Method of preparing ethylenediamine tetracetonitrile and ethylenediamine tetraacetic acid using hydroxy acetonitrile as raw material

A technology of ethylenediaminetetraacetonitrile and ethylenediaminetetraacetic acid, applied in the field of preparation of ethylenediaminetetraacetonitrile, can solve the problems of low price, high cost and poor safety of chloroacetic acid

Inactive Publication Date: 2007-05-23
SOUTHWEST UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] GB871380, JP55151537, etc. introduce the synthesis of EDTA with high-purity liquid hydrocyanic acid, ethylenediamine, and formaldehyde as raw materials. High-purity liquid hydrocyanic acid also has high cost and poor safety.
"Shandong Chemical Industry" 1994(4), pp. 24-25; "Zhejiang Chemical Industry" 1988(6), pp. 25-26 and "Guangzhou Food Industry Science and Technology" 15(1), pp. 15-46, 1999, introduction Ethylenediamine, chloroacetic acid, sodium carbonate, etc. are used as raw materials to prepare EDTA, because the price of chloroacetic acid is not competitive and the cost is high

Method used

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  • Method of preparing ethylenediamine tetracetonitrile and ethylenediamine tetraacetic acid using hydroxy acetonitrile as raw material
  • Method of preparing ethylenediamine tetracetonitrile and ethylenediamine tetraacetic acid using hydroxy acetonitrile as raw material
  • Method of preparing ethylenediamine tetracetonitrile and ethylenediamine tetraacetic acid using hydroxy acetonitrile as raw material

Examples

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Embodiment 1

[0022] In a three-neck round bottom flask equipped with a thermometer, reflux condenser, and constant pressure dropping funnel, adjust the pH of 6.7ml (6g, 0.1mol) of ethylenediamine solution to 6-8 with concentrated hydrochloric acid, and add it dropwise at room temperature 30ml (0.2mol) of hydroxyacetonitrile, the temperature was raised to 40°C-50°C, and the temperature was kept at 20°C-60°C for more than 30min (dropping and reacting for 1 hour). Heat up to 60°C-100°C, add 34ml (0.24mol) of hydroxyacetonitrile dropwise, react at 60°C-100°C for 3 hours, add saturated NaHCO 3 The pH was adjusted to about 6, and the reaction was continued for 3 hours. After cooling, suction filtration, washing and drying, EDTN was obtained, 18.4g (85% yield), with a melting point of 132-134°C. The product was confirmed by NMR and IR.

[0023] Dissolve 5.4g (25mmol) of EDTN obtained above in 10.3ml of 30% NaOH solution, stir at 40°C for 30min, heat to a slight boil, drive out most of the ammoni...

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Abstract

A process for preparing ethyldiamine tetraacetonitrile and ethyldiamine tetraacetic acid includes such steps as regulating the pH value of ethyldiamine solution to 6-8, adding hydroxyacetonitrile, reacting to obtain ethyldiamine diacetonitrile, heating to 60-100 deg.C, adding hydroxyaceto nitrile reacting to generate ethyldiamine tetraacetonitrile, cooling, filter, hydrolyzing in alkaline aqueous solution to obtain ethyldiamine tetraacetate, and adding acid to make pH=1-3 for obtaining ethyldiamine tetraacetic acid.

Description

technical field [0001] The invention relates to a method for preparing ethylenediaminetetraacetonitrile (EDTN), ethylenediaminetetraacetic acid (EDTA) and salts from hydroxyacetonitrile. Background technique [0002] Ethylenediaminetetraacetonitrile is the precursor of ethylenediaminetetraacetic acid (EDTA), and EDTA can be obtained after acid hydrolysis or alkali hydrolysis and acidification. EDTA has a wide range of uses. It is often used as a bleaching and fixing agent in the processing of color photosensitive materials. It is also used as a dyeing aid, fiber processing aid, cosmetic additive, metal ion complexation and separation masking agent, detergent, stabilizer, Synthetic rubber polymerization initiator, etc. EDTA is a representative substance of chelating agent, which can form extremely stable water-soluble complexes with alkali metals, rare earth elements and transition metals. In addition to sodium salts, there are amine salts and various salts such as iron, ma...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/24C07C253/30C07C229/16C07C227/26
Inventor 彭云贵田金平孟祥林吉昌云郑长春李星尹应武
Owner SOUTHWEST UNIV
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