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Preparation method of bifunctional hollow fibrous membrane with strong acidic catalysis and pervaporation

A pervaporation, inorganic hollow fiber technology, applied in the preparation of organic compounds, catalyst activation/preparation, preparation of carboxylate, etc., can solve rare problems, reduce separation steps, improve conversion rate, save equipment and operating costs Effect

Active Publication Date: 2012-01-25
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are relatively few patents related to the use of PFSA resin as a solid acid catalyst to prepare catalytic membranes.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Polyacrylonitrile (PAN), polyvinylpyrrolidone (PVP, K30) and N,N dimethylacetamide (DMAc) were dissolved in a mass ratio of 15:5:80 at 60°C for 24h, stirred and left to stand to obtain a cast film liquid. The hollow fiber membrane spinning device was self-made in the laboratory, and the spinneret used had an outer diameter of 1.5 mm and an inner diameter of 1.0 mm. Pour the casting liquid into the raw material tank and let it stand for 24 hours for defoaming. The casting liquid is filtered through a stainless steel filter before entering the spinneret to remove the tiny particles that may exist in the casting liquid. Under the action of nitrogen pressure, the casting liquid enters the spinneret, the core liquid (internal gel bath) is pumped into the spinneret by a non-pulsating precision metering pump (China, Xingda), and the casting liquid comes out of the spinneret. The material transfer of solvent and non-solvent occurs with the inner and outer gel bath, and the ho...

Embodiment 2

[0031] Dissolve PFSA in an aqueous solution of isopropanol with a mass ratio of 1:1, add nano-SiO 2 and PVA solution, PFSA, nano-SiO 2 The mass ratio to PVA is 8:2:3. Dip-coated on SHFCM-4 pervaporation hollow fiber separation membrane, dried at room temperature, treated with 5wt% hydrochloric acid, and dried at room temperature to obtain a hollow fiber membrane with dual functions of strong acid catalysis and pervaporation. The pervaporation separation column top crude ester (water: 8.91wt%, ethanol: 3.73wt%, ethyl acetate: 87.36wt%) was used to test the separation of the membrane, and the catalytic acetic acid-ethanol esterification reaction was used to test the catalytic activity of the membrane. The PFSA resin loaded on the hollow fiber membrane with the dual functions of strong acid catalysis and pervaporation is 4.0wt%, and the total permeation flux is 136g / m 2 h, the separation factor of water to ethanol is 404, without ethyl acetate permeation, the equilibrium conver...

Embodiment 3

[0033] Dissolve PFSA in an aqueous solution of isopropanol with a mass ratio of 1:1, add nano-SiO 2 and PVA solution, PFSA, nano-SiO 2 The mass ratio with PVA is 10:0:3. Dip-coated on SHFCM-4 pervaporation hollow fiber separation membrane, dried at room temperature, treated with 5wt% hydrochloric acid, and dried at room temperature to obtain a hollow fiber membrane with dual functions of strong acid catalysis and pervaporation. The pervaporation separation column top crude ester (water: 8.91wt%, ethanol: 3.73wt%, ethyl acetate: 87.36wt%) was used to test the separation of the membrane, and the catalytic acetic acid-ethanol esterification reaction was used to test the catalytic activity of the membrane. The PFSA resin loaded on the hollow fiber membrane with strong acid catalysis and pervaporation dual functions is 4.5wt%, and the total permeation flux is 117g / m 2 h, without the permeation of ethanol and ethyl acetate, the equilibrium conversion rate of ethanol in the esterif...

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Abstract

The invention relates to a preparation method of a bifunctional hollow fibrous membrane with strong acidic catalysis and pervaporation. The preparation method comprises the following steps: 1, preparing hollow fibrous basilemmas of a high molecular material and an inorganic material; 2, preparing an aqueous solution of polyvinyl alcohol (PVA); 3, dip-coating the aqueous solution of the PVA and anaqueous solution of PVA-GA (polyvinyl alcohol-glutaraldehyde) on the hollow fibrous basilemmas, carrying out surface crosslinking, and drying at room temperature to prepare a hollow fibrous pervaporation membrane; 4, placing a perfluorinated sulfonic acid (PFSA) resin in an aqueous solution of a lower boiling alcohol solvent, and heating for dissolving; 5, adding the PVA and an inorganic nanomaterial to the aqueous solution of the alcohol solvent containing the PFSA, or adding the PVA, the inorganic nanomaterial, GA and an acid catalyst to prepare a catalyst coating liquid; and 6, dip-coatingthe catalyst coating liquid on the hollow fibrous prevaporization membrane, and drying at room temperature to prepare the hollow fibrous membrane with the dual functions. The preparation method of the present invention has the advantages of simple preparation technology, no complex equipment requirement, and convenient and fast operation.

Description

【Technical field】 [0001] The invention relates to a preparation method of a dual-function membrane with strong acid catalysis and pervaporation, in particular to a preparation method of a perfluorosulfonic acid resin (PFSA) catalysis and pervaporation dual-function hollow fiber membrane. 【Background technique】 [0002] At present, catalytic membranes have been widely used in reforming reactions, selective oxidation reactions, dehydrogenation reactions, hydrogenation reactions, esterification reactions, and the like. But the vast majority of these membranes have only one skin layer, which provides both catalytic and separation properties. Such membranes tend to have either good catalytic activity or good separation. There are few membranes that have both high catalytic activity and high separation. Therefore, it is very important to prepare and optimize the bifunctional hollow fiber membrane with strong acid catalysis and pervaporation with two skin layers. The catalytic l...

Claims

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Application Information

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IPC IPC(8): B01D69/08B01J31/10B01J37/02C07C69/14C07C67/08C07C67/48
Inventor 许振良马晓华魏永明程亮
Owner EAST CHINA UNIV OF SCI & TECH
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