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Method for synthesizing silicoaluminophosphate molecular sieve by utilizing crystallization mother liquor

A technology for crystallization of mother liquor and silicoaluminophosphate, applied in the direction of molecular sieve characteristic silicoaluminophosphate, molecular sieve and alkali exchange phosphate, etc., can solve the problems of small synthesis range, difficult to enlarge, low crystallinity, etc., to improve selectivity, The effect of reducing dosage and improving lifespan

Inactive Publication Date: 2011-01-05
THE NORTHWEST RES INST OF CHEM IND +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In CN1314587C announced on May 9, 2007, a method for preparing SAPO-34 molecular sieve by vapor phase crystallization method is disclosed, but compared with hydrothermal synthesis method, the method has relatively low crystallinity, and the prepared molecular sieve has a silicon-aluminum ratio Compared with phosphorus and aluminum, the synthesis range is smaller, and the equipment is complicated, and it is not easy to enlarge and other defects

Method used

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  • Method for synthesizing silicoaluminophosphate molecular sieve by utilizing crystallization mother liquor
  • Method for synthesizing silicoaluminophosphate molecular sieve by utilizing crystallization mother liquor
  • Method for synthesizing silicoaluminophosphate molecular sieve by utilizing crystallization mother liquor

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Effect test

Embodiment 1

[0029] The source of crystallization mother liquor: the filtrate recovered from silicoaluminophosphate molecular sieve prepared by hydrothermal synthesis is used as the crystallization mother liquor of this embodiment;

[0030] The source of the seed crystal: the silicoaluminophosphate molecular sieve prepared by the hydrothermal synthesis method is used as the seed crystal of this embodiment;

[0031] (1) Mix the aluminum source and deionized water evenly to form a suspension A, deionized water and aluminum source (use Al 2 o 3 The molar ratio of meter) is 25: 1, and the aluminum source used is pseudo-boehmite;

[0032] (2) The phosphorus source and deionized water are mixed evenly to form solution B, and the deionized water and phosphorus source (in the form of P 2 o 5 The molar ratio of meter) is 25:1, and the phosphorus source used is orthophosphoric acid;

[0033] (3) Mix the suspension A with the solution B evenly, then add the template agent, silicon source, crystal...

Embodiment 2

[0038] The preparation process of this example is the same as that of Example 1, except that the crystallization mother liquor used is a mixture of the crystallization mother liquor used in Example 1 and the filtrate recovered in Example 1, and the aluminum source used is aluminum isopropoxide Or alumina, or at least two of aluminum isopropoxide, pseudoboehmite and alumina, the phosphorus source used is phosphorous acid or phosphorous acid and orthophosphoric acid, and the template used is tetraethylammonium hydroxide, triethylamine or diethylamine, or at least two of tetraethylammonium hydroxide, triethylamine, diethylamine and morpholine, and the silicon source used is ethyl orthosilicate or white carbon black, or ethyl orthosilicate At least two kinds of ester, white carbon black and silica sol, and the hydrothermal crystallization time under the condition of 180° C. is 12 hours, and the silicoaluminophosphate molecular sieve EX-2 is prepared.

Embodiment 3

[0040] The preparation process of this example is the same as that of Example 1, except that the crystallization mother liquor used is the mixed solution of the filtrate recovered in Example 1 and Example 2, and the aluminum source used is aluminum isopropoxide or aluminum oxide, or It is at least two of aluminum isopropoxide, pseudoboehmite and alumina, the phosphorus source used is phosphorous acid or phosphorous acid and orthophosphoric acid, and the template used is tetraethylammonium hydroxide, triethylamine or diethylamine, Or at least two of tetraethylammonium hydroxide, triethylamine, diethylamine and morpholine, the silicon source used is ethyl orthosilicate or white carbon black, or ethyl orthosilicate, white carbon black and at least two kinds of silica sols, and the hydrothermal crystallization time is 24 hours at a temperature of 180° C. to prepare the silicoaluminophosphate molecular sieve EX-3.

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Abstract

The invention discloses a method for synthesizing a silicoaluminophosphate molecular sieve by utilizing crystallization mother liquor, which comprises the following steps: 1) mixing an aluminum source with deionized water for forming suspension A, or mixing the aluminum source with the crystallization mother liquor for forming the suspension A; 2) mixing a phosphorus source with the deionized water for forming solution B, or mixing the phosphorus source with the crystallization mother liquor for forming the solution B; 3) mixing the suspension A with the solution B, and then adding a template agent, a silicon source, crystal seeds and the crystallization mother liquor for forming initial gel mixture; 4) placing the initial gel mixture in a crystallization kettle for hydrothermal crystallization, and then filtering for obtaining a filter cake and filtrate; 5) washing the filter cake, then drying and then calcining for obtaining the silicoaluminophosphate molecular sieve; and 6) recovering the filtrate, sealing and preserving. The method can reduce the using quantity of the template agent, realize zero emission of the crystallization mother liquor, and simultaneously regulate the grain size and the acid strength of the silicoaluminophosphate molecular sieve by fully utilizing the crystallization mother liquor.

Description

technical field [0001] The invention belongs to the technical field of molecular sieve synthesis, and in particular relates to a method for synthesizing silicon-aluminophosphate molecular sieves by using crystallization mother liquor. Background technique [0002] Low-carbon olefins, especially ethylene and propylene, as basic organic chemical raw materials, play a pivotal role in modern petroleum and chemical industries. The production methods of olefins can be divided into two categories: one is the petroleum route, and the other is the non-petroleum route. But for oil, the price continues to rise for a long time, the supply is unstable, and the resource reserves are limited. Therefore, it is not enough to increase the production of ethylene and propylene by relying on the traditional petroleum route. Methanol-to-Olefins (MTO for short) uses coal or natural gas as raw material to produce ethylene, propylene and other low-carbon olefins through methanol process, it is the...

Claims

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Application Information

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IPC IPC(8): C01B37/08C01B39/54
Inventor 高俊文宋庆锋潘蕊娟王瑞张勇高亚娜郭彦鑫
Owner THE NORTHWEST RES INST OF CHEM IND
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