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Method for preparing SAPO-II molecular sieve

A technology of SAPO-11 and molecular sieve, which is applied in the direction of molecular sieve and alkali-exchanged phosphate, molecular sieve characteristic silicoaluminophosphate, etc., can solve the unfavorable problems of industrial scale-up and production of SAPO-11, and achieve fewer defects, simple operation and perfect crystal Effect

Active Publication Date: 2013-03-20
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Using conventional synthesis methods, the obtained colloids are generally highly acidic, with a pH of about 4.0, and strong acidity is not conducive to the industrial scale-up and production of SAPO-11.

Method used

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  • Method for preparing SAPO-II molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] A: Weigh 10.85g of pseudoboehmite (Wenzhou Jingjing Alumina Co., Ltd., water content 25% by weight), dissolve it in 18.00g of deionized water to make a solution, heat, and stir for 0.5h;

[0040] B: Measure 9.7ml of di-n-propylamine (98% by weight) and add it dropwise to the solution obtained in step A, stir for 2 hours, then weigh 10.30g of silica sol (Qingdao Chengyu Chemical Co., Ltd., containing silicon dioxide 25% by weight) was added to the aforementioned solution, stirred for 2h to obtain an aqueous slurry;

[0041] C: When the aqueous slurry obtained in step B is heated to 80°C, 16.45g H 3 PO 4 (concentration is 85% by weight) the acid solution in 18.00g deionized water is added dropwise in the aqueous slurry at the speed of adding 2.8% phosphoric acid per minute, the pH of the slurry in the whole process is 7.3, add water, stir for 1h again, get A colloidal mixture whose molar composition is R:Al 2 o 3 :P 2 o 5 : 0.6SiO2 2 :50H 2 O, wherein R is di-n-pr...

Embodiment 2

[0047] A: Weigh 10.85g of pseudoboehmite (Wenzhou Jingjing Alumina Co., Ltd., water content 25% by weight), dissolve it in 18.00g of deionized water to make a solution, heat, and stir for 0.5h;

[0048] B: Measure 9.7ml of di-n-propylamine (98% by weight) and add it dropwise to the solution obtained in step A, stir for 2 hours, then weigh 10.30g of silica sol (Qingdao Chengyu Chemical Co., Ltd., containing silicon dioxide 25% by weight) was added to the aforementioned solution, stirred for 2h to obtain an aqueous slurry;

[0049] C: When the aqueous slurry obtained in step B is heated to 80°C, 16.45g H 3 PO 4 (concentration is 85% by weight) the acid solution in 18.00g deionized water is added dropwise in the aqueous slurry at the speed of adding 5.6% phosphoric acid per minute, the pH of the slurry in the whole process is 7.0, add water, stir for 1h again, get A colloidal mixture whose molar composition is R:Al 2 o 3 :P 2 o 5 : 0.6SiO2 2 :50H 2 O, wherein R is di-n-pr...

Embodiment 3

[0054] A: Weigh 10.85g of pseudoboehmite (Wenzhou Jingjing Alumina Co., Ltd., water content 25% by weight), dissolve it in 18.00g of deionized water to make a solution, heat, and stir for 1 hour;

[0055] B: Measure 9.7ml of di-n-propylamine (98% by weight) and add it dropwise to the solution obtained in step A, stir for 2 hours, then weigh 10.30g of silica sol (Qingdao Chengyu Chemical Co., Ltd., containing silicon dioxide 25% by weight) was added to the aforementioned solution, stirred for 2h to obtain an aqueous slurry;

[0056] C: When the aqueous slurry obtained in step B is heated to 85°C, 16.45g H 3 PO 4 (concentration is 85% by weight) the acid solution in 18.00g deionized water is added dropwise in the water-containing slurry at the speed of adding 8.4% phosphoric acid per minute, the pH of the slurry is 6.8 in the whole process, add water, stir again 1h, obtain A colloidal mixture whose molar composition is R:Al 2 o 3 :P 2 o 5 : 0.6SiO2 2 :50H 2 O, wherein R ...

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Abstract

The invention discloses a method for preparing an SAPO-II molecular sieve. The method comprises a step of forming a colloidal mixture and a step of crystallizing the colloidal mixture, and is characterized in that: the step of forming the colloidal mixture comprise the substeps of: mixing an aluminum source, an organic template agent and a silicon source in sequence to obtain water-containing serum, heating the water-containing serum to 80-100 DEG C, then adding a phosphorus source at the rate of 1.0-15% of the phosphorus source per minute to obtain the colloidal mixture with the molar ratio of aR:Al2O3:bP2O5:cSiO2:dH2O, wherein R represents the organic template agent, a is 0.2-2.0, b is 0.2-1.2, c is 0.1-1.5 and d is 15-80. By means of the method disclosed by the invention, the acidity of the serum in the entire production process is weaker, so that the reaction is performed under a condition with weaker acidity, the equipment is free from corrosion, the requirements on the equipment are reduced, and thus, the production cost is reduced.

Description

technical field [0001] The invention relates to a method for preparing SAPO-11 molecular sieves. Background technique [0002] Silicoaluminophosphate (SAPO) molecular sieve is a new type of non-zeolite molecular sieve launched by Union Carbide Corporation in 1984. SAPO-n is replaced by Si atoms for AlPO 4 AlO formed after P or Al atoms in the -n skeleton 4 、PO 4 and SiO 4 The non-neutral molecular sieve framework composed of tetrahedrons has exchangeable cations and has proton acidity; at the same time, the SAPO-n molecular sieve has a pore size of 0.3-0.8nm, almost including the entire range of zeolite molecular sieves; SAPO-n molecular sieve The pore volume (H 2 O) is 0.18~0.48cm 3 / g. As a new generation of molecular sieves, SAPO-n molecular sieves have been widely valued in the field of catalysis. As a member of the SAPO-n molecular sieve family, SAPO-11 molecular sieve is a medium-pore molecular sieve with three-dimensional non-intersecting 10-membered ring elli...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/54C01B37/08
Inventor 张利霞栗同林赵岚刘艳惠杨光裴庆君任行涛
Owner CHINA PETROLEUM & CHEM CORP