High performance molecular sieve membrane of silicon by using ceramics of silicon dioxide as carrier, and preparation method

A silicon molecular sieve and silicon dioxide technology, which is applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc., can solve the problems of reducing the hydrophobicity of siliconalite molecular sieve membrane, and achieve easy control of synthesis conditions, simple operation, and application. wide effect

Inactive Publication Date: 2006-07-05
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

A good formula is the key to the synthesis of silicalite molecular sieve membrane. For the use of alumina carrier, the influence of alkalinity cannot be ignored. Excessive alkalinity will easily cause the dissolution of the carrier, and finally reduce the hydrophobicity of silicalite molecular sieve membrane.

Method used

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  • High performance molecular sieve membrane of silicon by using ceramics of silicon dioxide as carrier, and preparation method
  • High performance molecular sieve membrane of silicon by using ceramics of silicon dioxide as carrier, and preparation method
  • High performance molecular sieve membrane of silicon by using ceramics of silicon dioxide as carrier, and preparation method

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Experimental program
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Effect test

Embodiment 1

[0037] The synthesis of embodiment 1 tubular silicalite molecular sieve membrane

[0038] The porous silica ceramic carrier used in the experiment has a ceramic tube with an outer diameter of 11 mm, an inner diameter of 7 mm, a length of 90 mm, an average pore diameter of 0.26 μm, and a porosity of about 45%. The flaky silica carrier used for XRD characterization has a diameter of 25 mm, a thickness of 2 mm, and the same average pore diameter and porosity as the tubular carrier. After the carrier is smoothed by 1000 mesh fine sandpaper, it is cleaned by ultrasonic waves in distilled water, and then treated at high temperature for later use. The dried ceramic tubes and sheet-like supports are directly used for synthesis without the need for pre-coated seeds.

[0039] The schematic diagram and schematic diagram of the preparation are as follows figure 1 and figure 2 shown.

[0040] Weigh a certain amount of NaOH and dissolve it in distilled water, stir to dissolve, add tetr...

Embodiment 2

[0043] The synthesis of embodiment 2 tubular silicalite molecular sieve membranes

[0044] The same operation as in Example 1 was carried out, except that the aging temperature used was different, and the aging condition before hydrothermal synthesis was aging at 75° C. for 12 hours. From the scanning electron microscope photo, it can be seen that a uniform and dense molecular sieve film is formed on the surface of the carrier, and the molecular sieve crystal is a typical MFI crystal shape (such as Figure 6 , 7 shown). See S-3 and S4 in Table 2 for the results of molecular sieve membrane pervaporation experiments on the two tubular supports.

[0045] membrane tube

Embodiment 3

[0046] The synthesis of embodiment 3 tubular silicalite molecular sieve membranes

[0047] Weigh a certain amount of NaOH and dissolve it in distilled water, stir to dissolve, add tetrapropylammonium bromide (TPABr), stir and dissolve for a period of time, add a certain amount of silica sol to the above mixed solution, and stir thoroughly. The composition (molar ratio) of each component in the final solution is: 1TPABr: 0.25Na 2 O: 10SiO 2 : 600H 2 o

[0048] Seal one end of the unseeded porous silica ceramic tube with a polytetrafluoroethylene bracket, fill it with a mixed solution of glycerin and water, seal the other end with a polytetrafluoroethylene bracket, and place it vertically on the Pour the reaction solution into a reaction kettle lined with a polytetrafluoroethylene liner, age it in an oven at 75°C for 8 hours before synthesis, then in-situ hydrothermally synthesize it at 180°C for 24 hours, cool it down to room temperature naturally, and wash it with distilled...

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Abstract

The invention relates to a high-performance silicon molecular sieve membrane. It uses porous silicon dioxide ceramics as carrier, and its surface has MFI crystal structure. The average pore diameter of said silicon dioxide ceramics carrier is 0.1-2 microns, and its average porosity is 10-60%. Its preparation method uses porous silicon dioxide ceramics as carrier, uses TPABr as template agent and adopts in-situ hydration process to synthesize the invented silicon molecular sieve membrane.

Description

Technical field: [0001] The invention relates to a new synthesis method and application of an all-silicon molecular sieve membrane, and in particular provides a method for synthesizing a high-performance molecular sieve membrane on a silica ceramic tube carrier. Background technique: [0002] Molecular sieves have the following advantages as inorganic membrane materials: 1) Molecular sieves have regular pores and a single pore size distribution, and the pore size of some molecular sieves is similar to the molecular size of many important industrial raw materials. Molecular sieve membranes, separated by molecular sieving or type-selective diffusion. 2) Molecular sieve membrane has good thermal stability, chemical stability, mechanical stability and biological stability. Compared with organic membranes, it has higher permeation flux and selectivity, and has a longer service life. 3) Different molecular sieves have different hydrophilicity and hydrophobicity, and the appropri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/02
Inventor 杨维慎陈红亮刘杰李砚硕
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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