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A kind of preparation method of multi-layer structured molecular sieve membrane

A technology of multi-layer structure and molecular sieve is applied in the field of preparation of multi-layer structure type molecular sieve membrane materials, which can solve the problems of high cost and complicated process, and achieve the effects of high success rate, simple process and excellent hydrophobic performance.

Inactive Publication Date: 2018-12-11
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that the synthesis liquid needs to form local supersaturation near the surface of the carrier, and crystal nuclei are generated on the surface of the carrier, and molecular sieve membranes are formed by continuous growth, mutual fusion, and crosslinking.
The disadvantage is that it needs to replace the synthetic mother liquor of the molecular sieve membrane, resulting in cumbersome process and high cost (Ma Ning, PhD thesis of Tianjin University, "Microstructure Control and Application of Oriented Beta Zeolite Membrane", 2011)

Method used

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  • A kind of preparation method of multi-layer structured molecular sieve membrane
  • A kind of preparation method of multi-layer structured molecular sieve membrane
  • A kind of preparation method of multi-layer structured molecular sieve membrane

Examples

Experimental program
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Effect test

example 1

[0042] In this example, the dynamic wetting method is used to coat the seed layer, and the periodic secondary growth method is used to synthesize the TS-1 molecular sieve membrane.

[0043] The first step, the dynamic wetting method to prepare the seed layer:

[0044] Disperse 0.20g of TS-1 molecular sieve with a particle size of 400nm in 19.80g of absolute ethanol at 75°C to obtain a 1wt.% seed crystal suspension; then immerse the carrier in the seed crystal solution and take it out after 10s; dry: Drying at 60°C for 0.5h; calcination: calcination at 600°C for 3h, the seeds are uniformly dispersed in the surface defects of the carrier.

[0045] The second step is to prepare TS-1 molecular sieve membrane by periodic secondary growth method:

[0046] The molar composition of the synthetic mother liquor used in the periodic secondary growth method is 1.00SiO 2 :0.33TiO 2 :0.08TPAOH:60H 2 O. Orthoethyl silicate (TEOS) is used as the silicon source, and butyl titanate is used...

example 2

[0060] The specific steps of this example 2 are the same as those in Example 1, during which there is no need to replace the synthetic mother liquor, the difference is that the molar composition of the synthetic mother liquor used by the periodic secondary growth method is 1.00SiO 2 :0.33TiO 2 :0.08TPAOH:100H 2 O, the crystallization temperature is 140°C. This example increases the amount of water (H 2 O:SiO 2 =100), for which TS-1 molecular sieve membrane was synthesized by increasing the crystallization temperature (140°C). The TS-1 molecular sieve membrane structure obtained in the experiment is similar to Example 1, and also has a dense cross-linked double-layer membrane structure, and effectively avoids the precipitation of aluminum elements from the surface of the support, while reducing the amount of template used.

example 3

[0062] The specific steps of this example 3 are the same as those in Example 1, during which there is no need to replace the synthetic mother liquor, the difference is that the molar composition of the synthetic mother liquor used in the periodic secondary growth method is 1.00SiO 2 :0.33TiO 2 :0.08TPAOH:800H 2 O, the crystallization temperature is 170°C. The structure of the TS-1 molecular sieve membrane obtained in this example is similar to Example 1. This example increases the amount of water (H 2 O:SiO 2 =800), for which the TS-1 molecular sieve membrane was synthesized by further increasing the crystallization temperature (170°C). The TS-1 molecular sieve membrane structure obtained in the experiment is similar to Example 1, and also has a dense cross-linked double-layer membrane structure, and effectively avoids the precipitation of aluminum elements from the surface of the support, while reducing the amount of template used.

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Abstract

The invention provides a method, i.e., periodic secondary growth method for preparing a multilayer-structured molecular sieve membrane. The method comprises the following steps: (1) preparing a seed crystal layer by a dynamic wetting method; (2) preparing a molecular sieve membrane by the periodic secondary growth method; and (3) activating the molecular sieve membrane. Periodic secondary growth means carrying out programmed control on the temperature of a molecular sieve membrane crystallization process, wherein programmed heating, constant-temperature crystallization and programmed cooling are known as a crystallization period, and the crystallization process may comprise a plurality of crystallization periods. Compared with the traditional secondary growth methods, the method has the advantages that the multilayer-structured molecular sieve membrane can be formed by using a periodic crystallization mode. The molecular sieve membrane has the advantage of no pinhole defect and has very good compactness. The method is simple and efficient in process, has very good repeatability and very high success rate and is applicable to industrial amplified application.

Description

technical field [0001] The invention relates to a preparation method for preparing a multilayer structured molecular sieve membrane material, specifically a method for preparing a dense molecular sieve membrane on a porous alumina ceramic carrier by using a periodic secondary growth method. Background technique [0002] Molecular sieve membrane is a new type of inorganic membrane developed in recent years. Among them, molecular sieve membranes with a pore size of less than 1 nm (for example, MFI, β-type) have the characteristics of general inorganic membranes, but also have a small and uniform pore size, and the cations in the molecular sieve crystal can be exchanged by other ions (such as Ti, Fe, etc.), The Si / Al ratio can be adjusted, and Si or Al atoms can be replaced by other heteroatoms. Among them, the important prerequisite for the application of molecular sieve membrane is that it has good compactness to ensure its excellent performance. Molecular sieve membranes w...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B41/89
Inventor 刘旭光刘勇王壮瑞张宝泉
Owner QINGDAO UNIV OF SCI & TECH