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Method for synthesizing phosphorus-silicate-aluminum molecular sieve with metal-amine-complex as template

A technology of phosphorus-silicon-aluminum molecular sieve and template agent, which is applied in the direction of molecular sieve and alkali-exchanged phosphate, molecular sieve characteristic silicon-aluminophosphate, etc., can solve the problems of insufficient dispersion and many metals, and achieve low cost, high specific surface area and simple method easy effect

Active Publication Date: 2011-11-30
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to adjust the acidity of SAPO-34 molecular sieve, metal ions can be introduced into SAPO-34 molecular sieve by ion exchange, but the metals introduced by the above method are not many and not dispersed enough

Method used

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  • Method for synthesizing phosphorus-silicate-aluminum molecular sieve with metal-amine-complex as template
  • Method for synthesizing phosphorus-silicate-aluminum molecular sieve with metal-amine-complex as template
  • Method for synthesizing phosphorus-silicate-aluminum molecular sieve with metal-amine-complex as template

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1: the preparation of Cu-SAPO-34 sample

[0029] First add boehmite to water, add phosphoric acid drop by drop, and after stirring for one hour, a viscous gel is obtained, then add amorphous silicon dioxide, stir to form a gel, add copper sulfate pentahydrate, and fully stir Then add tetraethylenepentamine, and after stirring for one hour, add n-propylamine to the above system, stir at room temperature for 12 hours, put it into a polytetrafluoroethylene-lined steel reactor, and react at 200 degrees for two days. The chemical ratio of the system is as follows: 1 Al 2 o 3 : 1.14P 2 o 5 : 0.57 SiO 2 : 75 H 2 O: 0.3 Cu-R1: 2.4 R2. After the reaction was completed, the obtained product was fully washed with deionized water and dried overnight at 80°C.

[0030] attached figure 1 According to the XRD characterization results of the product, it can be seen that the product has a typical SAPO-34 structure and has a high degree of crystallinity.

[0031] attac...

Embodiment 2

[0034] Embodiment 2: the preparation of Cu-SAPO-34 sample

[0035] The addition sequence and stirring time of gel preparation are the same as in Example 1. The chemical ratio of the system is: 1 Al 2 o 3 : 1.14P 2 o 5 : 0.57 SiO 2 : 85 H 2 O: 0.3 Cu-R1: 4.5 R2. React at 150 degrees for two days. After the reaction was completed, the obtained product was fully washed with deionized water and dried overnight at 80°C.

[0036] attached Figure 5 According to the XRD characterization results of the product, it can be seen that the product has a typical SAPO-34 structure and has a high degree of crystallinity.

[0037] attached Figure 6 It is the solid ultraviolet-visible absorption spectrum of the product.

Embodiment 3

[0038] Embodiment 3: the preparation of Cu-SAPO-34 sample

[0039] First add aluminum hydroxide to water, add phosphoric acid drop by drop, and after stirring for one hour, a viscous gel is obtained, then add amorphous silicon dioxide, stir to form a gel, add copper sulfate pentahydrate, after fully stirring Then add tetraethylenepentamine, and after stirring for one hour, add n-propylamine to the above system, stir for 12 hours at room temperature, put it into a polytetrafluoroethylene-lined steel reactor, and react at 200 degrees for two days. The chemical ratio of the system is as follows: 1 Al 2 o 3 : 1.14P 2 o 5 : 0.57 SiO 2 : 80 H 2 O: 0.3 Cu-R1: 2.4 R2. After the reaction was completed, the obtained product was fully washed with deionized water and dried overnight at 80°C.

[0040] attached Figure 7 According to the XRD characterization results of the product, it can be seen that the product has a typical SAPO-34 structure and has a high degree of crystallinity...

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Abstract

The invention relates to a synthesis of a molecular sieve and aims to provide a method for synthesizing a silicoaluminophosphate molecular sieve by the use of a metal-amine-complex as a template agent. The method provided by the invention comprises the following steps of: adding boehmite or aluminium hydroxide into deionized water, adding dropwisely phosphoric acid with stirring, and adding amorphous silica; successively adding a divalent metal salt and organic amine after uniformly mixing to make the PH value of a gel to reach 7-9, stirring at room temperature for 12 hours, placing into a reaction vessel for a crystallization reaction, washing a solid crystal product to a neutral one, and drying to obtain a molecular sieve powder. According to the invention, different metal ions can be introduced so as to adjust the acidity of the SAPO-34 molecular sieve; And the metal ions in the obtained molecular sieve can be dispersed uniformly and the metal ions can be introduced in larger amounts; in addition, the molecular sieve has higher specific surface area and has a high reaction activity in a catalytic reaction. The synthesis method provided by the invention requires a simple template agent and low cost, the crystallization temperature is controlled from 150 DEG C to 200 DEG C, and a method for removing the template agent is simple and easy to operate.

Description

technical field [0001] The present invention relates to the synthesis of molecular sieves, in particular to the rapid and efficient synthesis of phosphorus-containing silicon-aluminum heteroatom molecular sieves using metal-amine-complexes as a new template in a relatively wide range of hydrothermal crystallization temperatures method. Background technique [0002] Phosphosilicate SAPO-34 molecular sieve is a molecular sieve with chabazite-like structure composed of phosphorus, silicon, aluminum and oxygen. Its structural unit consists of PO 2 + , SiO 2 and AlO 2 - Tetrahedral structure, anhydrous chemical composition can be expressed as: mM (Si x ·Al y ·P z )O 2 , in the above formula, M is the template agent present in the molecular sieve crystal, m is the mole fraction of M, x, y, z are the mole fractions of Si, Al, and P respectively, and satisfy x+y+z=1. In the early 1980s Wilson S.T. and Flanigen E.M. of United Carbide Corporation (U.C.C) successfully synthes...

Claims

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Application Information

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IPC IPC(8): C01B39/54C01B37/08
Inventor 肖丰收朱龙凤任利敏张海燕孟祥举
Owner ZHEJIANG UNIV
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