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Preparation method of high-silicon ZSM-5 molecular sieve with mesoporous structure

A technology of ZSM-5 and mesoporous structure, which is applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of poor adsorption capacity of molecular sieve and weak hydrophobicity of molecular sieve, and achieve Improve the adsorption capacity, increase the ratio of silicon to aluminum, and increase the effect of specific surface area

Pending Publication Date: 2022-07-22
山东亮剑环保新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, industrial VOCs contain a large amount of water vapor. Due to the weak hydrophobicity of molecular sieves, there will be competition between water vapor and molecular sieves when adsorbing macromolecular organics, which will further cause the adsorption capacity of molecular sieves to deteriorate.

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0021] A method for preparing a high-silicon ZSM-5 molecular sieve with a mesoporous structure provided in the embodiment of the present invention mainly includes the following steps:

[0022] Step S10: Dissolve 30g of tetrapropylammonium bromide in 30mL of water, gradually add 100g of silica sol (20% content) at a temperature of 15-25°C, place it in an ultrasonic device for ultrasonic treatment for 2-3 hours, and filter to obtain pure ZSM-5 clusters of silicon.

[0023] Step S20: fully mix 2g of hexadecyltrimethoxysilane, 10g of ammonium carbonate and the ZSM-5 crystal cluster obtained above, add 10g of sodium hydroxide to adjust the pH to 9-11, and simultaneously add 5g of aluminum sol ( 20% content) and 200 g of silica sol (20% content), stirred at 30°C for 3 hours.

[0024] Step S30: put the crystallization liquid into a crystallization kettle and crystallize at 160° C. for 24 hours. After filtering, washing, and drying, calcining at 550° C. for 5 hours to obtain the high...

Embodiment 2

[0026] A method for preparing a high-silicon ZSM-5 molecular sieve with a mesoporous structure provided in the embodiment of the present invention mainly includes the following steps:

[0027] Step S10: Dissolve 30g of tetrapropylammonium bromide in 30mL of water, gradually add 150g of silica sol (20% content) at a temperature of 15-25°C, place it in an ultrasonic device for ultrasonic treatment for 2-3 hours, and filter to obtain pure ZSM-5 clusters of silicon.

[0028] Step S20: fully mix 2.5g of hexadecyltrimethoxysilane, 20g of ammonium carbonate and the ZSM-5 crystal cluster obtained above, add 10g of sodium hydroxide to adjust the pH to 9-11, and simultaneously add 5g of aluminum sol under stirring (20% content) and 150 g of silica sol (20% content), stirred at 30°C for 3 hours.

[0029] Step S30: put the crystallization liquid into a crystallization kettle and crystallize at 180°C for 72 hours. After filtering, washing and drying, calcining at 550°C for 5 hours to obta...

Embodiment 3

[0031] A method for preparing a high-silicon ZSM-5 molecular sieve with a mesoporous structure provided in the embodiment of the present invention mainly includes the following steps:

[0032] Step S10: Dissolve 30 g of tetrapropylammonium bromide in 30 mL of water, gradually add 50 g of silica sol (20% content) at a temperature of 15-25 °C, place it in an ultrasonic device for ultrasonic treatment for 2-3 hours, and filter to obtain pure ZSM-5 clusters of silicon.

[0033] Step S20: fully mix 2g of hexadecyltrimethoxysilane, 10g of ammonium carbonate and the ZSM-5 crystal cluster obtained above, add 10g of sodium hydroxide to adjust the pH to 9-11, and add 3g of aluminum sol ( 20% content) and 250 g of silica sol (20% content), stirred at 30°C for 3 hours.

[0034] Step S30: put the crystallization liquid into a crystallization kettle and crystallize at 160° C. for 24 hours. After filtering, washing, and drying, calcining at 550° C. for 5 hours to obtain the high-silicon ZSM...

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Abstract

The embodiment of the invention provides a preparation method of a high-silicon ZSM-5 molecular sieve with a mesoporous structure, and belongs to the technical field of molecular sieve preparation. The preparation method comprises the following steps: dissolving tetrapropylammonium bromide in water, gradually adding a silicon source at a certain temperature, placing the mixture in an ultrasonic device for ultrasonic treatment for 2-3 hours, and filtering to obtain a pure silicon ZSM-5 crystal cluster; the preparation method comprises the following steps: fully mixing an organic pore-enlarging agent, an inorganic pore-enlarging agent, ZSM-5 crystal clusters and water, adding sodium hydroxide to adjust the pH value to 9-11, simultaneously adding an aluminum source and a silicon source in a stirring state, and stirring for a period of time at a certain temperature; filling the crystallization liquid into a crystallization kettle, crystallizing for a certain time at a certain temperature, filtering, washing, drying and roasting to obtain the high-silicon ZSM-5 molecular sieve. The microporous molecular sieve is subjected to chambering modification and the hydrophobic property of the molecular sieve is improved, so that the adsorption capacity of the molecular sieve on macromolecular organic matters is improved.

Description

technical field [0001] The invention relates to the technical field of molecular sieve preparation, in particular to a preparation method of a high-silicon ZSM-5 molecular sieve with a mesoporous structure. Background technique [0002] At present, ZSM-5 molecular sieves have been widely used in the field of VOCs (Volatile Organic Compounds; volatile organic compounds) adsorption. However, as a kind of microporous molecular sieve with MFI topology, ZSM-5 molecular sieve has limited application in the adsorption of macromolecular organic substances. For macromolecular organics whose molecular size exceeds the pore size of zeolite, molecular sieves are powerless. At the same time, industrial VOCs contain a large amount of water vapor. Due to the weak hydrophobicity of molecular sieves, there will be competition between water vapor and molecular sieves when adsorbing macromolecular organic substances, which further causes the adsorption capacity of molecular sieves to deterior...

Claims

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Application Information

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IPC IPC(8): C01B39/40
CPCC01B39/40
Inventor 王冠庆梁飞杜忠杰曾褔厚陈亮
Owner 山东亮剑环保新材料有限公司
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