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Preparation method for silicon-phosphorus-aluminum molecular sieve

A silicon-phosphorus-aluminum molecular sieve and aluminum source technology, applied in the direction of molecular sieves and alkali-exchanged phosphates, molecular sieve characteristic silicon-aluminophosphates, etc., can solve the problems of low catalytic activity, large diffusion resistance, low mesopore content, etc., and achieve reduction Diffusion resistance, good hydrothermal stability, and high crystallinity

Active Publication Date: 2018-09-21
SHAANXI YANCHANG PETROLEUM GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to provide a method that can solve the problems of low mesoporous content, large diffusion resistance, low catalytic reactivity and easy deactivation of traditional silicon-phosphorus-aluminum molecular sieves, and has the advantages of simple process, high yield, good repeatability, hydrothermal Preparation method of silicon phosphorus aluminum molecular sieve with high stability

Method used

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  • Preparation method for silicon-phosphorus-aluminum molecular sieve
  • Preparation method for silicon-phosphorus-aluminum molecular sieve
  • Preparation method for silicon-phosphorus-aluminum molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] a) Fully mix aluminum isopropoxide, water, di-n-propylamine, concentrated phosphoric acid, and acidic silica sol according to the molar ratio of 1:70:0.4:1:0.8, stir evenly, adjust the pH value to 4.5 to obtain gel A, Put it into a crystallization kettle and crystallize for 12 hours under autogenous pressure at 160°C;

[0039] b) cetyltrimethylammonium bromide and (ethanol: water = 3:1 mass ratio) were mixed and stirred at a molar ratio of 0.15:1 to obtain solution B;

[0040] c) Stir the crystallized gel A in step a) fully and then slowly add solution B, wherein the molar ratio of the aluminum source of gel A to the solvent of solution B is 1:0.8, and then adjust the pH value to 4.5 with a template to obtain a gel. Glue C;

[0041] d) The gel C obtained in step c) was dehydrated by rotary evaporation at 120°C, and after being completely dehydrated, it was quickly placed in an oven at 220°C to dry to obtain a precursor;

[0042] e) Grinding and crushing the precursor ...

Embodiment 2

[0046] a) Fully mix pseudo-boehmite, water, tetraethylammonium hydroxide, concentrated phosphoric acid, and tetraethylorthosilicate at a molar ratio of 1:50:4:1:0.4, stir evenly, and adjust the pH value Gel A was obtained at 7.0, put into a crystallization kettle and crystallized under autogenous pressure at 180°C for 8 hours;

[0047] b) Chitosan and water are mixed and stirred at a molar ratio of 0.2:1 to obtain solution B;

[0048] c) Fully stir the crystallized gel A in step a) and then slowly add solution B, wherein the molar ratio of the aluminum source of gel A to the solvent of solution B is 1:1.5, and then adjust the pH value to 6.5 with a template agent to obtain Gel C;

[0049]d) The gel C obtained in step c) was dehydrated by rotary evaporation at 120°C, and after being completely dehydrated, it was quickly placed in an oven at 260°C to dry to obtain a precursor;

[0050] e) Grinding and crushing the precursor of step d), placing it in the upper part of the react...

Embodiment 3

[0054] a) Fully mix aluminum isopropoxide, water, morpholine, phosphorous acid, and acidic silica sol according to the molar ratio of 1:30:2:0.8:0.1, stir evenly, adjust the pH value to 3.5 to obtain gel A, pack Put into the crystallization kettle and crystallize for 45h under autogenous pressure at 120°C;

[0055] b) Mix and stir sucrose and dimethyl ether at a molar ratio of 0.05:1 to obtain solution A;

[0056] c) After fully stirring the gel A crystallized in step a), slowly add solution A, wherein the molar ratio of the gel A and the aluminum source in the solution A to the solvent is 1:1, and then adjust the pH value with a templating agent 3.5 Obtain gel B;

[0057] d) The gel B obtained in step c) was dehydrated by rotary evaporation at 80°C, and after being completely dehydrated, it was quickly placed in an oven at 160°C to dry to obtain a precursor;

[0058] e) Grinding and crushing the precursor of step d), placing it in the upper part of the reaction kettle, putt...

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Abstract

The invention provides a preparation method for a silicon-phosphorus-aluminum molecular sieve, belonging to the technical field of molecular sieves. The preparation method mainly overcomes the problems of low mesopore content, great diffusional resistance, low catalytic reaction activity, proneness to inactivation and the like of traditional silicon-phosphorus-aluminum molecular sieves. Accordingto the preparation method in the invention, an aluminum source, a phosphorus source, a silicon source, a template and water are fully mixed, and the silicon-phosphorus-aluminum molecular sieve rich inmesoporous structures is prepared by changing the preparation method and adding a pore expanding agent; so the diffusion resistance of reaction raw materials and a product can be effectively reduced,the catalytic activity of the molecular sieve is improved, the selectivity of the target product is enhanced, and the service life of the catalyst is prolonged. The prepared silicon-phosphorus-aluminum molecular sieve has important application value in hydroisomerization, methanol to olefins, denitration of automobile exhaust gas and the like.

Description

technical field [0001] The invention belongs to the field of molecular sieve synthesis, and in particular relates to a preparation method of a silicon, phosphorus, and aluminum molecular sieve. Background technique [0002] Silicon phosphorus aluminum molecular sieve is a non-metallic oxide crystal composed of silicon-oxygen tetrahedron, aluminum-oxygen tetrahedron and phosphorus-oxygen tetrahedron shared oxygen atom vertices. Its skeleton structure contains regular and orderly arranged pores or cages of molecular size ( Pore ​​diameter 0.33-1.5nm), is widely used in coal chemical industry, petrochemical industry and fine chemical industry and other fields. However, the pores of silicon phosphorus aluminum molecular sieve are small, the products are not easy to diffuse out, and secondary reactions are easy to occur and carbon deposits, resulting in rapid deactivation of the catalyst. Therefore, the pore structure and specific surface area of ​​the catalyst are important fac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/08C01B39/54
CPCC01B37/08C01B39/54C01P2004/03C01P2006/12C01P2006/14C01P2006/17
Inventor 黄传峰韩磊李大鹏刘树伟
Owner SHAANXI YANCHANG PETROLEUM GRP
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