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New process for preparing N-phosphonomethyl iminodiacetic acid

The technology of bisphosphonate and process is applied in the field of producing N-phosphonomethyliminodiacetic acid while by-producing chlorinated alkane, can solve the problems of high production cost, pollute the environment and the like, and achieve good environmental benefits and good economy. Effect

Inactive Publication Date: 2003-11-26
ZHEJIANG XINAN CHEM INDAL GROUP
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

[0006] Chloromethane is the main raw material for the production of methylchlorosilane. At present, it is mainly produced by the methanol hydrochlorination method. In the presence of a catalyst, methanol and hydrogen chloride react to form chloromethane, and then purified to obtain a high content of chloromethane. This process pollutes the environment. And the production cost is as high as 2,500 yuan / ton, and the development of organosilicon monomers urgently needs low-cost methyl chloride

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Embodiment 1: Get 70g raffinate and place in the 500ml four-neck flask that thermometer, stirrer, condenser are housed. The outlet of the condensing pipe is respectively connected with the washing bottle containing 20% ​​liquid caustic soda and the washing bottle of 98% concentrated sulfuric acid to collect the treated gas. Stir, then add 67.5g of iminodiacetic acid (98.5%, 0.5mol) and 336g of 31% hydrochloric acid respectively, heat up to 80-90°C, keep warm for 20-30 minutes, then add 76g of formazan recovered from the glyphosate production process Acetal (80%, the rest is water and methanol), reacted at 90-100 ° C for 2-10 hours, when there were almost no bubbles in the drying bottle equipped with concentrated sulfuric acid, the reaction was over, cooled to room temperature, filtered to obtain 128g wet Powder, mother liquor 286g. After drying the wet powder, 103.6 g of bisglyphosate dry powder with a content of 98.6% was obtained, and the yield was 90.0%. 105.2 g of...

Embodiment 2

[0036] Embodiment 2: get the mother liquor 143g in 46g phosphorous acid and embodiment 1, and hydrochloric acid amount is adjusted to 236g, all the other are with embodiment 1, get wet powder 131.6g, mother liquor 275g. After drying, 106.9 g of dry powder was obtained, the content of bisglyphosate was 98.3%, and the calculated yield was 92.5%. 68.7 g of methyl chloride was obtained, and its content was analyzed to be 99.5%.

Embodiment 3

[0037] Embodiment 3: get 50g content and be the mother liquor 143g among the formaldehyde of 36% and embodiment 1, and hydrochloric acid amount is adjusted to 110g, all the other are with embodiment 1, get wet powder 129.3g, mother liquor 177g. After drying, 104.8 g of dry powder was obtained, the content of bisglyphosate was 98.1%, and the calculated yield was 90.6%. 36.5 g of methyl chloride was obtained, and its content was analyzed to be 99.5%.

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Abstract

The new process of preparing N-phosphonomethyl iminodiacetic acid (NPMIDA) as the intermediate for synthesizing glyphosate features the materials including alkyl phosphite and / or C1-C4 formaldehyde alcohol. Especially, the residual liquid produced in the dimethyl phosphite producing process and acetal produced in dimethyl phosphite process of producing glyphosate are used. In the same time, chloromethane for synthesizing methyl chlorosilane may be obtained.

Description

technical field [0001] The invention relates to a process for producing N-phosphonomethyliminodiacetic acid (PMIDA) while by-producing chlorinated alkanes. Background technique [0002] The chemical name of glyphosate is N-phosphonomethylglycine (PMG), and its molecular formula is: It is a high-efficiency broad-spectrum herbicide. Because of its good systemic conductivity, it is very effective in the control of a variety of deep-rooted weeds. In recent years, the sales volume has gradually increased. With the glyphosate-resistant transgenic With the gradual promotion of crops, its application range has been further expanded. Now it has become the herbicide with the largest sales volume and the fastest growth rate in the world. There are two main production processes for glyphosate acid that are now industrialized. One is the IDA route using hydrocyanic acid or diethanolamine as the starting material used by Monsanto in the United States; The dial...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/36
Inventor 王伟任不凡周曙光郑红朝邵振威黎显文
Owner ZHEJIANG XINAN CHEM INDAL GROUP
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