Method of preparing high-oriented MFI type zeolite membrane by virtue of secondary growth under neutral condition

A secondary growth and orientation technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve problems such as danger, and achieve the effects of small destructiveness, continuous film layer, and low preparation cost

Inactive Publication Date: 2015-04-29
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can be seen that the synthetic fluid used uses highly corrosive hydrofluoric acid, which is very dangerous for both laboratory operations and industrial applications

Method used

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  • Method of preparing high-oriented MFI type zeolite membrane by virtue of secondary growth under neutral condition
  • Method of preparing high-oriented MFI type zeolite membrane by virtue of secondary growth under neutral condition
  • Method of preparing high-oriented MFI type zeolite membrane by virtue of secondary growth under neutral condition

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Wipe the micron-sized MFI type molecular sieve seed crystal powder on the surface of the glass sheet to get the b The glass sheet of the axis-oriented seed layer, the scanning electron microscope picture of the seed layer is as follows figure 1 As shown, the X-ray diffraction pattern is as figure 2 shown. The molar ratio is fumed silicon dioxide: tetrapropylammonium bromide: water = 1:0.1:165 synthetic solution was stirred at room temperature for 10 minutes, and then the synthetic solution and the glass sheet with the seed layer were put into In the synthesis kettle with polytetrafluoroethylene lining, the synthesis solution is immersed in the glass plate support, sealed and placed in a blast oven at 175°C for crystallization for 48 hours. After the reaction, the glass plate is taken out and washed with deionized water. After drying, get a high b The axis-oriented MFI molecular sieve membrane, the scanning electron microscope picture of the membrane layer is as foll...

Embodiment 2

[0026] The preparation method of the seed layer is the same as in Example 1, and the support body is a stainless steel sheet. The molar ratio is silica sol: tetrapropyl ammonium bromide: water = 1:5:2000 synthetic solution was stirred at room temperature for 10 minutes, then this synthetic solution was put into a In the polytetrafluoroethylene-lined synthesis kettle, the synthesis liquid is immersed in the stainless steel sheet support, sealed and placed in a blast oven at 200°C for crystallization for 72 hours. After the reaction, the stainless steel sheet is taken out, washed with deionized water, and then baked. dry, get high b Axially oriented MFI type molecular sieve membrane.

Embodiment 3

[0028] The preparation method of the seed layer is the same as in Example 1, and the support body is a glass sheet and a stainless steel sheet. The molar ratio is fumed silicon dioxide: tetrapropylammonium bromide: water=1:1:1650 synthetic solution was stirred at room temperature for 60 minutes, then this synthetic solution was mixed with stainless steel sheet and glass sheet with seed crystal layer Put them together into a synthetic kettle with a polytetrafluoroethylene liner, immerse the stainless steel sheet and glass sheet support in the synthetic solution, seal it and put it in a blast oven at 175°C for 24 hours of crystallization, and take out the glass sheet and glass sheet after the reaction is over. The stainless steel sheet was washed with deionized water and then dried to obtain a high b Axis-oriented MFI molecular sieve membrane, scanning electron microscope pictures of the membrane layer on the stainless steel sheet are as follows Figure 5 shown.

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Abstract

The invention discloses a method of preparing a high-oriented MFI type zeolite membrane by virtue of secondary growth under the neutral condition. The method comprises the following steps: 1) preparing a neutral synthetic fluid, wherein the synthetic fluid is prepared from the following components including a silica source, tetrapropylammonium bromide and water, and the molar ratio of the silica source to tetrapropylammonium bromide to water is 1 to (0.1-5) to (10-2000); and 2) stirring the synthetic fluid for 10-60 minutes at room temperature, charging into a reaction kettle, putting a supporting body coated with a b axis oriented crystal seed layer into the reaction kettle, immersing the supporting body with the synthetic fluid, sealing the reaction kettle, carrying out heating synthesis, washing, and drying to obtain the oriented MFI type zeolite membrane on the supporting body, wherein the synthesis temperature is 120-200 DEG C, and the synthesis time is 12-72h. According to the method disclosed by the invention, the synthesized MFI type zeolite membrane has high b axis orientation, the used synthetic fluid is neutral and is small in damage on the surface of the supporting body and low in raw material cost, and the cost is easily lowered.

Description

technical field [0001] The invention relates to the synthesis of MFI molecular sieve membranes, and in particular provides a method for preparing highly oriented MFI molecular sieve membranes under neutral synthesis conditions. Background technique [0002] Molecular sieve membranes have regular and ordered pore structures, excellent thermal and chemical stability, and good mechanical and electronic properties, so they are widely used in separation processes, membrane reactors, anti-corrosion coatings, chemical sensors and low-dielectric Electrical constant materials and many other fields. At present, the molecular sieve membranes reported in the literature mainly include MFI type, LTA type, T type, CHA type, FAU type and so on. Due to the pore size of the MFI molecular sieve ( b A straight channel with an axial orientation of 0.53×0.56 nm, a Sinusoidal channels with axial orientation of 0.51×0.55 nm) are comparable to the molecular size of many important industrial chemi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
CPCC01B39/04C01P2002/72C01P2004/03
Inventor 王正宝彭勇
Owner ZHEJIANG UNIV
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