Method for preparing iminodiacetic acid from iminodiacetic acid disodium salt

A technology of disodium iminodiacetic acid and sodium iminodiacetic acid, which is applied in the field of preparation of iminodiacetic acid, can solve the problems of low operating efficiency, large equipment investment, cumbersome process, etc., and achieve saving investment and energy consumption, and production cycle Short, easy-to-use effects

Active Publication Date: 2009-06-03
GUANGXI RES INST OF CHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Another example is the ion exchange method, electrodialysis technology, sodium filtration membrane technology, etc. reported at home and abroad. Either the equipment investment is large, the energy consumption is high, or the process is cumbersome and the operation efficiency is low.

Method used

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  • Method for preparing iminodiacetic acid from iminodiacetic acid disodium salt
  • Method for preparing iminodiacetic acid from iminodiacetic acid disodium salt
  • Method for preparing iminodiacetic acid from iminodiacetic acid disodium salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Weigh 200g of disodium iminodiacetic acid solid, add 150ml of tap water, stir and dissolve at 35-40°C, then slowly drop about 70ml into the filtrate with a stirring speed of 100r / min and a flow rate of 10ml / min. The mass concentration is 35-37 % hydrochloric acid, adjust pH = 1.98, iminodiacetic acid crystallizes out, let it stand for 10 minutes, filter to obtain IDA, dry at 100-105°C, and weigh to obtain a qualified product. Filtrate pH = 2.3, add 50ml of hydrochloric acid with a mass concentration of 35-37% to the filtrate, adjust pH = 1.35, concentrate in vacuo until a large amount of salt precipitates, filter with suction, dry and weigh the obtained salt and detect its content, and the filtrate is circulated to dissolve The second batch of iminodiacetic acid disodium solids, and thus repeated circulation 15 times. In the experiment, the total yield of IDA was 97.6%, the content was 98.7%, and the salt removal rate was 99.2%.

Embodiment 2

[0031] Weigh 200g of disodium iminodiacetic acid solid, add 180ml of tap water, stir and dissolve at 35-40°C, then slowly drop about 70ml into the filtrate with a stirring speed of 200r / min and a flow rate of 10ml / min. The mass concentration is 35-37 % hydrochloric acid, adjust the pH=1.95, iminodiacetic acid crystals precipitate out, stand still for 20 minutes, filter to obtain IDA, dry at 100-105°C, and weigh to obtain a qualified product, the filtrate pH=2.4. Add 50ml of hydrochloric acid with a mass concentration of 35-37% to the filtrate, adjust pH=1.32, concentrate in vacuo until a large amount of salt precipitates, filter with suction, dry and weigh the obtained salt, and detect its content, and the filtrate circulates to dissolve the second batch of sub Aminodiacetic acid disodium solid, and thus repeated cycle 25 times. In the experiment, the total yield of IDA was 98.1%, the content was 98.5%, and the salt removal rate was 98.2%.

Embodiment 3

[0033]Weigh 200g of disodium iminodiacetic acid solid, add 150ml of tap water, stir and dissolve at 35-40°C, then slowly drop about 70ml into the filtrate with a stirring speed of 200r / min and a flow rate of 10ml / min. 37% hydrochloric acid, adjust pH=1.98, iminodiacetic acid crystallizes out, stand still for 15 minutes, filter to obtain IDA, dry at 100-105°C, weigh to obtain qualified product, filtrate pH=2.5. Add 60ml of hydrochloric acid with a mass concentration of 35-37% to the filtrate, adjust pH=1.30, concentrate in vacuo until a large amount of salt is precipitated, filter with suction, dry and weigh the obtained salt, and detect its content, and circulate the filtrate to dissolve the second batch of sub Aminodiacetic acid disodium solid, and thus repeated 15 times. In the experiment, the total yield of IDA was 97.9%, the content was 98.3%, and the salt removal rate was 98.5%.

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Abstract

The invention discloses a method for preparing iminodiacetic acid from iminodiacetic acid disodium salt. The method comprises the following steps: acidifying aqueous solution of the iminodiacetic acid disodium salt by hydrochloric acid until pH of the aqueous solution is a little less than an isoelectric point of the iminodiacetic acid, wherein, the pH equals 1.9-2.1; standing to separate the iminodiacetic acid out; filtering followed by drying to obtain a dry product; adding a fixed volume of the hydrochloric acid to the filtrate until the pH of the filtrate equals 1.3-1.5; condensing the filtrate to separate sodium chloride out, and filtering to remove the sodium chloride; dissolving the iminodiacetic acid disodium salt solid of the second batch in acid pregnant liquor; and repeating the steps to prepare the iminodiacetic acid product. The method has the characteristics of simple and short process route, convenient operation, little wastes (waste gas, waste water and industrial residue), lower equipment investment and energy consumption, and obvious economic and social benefits.

Description

technical field [0001] The invention relates to a method for preparing iminodiacetic acid, an intermediate of chemical products, in particular to a method for preparing iminodiacetic acid using disodium salt of iminodiacetic acid as a raw material. Background technique [0002] Iminodiacetic acid is an important intermediate of the pesticide glyphosate. Glyphosate has not only become the world's largest herbicide in production and sales for many years, but also has an annual production and sales growth rate of 18% to 20%. The strong sales momentum of glyphosate makes iminodiacetic acid one of the few chemical intermediates in short supply in China. [0003] At present, there are many methods for synthesizing iminodiacetic acid at home and abroad, but the final process is to synthesize iminodiacetic acid sodium salt, and then obtain iminodiacetic acid through acidification, and simultaneously produce a large amount of sodium salt. Due to the solubility, the mother liquor sti...

Claims

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Application Information

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IPC IPC(8): C07C229/16C07C227/18C07C227/38
Inventor 王俊莫炳辉曾觉发李华锋柯珂
Owner GUANGXI RES INST OF CHEM IND CO LTD
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