Amination catalyst and preparation method thereof

A catalyst and amination technology, applied in physical/chemical process catalysts, molecular sieve catalysts, preparation of amino compounds, etc., can solve the problems of environmental pollution, large number of acid centers, low activity and selectivity of amination catalysts, etc., and achieve catalytic activity. and highly selective effects

Active Publication Date: 2009-04-15
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When dichloroethane is used to produce ethylenediamine, salt is unavoidable and causes environmental pollution problems due to the discharge of waste water
[0006] This patent does not report the proportion of mesopores of the amination catalyst. From its data, it is inferred that the proportion of mesopores (pore diameter is 2nm to 50nm) o

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The present invention is implemented with reference to the following composition by weight percentage:

[0032] 16% Aluminum Oxide, 7% Titanium Oxide, 1% Bi 3+ , 1.5% Cs + , and the balance is hydrogen mordenite.

[0033] 1.1 Preparation of hydrogen mordenite

[0034] Get sodium-type mordenite and stir in 0.5mol / L ammonium citrate solution at 90°C to make ammonium-type mordenite (SiO 2 / Al 2 o 3 Molar ratio 15), it was calcined at 480° C. for 6 hours to obtain hydrogen mordenite.

[0035] 1.2 Catalyst preparation

[0036] 1) Preparation containing metal ion Bi 3+ and metal ions Cs + The mixed solution, the hydrogen-type mordenite is immersed in the mixed solution, the immersion temperature is 70°C, the immersion time is 18 hours, and the impregnated hydrogen-type mordenite is dried at 95°C for 10 hours;

[0037] 2) Mix the hydrogen-form mordenite impregnated in step 1 with alumina and dodecyl ethanolamine titanate evenly, age at 150° C. for 24 hours, shape it, ...

Embodiment 2

[0043] The present invention is implemented with reference to the following composition by weight percentage:

[0044] 23% Aluminum Oxide, 8% Titanium Oxide, 2% Re 7+ , 0.5% Cs + , and the balance is hydrogen mordenite.

[0045] 2.1 Preparation of hydrogen mordenite

[0046] Get sodium-type mordenite and stir in 0.8mol / L ammonium citrate solution at 90°C to make ammonium-type mordenite (SiO 2 / Al 2 o 3 Molar ratio 20), it was calcined at 530° C. for 6 hours to obtain hydrogen-form mordenite.

[0047] 2.2 Catalyst preparation

[0048] 1) Preparation containing metal ion Re 7+ and metal ions Cs + The mixed solution, the hydrogen-type mordenite is immersed in the mixed solution, the immersion temperature is 70°C, the immersion time is 18 hours, and the impregnated hydrogen-type mordenite is dried at 95°C for 10 hours;

[0049] 2) Mix the hydrogen-form mordenite impregnated in step 1 with alumina and dodecyl ethanolamine titanate evenly, age at 170° C. for 24 hours, shape...

Embodiment 3

[0055] The present invention is implemented with reference to the following composition by weight percentage:

[0056] 25% Aluminum Oxide, 5% Titanium Oxide, 3% W 6+ , 0.1% Cs + , the balance being hydrogen mordenite;

[0057] 3.1 Preparation of hydrogen mordenite

[0058] Get sodium-type mordenite and stir in 0.8mol / L ammonium citrate solution at 90°C to make ammonium-type mordenite (SiO 2 / Al 2 o 3 Molar ratio 18), it was calcined at 580° C. for 4 hours to obtain hydrogen mordenite.

[0059] 3.2 Catalyst preparation

[0060] 1) Preparation containing metal ion W 6+ and metal ions Cs + The mixed solution of hydrogen-form mordenite is impregnated in the mixed solution, the immersion temperature is 85°C, the immersion time is 18 hours, and the impregnated hydrogen-form mordenite is dried at 95°C for 10 hours;

[0061] 2) Mix the hydrogen-form mordenite impregnated in step 1 with alumina and dodecyl ethanolamine titanate evenly, age at 200° C. for 24 hours, shape it, an...

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Abstract

The invention discloses an amination catalyst and a preparation method thereof, which aims to solve the problem that the amination catalyst is not high in activity and selectivity. The compositions in weight percentage of the amination catalyst are: 15 to 25 percent of A, 5 to 10 percent of B, 1 to 3 percent of C, 0.1 to 1.5 percent of D, and the balance being h-type mordenite, wherein the A is alumina; the B is titanium oxide; the C is metallic ion W<6+>, Re<7+> or Bi<3+>; the D is metallic ion Cs<+>; and the metals exist in the form of elements or oxides. The preparation method comprises the following steps of loading the components C and D on the h-type mordenite, well mixing the components C and D with the alumina and ethanolamine titanate dodecane alcohol ester, molding, roasting and activating the mixture. The catalyst is used for synthesizing ethylene dimine under the conditions of ethanolamine and ammonia phase.

Description

technical field [0001] The invention relates to an amination catalyst and a preparation method thereof. technical background [0002] Ethylenediamine is an important organic chemical raw material, mainly used in epoxy resin curing agent, pesticide, high molecular polymer and other fields. [0003] There are currently two ways to produce ethylenediamine, namely the dichloroethane method and the ethanolamine method. Salt is unavoidably formed during the production of ethylenediamine by the dichloroethane method, which causes environmental pollution problems due to the discharge of waste water. Compared with it, the ethanolamine method overcomes this defect and has become the preferred method for the production of ethylenediamine. [0004] The ethanolamine method uses ethanolamine and ammonia as raw materials to react in the gas phase in the presence of an amination catalyst to obtain ethylenediamine. Generally, microporous zeolite with regular pore structure is used as the ...

Claims

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Application Information

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IPC IPC(8): B01J29/26B01J29/18C07C209/14
Inventor 吕剑杨建明赵锋伟余秦伟杜咏梅寇联岗
Owner XIAN MODERN CHEM RES INST
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