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Preparation method of green chelating agent methyl glycine diacetic acid (MGDA) sodium salt

A technology of sodium methyl glycine diacetate and chelating agent is applied in the field of preparation of green chelating agent methyl glycine diacetate sodium salt, which can solve the problems of affecting chelating performance, high chloride ion content, strong corrosiveness, etc. The effect of production cost, simple reaction steps and short reaction period

Active Publication Date: 2020-12-01
HENAN QINGSHUIYUAN TECH
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

In the above-mentioned method for preparing MGDA 3Na, most of them use hydrocyanic acid, which will produce a large amount of cyanide-containing wastewater in the production process, and is highly corrosive, pollutes the environment, and does not meet the current clean production; although chloroacetic acid is used instead The method of hydrocyanic acid can effectively reduce the formation of pollutants, but the content of chloride ions is high, and the effective content of prepared MGDA·3Na is low, which will affect its chelating performance

Method used

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  • Preparation method of green chelating agent methyl glycine diacetic acid (MGDA) sodium salt

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Effect test

Embodiment 1

[0027] Add 4.5g of L-alanine and 10g of deionized water into a 100mL three-necked flask, stir at room temperature for 10min, then add 15.9g of glyoxylic acid (40wt%), control the reaction temperature of the solution at 30±2°C, React for 30 minutes. A reflux condenser was connected to the mouth of the three-necked flask, and the reaction temperature was raised to 95°C. Take 6.7g of formic acid with a mass fraction of 88% and put it in a constant pressure dropping funnel, control the opening of the glass stopper, slowly add formic acid dropwise, and control the reaction temperature at 95±2°C. After the dropwise addition, keep warm for 4h. The temperature was lowered to 75° C., and 32 wt % liquid caustic soda was added dropwise to the solution to adjust the pH to 10.0. Concentrate in vacuum at -0.01Mpa for 0.5h, and cool to room temperature. 30.1 g of methylglycine diacetic acid sodium salt solution was obtained, the mass concentration was 45%, the effective content was 40%, a...

Embodiment 2

[0029] Add 4.5g of L-alanine and 10g of deionized water into a 100mL three-necked flask, stir at room temperature for 10min, then add 18.5g of glyoxylic acid (40wt%), control the reaction temperature of the solution at 45±2°C, React for 30 minutes. A reflux condenser was connected to the mouth of the three-necked flask, and the reaction temperature was raised to 80°C. Take 9.2g of formic acid with a mass fraction of 88% and put it in a constant pressure dropping funnel, control the opening of the glass stopper, slowly add formic acid dropwise, and control the reaction temperature at 80±2°C. After the dropwise addition, keep warm for 3h. The temperature was lowered to 60° C., and 32 wt % liquid caustic soda was added dropwise to the solution to adjust the pH to 10.2. Concentrate in vacuum at -0.02Mpa for 0.5h, cool to room temperature, and obtain 29.3g of methylglycine diacetic acid sodium salt solution, with a mass concentration of 48%, an effective content of 45%, and a tot...

Embodiment 3

[0032] Add 4.5g of L-alanine and 10g of deionized water into a 100mL three-necked flask, stir at room temperature for 10min, then add 13.0g of formic acid (88wt%), control the reaction temperature of the solution at 25±2°C, and react for 30min . A reflux condenser was connected to the mouth of the three-necked flask, and the reaction temperature was raised to 80°C. Take 27.8g of glyoxylic acid with a mass fraction of 40% and put it into a constant pressure dropping funnel, control the opening of the glass stopper, slowly add glyoxylic acid dropwise, and control the reaction temperature at 80±2°C. After the dropwise addition, keep warm for 5h. The temperature was lowered to 50° C., and 50 wt % liquid caustic soda was added dropwise to the solution to adjust the pH value to 11.0. Concentrate in vacuum at -0.03Mpa for 0.5h, cool to room temperature, and obtain 28.5g of methylglycine diacetic acid sodium salt solution, with a mass concentration of 48%, an effective content of 46...

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Abstract

The invention relates to a preparation method of a green chelating agent, namely MGDA sodium salt. Specifically, in an aqueous solution reaction system, L-alanine, glyoxylic acid and formic acid are subjected to a reductive amination reaction, so two hydrogen atoms, connected with N, on L-alanine are substituted, and two carboxymethyl groups are introduced into L-alanine to prepare a MGDA sodium salt solution. Through detection, the effective content of the MGDA sodium salt can reach 40% or above, and yield can reach 86% or above on a dry basis. The method is short in production period, simpleand clean in process, and mild in reaction condition, a new thought is provided for preparation of the MGDA sodium salt, highly toxic substances such as hydrocyanic acid are replaced, the reaction becomes safe and environmentally friendly, and industrial production difficulty is reduced; and substances such as chloroacetic acid are replaced, and a produced MGDA sodium salt product does not contain chloride ions and is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the field of organic chemical synthesis, and specifically provides a method for preparing a green chelating agent methylglycine diacetic acid sodium salt. Background technique [0002] At present, the common chelating agents are mainly composed of silicate, phosphate hydrochloric acid, amino carboxylate and phosphonate. MGDA (methylglycine diacetic acid) is widely used in most cleaning processes because of its non-toxic and easy biodegradable advantages. Its molecules interact with cations to form a perfect three-dimensional space structure, usually forming a 1:1 complex. These complexes are stable, even under alkaline conditions or at temperatures up to 100°C. [0003] The synthetic method of methylglycine diacetate can be divided into four major classes in general: the one is to carry out Strecker reaction by iminodiacetonitrile or iminodiacetic acid and cyanide and acetaldehyde, then obtain product through hydrolysis; Where...

Claims

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Application Information

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IPC IPC(8): C07C227/18C07C229/16
CPCC07C227/18C07C229/16
Inventor 敬元元马高奇邱培辉贺潇潇卢亚楠原金妮
Owner HENAN QINGSHUIYUAN TECH
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