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Catalyst for amination of ethanolamine to sysnthsize ethylene diamine and preparation method thereof

A technology of ethanolamine amine and catalyst, which is applied in the field of catalyst and its preparation for the amination of ethanolamine to ethylenediamine, which can solve the problems of polluted products, difficult separation, increased process operation complexity and production cost, and achieve high activity and selectivity , good mechanical strength and stability, excellent selectivity effect

Active Publication Date: 2012-05-02
GUANGXI RES INST OF CHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The conversion rate of ethanolamine and the selectivity of ethylenediamine of the catalyst are difficult to meet the requirements, and the repeated and continuous addition of precious metals in the preparation process increases the complexity of the process operation and the production cost.
[0007] US6534441 has reported a kind of Ni-Re-B / Al 2 o 3 Catalyst, which can increase the selectivity of ethylenediamine to 70% to 80%, but the loss of B in the reaction will pollute the product and cause difficulties in separation, and the addition of B makes the preparation process of the catalyst more complicated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1.1 Catalyst preparation

[0024] (1) 30.63gNi(NO 3 ) 2 , 12.45gCo(NO 3 ) 2 , 8.51gCu(NO 3 ) 2 , 11.53gCr(NO 3 ) 3 and 0.35g (NH 4 ) 3 ReO 5 respectively dissolved in deionized water to form a solution;

[0025] (2) Weigh 102.02g of small spherical Al 2 o 3 Carrier, Al 2 o 3 The specific surface area is 180m 2 / g, with a pore volume of 0.6ml / g, dried in a vacuum oven at 200°C for 2h, then mixed the dried carrier and the metal salt solution obtained in step (1) into a beaker and oscillated and impregnated in an ultrasonic wave for 2h;

[0026] (3) Filter off excess liquid to obtain a carrier that has adsorbed metal ions, dry it in a vacuum oven at 150°C for 3 hours, and then continue to impregnate it in the remaining solution;

[0027] (4) The carrier impregnated twice is calcined at 550-650° C. for 3 hours in a box-type resistance furnace to prepare the catalyst.

[0028] 1.2. Catalyst activation

[0029] The catalyst is reductively activated in a tubu...

Embodiment 2

[0040] 2.1. Catalyst preparation

[0041] (1) 35.86gNi(NO 3 ) 2 , 28.45gCo(NO 3 ) 2 , 7.09gCu(NO 3 ) 2 , 1.05gZn(NO 3 ) 2 and 0.52g (NH 4 ) 3 ReO 5 respectively dissolved in deionized water to form a solution;

[0042] (2) Weigh 99.60g TiO 2 Carrier, TiO 2 The specific surface area is 95m 2 / g, with a pore volume of 0.6ml / g, dried in a vacuum oven at 200°C for 2h, then mixed the dried carrier and the metal salt solution obtained in step (1) into a beaker and oscillated and impregnated in an ultrasonic wave for 1.5h;

[0043] (3) Filter off excess liquid, and dry the obtained metal ionophore adsorbed in a vacuum drying oven at 150° C. for 2 hours, and then continue to immerse in the remaining solution;

[0044] (4) The carrier impregnated twice is calcined at 500-600° C. for 4 hours in a box-type resistance furnace to prepare the catalyst.

[0045] 2.2. Catalyst activation and catalyst activity test The reaction process is the same as in Example 1.

[0046] The re...

Embodiment 3

[0053] 3.1 Catalyst preparation

[0054] (1) 33.24gNi(NO 3 ) 2 , 52.75gCo(NO 3 ) 2 , 13.82gCu(NO 3 ) 2 and 0.52g (NH 4 ) 3 ReO 5 respectively dissolved in deionized water to form a solution;

[0055] (2) Weigh 93.60g SiO2 2 -Al 2 o 3 Carrier, SiO 2 -Al 2 o 3 The specific surface area is 150m 2 / g, the pore volume is 0.5ml / g, dry in a vacuum oven at 200°C for 2h, then mix the dried carrier and the metal salt solution obtained in step (1) into a beaker and oscillate and impregnate in an ultrasonic wave for 3h;

[0056] (3) Filter off excess liquid to obtain a carrier that has adsorbed metal ions, dry it in a vacuum oven at 150°C for 2.5 hours, and then continue to impregnate it in the remaining solution;

[0057] (4) The carrier impregnated twice is calcined at 450-550° C. for 6 hours in a box-type resistance furnace to prepare the catalyst.

[0058] 3.2. Catalyst Activation and Catalyst Activity Test The reaction process is the same as in Example 1.

[0059] T...

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Abstract

The invention discloses a catalyst for amination of ethanolamine to sysnthsize ethylene diamine and a preparation method thereof. The catalyst is prepared by using a Ni-Co bifunctional reactive component as a base stock and adding mixing metal of two or more of Cu, Fe, Zn, Cr and Re to be loaded on a porous material carrier, wherein in the catalyst, the content of the porous material carrier accounts for 65-90 percent by weight, and the content of the mixing metal accounts for 10-35 percent by weight. The preparation method of the catalyst comprises the steps of: dipping the porous material in a metal salt solution of Ni, Co, Cu and the like twice, and then roasting at high temperature. The service life of the catalyst lasts for 400 hours, the conversion rate of the ethanolamine reaches 68.85 percent and the selectivity of the ethylene diamine reaches 71.05 percent.

Description

technical field [0001] The invention belongs to the technical field of chemical catalyst preparation, in particular to a catalyst for amination of ethanolamine to ethylenediamine and a preparation method thereof. Background technique [0002] Ethylenediamine (EDA), also known as 1,2-diaminoethane and ethylenediamine, is an important chemical raw material and fine chemical intermediate. It has the characteristics of alkalinity and surface activity, and is widely used in organic compounds, high In molecular compound, medicine, dyestuff, pesticide and other industries, it can be used to produce chelating agent, insect repellant, soil improver, lubricant, rubber accelerator, emulsifier, antifreeze agent and organic solvent, etc. [0003] There are many production methods of ethylenediamine, including dichloroethane method, ethanolamine method, ethylene ammoniation method, formaldehyde-hydrocyanic acid method, diethylene glycol ammoniation method, chloroacetyl chloride ammonia me...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/889B01J37/34B01J35/10C07C211/10C07C209/16
Inventor 孙果宋李华锋雷朝快韦志明王俊黄科林
Owner GUANGXI RES INST OF CHEM IND CO LTD