Preparation method for glyphosate

A technology of glyphosate and glyphosate, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve problems such as side reactions, unfavorable industrial production, and poor effect of activated carbon.

Inactive Publication Date: 2012-08-29
CHONGQING UNISPLENDOUR CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0003] Glycine method is a traditional production process in my country that started earlier. After years of development, the process technology has matured, but the process has the following disadvantages: long process route, complicated process, many by-products, a large amount of organic recovery solvents are used in the process, and environmental pollution. The impact is large and the energy consumption is also large, which is not conducive to industrial production. The glyphosate powder is directly obtained by the glycine method. In this method, the solid-liquid separation mother liquor is used to produce the water preparation, and the NaCl content in the produced water preparation is high. If the dosage is large Cause negative effects such as land compaction, which is not good for the environment
Among them, the air oxidation method using precious metals as catalysts is the method adopted by Monsanto, the leader in glyphosate production. The glyphosate obtained by this method has a high content and a purity of up to 97%, and the selectivity and conversion rate of the reaction are also very good. Good, the yield is as high as 96%, but precious metals are expensive in this method, difficult to recycle, and the catalyst is easily deactivated. The most important thing is that this method is a patent of Monsanto, and it is urgent to develop a new process ...

Method used

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  • Preparation method for glyphosate
  • Preparation method for glyphosate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] A kind of preparation method of glyphosate, carries out according to the following steps:

[0051] Add 350g of bisglyphosate, 350g of deionized water or tap water and 1.1g of sodium tungstate into a 1000ml four-necked bottle, measure the pH after stirring, it is generally about 1.5-2, raise the temperature to T=64-65°C, and start to drop the content of 228g of 27.5% hydrogen peroxide, the temperature of hydrogen peroxide dripping is controlled at 66±1°C, and the dropping time is generally 40-50min. Impurity activated carbon obtains oxidized liquid.

[0052] Cool the oxidizing solution with ice-salt water until T<25°C, use KI starch test paper to test that the test paper turns blue, add 76g of 20% sodium sulfite aqueous solution to consume excess hydrogen peroxide, and test with KI starch test paper, when the test paper is white or colorless When, stop adding sodium sulfite aqueous solution.

[0053]Cool the oxidizing solution to 10°C, start to drop 33.5g of ferrous su...

Embodiment 2

[0055] A kind of preparation method of glyphosate, carries out according to the following steps:

[0056] Add 250Kg of bisglyphosate, 240Kg of deionized water or tap water and 0.9Kg of sodium tungstate into a 1000l enamel kettle, measure the pH after stirring, generally around 1.5-2, raise the temperature to T=64-65°C, and start to drop the content of 171Kg of 28.1% hydrogen peroxide, the temperature of hydrogen peroxide is controlled at 66±1°C, the time of dropping is generally 40-50min, the mixture becomes clear after about 40min after the addition, keep warm for 30min, add a small amount of activated carbon to decolorize, filter to remove mechanical Impurities and activated carbon get oxidized liquid.

[0057] Cool the oxidizing solution with ice-salt water to T<25°C, use KI starch test paper to detect that the test paper turns blue, add 26.5Kg of 20% sodium sulfite aqueous solution, consume excess hydrogen peroxide, and test with KI starch test paper, when the test paper i...

Embodiment 3

[0060] A kind of preparation method of glyphosate, carry out as follows:

[0061] Add bisglyphosate, soft water and sodium phosphotungstate into the reaction kettle, then add hydrogen peroxide to react to obtain an oxidation solution, consume excess hydrogen peroxide with a sodium sulfite aqueous solution with a concentration of 10-30% by mass, and use KI starch test paper to detect the concentration of the oxidation solution. Whether the excess hydrogen peroxide is consumed, the temperature in the process of consuming excess hydrogen peroxide is 10-50°C; then add ferrous sulfate for reduction reaction, crystallization, and drying to obtain glyphosate raw powder, bisglyphosate: soft water: phosphotungsten The molar ratio of sodium acid: hydrogen peroxide: ferrous sulfate is 1: 20: 0.005: 1.5: 0.02, and the HPLC purity and yield of glyphosate finally obtained can reach the beneficial effects described in the present invention.

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Abstract

A preparation method for glyphosate comprises the steps as follows: oxydol is adopted for catalytic oxidation of a pmida raw material to obtain oxidation liquid, sulfide reductant with weaker reducibility is added into the oxidation liquid to consume excess oxydol in the oxidation reaction, then ferrous sulfate is added for reduction, and finally separation and drying are conducted so as to prepare the glyphosate; and the sulfide reductant with the weaker reducibility is any one or any combination of sodium sulfite, ammonium sulfite, potassium sulfite, ammonium bisulfite, sodium thiosulfate and sodium bisulfite. According to the method provided by the invention, the amount of the ferrous sulfate reductant is low, so as to save the raw material cost; the technical problem that the glyphosate prepared by the process in the prior art is yellowish is solved due to oxidation, reduction and other treatments in the method; meanwhile, the purity of the glyphosate prepared by using the method is high, the content of the glyphosate in solid powder is more than 96 percent, and the yield is more than 82 percent; and through the adoption of the method, the consumption of raw and auxiliary materials is lower, ammonia water, sulfuric acid and other raw materials are not used in the process.

Description

technical field [0001] The invention relates to a preparation method of glyphosate, in particular to a preparation method of glyphosate with high yield, and belongs to the field of chemical synthesis. Background technique [0002] Glyphosate is a high-efficiency, low-toxicity, post-emergent herbicide, and its sales volume occupies an important position in pesticide products. Glyphosate was originally synthesized by Monsanto Chemical Company of the United States; the current production process of glyphosate mainly includes glycine Method and IDA method two process routes. [0003] Glycine method is a traditional production process in my country that started earlier. After years of development, the process technology has matured, but the process has the following disadvantages: long process route, complicated process, many by-products, a large amount of organic recovery solvents are used in the process, and environmental pollution. The impact is large and the energy consumptio...

Claims

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Application Information

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IPC IPC(8): C07F9/38
Inventor 王友仁王冬林杨建川李俊锋罗延谷罗丹丹李文艳陈勇董远萍陈敬任权龙晓钦
Owner CHONGQING UNISPLENDOUR CHEM
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