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Mordenite/SAPO-34 composite molecular sieve amination catalyst and method for preparing same

A SAPO-34 and composite molecular sieve technology, which is applied in the field of mordenite/SAPO-34 composite molecular sieve amination catalyst and its preparation, can solve the problems of difficult desorption, low low temperature activity, fast coking and the like, and achieves simplified preparation steps, The effect of high overall selectivity and high low temperature activity

Active Publication Date: 2014-08-27
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the low selectivity of the catalyst, more by-products are generated, and the total selectivity is generally lower than 70%.
[0005] In the prior art, the amination reaction raw materials are ethanolamine and liquid ammonia, and the reaction products are ethylenediamine, piperazine, triethylenediamine, aminoethylpiperazine, diethylenetriamine, etc., and the reactants and products are strong Alkaline substances are easy to adsorb and difficult to desorb on various acidic sites of modified zeolite molecular sieve catalysts, and are easy to further react to form various alkaline coking compounds, which block the catalyst pores and cover the active sites of the catalyst, so there is low temperature activity Not high, and the problem of fast coking when the temperature is high

Method used

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  • Mordenite/SAPO-34 composite molecular sieve amination catalyst and method for preparing same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Mix 3.5g of pseudo-boehmite and 6g of deionized water at 60°C, slowly add 5.7g of orthophosphoric acid with a weight percentage of 85% and 0.05g of hydrofluoric acid dropwise, stir for 1h, then add 24g of silica sol, and stir for 1h , then drop 5 g of 4-hydroxypiperidine, adjust the pH of the mixture to 5-6, and keep stirring for 1 h; add SiO 2 / Al 2 o 3 5g of 20-80 mordenite molecular sieves, continuously stirred for 1h, mixed evenly, and aged for 1h; the mixture was hydrothermally crystallized at 130°C for 10h in a polytetrafluoroethylene-lined autoclave, and then heated to 180°C, Constant temperature hydrothermal crystallization for 24 hours, the product was filtered, washed with deionized water, dried at 120°C for 6 hours, and calcined at 500°C in air atmosphere for 2 hours to obtain mordenite / SAPO-34 composite molecular sieve;

[0034]Mix 80 g of mordenite / SAPO-34 composite molecular sieve, 15 g of titanium oxide, and 5 g of alumina evenly, granulate, press and s...

Embodiment 2

[0036] Embodiment 2 is substantially the same as the preparation process in Example 1, and the difference is that adopting 2.2g weight percent is 85% orthophosphoric acid, template agent morpholine is 1.2g, and deionized water is 5.2g, and prepared mordenite / SAPO-34 Composite Molecular Sieve Amination Catalyst B.

Embodiment 3

[0038] The preparation process of embodiment 3 is basically the same as that of embodiment 1, and the difference is that adopting 6.6g of orthophosphoric acid with a weight percentage of 85%, the templating agent 4-hydroxymethyl piperidine is 7.9g, and deionized water is 52g to prepare Mordenite / SAPO-34 composite molecular sieve amination catalyst C was obtained.

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Abstract

The invention discloses a mordenite / SAPO-34 composite molecular sieve amination catalyst and a method for preparing the same. The amination catalyst comprises the following raw materials by weight percent: 75-90% of mordenite / SAPO-34 composite molecular sieve, 5-15% of titanium oxide, and 5-10% of alumina binder. The mordenite with the ratio of SiO2 to Al2O3 being 20-80 in the mordenite / SAPO-34 composite molecular sieve accounts for 50-80% of the total weight of the mordenite / SAPO-3 composite molecular sieve, and the SAPO-34 molecular sieve accounts for 20-60% of the total weight of the mordenite / SAPO-3composite molecular sieve. The method for preparing the mordenite / SAPO-34 composite molecular sieve amination catalyst comprises the following steps of: mixing an aluminum source, a phosphorus source, a silicon source and a template agent, adding the mordenite, putting the materials in a high-pressure kettle, and crystallizing to obtain the mordenite / SAPO-34 composite molecular sieve, mixing the mordenite / SAPO-34 composite molecular sieve, the titanium oxide and the alumina uniformly, pressing and moulding, and sintering at 450 DEG C for 8 hours to obtain the amination catalyst.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a mordenite / SAPO-34 composite molecular sieve amination catalyst and a preparation method thereof. Background technique [0002] Ethyleneamine is a general term for compounds including ethylenediamine, piperazine, triethylenediamine, aminoethylpiperazine and diethylenetriamine. Usually, ethanolamine and ammonia are used as raw materials to carry out amination reaction to synthesize ethyleneamine in the presence of an amination catalyst. [0003] The preparation of the amination catalyst is generally obtained by modifying a single mordenite or HZSM-5. US Patent (US5731449) discloses a zeolite catalyst treated with alkali solution to synthesize triethylenediamine and piperazine from amides. Soak ZSM-5 with NaOH aqueous solution to convert it into NaZSM-5, and then use NH 4+ The aqueous solution is ion-exchanged and converted into NH 4 ZSM-5, and finally ge...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/85C07B43/04
Inventor 杨建明吕剑赵锋伟何飞魏阿宝石磊陈涛余秦伟梅苏宁王为强周继华
Owner XIAN MODERN CHEM RES INST
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