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Method for producing ethylene glycol-bis (2-aminoethyl ether) tetraacetic acid (EGTA)

A production method, the technology of disodium iminodiacetic acid, which is applied in chemical instruments and methods, the preparation of organic compounds, organic chemistry, etc., can solve the problems that the purity of EGTA cannot meet the requirements of biochemical reagents, etc., so as to improve the yield and equipment Utilization rate, simple reaction principle, and the effect of reducing the concentration of organic matter

Inactive Publication Date: 2010-12-01
HUZHOU XULONG BIOCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the purity of EGTA produced by existing technologies at home and abroad often does not meet the requirements of biochemical reagents

Method used

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  • Method for producing ethylene glycol-bis (2-aminoethyl ether) tetraacetic acid (EGTA)
  • Method for producing ethylene glycol-bis (2-aminoethyl ether) tetraacetic acid (EGTA)
  • Method for producing ethylene glycol-bis (2-aminoethyl ether) tetraacetic acid (EGTA)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Put glycerin into a 500-liter dry reaction pot first, then put in disodium iminodiacetate and sodium carbonate, then slowly raise the temperature to 60°C, then slowly add dichlorotriethyl ether dropwise, and then slowly raise the temperature to 99°C Keep at ℃ for more than 5 hours, then slowly cool naturally to 50℃, slowly add hydrochloric acid dropwise until the pH is 5, slowly raise the temperature to 90℃, filter it into another reaction pot with a filter rod, and then add hydrochloric acid dropwise To pH 1, after standing for 8 hours, add 2 times the amount of water, stir for 20 minutes, dry with a centrifuge, rinse with a large amount of water, rinse with an appropriate amount of methanol, and dry with a centrifuge to obtain a crude product; Dissolve the crude product in boiling water and reflux for about 1 to 1.5 hours; then pour in excess water, stir for 7 hours under boiling, cool to room temperature, then centrifuge, dehydrate and dry to obtain the finished produ...

Embodiment 2

[0029] Put glycerin into a 500-liter dry reaction pot first, then put in disodium iminodiacetate and sodium carbonate, then slowly raise the temperature to 65°C, then slowly add dichlorotriethyl ether dropwise, and slowly raise the temperature to 101 Keep at ℃ for more than 5 hours, then slowly cool naturally to 60℃, slowly add hydrochloric acid dropwise until the pH is 7, slowly raise the temperature to 95℃, filter it into another reaction pot with a filter rod, and then add hydrochloric acid dropwise until the pH is 1.5, after standing for 10 hours, add 4 times the amount of water, stir for 40 minutes, dry with a centrifuge, rinse with a large amount of water, rinse with an appropriate amount of methanol, and dry with a centrifuge to obtain a crude product; Dissolve the crude product in boiling water and reflux for about 2 to 3 hours; then pour in excess water, stir for 9 hours in a boiling state, cool to room temperature, then centrifuge, dehydrate and dry to obtain the fini...

Embodiment 3

[0031] Put glycerin into a 500-liter dry reaction pot first, then put in disodium iminodiacetate and sodium carbonate, then slowly raise the temperature to 60°C, then slowly add dichlorotriethyl ether dropwise, and then slowly raise the temperature to 100°C Keep at ℃ for more than 5 hours, then slowly cool naturally to 55℃, slowly add hydrochloric acid dropwise until there is no solid content in the liquid, then slowly increase the temperature to 90℃, filter it into another reaction pot with a filter stick, and then Then add hydrochloric acid dropwise until the pH is 1, and after standing for 12 hours, add 3 times the amount of water, stir for 30 minutes, dry it with a centrifuge, rinse with a large amount of water, rinse with an appropriate amount of methanol, and shake it with a centrifuge. Dry to obtain the crude product; dissolve the crude product in boiling water and reflux for about 2 to 3 hours; then pour in excess water, stir for 8 hours in a boiling state, cool to room...

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Abstract

The invention relates to a method for synthesizing a chelating reagent commonly used in the chemistry, medicine or molecular biology, in particular to a method for producing ethylene glycol-bis (2-aminoethyl ether) tetraacetic acid (EGTA) and belongs to the technical field of fine chemical engineering. In the method for producing the EGTA, disodium iminodiacetate and triethylene glycol dichlorideare taken as production raw materials, parameters such as temperature, pH and the like in a production process are controlled strictly to synthesize the EGTA at the same time, and the purification ofthe EGTA is realized by a boiling water rinsing method. The EGTA prepared by the method of the invention has the advantage of high purity.

Description

technical field [0001] The invention relates to a synthesis method of a chelating reagent commonly used in chemistry, medicine or molecular biology, in particular to a production method of EGTA, and belongs to the technical field of fine chemicals. Background technique [0002] The chemical name of EGTA is ethylene glycol diether (2-aminoethyl) tetraacetic acid, the chelating property is similar to EDTA, but it has a higher Ca than EDTA 2+ Choose Complexity. The magnesium complex of EGTA is very unstable, while the calcium complex of EGTA is still very stable. 2+ Determination of Ca in the presence of 2+ EGTA can be used for direct titration, ΔlgK=10.97-5.21=5.76>5, and the titration error is less than 0.3%. Therefore, choosing EGTA as the titrant is beneficial to improve the selectivity. In addition, the stability of its complexes with other metal ions is generally worse than that of the corresponding EDTA complexes. Therefore, EGTA has wider application value. Howe...

Claims

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Application Information

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IPC IPC(8): C07C229/16C07C227/18
Inventor 褚刚文
Owner HUZHOU XULONG BIOCHEM
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