glyphosate potassium salt technical product

A technology of glyphosate potassium salt and synthesis method, which is applied in the fields of chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., and can solve the problem of low crystallization rate, low utilization rate of equipment, and low economic issues

Active Publication Date: 2015-01-14
HANGZHOU JINFADA CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The patent CN101186622A uses the crystallization of the relationship between solubility curves at different temperatures to obtain glyphosate potassium salt. However, due to the high solubility of glyphosate potassium salt, the solubility of glyphosate potassium salt at room temperature reaches more than 160 grams, and the concentration is as high as 60%. In order to obtain a larger amount of primary crystallization, the concentration of potassium salt must be increased as much as possible. When the concentration of potassium salt is too high, the viscosity will increase significantly and become very viscous. Not only does it require high mixing equipment, but the main reason is that the crystallization rate is not high. , the obtained mother liquor has a high content of potassium salt of glyphosate, and the utilization rate of the equipment is not high, which is uneconomical
Attempts to extract a well-formed solid from its potassium glyphosate brine solution using conventional organic solvents were unsuccessful

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 50g of water and 100g of dry glyphosate raw powder (purity 95%) to the reaction with a stirring and cooling device, stir evenly to form a suspension containing glyphosate, and gradually increase the concentration of 65g to 48% under stirring Potassium hydroxide solution (potassium carbonate or potassium bicarbonate solution of the same concentration or a mixed solution of potassium hydroxide, potassium carbonate and potassium bicarbonate can also be used) is added dropwise to the glyphosate suspension to make it react. A large amount of heat is generated during the reaction, and the reaction system gradually changes from a white suspension system to a colorless and transparent solution, and an aqueous solution of glyphosate potassium salt is obtained. After the dropwise addition, the mass concentration of the glyphosate potassium salt solution was 40%, and the pH value was adjusted to 4.0. When the aqueous solution of glyphosate potassium salt is cooled to 50°C or 4...

Embodiment 2

[0029] Add 40g of water and 200g of dry glyphosate powder (purity 95%) to the reaction with a stirring and cooling device, stir evenly to form a suspension containing glyphosate, and gradually add 140g of glyphosate to a concentration of 48% under stirring Potassium hydroxide solution (potassium carbonate or potassium bicarbonate solution of the same concentration can also be used) is added dropwise to the glyphosate suspension to make it react. A large amount of heat is generated during the reaction, and the reaction system gradually changes from a white suspension system to a colorless and transparent solution, and an aqueous solution of glyphosate potassium salt is obtained. After the dropwise addition, the mass concentration of the glyphosate potassium salt solution was 45%, and the pH value was adjusted to 4.2. When the aqueous solution of glyphosate potassium salt is cooled to 40°C or 35°C, gradually add 320g of methanol (ethanol or other lower alcohols can also be used)...

Embodiment 3

[0031]Add 130g of water and 200g of dry glyphosate powder (purity: 95%) to the reaction with a stirring and cooling device, stir evenly to form a suspension containing glyphosate, and gradually increase the concentration of 144g to 48% under stirring The potassium hydroxide solution was added dropwise to the glyphosate suspension to make it react. A large amount of heat is generated during the reaction, and the reaction system gradually changes from a white suspension system to a colorless and transparent solution, and an aqueous solution of glyphosate potassium salt is obtained. After the dropwise addition, the mass concentration of the glyphosate potassium salt solution was 50%, and the pH value was 4.5. When the aqueous solution of glyphosate potassium salt is cooled to 30°C or 25°C, gradually add 540g of methanol (methanol or other lower alcohols can also be used) dropwise under stirring. Control at 140r / min, 160r / min or 180r / min. During the dropwise addition, the soluti...

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Abstract

The invention discloses a synthesis method of a glyphosate potassium salt technical product, belonging to the pesticide technical field. The synthesis method comprises the following process steps of: 1) mixing glyphosate, alkali with potassium ions which are positive ions, and water to react and form a glyphosate potassium salt aqueous solution, and controlling the pH value of the glyphosate potassium salt aqueous solution after the reaction; 2) reducing the temperature of the glyphosate potassium salt aqueous solution, dropwise adding an organic solvent in the glyphosate potassium salt aqueous solution under stirring to perform alcohol precipitation; and 3) filtering after the precipitation of crystals to obtain a wet potassium salt technical product, and then drying to obtain the glyphosate potassium salt technical product. The synthesis method of the glyphosate potassium salt technical product is reasonable in design, the content of the glyphosate obtained by the method is up to above 97%, the yield of the glyphosate potassium salt is above 98%; and compared with the glyphosate potassium salt yield of the prior art which is 20%, the efficiency is increased by nearly 5 times and every unit of energy consumption is reduced.

Description

technical field [0001] The invention belongs to the technical field of pesticides, in particular to a synthesis method of glyphosate potassium salt original drug. Background technique [0002] Glyphosate is the systemic herbicide with the largest sales volume and the fastest growth rate in the world, and with the successful development and popularization of glyphosate-transgenic crops and the shortage of energy sources, it has led to the sowing and promotion of biofuel crops. The production of phosphine offers new opportunities. [0003] Glyphosate (glyphosate), the chemical name is N-(phosphine carboxymethyl) glycine, the pure product is a non-volatile white solid, the specific gravity is 0.5, it melts at about 230 ° C, and it is accompanied by decomposition. The solubility in water at room temperature Only 1.2 grams, insoluble in common organic solvents, and its isopropylamine salt, potassium salt, ammonium salt, and sodium salt are soluble in water. Glyphosate is a syst...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/38
Inventor 孔鑫明周海杨刘劭农汤晓娟邓青松程晨杰周锦枫孙晓昂
Owner HANGZHOU JINFADA CHEM IND
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