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Preparation method of ethanol-permselective POSS (polyhedral oligomeric silsesquioxanes)/silicone rubber composite membrane

A polysilsesquioxane and silicone rubber composite membrane technology, which is applied in semipermeable membrane separation, chemical instruments and methods, membrane technology, etc., can solve the problems of poor stability of separation performance, poor uniformity, repeatability, and poor compatibility, etc. question

Active Publication Date: 2014-03-26
BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are two serious defects in the preparation of zeolite particle-filled PDMS composite membranes by simple physical filling: first, in the process of composite membrane preparation, due to the significant difference in the physical and chemical properties of the organic phase and inorganic particles, the compatibility between the two is poor, and the inorganic The particles are unevenly dispersed in the PDMS phase and are easy to agglomerate, resulting in poor structural uniformity and preparation repeatability of the organic / inorganic composite film; secondly, the currently used inorganic particles are relatively large in size (0.05μm-5μm), generally The molecular size of ethanol and water (dynamic radius: 0.52nm, 0.37nm) is hundreds or even tens of thousands of times, so it is difficult to give full play to the synergistic effect of organic / inorganic composite materials, and there is only a weak van der Waals between the inorganic phase and the organic phase. Under the action of long-term swelling of small solvent molecules, the stability of the interface structure and separation performance of the filled membrane is poor, and the pervaporation performance is prone to obvious trade-off phenomenon and irreversible attenuation, which seriously restricts the organic and inorganic phases of the filled membrane. The Exertion of Synergistic Effect and Its Industrial Application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 1) Dissolve 15g PVDF in 85g triethyl phosphate (TEP) to make a solution with a concentration of 15wt%, stir evenly at 70°C, filter, defoam, scrape the film on polyester non-woven fabric, and use water as a gel bath , using the immersion precipitation phase inversion method to obtain the PVDF porous bottom membrane supported by non-woven fabrics, and after the solvent exchange is complete, let it dry naturally;

[0021] 2) The method of preparing polysilsesquioxane / silicone rubber film liquid: mix polydimethylsiloxane, octaphenyl polysilsesquioxane, tetraethyl orthosilicate, dibutyltin dilaurate and tetrahydrofuran , Stir evenly, filter and defoam; polydimethylsiloxane: octaphenyl polysilsesquioxane: ethyl orthosilicate: dibutyltin dilaurate: tetrahydrofuran The mass ratio is 100:10:5:1.2: 200;

[0022] 3) Membrane-making method of silicone rubber composite membrane, the membrane solution obtained in 2) is coated on the PVDF porous supporting base membrane obtained in 1...

Embodiment 2

[0025] 1) Dissolve 8g of PVDF in 92g of N,N-dimethylformamide to form a solution with a concentration of 12wt%, stir evenly at 70°C, filter, defoam, scrape the film on polyester non-woven fabric, and the water will become a gel Bath, using the immersion precipitation phase inversion method to obtain the PVDF porous bottom membrane supported by non-woven fabric, after the solvent exchange is complete, let it dry naturally;

[0026] 2) The method of preparing polysilsesquioxane / silicone rubber membrane liquid: polytrimethylsilacylpropyne, octamethoxypolysilsesquioxane, phenyltrimethoxysilane, monobutyltin oxide and Mix toluene, stir evenly, filter and defoam; polytrimethylsilapropyne: octavinylpolysilsesquioxane: phenyltrimethoxysilane: monobutyltin oxide: toluene mass ratio is 100:0.5:5 :1:500;

[0027] 3) Membrane-making method of silicone rubber composite membrane, the membrane solution obtained in 2) is coated on the PVDF porous support base membrane obtained in 1), and aft...

Embodiment 3

[0030] 1) Dissolve 20g of PVDF in 80g of N-methylpyrrolidone to make a solution with a concentration of 18wt%, stir evenly at 70°C, filter, defoam, scrape the film on polyester non-woven fabric, use water as a gel bath, and use immersion precipitation The PVDF porous bottom membrane supported by non-woven fabric was obtained by phase inversion method, and after the solvent exchange was complete, it was dried naturally;

[0031] 2) The method of preparing polysilsesquioxane / silicone rubber film liquid: polymethylphenylsiloxane, hydrogen polysilsesquioxane, phenyl triethoxysiloxane, dibutyl oxide Mix tin and n-heptane, stir well, filter and defoam; polymethylphenylsiloxane: hydrogen polysilsesquioxane: phenyltriethoxysiloxane: dibutyltin oxide: n-heptane The mass ratio is 100:20:15:3:300;

[0032]3) Membrane-making method of silicone rubber composite membrane, the membrane solution obtained in 2) is coated on the PVDF porous supporting base membrane obtained in 1), and after de...

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Abstract

The invention discloses a preparation method of an ethanol-permselective POSS (polyhedral oligomeric silsesquioxanes) / silicone rubber composite membrane and belongs to the technical field of pervaporation membrane separation. A membrane liquid formed by mixing of silicone rubber, POSS, a cross-linking agent, a catalyst and a solvent is prepared; a porous support PVDF (polyvinylidene fluoride) base membrane is coated with the membrane liquid; and the POSS / silicone rubber composite membrane is obtained through deep cross-linking. The obtained POSS / silicone rubber composite membrane has excellent ethanol-permselective performance for ethanol aqueous solutions with low concentration (1wt%-30wt%), and the separation factor alpha obtained is 1.70 and the permeation flux J is 0.15 kg / m2h under the optimum condition for ethanol aqueous solutions with the concentration of 10wt%.

Description

technical field [0001] The invention discloses a preparation method for a polysilsesquioxane / silicone rubber composite membrane which is preferentially permeable to alcohol, and belongs to the technical field of pervaporation membrane separation. Prepare a membrane liquid mixed with silicone rubber, polysilsesquioxane, cross-linking agent, catalyst, and solvent, and coat the membrane liquid on a polyvinylidene fluoride (PVDF) porous support base film, and obtain it through deep cross-linking Polysilsesquioxane / silicone rubber composite film. The polysilsesquioxane / silicone rubber composite membrane obtained in the present invention has excellent performance of preferentially permeating alcohol for low-concentration ethanol aqueous solution (1wt%-30wt%), and for a concentration of 10wt% ethanol aqueous solution, the separation factor α =17.0, the permeation flux is J=0.15kg / m 2 h. Background technique [0002] At present, the most researched and most promising pervaporatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/70B01D69/12B01D67/00
Inventor 展侠刘吉辉
Owner BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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