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A method for preparing sapo-35 molecular sieves using n-methylpiperidine as a template

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: 2022-04-08
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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  • A method for preparing sapo-35 molecular sieves using n-methylpiperidine as a template
  • A method for preparing sapo-35 molecular sieves using n-methylpiperidine as a template
  • A method for preparing sapo-35 molecular sieves using n-methylpiperidine as a template

Examples

Experimental program
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Effect test

Embodiment 1

[0025] At 25°C, 1 g of pseudo-boehmite was dissolved in 16 mL of deionized water, and then 3.3 g of phosphoric acid (85% by mass) was added dropwise to continue stirring, and then 0.31 g of ethyl orthosilicate and 5.4 mL of N -Methyl piperidine, stir evenly, transfer to a stainless steel reaction kettle, stand for crystallization at 180 °C for 3 days, 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 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 1 g of pseudo-boehmite with 16 mL of deionized water, then dropwise add 3.3 g of phosphoric acid (85% by mass) and continue to stir evenly, then add 0.62 g of ethyl orthosilicate, 5.4 mL of N -Methyl piperidine, stir evenly, transfer to a stainless steel reaction kettle, stand for crystallization at 180 °C for 3 days, 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, 1 g of pseudo-boehmite was dissolved in 16 mL of deionized water, then 3.3 g of phosphoric acid (85% by mass) was added dropwise to continue stirring, and then 0.93 g of ethyl orthosilicate and 5.4 mL of N -Methyl piperidine, stir evenly, transfer to a stainless steel reaction kettle, stand for crystallization at 180 °C for 3 days, 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 SAPO-35 molecular sieves by using N-methylpiperidine as a template agent, belonging to the technical field of SAPO molecular sieve preparation. It is to mix the silicon source, aluminum source, phosphorus source, N-methylpiperidine organic template and water and stir at 10-40°C to obtain the initial synthetic gel, and then the initial synthetic gel is heated at 160-200 ℃ and autogenous pressure conditions for hydrothermal crystallization for 1-5 days, and finally the hydrothermal crystallization products were collected, washed with water, separated, and dried in an oven at 50-100 ℃ to obtain SAPO‑35 molecular sieves. The prepared SAPO-35 molecular sieve has good crystallinity, is basically free of impurities, has a wide adjustable range of silicon content, and has better thermal stability and hydrothermal stability. The method has simple steps and convenient operation, and the prepared SAPO‑35 molecular sieve is suitable for hydrocarbon conversion processes and the like, such as the process of methanol to olefins, and its ethylene selectivity is relatively high. The prospect of industrial development is good.

Description

technical field [0001] The invention belongs to the technical field of SAPO molecular sieve preparation, in particular to a method for preparing SAPO-35 molecular sieve by using N-methylpiperidine as a template agent. Background technique [0002] Aluminum phosphate molecular sieve is a new generation of molecular sieve (US4310440) invented by UCC 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] When silicon is introduced into the framework of aluminum phosphate molecular sieve, it becomes silicoaluminophosphate molecular sieve, namely SAPO series molecular sieve (US4440871). There are balance cations outside the framework, so it has cation exchange performance, when the extra framework cation is H + When the molecular sieve has an acidic center, it has the performance of acidic catalytic reaction. As the active compone...

Claims

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Application Information

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Patent Type & Authority Patents(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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