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Method for preparing highly-oriented MFI-type molecular sieve membrane by secondary growth process

A secondary growth and orientation technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of corrosiveness of synthesis liquid, harsh conditions, and relatively high carrier requirements, and achieve simple operation, continuous film layer, and good orientation Effect

Inactive Publication Date: 2015-09-09
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In summary, although people have a high degree of synthetic b The axis-oriented MFI molecular sieve membrane has made a lot of efforts and made some progress, but the current secondary growth method b The method of axially oriented MFI type molecular sieve membrane, some conditions are harsh, some synthetic liquids are corrosive, have relatively high requirements on the carrier, and some cannot completely suppress the formation of twins
That is to say, there is no simple and effective preparation of high b Axial Oriented MFI Molecular Sieve Membrane Method

Method used

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  • Method for preparing highly-oriented MFI-type molecular sieve membrane by secondary growth process
  • Method for preparing highly-oriented MFI-type molecular sieve membrane by secondary growth process
  • Method for preparing highly-oriented MFI-type molecular sieve membrane by secondary growth process

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Embodiment 1

[0029] 1) The preparation of the secondary growth synthesis solution, according to the molar ratio of the composition of the synthesis solution: Tetraethyl orthosilicate (TEOS): tetrapropylammonium hydroxide (TPAOH): water = 1:0.2:200, TEOS, TPAOH Mix with water, stir at room temperature for 3 hours, add the calculated amount of ammonium sulfate aqueous solution to the clarified mixed solution, and continue stirring for 1 hour to obtain the final synthetic solution; the molar composition of the final synthetic solution is: TEOS:TPAOH:H 2 O: ammonium sulfate=1:0.2:200:0.075

[0030] 2) Put the carrier coated with the b-axis orientation seed layer into a high-pressure synthesis kettle, pour the above synthesis liquid, and seal; crystallize at 150°C for 3 hours;

[0031] 3) Cool the synthesis kettle, take out the carrier, wash and dry, and obtain an oriented MFI molecular sieve membrane on the carrier, such as figure 2 .

Embodiment 2

[0033] With embodiment 1, the molar composition of final synthetic liquid is: TEOS:TPAOH:H 2 O: ammonium sulfate=1:0.2:200:0.1; crystallize at 150°C for 4 hours; obtain MFI molecular sieve membrane on the carrier, such as image 3 , and its X-ray diffraction pattern is as Figure 4 , the resulting molecular sieve membrane is of height b Axially oriented MFI type molecular sieve membrane.

Embodiment 3

[0035] 1) The preparation of the secondary growth synthetic solution, according to the molar ratio of the synthetic solution: TEOS:TPAOH:H 2O=1:0.1:250, mix TEOS, TPAOH and water, stir at room temperature for 5 hours, add the calculated amount of ammonium bicarbonate aqueous solution into the clear mixed solution, and continue stirring for 1 hour to obtain the final synthetic solution; finally synthesize The molar composition of the liquid is: TEOS:TPAOH:H 2 O: ammonium bicarbonate=1:0.1:250:0.1;

[0036] 2) Put the carrier coated with the b-axis orientation seed layer into a high-pressure synthesis kettle, pour the above synthesis liquid, and seal; crystallize at 180°C for 3 hours;

[0037] 3) Cool the synthesis kettle, take out the carrier, wash and dry, and obtain an oriented MFI molecular sieve membrane on the carrier, such as Figure 5 .

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Abstract

The invention discloses a method for preparing a highly-oriented MFI-type molecular sieve membrane by a secondary growth process, which comprises the following steps: 1) preparation of a secondary growth synthesis liquid: mixing certain amounts of ethyl orthosilicate, tetrapropyl ammonium hydroxide and water, stirring at room temperature for 3-5 hours, adding an ammonium salt water solution with a certain concentration into the clear synthesis liquid, and continuing stirring for 1-3 hours to obtain the final synthesis liquid, wherein the synthesis liquid is composed of the following components in parts by mole: 1 part of ethyl orthosilicate, 0.1-0.4 part of tetrapropyl ammonium hydroxide, 100-500 parts of water and 0.075-0.3 part of water; 2) putting a carrier coated with a b-axis-oriented crystal seed layer into a high-pressure synthesis kettle, pouring the synthesis liquid, and sealing; crystallizing at 120-180 DEG C for 3-12 hours; and 3) cooling the synthesis kettle, taking out the carrier, washing and drying to obtain the oriented MFI-type molecular sieve membrane on the carrier. The ammonium salt added into the traditional synthesis liquid can effectively inhibit the twin crystal from generation in the secondary growth process. The method is simple to operate, and has the advantages of wide application range, no special requirements for the carrier and low preparation cost.

Description

technical field [0001] The invention relates to the synthesis of MFI molecular sieve membranes, and in particular provides a method for synthesizing highly oriented MFI molecular sieve membranes by adding crystallization regulators into traditional synthesis liquids. Background technique [0002] Zeolite molecular sieve is an excellent inorganic membrane material, which has the advantages of regular pore structure and adjustable pore size distribution, excellent thermal stability, chemical stability and biological stability, and has broad application prospects in the field of advanced functional materials; it Not only can it be used as catalytic membrane, separation membrane, microreactor element, chemical sensor, modified electrode, but also as photoelectric material, low dielectric constant material, proton exchange membrane, anti-corrosion coating and hydrophobic antibacterial material, etc.; The research on zeolite molecular sieve membrane has been widely concerned by sc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 王正宝路晓飞彭勇
Owner ZHEJIANG UNIV
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