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Preparation of osmotic vaporizing alcohol permselective zeolite filling silicon rubber compound film

A silicone rubber composite membrane, preferential alcohol permeation technology, applied in chemical instruments and methods, semi-permeable membrane separation, membrane technology and other directions, can solve the problems of low separation membrane strength, high production cost, restricting large-scale industrial applications, etc. The production process is simple, the production cost is low, and the effect of good pervaporation and alcohol permeability

Active Publication Date: 2008-09-17
北京清源洁华膜技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] "Method for Separating Ethanol Aqueous Solution Using Polyvinylidene Fluoride Pervaporation Membrane" (CN1239012A) discloses a method of using vinylidene fluoride to prepare a preferential alcohol permeation membrane, but the separation membrane has low strength, poor pressure resistance, and separation The concentration of ethanol in membrane separation is limited between 0.1wt% and 20wt%, which limits its industrial application
"A Preparation Method for Preferential Alcohol Permeation Separation Membrane" (CN1640534A) discloses a method for preparing cyclosiloxane preferential alcohol permeation separation membrane by means of concentrated emulsion polymerization, but the polymer preparation process is relatively complicated, and its separation system Limited to 25vol% ethanol aqueous solution, its permeation flux is only 36.2-100.3g / m 2 h, which greatly limits its application in industry
"A Pervaporation Separation Membrane for Separating Liquid Mixtures" (US5254251) discloses a preparation method of a double-layer composite membrane. The selection layer is a polyether-polyamide block copolymer, and the reinforcement matrix layer is a silk screen. The matrix strength Higher, selectivity and permeation flux are also greatly improved, but the production cost of polyether-polyamide copolymer is relatively high, which limits its large-scale industrial application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 1) Dissolve 6g of PVDF in 34g of N,N-dimethylformamide to make a solution with a concentration of 15wt%, stir evenly at 70°C, filter, defoam, and directly scrape the film on one side of the polyester non-woven fabric, Water is used as a gel bath, and the PVDF porous bottom membrane supported by non-woven fabric is obtained by immersion precipitation phase inversion method. After the solvent exchange is complete, it is naturally dried.

[0021] 2) Disperse the MFI type zeolite with a silicon-aluminum ratio of 25 in acetone, add hydrofluoric acid (HF) aqueous solution, and prepare a hydrofluoric acid solution with a concentration of 20 g / ml, magnetically stir for 5 minutes, wash with acetone after filtering, Baking at 550°C for 12 hours.

[0022] 3) Dissolve 0.9g of acid-treated zeolite, 9g of PDMS with a viscosity of 5000Pa·s, 1.2g of phenyltriethoxysilane crosslinking agent, and 0.5g of catalyst dibutyltin dilaurate in 30g of toluene to prepare solution, stirred evenly...

Embodiment 2

[0029] 1) Dissolve 6g of PVDF in 34g of N,N-dimethylacetamide to make a solution with a concentration of 15wt%, stir evenly at 70°C, filter, defoam, and directly scrape the film on one side of the polyester non-woven fabric, Water is used as a gel bath, and the PVDF porous bottom membrane supported by non-woven fabric is obtained by immersion precipitation phase inversion method. After the solvent exchange is complete, it is naturally dried.

[0030] 2) Disperse the MFI type zeolite with a silicon-aluminum ratio of 50 in acetone, add hydrofluoric acid (HF) aqueous solution, and prepare a hydrofluoric acid solution with a concentration of 15 g / ml, magnetically stir for 5 minutes, wash with acetone after filtering, Baking at 450°C for 8 hours.

[0031] 3) Dissolve 1.8g of acid-treated zeolite, 9g of PDMS with a viscosity of 10000Pa·s, 1.2g of ethyl orthosilicate crosslinking agent, and 0.5g of catalyst dibutyltin dilaurate in 30g of tetrahydrofuran to prepare a solution, Stir e...

Embodiment 3

[0039] 1) Dissolve 6g of PVDF in 34g of triethyl phosphate to make a solution with a concentration of 15wt%, stir evenly at 70°C, filter, defoam, scrape the film directly on one side of the polyester non-woven fabric, and use water as a gel bath , the PVDF porous bottom membrane supported by non-woven fabric was obtained by immersion precipitation phase inversion method, and after the solvent exchange was complete, it was dried naturally.

[0040] 2) Disperse the MFI type zeolite with a silicon-aluminum ratio of 300 in acetone, add hydrofluoric acid (HF) aqueous solution, and prepare a hydrofluoric acid solution with a concentration of 6 g / ml, magnetically stir for 5 minutes, wash with acetone after filtering, Baking at 350° C. for 5 hours.

[0041] 3) Dissolve 2.7g of acid-treated zeolite, 9g of PDMS with a viscosity of 50000Pa·s, 1.2g of phenyltrimethoxysilane crosslinking agent, and 0.5g of catalyst dibutyltin dilaurate in 30g of n-heptane to prepare into a solution, stirr...

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Abstract

The invention relates to a pervaporation alcohol permselective zeolite filled silicone rubber composite membrane, belonging to pervaporation membrane separation technological field, which is characterized in that a polyester non-woven fabric support layer is film-wiped by polyvinylidene fluoride (PVDF) solution; a PVDF porous basement membrane is obtained by using an immerse precipitation transformation method; after the MFI type zeolite is processed by hydrofluoric acid, a membrane solution containing the MFI type zeolite, dimethyl silicone polymer(PDMS), a cross-linking agent and a catalyst is prepared; the PVDF porous basement membrane is film-wiped and air-dried in ambient temperature to cross-link completely. The separation performance of prior non-zeolite filled PDMS membrane to ethanol water solution is bad, and the separation factor and permeation flux are low. The pervaporation alcohol permselective zeolite filled silicone rubber composite membrane processed in acid has the advantages of good performance; the ethanol water solution concentration is 5 wt%, the separation factor Alpha in 50 DEG C is 16.3, and the permeation flux is J=132.7g / m2h.

Description

technical field [0001] The invention relates to a preparation method of a zeolite-filled silicon rubber composite membrane which can be used for pervaporation with alcohol-preferential permeation, and belongs to the field of pervaporation membrane separation. Background technique [0002] The energy crisis in the 1970s prompted people to explore the renewable energy-fermentation method to prepare ethanol and energy-saving separation technology. And in the process of producing ethanol by biological fermentation, when the ethanol content in the fermented liquid reaches a certain concentration (5wt%~8wt%), it will seriously inhibit the carrying out of the fermentation process, so ethanol must be continuously separated from the fermented liquid , in order to ensure that the production process has been maintained in an efficient state. [0003] As an emerging membrane separation technology, pervaporation technology is especially suitable for the separation of mixture systems wit...

Claims

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Application Information

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IPC IPC(8): B01D71/34B01D71/70B01D69/12
Inventor 李继定展侠黄军其
Owner 北京清源洁华膜技术有限公司
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