Catalyst for gas phase synthesis of ethylenediamine and preparation method thereof

A gas-phase synthesis and catalyst technology, which is applied in the preparation of organic compounds, molecular sieve catalysts, and amino compounds, etc., can solve the problems of complex reaction products, low catalytic activity of molecular sieves, and low selectivity, etc. requirements, the effect of catalyst stabilization

Active Publication Date: 2007-05-16
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ethanolamine is an aminoalcohol compound, which has two functional groups with close activity. When ammonia is used as an amination reagent, it can be expected to obtain a wide range of binary primary amines or cyclic amines, but the general reaction intermediate amine has a higher reaction rate than ammonia. Activity, the reaction product is relatively complex, the selectivity is low, and the catalytic amination reaction of intramolecular alcohols is prone to occur to obtain products mainly composed of cyclic amines
[0004] In the current prior art, hydrogen-type molecular sieves are used as catalysts in the ethanolamine condensation method, which has the disadvantage of low catalytic activity of molecular sieves.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The present invention is implemented with reference to the following weight percentage composition:

[0024] Alumina: 23%;

[0025] Metal ion: 15%;

[0026] The balance is hydrogen mordenite.

[0027] The metal ions are Zr and Zn, Zr 4+ And Zn 2+ The molar ratio is 1:1.

[0028] 1.1 Catalyst preparation:

[0029] (1) Treat sodium-type mordenite with 0.1mol / L citric acid solution, filter and dry to prepare hydrogen-type mordenite (SiO 2 / Al 2 O 3 The molar ratio is 20-30);

[0030] (2) Take ZrOCl 2 ·8H 2 O(25.82g 0.080mol) and Zn(NO 3 ) 2 ·6H 2 O (23.83g 0.080mol), prepared into a mixed solution, immersed 62g of the hydrogen-type mordenite in step 1 in the solution at a temperature of 80-90°C, and an immersion time of 10-18 hours;

[0031] (3) Dry the mordenite obtained in step 3 from step 2 at 90-110°C for 10-12 hours;

[0032] (4) The mordenite obtained in step 3 is uniformly mixed with 23 g of alumina and graphite powder as a release agent, pressed into a shape, and calci...

Embodiment 2

[0036] The present invention is implemented with reference to the following weight percentage composition:

[0037] Alumina: 25%;

[0038] Metal ion: 10%;

[0039] The balance is hydrogen mordenite.

[0040] Metal ions are Nb and Fe, Nb 5+ And Fe 3+ The molar ratio is 5:1.

[0041] 2.1 Catalyst preparation

[0042] (1) Treat sodium-type mordenite with 0.3mol / L citric acid solution, filter and dry to prepare hydrogen-type mordenite (SiO 2 / Al 2 O 3 Molar ratio 20~30);

[0043] (2) Take NbCl 5 (20.31g 0.075mol) and Fe(NO 3 ) 3 ·9H 2 O (6.07g 0.015mol), prepared into a mixed solution, and immersed 65g of the hydrogen-type mordenite in step 1 in the solution at a temperature of 80-90°C and an immersion time of 10-18 hours;

[0044] (3) Dry the mordenite obtained in step 3 from step 2 at 90-110°C for 10-12 hours;

[0045] (4) The mordenite obtained in step 3 is uniformly mixed with 25 g of alumina and graphite powder as a release agent, pressed into a shape, and calcined at 400-600° C....

Embodiment 3

[0049] The present invention is implemented with reference to the following weight percentage composition:

[0050] Alumina: 28%;

[0051] Metal ion: 8%;

[0052] The balance is the treated hydrogen mordenite.

[0053] Metal ions are Mo and Zn, Mo 6+ And Zn 2+ The molar ratio is 8:1.

[0054] 3.1 Catalyst preparation

[0055](1) The sodium mordenite is exchanged with 0.7mol / L citric acid solution, filtered and dried to prepare hydrogen mordenite (SiO 2 / Al 2 O 3 Molar ratio 20~30);

[0056] (2) Take (NH 4 ) 2 MoO 4 (15.06g 0.077mol) and Zn(NO 3 ) 2 ·6H 2 O (2.97g 0.010mol), prepared into a mixed solution, immerse 68g of the hydrogen-type mordenite in step 1 in the solution at a temperature of 80-90°C, and an immersion time of 10-18 hours;

[0057] (3) Dry the mordenite obtained in step 3 from step 2 at 90-110°C for 10-12 hours;

[0058] (4) The mordenite obtained in step 3 is uniformly mixed with 28 g of alumina and graphite powder as a release agent, pressed into a shape, and cal...

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Abstract

The invention relates to a catalyst used to composite ethanediamine from gas phase and relative production, wherein it comprises 20-30% alumina, 5-15% metal ion, and left is hydrogen mordenite treated by acid, while metal ion can be one of Zr4+, Nb5+, Mo6+, Sn4+, Sb5+ with one of Zn2+, Fe3+, while their mol ratio is 1-10:1. And its production comprises loading the metal ion on the treated hydrogen mordenite, drying, and mixing with alumina, compressing, baking and activating. The invention is used to composite ethanediamine from ethanolamine and ammonia gas.

Description

Technical field [0001] The invention relates to a catalyst for gas phase synthesis of ethylene diamine and a preparation method thereof. Background technique [0002] Ethylenediamine is an important organic chemical product, mainly used in the fields of epoxy resin curing agent, pesticide, medicine, low molecular weight polyamide resin, chelating agent, surfactant, lubricating oil additive, paper wet strength agent, etc. [0003] There are currently two methods for producing ethylene diamine in the world, namely the dichloroethane method and the ethanolamine method. Ethanolamine is an amino alcohol compound with two functional groups with close reactivity. When ammonia is used as the amination reagent, it can be expected to obtain a wide range of dibasic primary amines or cyclic amines, but generally the reaction intermediate amine has a higher reaction than ammonia The activity, the reaction product is more complicated, the selectivity is low, and it is prone to the catalyzed am...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/20C07C211/10C07C209/16
Inventor 杨建明吕剑赵锋伟寇联岗石强
Owner XIAN MODERN CHEM RES INST
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