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Preparation method of all-silicon MFI type molecular sieve membrane with high stability

A high-stability, zeolite molecular sieve membrane technology, applied in chemical instruments and methods, pervaporation, membrane technology, etc., can solve problems such as poor membrane stability, and achieve good stability and good industrial application prospects.

Active Publication Date: 2014-07-23
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention aims at the problem that the all-silicon MFI type molecular sieve membrane is prone to poor membrane stability in the prior art by using a strong alkaline synthetic solution, and proposes a preparation of an all-silicon MFI type zeolite molecular sieve membrane with high stability under neutral conditions method

Method used

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  • Preparation method of all-silicon MFI type molecular sieve membrane with high stability
  • Preparation method of all-silicon MFI type molecular sieve membrane with high stability
  • Preparation method of all-silicon MFI type molecular sieve membrane with high stability

Examples

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Effect test

Embodiment 1

[0028] Example 1: Preparation of all-silicon MFI type zeolite molecular sieve membrane under neutral conditions

[0029] Mix 0.47g of tetrapropylammonium bromide, 1.64g of ammonium fluoride and 40.03g of water evenly, and slowly add 1.33g of fumed silica at 80°C, shake vigorously to form a stable transparent sol (nSiO 2 :nTPABr:nNH 4 F: nH 2 O=1:0.08:2:100), pour it into a polytetrafluoroethylene-lined stainless steel reactor, and then put the reactor into an oven at 180°C for crystallization for 10 hours. After the synthesis is completed, the reaction product is centrifuged, washed, and dried to obtain an all-silicon MFI zeolite molecular sieve. Using YSZ hollow fiber as a support, it was ultrasonically cleaned in deionized water for 20 min, and then dried for later use. Put the molecular sieve particles into a ball mill tank, use water as the dispersant, and ball mill for 8 hours at a speed of 200r / min. The mass ratio of water to molecular sieve is 30:1. After the ball mi...

Embodiment 2

[0031] Example 2: Preparation of all-silicon MFI type zeolite molecular sieve membrane under neutral conditions

[0032] Mix 2.36g of tetrapropylammonium bromide, 2.05g of ammonium fluoride and 40.03g of water evenly, heat in a water bath at 90°C until completely dissolved, then add 3.33g of fumed silica, and shake vigorously until a transparent sol (nSiO2:nTPABr : nNH 4 F: nH 2 O=1:0.16:1.0:40). The synthesis temperature is 160°C and the synthesis time is 24h. The obtained molecular sieve particles were put into a ball mill tank with water as a dispersant, and ball milled for 2 hours at a rotational speed of 600 r / min. The mass ratio of water to molecular sieve was 50:1. Chip α-Al 2 o 3as a support material. Preparation of molecular sieve membrane synthesis mother liquor: mix 1.18g tetrapropylammonium bromide, 0.33g ammonium fluoride and 40.03g water and heat to 90°C, add 3.33g fumed silica (nSiO 2 :nTPABr:nNH 4 F: nH 2 O=1:0.1:0.2:50), and hydrothermally synthesized...

Embodiment 3

[0033] Example 3: Preparation of all-silicon MFI type zeolite molecular sieve membrane under neutral conditions

[0034] The synthetic liquid composition of molecular sieve seed crystal is 6.67g fumed silica, 7.09g tetrapropyl ammonium bromide, 1.64g ammonium fluoride and 40.03g water (nSiO 2 :nTPABr:nNH 4 F: nH 2 O=1:0.24:0.4:20). Put the obtained molecular sieve particles into a ball mill tank, use water as a dispersant, and ball mill for 4 hours at a speed of 400 r / min. The mass ratio of water to molecular sieve is 20:1. All the other conditions and steps are the same as in Example 1.

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Abstract

The invention relates to a preparation method of an all-silicon MFI type molecular sieve membrane with high stability. The preparation method comprises the following steps: in a neutral synthetic liquid, preparing an MFI molecular sieve seed crystal and an MFI molecular sieve membrane by using villiaumite as a mineralizer and tetrapropylammonium bromide as a template agent under a neutral synthesis condition; crushing the MFI molecular sieve seed crystal by high-energy ball milling and then applying the crushed seed crystal to the surface of a porous support body; and preparing an MFI zeolite molecular sieve membrane by secondary growth. Compared with the MFI type molecular sieve membrane synthesized from an alkali system, the fluorine-containing MFI type molecular sieve membrane prepared by the method shows good stability in the process of removing ethanol from an ethanol / water mixture by pervaporation and has an excellent industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of pervaporation membranes, and in particular relates to a preparation method of a highly stable all-silicon MFI type molecular sieve membrane material under neutral conditions. Background technique [0002] Fuel ethanol, as a clean and efficient renewable energy, has attracted widespread attention from all over the world in recent years. The traditional fermentation method is used to prepare fuel ethanol, and the rectification method is generally used to separate the ethanol in the fermentation broth, and the whole process consumes a lot of energy. Pervaporation membrane separation technology is a new type of separation technology applied to organic solvents and water systems. It has the characteristics of high efficiency, low energy consumption, no pollution and simple operation. In recent years, many researchers have devoted themselves to applying this technology to the production process of fuel ethanol...

Claims

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Application Information

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IPC IPC(8): B01D71/02B01D69/12B01D67/00B01D61/36C07C31/08C07C29/76
Inventor 顾学红孔晴晴张春王学瑞
Owner NANJING UNIV OF TECH
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