Method for preparing b-axial oriented ZSM-5 molecular sieve nano-ceramic composite membrane

A nano-ceramic, ZSM-5 technology, applied in the fields of inorganic porous materials, membrane separation and membrane catalysis, to achieve the effect of improving completeness, promoting directional growth and wide applicability

Active Publication Date: 2017-03-22
GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the preparation process of molecular sieve membranes has been developed rapidly in the past ten years, there are still many difficult problems in the preparation and application of ZSM-5 molecular sieve membranes due to the limitation of carrier flatness and other aspects.

Method used

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  • Method for preparing b-axial oriented ZSM-5 molecular sieve nano-ceramic composite membrane
  • Method for preparing b-axial oriented ZSM-5 molecular sieve nano-ceramic composite membrane
  • Method for preparing b-axial oriented ZSM-5 molecular sieve nano-ceramic composite membrane

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preparation example Construction

[0029] A method for preparing a b-axis oriented ZSM-5 molecular sieve nano-ceramic composite membrane, comprising the steps of:

[0030] (1) Preparation of ZSM-5 molecular sieve seed crystal: using aluminum source, silicon source, organic template and water as raw materials, the molar composition of raw materials in the reaction system is calculated as oxide: 1Al 2 o 3 :aSiO 2 :bTemplate:cH 2 O, a=10~1000, b=0.5~3, c=4.5~100, Template is an organic template, according to the above dosage, add the silicon source into the water, stir until it is completely dissolved and become a silica sol, under stirring, The aluminum source and the organic template are gradually added dropwise to the silica sol, and the stirring is continued until uniform, and the pH of the reaction solution is adjusted to 11-12 to obtain the ZSM-5 molecular sieve synthetic solution;

[0031] Put the ZSM-5 molecular sieve synthesis solution into a reaction container, then put the reaction container into a h...

Embodiment 1

[0038] (1) Preparation of ZSM-5 molecular sieve seed crystals

[0039] According to 1Al 2 o 3 :1000SiO2 2 :3TEA:100H 2 The material ratio of O is used to prepare the synthetic liquid. The aluminum source and silicon source in the reaction are AlCl 3 And ethyl orthosilicate, while using triethylamine as template agent. Add a certain amount of NaOH in pure water, so that the pH value of the solution is 11-12, dissolve ethyl orthosilicate for 5 hours under stirring conditions, and make it completely hydrolyzed; after the aqueous solution is clarified, add a proportioned amount of AlCl 3 , stirring and dissolving for 3 hours. After the substances are completely dissolved, adjust the pH value of the reaction solution to 11-12, and age it at room temperature for 10 hours, and then add it to the reaction kettle. Place the reaction kettle in an oven that has been heated to 140°C, and react under stirring conditions for 100 hours. After the reaction is completed, the reaction ket...

Embodiment 2

[0048] (1) Preparation of ZSM-5 molecular sieve seed crystals

[0049] It is basically the same as Example 1, except that in the process of preparing the ZSM-5 molecular sieve synthetic solution, the aluminum source and silicon source used are respectively pseudo-boehmite and water glass, and tetrapropylammonium bromide is used as a template .

[0050] (2) Preparation of aluminum sol

[0051] It is basically the same as Embodiment 1, except that aluminum sulfate is used as the aluminum source.

[0052] (3) Preparation of ZSM-5 molecular sieve nano-ceramic composite membrane with b-axis orientation

[0053] Basically the same as Example 1, the difference is that the carrier used is porous stainless steel, and the air flow rate becomes 1m 3 / h, the calcination temperature becomes 480°C.

[0054] The ZSM-5 molecular sieve nano-ceramic composite membrane prepared by embodiment 2 is detected by SEM, and the results are as follows: image 3 It can be seen that the prepared ZSM-...

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Abstract

The invention relates to a method for preparing a b-axial oriented ZSM-5 molecular sieve nano-ceramic composite membrane. The method comprises the following steps: (1) preparing ZSM-5 molecular sieve synthetic liquid by using an aluminum source, a silicon source, an organic template agent and water as raw materials, and reacting the synthetic liquid to obtain a ZSM-5 molecular sieve seed crystal; (2) dissolving the aluminum source in distilled water to prepare alumina sol, heating the alumina sol to 80-95 DEG C, and adding chitosan and dissolving; and (3) adding the ZSM-5 molecular sieve seed crystal into the mixed solution, coating the mixed solution on the outer surface of a carrier, putting the carrier into a heating device, heating to 480-800 DEG C, and keeping temperature constant to obtain the b-axial oriented ZSM-5 molecular sieve nano-ceramic composite membrane. The preparation process is mild in condition and simple in operation, can be used for developing a novel composite membrane, and is beneficial to industrialization of gas separation, purification, alcohol-water low-energy-consumption membrane separation and other technologies by combining the advantages of the oriented ZSM-5 molecular sieve membrane and a nano-ceramic membrane.

Description

technical field [0001] The invention belongs to the technical fields of inorganic porous materials, membrane separation and membrane catalysis, and in particular relates to a method for preparing a b-axis oriented ZSM-5 molecular sieve nano-ceramic composite membrane. Background technique [0002] ZSM-5 is a kind of zeolite molecular sieve with a wide range of applications. It has a two-dimensional pore structure and its effective pore size is about 0.55nm. It is suitable for adsorption and separation of various important industrial raw materials, and has good shape-selective catalytic performance; and Due to the higher silicon-aluminum ratio (Si / Al ratio), its hydrothermal stability and chemical stability are better. Therefore, the ZSM-5 molecular sieve membrane is considered to be the most potential molecular sieve membrane. Pure silicon or high silicon ZSM-5 (silicalite-1) molecular sieve membrane not only has high stability, but also has good hydrophobic properties. It ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/02B01D67/00B01D53/22B01J29/40B01J35/02
CPCB01D53/228B01D67/0039B01D71/028B01J29/40B01J35/02
Inventor 杨文申郎林阴秀丽吴创之
Owner GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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