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Method for recovering mesoporous molecular sieve organic template

A technology of organic templates and mesoporous molecular sieves, applied in solid solvent extraction, etc., can solve problems such as no relevant literature reports

Inactive Publication Date: 2012-09-26
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Mesoporous molecular sieves with high hydrothermal stability can be prepared by using P123 to assemble the precursor of Y-type molecular sieves. There is no relevant literature report on the recovery technology of the template agent in this molecular sieve.

Method used

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  • Method for recovering mesoporous molecular sieve organic template
  • Method for recovering mesoporous molecular sieve organic template

Examples

Experimental program
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Effect test

Embodiment 1

[0019] The raw material is the mesoporous molecular sieve obtained by assembling the precursor of the Y-type molecular sieve by using P123, wherein the content of the template agent is 30-45%. Weigh 10 g of raw material and add it to the extractor, supercritical CO 2 After fully mixing with the entrainer n-hexane, it is added into the extractor from the bottom of the extractor. Control the pressure of the extractor at 25±2MPa, the temperature at 40±3°C, supercritical CO 2 The flow rate is 40L / h, the extraction time is 2.5h, the molar ratio of entrainer n-hexane is 0.035, and the recovery rate of template agent is about 72%.

Embodiment 2

[0021] The raw material is the mesoporous molecular sieve obtained by assembling the precursor of the ZSM-5 molecular sieve with P123, wherein the content of the template agent is 30-45%. Take by weighing 35g of raw material and add in the extractor, entrainer acetone and supercritical CO 2 After mixing well, add to the extractor from the bottom of the extractor. Control the pressure of the extractor at 13.5±2MPa and the temperature at 65±2°C. Static extraction was carried out for 2 hours first, and the molar ratio of entrainer acetone was 0.05. Reconditioning supercritical CO 2 The flow rate is 45L / h, the dynamic extraction time is 2.5h, and the recovery rate of template agent is about 81%.

Embodiment 3

[0023] The raw material is the mesoporous molecular sieve obtained by assembling the precursor of the BETA molecular sieve by using P123, wherein the content of the template agent is 30-45%. Weigh raw material 9.9g and add in the extractor, entrainer ethyl ester and supercritical CO 2 After mixing well, add to the extractor from the bottom of the extractor. Control the pressure of the extractor to 20±2MPa, the temperature to 65±2°C, the molar fraction of entrainer ethyl ester to be 0.10, supercritical CO 2 The flow rate is 50L / h, and the extraction time is 4h. The recovery rate of the templating agent was about 88%.

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Abstract

The invention relates to a method for recovering a mesoporous molecular sieve organic template. The method comprises the following steps of: filling mesoporous molecular sieve with 30-45 wt% of organic template into an extractor; flowing supercritical carbon dioxide and entrainer into the extractor simultaneously, with extraction pressure of 10-30 MPa, supercritical carbon dioxide flow of 40-60 L / h and extraction time of 2-6 h, at 40-70 DEG C, wherein the entrainer is hexane, acetone, ethyl ester or a mixture of ethanol and ethyl ester in a volume ratio of 1:1, and a molar ratio of entrainer to carbon dioxide is 0.03-0.15; separating the organic template, entrainer and carbon dioxide in the extract at normal temperature and normal pressure; and evaporating to remove the entrainer and recovering the organic template. A recovery rate of the template reaches more than 80%.

Description

technical field [0001] The invention relates to a method for recovering an organic template of a mesoporous molecular sieve, in particular to a method for recovering an organic template by using a supercritical fluid containing an entrainer. Background technique [0002] As an efficient green separation technology, supercritical fluid extraction may realize the effective recycling of template agents. Supercritical CO as a supercritical fluid 2 (Critical temperature: 31.04°C; Critical pressure: 7.38MPa) It has the advantages of being safe, non-toxic, non-flammable and explosive, inert, cheap and easy to obtain. Supercritical CO 2 It has many special properties, such as strong dissolving ability and transmission performance, and small changes in temperature and pressure near its critical point will cause obvious changes in its density, which in turn will cause significant changes in solute solubility. non-polar supercritical CO 2 It has a strong dissolving ability for non-...

Claims

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Application Information

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IPC IPC(8): B01D11/02
Inventor 谭青峰刘洪涛兰玲徐春艳袁晓亮胡胜
Owner PETROCHINA CO LTD
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