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Method for synthesizing silicalite-1 zeolite membranes

A synthetic method and technology of molecular sieves, applied in the direction of molecular sieve compounds, molecular sieves and base exchange compounds, chemical instruments and methods, etc., to achieve good repeatability

Inactive Publication Date: 2010-04-21
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the synthesis solution of the current secondary growth method contains organic templates, so the calcination stage is inevitable, and the defects caused are also inevitable.

Method used

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  • Method for synthesizing silicalite-1 zeolite membranes
  • Method for synthesizing silicalite-1 zeolite membranes
  • Method for synthesizing silicalite-1 zeolite membranes

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The aluminum oxide with a thickness of 2 mm and a diameter of 20 mm is used as a carrier, its porosity is 45%, and the average diameter of the void is 0.2 μm. Carrier pretreatment: smooth one side of the carrier with 1000-mesh sandpaper, ultrasonic cleaning, and dry at 40°C for two days. stand-by.

[0029] Put the TPAOH (1M) solution in a sealable polytetrafluoroethylene conical flask, and dissolve sodium hydroxide in the solution, heat to 80°C, and at 500rpm, put the fumed silica at a speed of 0.2g per minute This was added in portions to the solution to give a clear solution in the ratio 1 g (silica): 5 ml (TPAOH): 0.7 g (sodium hydroxide). Cool naturally to room temperature and age for 3 hours. Pour the synthesis liquid into a reaction kettle, conduct hydrothermal crystallization at 120° C. for 0.5 days, prepare the obtained seed crystals into a 10-50% solution, and adjust the pH value to about 10.

[0030] A small amount of the above seed crystal solution was tak...

Embodiment 2

[0033] In this experiment, aluminum oxide with a thickness of 2 mm and a diameter of 20 mm was used as a carrier, and its porosity was 45%, and the average diameter of the voids was 0.2 microns. Carrier pretreatment: smooth one side of the carrier with 1000-mesh sandpaper, ultrasonic cleaning, and dry at 40°C for two days. stand-by.

[0034] Put the TPAOH (1M) solution in a sealable polytetrafluoroethylene conical flask, and dissolve sodium hydroxide in the solution, heat to 80°C, and at 500rpm, put the fumed silica at a rate of 0.2g per minute This was added in portions to the solution to give a clear solution in the ratio 1 g (silica): 5 ml (TPAOH): 0.7 g (sodium hydroxide). Cool naturally to room temperature and age for 3 hours. Pour the synthesis solution into a reaction kettle, conduct hydrothermal crystallization at 120° C. for 1 day, prepare the obtained seed crystals into a 10-50% solution, and adjust its pH value to about 10.

[0035]A small amount of the above see...

Embodiment 3

[0038] In this experiment, aluminum oxide with a thickness of 2 mm and a diameter of 20 mm was used as a carrier, and its porosity was 45%, and the average diameter of the voids was 0.2 microns. Carrier pretreatment: smooth one side of the carrier with 1000-mesh sandpaper, ultrasonic cleaning, and dry at 40°C for two days. stand-by.

[0039] Put the TPAOH (1M) solution in a sealable polytetrafluoroethylene conical flask, and dissolve sodium hydroxide in the solution, heat to 80°C, and at 500rpm, put the fumed silica at a rate of 0.2g per minute This was added in portions to the solution to give a clear solution in the ratio 1 g (silica): 5 ml (TPAOH): 0.7 g (sodium hydroxide). Cool naturally to room temperature and age for 3 hours. Pour the synthesis solution into a reaction kettle, conduct hydrothermal crystallization at 120° C. for 2 days, prepare the obtained seed crystals into a 10-50% solution, and adjust its pH value to about 10.

[0040] A small amount of the above s...

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Abstract

The invention discloses a method for synthesizing silicalite-1 zeolite membranes. The method comprises: preparing synthetic fluid of crystal seeds, performing hydrothermal synthesis for 0.5 to 3 days, obtaining crystal seeds uniform in particle size and preparing a crystal-seed solution; impregnating a carrier with the crystal-seed solution for 5 to 10 seconds, drying and roasting the obtained product; preparing template-free zeolite membrane mother liquor, placing diaphragms containing crystal-seed layers in the mother liquor and performing hydrothermal reaction in a reaction kettle for 4 to 8 hours; and washing and drying membranes. As the synthetic fluid has no template, roasting is not needed after secondary growth, so that defect-free pure silicon zeolite membranes can be obtained. The zeolite membranes are resistant to heat and chemicals, have good stability, and can be applied to the permeation and separation of gas and liquid steam at high temperature and other aspects.

Description

Technical field: [0001] The invention relates to a synthesis method of a molecular sieve membrane, in particular to a synthesis method of a template-free silicalite-1 molecular sieve membrane. technical background: [0002] With the shortage of energy, people pay more and more attention to the development and utilization of new energy, and the requirements for the preparation and separation of many new energy are getting higher and higher. The heat resistance and chemical resistance of the organic film cannot meet its requirements, so more and more attention has been paid to the research on inorganic materials. [0003] Molecular sieve is a kind of inorganic membrane material with regular channels, which is based on silicon-oxygen tetrahedron and aluminum-oxygen tetrahedron. The pore size of some molecular sieve crystal channels is similar to that of many industrial raw material molecules. The molecules of the raw material are separated by molecular sieving or selective dif...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/00C01B37/00
Inventor 袁文辉王德临李莉
Owner SOUTH CHINA UNIV OF TECH
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