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Catalyst for preparing ethylene diamine through amination of ethylene glycol and preparation method thereof

A catalyst, ethylenediamine technology, applied in the field of catalysts, can solve problems such as easy sintering, heat sensitivity, and deactivation of copper-based catalysts

Inactive Publication Date: 2011-11-09
ZHANGJIAGANG HUIER CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0017] A good catalyst for alcohol dehydrogenation is a copper-based catalyst. There are two problems with the copper-based catalyst in this dehydrogenation reaction. One is ammonia poisoning, and the other is heat sensitivity. The reaction is an exothermic reaction. At high temperatures, copper-based The catalyst is easily sintered and deactivated

Method used

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Effect test

preparation example Construction

[0037] The preparation method of the catalyst is not limited to the steps of reduction and recalcination once. In order to pursue better catalyst activity and stability, after the catalyst undergoes calcination, reduction, and re-calcination, it can go through the process of second reduction and third calcination. The performance of the obtained catalyst will be better, but the effect will increase with the reduction , The number of re-roasting process increases and weakens.

[0038] The role of reduction and recalcination is to better disperse the metal components in the catalyst and form a specific crystal form. This crystal form makes the metal components work better together to achieve better activity and stability of the catalyst. .

[0039] The preparation method of catalyst is as follows:

[0040] Prepare 0.5-1 mol / liter copper nitrate and nickel nitrate solution, 0.5-1 mol / liter zirconium oxychloride solution, and 0.5-1 mol / liter nitric acid solution of other metals,...

Embodiment 1

[0048] The metal components are copper 40%, nickel 30%, zirconium 30% catalyst, prepared by co-precipitation method, only calcined at 500 ° C for 12 hours, the result of activity evaluation is that the conversion rate of ethylene glycol is 46%, and the conversion rate of ethylenediamine is 46%. Selectivity 52%. After being reduced by a mixed gas of hydrogen and nitrogen containing 10% hydrogen, and then calcined at 300°C for 24 hours, the conversion rate of ethylene glycol is 66%, and the selectivity of ethylenediamine is 73%.

Embodiment 2

[0050] The metal components are 30% copper, 20% nickel, 15% zirconium, 20% cerium, and 15% manganese. The catalyst is prepared by co-precipitation method and calcined at 500°C for 12 hours. The result of activity evaluation is that ethylene glycol conversion The rate is 55%, and the selectivity of ethylenediamine is 61%. After being reduced by a mixed gas of hydrogen and nitrogen containing 10% hydrogen, and then calcined at 300°C for 24 hours, the conversion rate of ethylene glycol is 68%, and the selectivity of ethylenediamine is 78%.

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Abstract

The invention provides a solid catalyst for preparing ethylene diamine through catalytic amination of ethylene glycol. The catalyst takes copper and nickel as main components and zirconium as an auxiliary component; and other metal components can be one or more than one of zinc, aluminum, titanium, manganese and cerium. The invention further provides a preparation method of the solid catalyst. The preparation method is characterized in that the catalyst is prepared through the processes of roasting, reducing and re-roasting by utilizing a coprecipitation method.

Description

technical field [0001] The invention relates to a catalyst mainly composed of copper and nickel, which catalyzes the reaction of ethylene glycol and ammonia hydroamination to prepare ethylenediamine. The reaction equation is as follows: [0002] HOCH 2 CH 2 OH+2NH 3 -->NH 2 CH 2 CH 2 NH 2 +2H 2 o [0003] The preparation method of the catalyst involved in the invention is an improved co-precipitation method, and the method of the invention improves the roasting process in the co-precipitation method to roasting, reduction and re-calcining. technical background [0004] Ethylenediamine is an important basic chemical raw material, used as solvent, stabilizer, chelating agent, synthetic resin, drug, inhibitor. In recent years, as the demand for TEAD (tetraacetylethylenediamine) used in phosphorus-free detergents has greatly increased, the demand for ethylenediamine as a raw material for TEAD has increased accordingly. [0005] Methods for the preparation of ethyle...

Claims

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Application Information

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IPC IPC(8): B01J23/755B01J23/889B01J23/80B01J23/83B01J37/03C07C211/10C07C209/16
Inventor 左卫雄刘胜
Owner ZHANGJIAGANG HUIER CHEM TECH
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