All-silicon/high-silicon molecular sieve membrane and quick preparation method thereof

A molecular sieve and high silicon technology, which is applied in the field of full silicon/high silicon molecular sieve membrane and its rapid preparation, can solve the problems of low permeability, large mass transfer resistance, and unfavorable commercial application of molecular sieve membrane.

Active Publication Date: 2021-05-04
SHANGHAI UNIV OF ENG SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional hydrothermal synthesis method to prepare molecular sieve membranes has the advantages of simple methods, but the thickness of the prepared membranes is usually 2-10 microns, resulting in large mass transfer resistance and low permeability, which is not conducive to the commercial application of molecular sieve membranes

Method used

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  • All-silicon/high-silicon molecular sieve membrane and quick preparation method thereof
  • All-silicon/high-silicon molecular sieve membrane and quick preparation method thereof
  • All-silicon/high-silicon molecular sieve membrane and quick preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] In this example, an all-silicon MFI molecular sieve membrane was synthesized under mild conditions (synthesized at 100°C for 2 hours). The specific steps are as follows:

[0064] Step 1: Tetrapropylammonium hydroxide was mixed with deionized water, then added tetraethyl orthosilicate (TEOS), stirred for 4 hours to obtain a synthetic liquid for seed crystals, and the molar ratio of the reaction liquid was: 25SiO 2 : 9TPAOH (tetrapropyl ammonium hydroxide): 360H 2 O: 100EtOH, hydrothermal crystallization at 120°C for 24 hours to obtain all-silicon MFI molecular sieve seed crystals (all-silicon MFI molecular sieves can also be called Silicalite-1 molecular sieves), and obtain nano-scale all-silicon MFI molecular sieve molecular sieve crystal seeds after ball milling;

[0065] Step 2: Select a porous ceramic tube with a pore size of 100nm as the carrier, seal the two ends of the carrier with glaze, wash and dry, seal the outer surface with PTFE tape, and brush the nano-scal...

Embodiment 2

[0075] In this example, an all-silicon MFI molecular sieve membrane was synthesized under mild conditions, and the only difference from Example 1 was that the synthesis time was 4 hours (100 degrees Celsius).

[0076] The surface and profile of gained all-silicon MFI molecular sieve membrane are as follows figure 2 As shown, it can be seen from the figure that the surface of the carrier is completely covered by MFI crystals (typical coffin-shaped crystals), and the cross-linking between crystals is perfect (see figure a); as the synthesis time increases, the thickness of the film increases to 0.65 microns ( See Figure b). It is extremely difficult to prepare an all-silicon MFI molecular sieve membrane with a thickness of less than 1 micron by a simple hydrothermal synthesis method.

[0077] The CO of the membrane tube containing the obtained all-silicon MFI molecular sieve membrane 2 / CH 4 Gas separation test results, at 0.14 MPa, its CO 2 The average permeability of CO...

Embodiment 3

[0079] In this example, an all-silicon MFI molecular sieve membrane is synthesized under mild conditions, the only difference from Example 1 is that the synthesis time is 6 hours (100 degrees Celsius).

[0080] The surface and profile of gained all-silicon MFI molecular sieve membrane are as follows image 3 As shown, it can be seen from the figure that the surface of the carrier is completely covered by MFI crystals (typical coffin-shaped crystals), and the cross-linking between crystals is perfect (see figure a); the thickness of the film is relatively uniform, about 1.03 microns (see figure b) . It is extremely difficult to prepare an all-silicon MFI molecular sieve membrane with a thickness of less than 1 micron by a simple hydrothermal synthesis method.

[0081] The CO of the membrane tube containing the obtained all-silicon MFI molecular sieve membrane 2 / CH 4 Gas separation test results, at 0.14 MPa, its CO2 The average permeability of CO 2 / CH 4 The average sepa...

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Abstract

The invention relates to an all-silicon / high-silicon molecular sieve membrane and a preparation method thereof. The method comprises the following steps: (1) preparing a nanoscale molecular sieve seed crystal; (2) coating a porous carrier tube with the nanoscale molecular sieve seed crystal; (3) preparing molecular sieve membrane synthesis mother liquor; (4) crystallizing the porous carrier tube obtained in the step (2) and the mother liquor obtained in the step (3); (5) after the crystallization is finished, washing and drying the obtained membrane tube; and (6) roasting to remove the template agent, and cooling to obtain the activated all-silicon / high-silicon molecular sieve membrane. Compared with the prior art, the sieve membrane has the advantages of mild conditions, high speed, reduced equipment investment, suitability for various molecular sieve structures and the like.

Description

technical field [0001] The invention relates to the field of synthesis of molecular sieve membranes, in particular to an all-silicon / high-silicon molecular sieve membrane and a rapid preparation method thereof. Background technique [0002] Inorganic molecular sieve membrane is obtained by preparing a layer of continuous, dense and uniform molecular sieve on a porous carrier. Due to the advantages of uniform pore size, high temperature resistance, chemical solvent resistance and ion exchange, inorganic molecular sieve membranes have great application potential in the fields of membrane catalytic reaction, gas separation, liquid pervaporation separation and environmental protection. For example, ZSM-5 and Silicalite-1 molecular sieve membranes with MFI structure have a pore diameter of about 0.55 nanometers, which are suitable for the separation of n-paraffin-isoparaffin, alcohol-water separation, and xylene isomer separation. [0003] At present, the methods for preparing i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/02B01D67/00B01D71/02
CPCC01B37/02B01D71/028B01D67/0039
Inventor 张延风邱恒娥徐宁张野
Owner SHANGHAI UNIV OF ENG SCI
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