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Method for reclaiming diglycolamidic acid from acidified mother liquor of diglycolamidic acid

A technology of iminodiacetic acid and iminodiacetic acid calcium, applied in organic chemistry, oxime preparation, etc., can solve the problems of high cost and complicated process, and achieve the effect of low recycling cost, simple process and cheap price

Inactive Publication Date: 2005-09-07
NANJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are many research reports at home and abroad on the recovery method of iminodiacetic acid in the mother liquor, such as adopting the recovery methods such as step-by-step concentration crystallization method, ion exchange method, electrodialysis technology, and adding alkali metal sulfate. These methods are either complicated in technology or high cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1: Get 100ml of iminodiacetic acid saturated solution (containing 6g of iminodiacetic acid, the same below.) Stir in a 250ml beaker, slowly add 3.5g Ca(OH) 2 , adjust the pH value of the solution to 11.67 with hydrochloric acid. The solution was transferred to a 250ml three-necked flask, stirred and reacted at 80°C for 1 hour, allowed to stand, cooled, and suction filtered to obtain 7.25g of calcium iminodiacetic acid wet filter cake with a content of 80.0% and a calcium salt yield of 79.1%.

Embodiment 2

[0018] Embodiment 2: Get 100ml iminodiacetic acid saturated solution and stir in 250ml beaker, slowly add 3.5gCa(OH) 2 , adjust the pH value of the solution to 11.67 with hydrochloric acid. The solution was transferred to a 250ml three-necked flask, stirred and reacted at 90°C for 1 hour, allowed to stand, cooled, and suction filtered to obtain 6.75g of calcium iminodiacetic acid wet filter cake with a content of 81.4% and a calcium salt yield of 71.2%.

Embodiment 3

[0019] Embodiment 3: Get 100ml iminodiacetic acid saturated solution and stir in 250ml beaker, slowly add 3.5gCa(OH) 2 , adjust the pH value of the solution to 11.67 with hydrochloric acid. Transfer the solution into a 250ml three-necked flask, stir and react at 80°C for 2h, let stand, cool, and filter with suction to obtain 7.85g of calcium iminodiacetate wet filter cake with a content of 82.2% and a calcium salt yield of 83.7%.

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PUM

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Abstract

The invention discloses a method for reclaiming diglycolamidic acid from acidified mother liquor of diglycolamidic acid, which comprises charging calcium salts into iminodiacetic acid acidulation mother liquid, wherein the mole ration of the iminodiacetic acid and the calcium salts is 1:1.0-1:1.8, adjusting and controlling pH between the range of 10.0-11.67, carrying out complex reaction at the temperature of 70-90 deg. C, filtering the reaction solution, obtaining iminodiacetic acid calcium and charging hydrochloric acid, so as to obtain iminodiacetic acid, finally cooling down for crystallization. The mol ratio of iminodiacetic acid calcium and HCL is 1:2-1:5.

Description

technical field [0001] The invention relates to a method for recovering iminodiacetic acid from iminodiacetic acid acidification mother liquor. Background technique [0002] Iminodiacetic acid is an important intermediate in fine chemical industry. Its largest consumption is the production of the herbicide glyphosate. Because of the chelating effect of iminodiacetic acid and metal ions, it is also widely used in process water treatment in the fields of electroplating, chemical plating, electronics, medical treatment, pharmaceuticals, and atomic energy. The production method of iminodiacetic acid has many processes according to the use of different starting materials. However, most of the processes first generate iminodiacetic acid sodium salt, and then acidify with hydrochloric acid to obtain iminodiacetic acid product. Due to the solubility, the acidified mother liquor still contains a certain amount of iminodiacetic acid. There are many research reports at home and abr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C249/14C07C251/08
Inventor 彭盘英王玉萍刘勇
Owner NANJING NORMAL UNIVERSITY
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