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Synthesis method of triethylene diamine from piperazine by product

A technology of triethylenediamine and by-products, applied in the direction of organic chemistry, etc., can solve problems such as low yield of triethylenediamine

Inactive Publication Date: 2004-03-03
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing TEDA synthesis technology basically uses a single raw material as a reactant, and the yield of triethylenediamine is also low except for the process using hydrogen phosphate as a catalyst. Therefore, it is necessary to study the synthesis process of TEDA

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0029] Add 450ml of deionized water to the mixture of 100g of barium nitrate, 100g of strontium nitrate, 50g of copper nitrate and 50g of magnesium nitrate to completely dissolve the nitrate, then dropwise add 250ml of saturated diammonium hydrogen phosphate solution to the system to precipitate the nitrate in the solution After the reaction is completed, the desired catalyst is obtained by standing, filtering, washing, drying and shaping. Example 2:

example 2

[0030] 80g barium nitrate, 50g strontium nitrate, 50g copper nitrate and 180g γ-Al 2 O 3 Add 300ml of deionized water to the mixture to dissolve the nitrate completely, then add 180ml of saturated diammonium hydrogen phosphate solution dropwise to the system to precipitate the nitrate in the solution. get the required catalyst. Example 3:

example 3

[0031] Use a metering pump to input a 40% aqueous solution of the piperazine by-product at a speed of 0.5ml / min, vaporize it through preheating, pass through a catalyst bed containing 25g of catalyst, the reaction temperature is 300 ° C, and the obtained reaction mixture Analysis contained 23.7% piperazine, 32.7% N-hydroxyethylpiperazine, and 28.5% triethylenediamine.

[0032] After diluting 200 g of the reaction mixture obtained in the previous step with 100 ml of water, heated to boiling, passed ethylene oxide at a speed of 40 ml / min, reacted for 2 h, and then analyzed by gas chromatography to obtain that the reaction solution contained 0.8% piperazine. , hydroxyethylpiperazine 27.5%, dihydroxyethylpiperazine 23.2%, triethylenediamine 24.3%

[0033] After the reaction mixture obtained in the previous step was diluted with 50 ml of water, it was passed into a catalyst bed containing 25g of catalyst at a speed of 0.4ml / min, and the reaction temperature was 320 ° C. The obtaine...

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PUM

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Abstract

A process for synthesizing the trivinyldiamine from the by-product of piperazine, which is the mixture of N-beta-hydroxyethyl piperazine, N-beta-hydroxyethyl ethanediamine, N-beta-aminoethyl piperazine, and pinerazine, includes primary catalytic reaction, hydroxyethylating reaction, and secondary catalytic reaction. Its advantages are long service life of catalyst, high output rate, and high purity.

Description

technical field [0001] The invention belongs to a synthesis process of polyurethane catalyst triethylenediamine, specifically a method for synthesizing triethylenediamine from a by-product of synthesizing piperazine. Background technique [0002] Triethylenediamine (TEDA) is the most widely used catalyst with the best performance among the polyurethane foaming amine catalysts. There are many foreign patents related to the research on the synthesis process of triethylenediamine. According to the different raw materials used, there are mainly two synthetic routes, using chain amine and cyclic amine as raw materials respectively, and the catalysts used are zeolite catalysts modified by zeolite and metal ions, metal oxide catalysts, and phosphoric acid of alkali metals and alkaline earth metals. Salt catalysts, etc. For example, US 4,017,494 reports the use of Al 2 O 3 It is a process route for synthesizing triethylenediamine as a catalyst; patents suc...

Claims

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Application Information

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IPC IPC(8): C07D487/08
Inventor 陈立功白国义李阳宋健王东华
Owner TIANJIN UNIV
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