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Method for preparing silicoaluminophosphate 11 (SAPO-11) molecular sieve with adjustable mesoporous aperture

A SAPO-11, molecular sieve technology, applied in the field of catalysis, can solve the problem of less SAPO-n molecular sieves

Active Publication Date: 2013-04-17
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are few reports on the synthesis of SAPO-n molecular sieves with hierarchical pore structure.

Method used

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  • Method for preparing silicoaluminophosphate 11 (SAPO-11) molecular sieve with adjustable mesoporous aperture
  • Method for preparing silicoaluminophosphate 11 (SAPO-11) molecular sieve with adjustable mesoporous aperture
  • Method for preparing silicoaluminophosphate 11 (SAPO-11) molecular sieve with adjustable mesoporous aperture

Examples

Experimental program
Comparison scheme
Effect test

Embodiment -1

[0023] Dissolve 2 g of cetyl triethoxy organosilicon quaternary ammonium salt in 18 g of ethanol to obtain an ethanol solution with a mass concentration of 10% cetyl triethoxy organosilicon quaternary ammonium salt.

[0024] Mix 23.1 g of phosphoric acid (AR, 85%) and 72.0 g of deionized water in a 38 °C water bath, add 15.2 g of pseudoboehmite (Shandong aluminum powder, aluminum oxide content 67.0%), and place in a 38 °C water bath Stir with medium magnetic force for 0.5 h to obtain aluminum phosphate sol; slowly add 11.2 g of di-n-propylamine (DPA, AR, 99%), continue stirring for 0.5 h to form a uniform sol (mixed solution), add 6.3 g of ethyl orthosilicate (AR , 99%), continue stirring for 0.5 h, add 20 g ethanol solution of cetyl triethoxy organosilicon quaternary ammonium salt with a mass concentration of 10%, and continue stirring in a water bath at 38 °C for 2 h, the reaction The molar ratio of materials in the system is Al 2 o 3 :P 2 o 5 :SiO2 2 :DPA:H 2 O=1:1:0....

Embodiment -2

[0028] Dissolve 2 g of cetyltrimethoxyorganosilicon quaternary ammonium salt in 18 g of methanol to obtain a methanol solution of cetyltrimethoxyorganosilicon quaternary ammonium salt with a mass concentration of 10%.

[0029] Mix 23.1 g of phosphoric acid (AR, 85%) and 72.0 g of deionized water in a 38 °C water bath, add 15.2 g of pseudoboehmite (Shandong aluminum powder, aluminum oxide content 67.0%), and place in a 38 °C water bath Stir with medium magnetic force for 0.5 h to obtain aluminum phosphate sol; slowly add 11.2 g of di-n-propylamine (DPA, AR, 99%), continue stirring for 0.5 h to form a uniform sol (mixed solution), add 6.3 g of ethyl orthosilicate (AR , 99%), continue to stir for 0.5 h, add 20 g methanol solution of cetyltrimethoxyorganosilicon quaternary ammonium salt with a mass concentration of 10%, and continue stirring in a water bath at 38 °C for 2 h, the reaction system The material molar ratio in Al 2 o 3 :P 2 o 5 :SiO2 2 :DPA:H 2 O=1:1:0.3:1.1:40; ...

Embodiment -3

[0032] Dissolve 2 g of dodecyl triethoxy organosilicon quaternary ammonium salt in 18 g of ethanol to obtain an ethanol solution of hexadecyl triethoxy organosilicon quaternary ammonium salt with a mass concentration of 10%.

[0033] Mix 23.1 g of phosphoric acid (AR, 85%) and 72.0 g of deionized water in a 38 °C water bath, add 15.2 g of pseudoboehmite (Shandong aluminum powder, aluminum oxide content 67.0%), and place in a 38 °C water bath Stir with medium magnetic force for 0.5 h to obtain aluminum phosphate sol; slowly add 11.2 g of di-n-propylamine (DPA, AR, 99%), continue stirring for 0.5 h to form a uniform sol (mixed solution), add 6.3 g of ethyl orthosilicate (AR , 99%), after stirring for 0.5 h, add 20 g of ethanol solution of dodecyl triethoxy organosilicon quaternary ammonium salt with a mass concentration of 10%, and continue stirring in a water bath at 38 °C for 2 h, the reaction The molar ratio of materials in the system is Al 2 o 3 :P 2 o 5 :SiO2 2 :DPA:H ...

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Abstract

The invention relates to a method for preparing a silicoaluminophosphate 11 (SAPO-11) molecular sieve. The method is characterized by comprising the following synthesis steps of: 1) dissolving long-chain alkylated organic silicon quaternary ammonium salt into a corresponding alcohol to obtain an alcohol solution of the long-chain alkylated organic silicon quaternary ammonium salt; 2) mixing deionized water, phosphor source, aluminum source, small molecular organic amine and silicon source uniformly to obtain a mixed solution; 3) adding the alcohol solution of the long-chain alkylated organic silicon quaternary ammonium salt into the mixed solution, and mixing uniformly to obtain a mixed solution; 4) charging the mixed solution into a polytetrafluoroethylene reaction kettle, putting the reaction kettle into a dynamic crystallization reaction oven, and performing sectional crystallization; 5) separating, washing and drying the solid product to obtain raw SAPO-11 molecular sieve powder; and 6) roasting the raw SAPO-11 molecular sieve powder, and thus obtaining the micropore-mesoporous SAPO-11 molecular sieve.

Description

technical field [0001] The invention relates to the technical field of catalysis, in particular to a method for preparing SAPO-11 molecular sieves with adjustable mesoporous diameters, in particular to a synthesis method for microporous-mesoporous SAPO-11 molecular sieves with adjustable mesoporous diameters. Background technique [0002] The silicoaluminophosphate molecular sieve SAPO-n is a new type of molecular sieve material developed by the UOP company in the United States. SAPO-n molecular sieve is made of SiO 2 , AlO 2 + and PO 2 - A microporous crystal structure composed of three tetrahedral units, where n represents a different crystal structure. SAPO-11 molecular sieve is a member of its family. It is a non-zeolite mesoporous molecular sieve with AEL structure. It has a one-dimensional ten-membered ring channel structure and an elliptical channel (0.64 nm×0.39 nm). SAPO-11 molecular sieve has been widely used in petrochemical fields such as normal hydrocarbon...

Claims

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Application Information

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IPC IPC(8): C01B39/54C01B37/08
Inventor 李孝国肖寒于海斌孙国方裴仁彦费亚南张耀日李佳赵甲隋芝宇张永惠
Owner CNOOC TIANJIN CHEM RES & DESIGN INST