Method used for electrochemical reduction preparation of diethylenetriamine from iminodiacetonitrile

A technology of iminodiacetonitrile and diethylenetriamine, applied in electrolysis process, electrolysis components, electrolysis organic production and other directions, can solve the problems of low selectivity of target products, deactivation of catalysts, etc. The effect of mild conditions and simple product separation process

Active Publication Date: 2019-11-12
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the problem is that the selectivity of the target product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The electrolytic reaction is carried out in an H-type electrolytic cell, which includes an anode pool and a cathode pool, and the volume of the anode pool and the cathode pool is 150mL. The anode pool and the cathode pool are separated by a cation exchange membrane, and the cation exchange membrane is DuPont's Nafion100. The cathode is a lead electrode and the anode is a graphite electrode.

[0031] Add 100g of catholyte in the catholyte, containing 5g of 98% sulfuric acid and 5g of IDAN in the catholyte, then add cobalt chloride accounting for one millionth of the total mass of the catholyte in the catholyte. Add dilute sulfuric acid with a concentration of 1wt% into the anode pool until the liquid level of the catholyte is equal to that of the catholyte. The electrolysis reaction temperature is controlled at 20°C, and the current density is 5mA / cm 2 . After no bubbles are produced at the anode, stop the reaction.

[0032] 100 mL of dioxane was added to the obtaine...

Embodiment 2

[0034] The electrolytic reaction is carried out in an H-type electrolytic cell, which includes an anode pool and a cathode pool, and the volume of the anode pool and the cathode pool is 150mL. The anode pool and the cathode pool are separated by a cation exchange membrane, and the cation exchange membrane is F775 of Asahi Glass. The cathode is a lead electrode and the anode is a 316L stainless steel electrode.

[0035] Add 100g of catholyte in the cathodic pool, containing 41g of 98% sulfuric acid and 20g of IDAN in the catholyte, then add cobalt chloride in the cathodic pool, after adding, cobalt chloride accounts for 2.5ppm of the total mass of the system. Add dilute sulfuric acid with a concentration of 5wt% into the anode pool until the liquid level of the catholyte is equal to that of the catholyte. The electrolysis reaction temperature is controlled at 50°C, and the current density is 20mA / cm 2 . After no bubbles are produced at the anode, stop the reaction.

[0036]...

Embodiment 3

[0038] The electrolytic reaction is carried out in an H-type electrolytic cell, which includes an anode pool and a cathode pool, and the volume of the anode pool and the cathode pool is 150mL. The anode pool and the cathode pool are separated by a cation exchange membrane, and the cation exchange membrane is DuPont Nafion's Nx-961. The cathode is a Pb / Hg electrode, and the anode is a graphite electrode.

[0039] Add 100g catholyte in the cathode pool, catholyte contains 98% sulfuric acid 17.1g, contains IDAN 12.5g, then adds cobalt chloride in the cathode pool, after adding, cobalt chloride accounts for 5ppm of system gross mass. Add dilute sulfuric acid with a concentration of 3wt% to the anode pool until the liquid level of the catholyte is equal to that of the catholyte. The electrolysis reaction temperature is controlled at 35°C, and the current density is 15mA / cm 2 . After no bubbles are produced at the anode, stop the reaction.

[0040] Add 100 mL of dioxane to the o...

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PUM

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Abstract

The invention provides a method used for electrochemical reduction preparation of diethylenetriamine from iminodiacetonitrile. According to the method, in an electrolytic tank, iminodiacetonitrile dissolved in a cathode liquid is subjected to electrolytic reaction on a cathode to produce diethylenetriamine. Electrochemical reduction is adopted, iminodiacetonitrile can be converted into diethylenetriamine at high selectivity, and generation of secondary amines such as piperazine is avoided. Iminodiacetonitrile is stable at partially acidic conditions, so that iminodiacetonitrile decomposition problem in the prior art is avoided, problems in the prior art that catalyst positioning is caused by iminodiacetonitrile decomposition products and continuous reaction is impossible to realize are solved. The reaction conditions are mild; diethylenetriamine product yield is high; product separation technology is simple; and industrialized application prospect is promising.

Description

technical field [0001] The invention belongs to the technical field of synthesis of organic amines, and relates to a method for preparing diethylenetriamine by electrochemically reducing iminodiacetonitrile. Background technique [0002] Diethylenetriamine (Diethylenetriamine), molecular formula C 4 h 13 N 3 , referred to as DETA, alias N 1 -(2-aminoethyl)-1,2-ethylenediamine, commonly known as diethylenetriamine, diethylenetriamine, diethylenetriamine, diethylenetriamine, etc., is a saturated fatty amine, yellow Hygroscopic transparent viscous liquid with irritating ammonia odor, easy to absorb moisture and carbon dioxide in the air. It is mainly used as a solvent and organic synthesis intermediate, and can be used to prepare carbon dioxide absorbers, lubricating oil additives, emulsifiers, photographic chemicals, surfactants, fabric finishing agents, paper strengthening agents, ammonia carboxy complexing agents, ashless additives , metal chelating agent, heavy metal h...

Claims

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Application Information

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IPC IPC(8): C25B3/04C25B3/25
CPCC25B3/25
Inventor 陈长生杜旺明刘释水李俊平黎源华卫琦
Owner WANHUA CHEM GRP CO LTD
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