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A kind of pure silicalite membrane and its preparation method and application

A zeolite membrane and pure silicon technology, applied in the field of pure silica zeolite membrane and its preparation, can solve the problems of waste of raw materials and many defects of zeolite membrane, and achieve the effect of promoting full growth, excellent performance and good separation performance

Inactive Publication Date: 2021-12-14
刘金梅
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention is to provide a kind of pure silicalite membrane, has good separation performance in ethanol / water separation; Another object of the application is to provide a kind of preparation method of pure silicalite membrane, has overcome traditional hydrothermal crystallization There are many defects in the preparation of zeolite membranes, waste of raw materials and other problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A method for preparing a pure silicalite membrane, specifically comprising the steps of:

[0032] (1) Pretreatment of porous carrier: select a tubular porous aluminum oxide with an average pore diameter of 0.5 μm, an inner diameter of 10 mm, and an outer diameter of 12 mm as the carrier, and wash the carrier with 10% dilute hydrochloric acid for 20 minutes under the assistance of ultrasonic waves , then treated in acetone for 15 minutes, and then washed the carrier with deionized water for 20 minutes to remove impurities on the surface of the carrier; finally, the carrier tube was dried at 120°C and set aside;

[0033] (2) Coating the zeolite seed layer: disperse pure silicalite with a particle size of about 300nm in deionized water to form a seed crystal suspension with a concentration of 2%, seal the two ends of the above-mentioned impurity-removed carrier tube, and immerse the crystal Seed solution, kept for 30s, then taken out, and further heat treated at 220°C for ...

Embodiment 2

[0039] A method for preparing a pure silicalite membrane, specifically comprising the steps of:

[0040] (1) Pretreatment of the porous carrier: choose a tubular porous zirconia with an average pore diameter of 2 μm, an inner diameter of 10 mm, and an outer diameter of 14 mm as the carrier. Under the assistance of ultrasonic waves, the carrier is cleaned with 5% dilute hydrochloric acid for 30 minutes, and then Treat in acetone for 10 minutes, then wash the carrier with deionized water for 30 minutes to remove impurities on the surface of the carrier, and finally dry the carrier tube at 150°C for later use;

[0041](2) Coating the zeolite seed crystal layer: disperse pure silica zeolite with a particle size of about 1000nm in deionized water to form a seed crystal suspension with a concentration of 1%, seal the two ends of the above-mentioned impurity-removed carrier tube, and immerse the crystal seed crystal Seed solution, kept for 30s, then taken out, and further heat treate...

Embodiment 3

[0047] A method for preparing a pure silicalite membrane, specifically comprising the steps of:

[0048] (1) Pretreatment of porous carrier: choose tubular porous titanium oxide with an average pore diameter of 0.2 μm, an inner diameter of 10 mm, and an outer diameter of 11 mm as the carrier, and under the assistance of ultrasonic waves, use dilute hydrochloric acid with a concentration of 10% to clean the carrier for 10 minutes, and then Treat in acetone for 5 minutes, then wash the carrier with deionized water for 20 minutes to remove impurities on the surface of the carrier, and finally dry the carrier tube at 100°C for later use;

[0049] (2) Coating the zeolite seed crystal layer: disperse pure silicalite with a particle size of about 50nm in deionized water to form a seed crystal suspension with a concentration of 3.5%, seal the two ends of the above-mentioned impurity-removed carrier tube, and immerse the crystal Seed solution, kept for 60s, then taken out, and further ...

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PUM

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Abstract

The invention discloses a pure silica zeolite membrane and its preparation method and application. The preparation method firstly modifies a porous carrier with zeolite grains of appropriate size, and then coats silica sol on the surface of the modified grain carrier. Under the condition of hydrothermal crystallization liquid, the silicon source and template agent in the traditional crystallization liquid are supplied separately, and the vapor pressure of the template agent and the pressure of deionized water are precisely regulated to directly prepare pure silicalite membrane, which improves the material utilization rate. Optimizing the structure of pure silicalite membranes overcomes the problems of many defects and waste of raw materials in the preparation of zeolite membranes by traditional hydrothermal crystallization, and the microstructure of pure silicalite membranes can be controlled only by precisely controlling the template agent and deionized water pressure. The pure silicalite membrane prepared by the method of the invention has few defects and high yield, and exhibits excellent performance in the separation of water-alcohol mixture.

Description

technical field [0001] The invention belongs to the technical field of chemical separation, and in particular relates to a pure silicalite membrane and its preparation method and application. Background technique [0002] Zeolite molecular sieve membrane material is a kind of aluminosilicate crystal with regular microporous structure. It has the advantages of excellent thermal stability, mechanical stability, microbial erosion resistance and oxidation resistance inherent in inorganic membrane materials, and is more unique. Its uniform and regular crystalline channel system and its adjustable surface properties endow the zeolite molecular sieve membrane with incomparable uniqueness of organic membranes, such as high selectivity, high flux, solvent resistance, High temperature resistance, etc., making it one of the most potential and promising membranes. [0003] Pure silicalite membranes have three-dimensional intercommunicating channels, which include elliptical pores conne...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04C01B37/02
CPCC01B39/04C01B37/02
Inventor 刘金梅吴苏州陈俊孚任嵬
Owner 刘金梅
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