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Method for preparing metal modified SAPO-34 molecular sieve

A SAPO-34 and metal modification technology, applied in the field of molecular sieves, can solve the problems of poor dispersion of SAPO-34 molecular sieves and low metal content, and achieve the effects of lowering temperature, reducing difficulty, and large specific surface area

Active Publication Date: 2015-04-08
SHANDONG QILU HUAXIN HIGH TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the metal content introduced by the current method is less and concentrated, and cannot be well dispersed in SAPO-34 molecular sieve

Method used

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  • Method for preparing metal modified SAPO-34 molecular sieve
  • Method for preparing metal modified SAPO-34 molecular sieve

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preparation example Construction

[0025] A kind of preparation method of metal modified SAPO-34 molecular sieve, comprises the steps:

[0026] (1) Mix the aluminum source and the mixed template agent and stir evenly, add deionized water, phosphorus source, and silicon source in turn, and stir at 20~30°C for 1~2 hours to mix evenly to obtain a mixed reaction solution; the mixed reaction Al in liquid 2 o 3 :P 2 o 5 : SiO 2 : mixed templating agent: H 2 The molar ratio of O is 0.8~1.2: 0.8~1.2: 0.2~0.4: 1.5~2.5: 50~70; the mixed templating agent is composed of tetraethylammonium hydroxide and morpholine, tetraethylammonium hydroxide and morpholine The molar ratio of morphine is 1:2~4;

[0027] (2) Mix the sodium carboxymethyl cellulose and the mixed reaction solution obtained in step (1) evenly, then put it into a high-temperature reactor and pre-crystallize it at 140-160°C for 20-24 hours, then raise the temperature to 160-180°C Crystallize for 40-50 hours, and centrifuge the mixed reaction solution to ob...

Embodiment 1

[0043] A kind of preparation method of copper metal modified SAPO-34 molecular sieve, comprises the steps:

[0044] (1) Mix the aluminum source and the mixed template agent and stir evenly, add deionized water, phosphorus source, and silicon source in turn, and stir at 30°C for 2 hours to mix evenly to obtain a mixed reaction solution; the Al in the mixed reaction solution 2 o 3 :P 2 o 5 : SiO 2 : mixed templating agent: H 2 The molar ratio of O is 0.8:0.8:0.2:1.5:50; the mixed template is composed of tetraethylammonium hydroxide and morpholine, and the molar ratio of tetraethylammonium hydroxide and morpholine is 1:2;

[0045] (2) Mix the sodium carboxymethyl cellulose and the mixed reaction liquid obtained in step (1) evenly, then put it into a high-temperature reactor and pre-crystallize at 160°C for 24 hours, then raise the temperature to 180°C for 50 hours, and put The mixed reaction solution is centrifuged to obtain filter cake and mother liquor; the mass ratio of s...

Embodiment 2

[0050] A kind of preparation method of nickel metal modified SAPO-34 molecular sieve, comprises the steps:

[0051] (1) Mix the aluminum source and the mixed template agent and stir evenly, add deionized water, phosphorus source, and silicon source in turn, and stir at 20°C for 1 hour to mix evenly to obtain a mixed reaction solution; the Al in the mixed reaction solution 2 o 3 :P 2 o 5 : SiO 2 : mixed templating agent: H 2 The molar ratio of O is 1.2:1.2:0.4:2.5:70; the mixed template is composed of tetraethylammonium hydroxide and morpholine, and the molar ratio of tetraethylammonium hydroxide and morpholine is 1:4;

[0052] (2) Mix the sodium carboxymethyl cellulose and the mixed reaction solution obtained in step (1) evenly, then put it into a high-temperature reaction kettle for pre-crystallization at 140°C for 20 hours, then raise the temperature to 160°C for crystallization for 40 hours, and mix The reaction solution is centrifuged to obtain filter cake and mother ...

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Abstract

The invention discloses a metal modified SAPO-34 molecular sieve. The preparation method comprises the following steps: adopting a mixed template agent of tetraethylammonium hydroxide and morpholine, adding a proper silicon source, an aluminum source and a phosphorus source, controlling the pre-crystallization and crystallization conditions, and adding sodium carboxymethyl cellulose in a proper ratio, thereby obtaining the SAPO-34 molecular sieve filter cake and a mother solution; mixing a metal salt and the mother solution to generate a metal complex, finally, adding dextrin into the metal complex and the SAPO-34 molecular sieve filter cake, performing centrifugal separation to obtain a filter cake, performing ion exchange between the filter cake and ammonium chloride to obtain metal modified SAPO-34 molecular sieve raw powder, and roasting, thereby obtaining the metal modified SAPO-34 molecular sieve. According to the process disclosed by the invention, the regular pore structure and large specific surface area of the SAPO-34 molecular sieve can be effectively maintained, the ratio of the pores can be improved to be about 90 percent by effectively regulating the acidity and pore size, and the ethylene / propylene selectivity of the reaction for producing olefins from methanol is improved to be 94 percent. According to the process disclosed by the invention, metals can be uniformly distributed in the SAPO-34 molecular sieve, and the mother solution treatment difficulty can be reduced.

Description

technical field [0001] The invention relates to the technical field of molecular sieves, in particular to a preparation method of metal-modified SAPO-34 molecular sieves. Background technique [0002] SAPO-34 molecular sieve is currently recognized as the best MTO catalyst. The main problems faced by this catalyst are low catalytic life due to carbon deposition and low selectivity of low-carbon olefins. The selectivity of low-carbon olefins is mainly affected by the strength and number of acid sites in the molecular sieve framework. Stronger acid sites are conducive to the formation of alkane molecules, while weaker acid sites affect the conversion rate of methane; currently, changing the acid site intensity There are mainly two ways of summing and number, introducing metal ions into the SAPO-34 molecular sieve framework or changing the coordination environment and relative content of silicon in the molecular sieve framework; among them, introducing metal ions into the SAPO-...

Claims

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Application Information

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IPC IPC(8): C01B39/54C01B37/08
Inventor 梁光华明曰信陈文勇彭立
Owner SHANDONG QILU HUAXIN HIGH TECH
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