Method for preparing SAPO-35 molecular sieve with N-methyl piperidine being template agent

A technology of SAPO-35 and methylpiperidine, which is applied in the field of preparing SAPO-35 molecular sieves, can solve the problems of long crystallization time and narrow silicon content of SAPO-35, and achieve good crystallinity, good thermal stability and hydrothermal The effect of stability and convenient operation

Active Publication Date: 2019-04-16
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In 1984, US4440871 disclosed a method for the hydrothermal synthesis of SAPO-35 molecular sieve using quinucidine as an organic template for the first time. The SAPO-35 prepared by this method has a narrow silicon content and a long crystallization time

Method used

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  • Method for preparing SAPO-35 molecular sieve with N-methyl piperidine being template agent
  • Method for preparing SAPO-35 molecular sieve with N-methyl piperidine being template agent
  • Method for preparing SAPO-35 molecular sieve with N-methyl piperidine being template agent

Examples

Experimental program
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Effect test

Embodiment 1

[0025] At 25°C, dissolve 1g of pseudo-boehmite with 16mL of deionized water, then dropwise add 3.3g of phosphoric acid (85% by mass) and continue stirring evenly, then add 0.31g of tetraethyl orthosilicate, 5.4mL of N -Methyl piperidine, stir evenly, transfer to a stainless steel reaction kettle, put it in an oven at 180°C for 3 days to crystallize, then cool the reaction kettle, collect the product, wash with deionized water until neutral, centrifuge, and dry at 75°C , the acquired product SAPO-35 molecular sieve, the product quality is 0.65g. In this example, the molar ratio of the synthesized gel is 6.15R:0.2SiO 2 :Al 2 o 3 : 2.0P 2 o 5 : 124H 2 O.

Embodiment 2

[0027] At 25°C, dissolve 1g of pseudo-boehmite with 16mL of deionized water, then dropwise add 3.3g of phosphoric acid (85% mass fraction) and continue to stir evenly, then add 0.62g of tetraethyl orthosilicate, 5.4mL of N -Methyl piperidine, stir evenly, transfer to a stainless steel reaction kettle, put it in an oven at 180°C for 3 days to crystallize, then cool the reaction kettle, collect the product, wash with deionized water until neutral, centrifuge, and dry at 75°C , the obtained product SAPO-35 molecular sieve, the product quality is 1.4g. In this example, the molar ratio of the synthesized gel is 6.15R:0.4SiO 2 :Al 2 o 3 : 2.0P 2 o 5 : 124H 2 O.

Embodiment 3

[0029] At 25°C, dissolve 1g of pseudo-boehmite with 16mL of deionized water, then dropwise add 3.3g of phosphoric acid (mass fraction 85%) and continue stirring evenly, then add 0.93g of tetraethyl orthosilicate, 5.4mL of N -Methyl piperidine, stir evenly, transfer to a stainless steel reaction kettle, put it in an oven at 180°C for 3 days to crystallize, then cool the reaction kettle, collect the product, wash with deionized water until neutral, centrifuge, and dry at 75°C , the obtained product SAPO-35 molecular sieve, the product quality is 1.4g. In this example, the molar ratio of the synthesized gel is 6.15R:0.6SiO 2 :Al 2 o 3 : 2.0P 2 o 5 : 124H 2 O.

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Abstract

The invention discloses a method for preparing an SAPO-35 molecular sieve with N-methyl piperidine being a template agent, and belongs to the technical field of SAPO molecular sieve preparation. A silicon source, an aluminum source, a phosphorus source and the N-methyl piperidine template agent are mixed and then stirred at the temperature of 10-40 DEG C uniformly to obtain initial synthesized gel; then the initial synthesized gel is subjected to hydrothermal crystallization for 1-5 days at the temperature of 160-200 DEG C and under a self-generated pressure condition; finally, hydrothermal crystallization products are collected, washed and separated and dried in a drying oven at the temperature of 50-100 DEG C to obtain the SAPO-35 molecular sieve. The prepared SAPO-35 molecular sieve isgood in crystallization degree, basically free of impurities and better in thermal stability and hydrothermal stability, and the adjustable range of the content of silicon is wide. The method is simple in step and convenient to operate, and the prepared SAPO-35 molecular sieve is suitable for a hydrocarbon conversion technology and others, suitable for an methanol-to-olefin process, and high in selectivity for ethylene, and has good prospects of industrial development.

Description

technical field [0001] The invention belongs to the technical field of preparing SAPO molecular sieves, and in particular relates to a method for preparing SAPO-35 molecular sieves by using N-methylpiperidine as a template. Background technique [0002] Aluminum phosphate molecular sieve is a new generation of molecular sieve (US4310440) invented by UCC Company in the United States in the early 1980s after aluminum silicate molecular sieve. Since the molecular sieve framework is electrically neutral, it has no cation exchange performance and catalytic reaction performance. [0003] Introducing silicon into the framework of aluminum phosphate molecular sieve will become silicoaluminophosphate molecular sieve, that is, SAPO series molecular sieve (US4440871). The molecular sieve framework is composed of phosphorus oxygen tetrahedron, aluminum oxygen tetrahedron and silicon oxygen tetrahedron. There are balance cations outside the framework, so it has cation exchange performan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/54C01B37/08
CPCC01B37/08C01B39/54C01P2002/72C01P2004/03
Inventor 于吉红李妍
Owner JILIN UNIV
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