Triethylene diamine synthesis method

A technology of triethylenediamine and its synthesis method, which is applied in the direction of chemical instruments and methods, molecular sieve catalysts, physical/chemical process catalysts, etc., can solve the problems affecting the yield of triethylenediamine, affecting catalytic activity, catalyst poisoning, etc., to achieve Effects of reducing acidity and acid content, increasing product yield, and lowering reaction temperature

Inactive Publication Date: 2017-09-15
SHAOXING XINGXIN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The reaction of synthesizing triethylenediamine usually needs to be completed under the catalysis of an acidic catalyst, but if the catalyst is too acidic, many side reactions may occur and a large amount of carbon deposits will be generated
On the one hand, the occurrence of side reactions will seriously affect the yield of triethylenediamine, on the other hand, carbon deposition will poison the catalyst and affect its catalytic activity and service life

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0040] 1. Preparation of modified molecular sieve catalyst

[0041] (1) Get 14.7g barium nitrate and join in 46.2ml water, stir and make it be dissolved in water completely, obtain barium nitrate aqueous solution;

[0042] (2) Get 30.0g of powdery HZSM-5 all-silicon molecular sieves and impregnate them in the aqueous solution of barium nitrate for 3 times, each time for 4 hours; Appropriate amount of water extrusion molding;

[0043] (3) The molded catalyst was calcined at 800° C. for 3 hours to obtain a modified molecular sieve catalyst with an alkaline earth metal content of 20 wt %.

[0044] Two, the synthesis of triethylenediamine

[0045] Continuous operation is carried out in a single-tubular fixed-bed reactor, and the aqueous solution containing 90wt% ethylenediamine is preheated and gasified; -1 The mass space velocity of the gas is passed through a bed layer equipped with a modified molecular sieve catalyst to carry out a contact reaction at a reaction temperature ...

Embodiment 2

[0055] 1. Preparation of modified molecular sieve catalyst

[0056] (1) Get 6.4g strontium nitrate and join in 15.4ml water, stir to make it dissolve in water completely, obtain strontium nitrate aqueous solution;

[0057] (2) Take 30.0g of powdered HZSM-5 molecular sieve with a silicon-aluminum ratio of 800 and immerse it in the aqueous solution of strontium nitrate for 12 hours; after the immersion is finished, dry it, then add 0.9g of binder scallop powder and an appropriate amount of water to extrude forming;

[0058] (3) The molded catalyst was calcined at 800° C. for 3 hours to obtain a modified molecular sieve catalyst with an alkaline earth metal content of 8 wt %.

[0059] Two, the synthesis of triethylenediamine

[0060] Continuous operation is carried out in a single-tubular fixed-bed reactor, and the aqueous solution containing 50wt% ethylenediamine and 20wt% 2-hydroxyethylamine is preheated and gasified; -1 The mass space velocity of the gas is passed through t...

Embodiment 3

[0070] 1. Preparation of modified molecular sieve catalyst

[0071] (1) Get 5.2g calcium nitrate and join in 30.8ml water, stir to make it dissolve in water completely, obtain calcium nitrate aqueous solution;

[0072] (2) Take 30.0g of powdery HZSM-5 molecular sieve with a silicon-aluminum ratio of 200 and impregnate it in the calcium nitrate aqueous solution, and impregnate twice, each time for 4 hours; after the impregnation, dry it, and add 0.9g of binder Squash powder and appropriate amount of water to extrude;

[0073] (3) The molded catalyst was calcined at 550° C. for 5 hours to obtain a modified molecular sieve catalyst with an alkaline earth metal content of 4 wt %.

[0074] Two, the synthesis of triethylenediamine

[0075] Continuous operation is carried out in a single-tubular fixed-bed reactor, and the aqueous solution containing 5wt% piperazine is preheated and gasified; -1 The mass space velocity of the gas is passed through the bed layer equipped with a modi...

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Abstract

The invention discloses a triethylene diamine synthesis method, which comprises the following steps of performing preheating gasification on a water solution of raw materials; then, at 180 to 400 DEG C, performing contact reaction with modified molecular sieve catalysts to obtain triethylene diamine, wherein the modified molecular sieve catalysts are obtained by soaking HZSM type molecular sieves into a water solution of alkaline earth metal compounds and then performing drying and roasting; the raw materials are at least one kind of materials from piperazidine, piperazidine derivatives, straight chain alcohol amine and amines. The molecular sieve catalysts are modified through the alkaline earth metal, so that the acidity and the acid size of Brphinsted acid on the surfaces of the molecular sieve catalysts are obviously reduced; the proportion of the Lewis acid sites is improved; the reaction temperature is greatly lowered; the universality of the catalysts is good; the product yield is improved. Compared with a conventional triethylene diamine synthesis method, the triethylene diamine synthesis method achieves economic effects, green effects and high efficiency.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a synthesis method of triethylenediamine. Background technique [0002] In recent years, with the increasingly wide range of applications, the polyurethane foam industry has developed rapidly. As its hardener, the market demand for triethylenediamine (TEDA) hits new highs; not only that, triethylenediamine (TEDA) can also be used as an ethylene polymerization catalyst and an ethylene oxide polymerization catalyst; its derivatives can also be used For emulsifiers and corrosion inhibitors. Therefore, the synthesis of triethylenediamine has been widely concerned by scientists. [0003] The US patent US6350874 reports the technology of using chain or cyclic amines as raw materials and using zeolite molecular sieves as catalysts to co-produce triethylenediamine and piperazine. However, the process reaction conditions are severe and the yield of triethylenediamine is not ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/08B01J29/40
CPCC07D487/08B01J29/40B01J2229/186
Inventor 叶汀袁斌炜刘帅
Owner SHAOXING XINGXIN CHEM
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