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Preparation method of molecular sieve membrane

A molecular sieve and seed crystal technology, applied in molecular sieve compounds, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., can solve the problems of complex operation, inability to realize large-scale application, and high requirements for condition control, and achieve good repeatability , High secondary growth activity, high success rate effect

Inactive Publication Date: 2015-03-18
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.
Other methods cannot be applied on a large scale due to complex operations and high requirements for condition control

Method used

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  • Preparation method of molecular sieve membrane
  • Preparation method of molecular sieve membrane
  • Preparation method of molecular sieve membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] In this embodiment, the dynamic wetting method is used to coat the seed layer, and the secondary growth method is used to synthesize the TS-1 molecular sieve membrane.

[0051] The first step, the dynamic wetting method to prepare the seed layer:

[0052]Disperse 0.20 g of TS-1 molecular sieve with a particle size of 400 nm in 19.80 g of absolute ethanol at 75°C to prepare a 1wt.% seed crystal suspension; then immerse the carrier in the seed crystal solution and take it out after 10 s; Drying: drying at 60 °C for 0.5 h; roasting: roasting at 600 °C for 3 h, the seeds are evenly dispersed in the surface defects of the carrier, and the XRD and SEM of the seed layer are shown in the attached figure 1 , 2 , a small amount of nano-crystal seeds are embedded on the surface of the carrier.

[0053] The second step, the secondary growth method to prepare TS-1 molecular sieve membrane:

[0054] The molar composition of the secondary growth solution is 1.00 TEOS : 0.05 TiO 2 ...

Embodiment 2

[0068] In this embodiment, the dynamic wetting method is used to coat the seed layer, and the secondary growth method is used to synthesize the Silicalite-1 molecular sieve membrane.

[0069] The same part of this embodiment and embodiment 1 will not be repeated, the difference is:

[0070] In the second step, the Silicalite-1 molecular sieve membrane is prepared by the secondary growth method,

[0071] Concrete synthetic steps are identical with example 1, but do not add titanium source. The structure of the synthesized Silicalite-1 molecular sieve membrane is similar to that of TS-1 molecular sieve membrane, and its XRD is shown in Figure 5 (d). Single-component He gas permeation experiment detects that its flux is less than 10 -10 mol / (m 2 ·s·Pa), indicating that the molecular sieve membrane has good compactness.

Embodiment 3

[0073] In this embodiment, the dynamic wetting method is used to coat the seed layer, and the secondary growth method is used to synthesize the TPAO-5 molecular sieve membrane.

[0074] The same part of this embodiment and embodiment 1 will not be repeated, the difference is:

[0075] In the first step, in the preparation of the seed layer by the dynamic wetting method, 0.20 g of semi-crystalline TAPO-5 molecular sieve was dispersed in 19.80 g of absolute ethanol at 75°C to obtain a 1wt.% seed crystal suspension; the remaining steps Same as Example 1. The seeds are uniformly dispersed in the surface defects of the carrier, and the seed layer XRD and SEM respectively see Figure 11 (a), Figure 12 .

[0076] The second step, the secondary growth method to prepare TAPO-5 molecular sieve membrane:

[0077] The molar composition of the growth solution is 0.05 TiO 2 : 1.00 Al 2 o 3 : 1.10 P 2 o 5 : 1.50 TEA : 105 H 2 O: 0.10H 2 o 2 . Phosphoric acid (H 3 PO 4 , 85...

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Abstract

The invention provides a preparation method of a molecular sieve membrane. The preparation method comprises the following steps: firstly, preparing a crystal seed layer by virtue of a dynamic wetting method; secondly, preparing the molecular sieve membrane by virtue of a secondary growth method; and thirdly, activating the molecular sieve membrane. Compared with the traditional secondary growth method, according to the preparation method, the crystal seed layer is coated by virtue of the dynamic wetting method instead of the traditional dip-coating method so as to improve the coating method of the crystal seed layer, and by the spreading wetting principle of a solid-liquid interface and adopting alcohol having low surface tension as a dispersion liquid, the crystal seeds are uniformly dispersed in defects on the surface of a carrier; the molecular sieve membrane is then prepared by virtue of the secondary growth method; the molecular sieve membrane is moderately activated so that the molecular sieve membrane can maintain intact denseness and has good repeatability and high success rate and is suitable for industrial amplification application.

Description

technical field [0001] The invention relates to a preparation method for preparing molecular sieve membrane materials, in particular to a method for preparing molecular sieve membranes on porous ceramic carriers by adopting a secondary growth method. Background technique [0002] Molecular sieve membrane is a new type of inorganic membrane developed in recent years. In addition to the characteristics of general inorganic membranes, molecular sieve membranes also have the characteristics of small and uniform pore size, cations in molecular sieve crystals can be exchanged by other ions, Si / Al ratio can be adjusted, and Si or Al atoms can be replaced by other heteroatoms. The important prerequisite for the application of molecular sieve membrane is that it has good compactness to ensure its excellent performance. Molecular sieve membranes with different structure types, pore sizes, and surface properties can meet different needs in the field of separation and catalysis. Theref...

Claims

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Application Information

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IPC IPC(8): C01B39/02C01B37/00
Inventor 刘旭光刘勇马欣张宝泉
Owner QINGDAO UNIV OF SCI & TECH
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