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Preparation for silicone hydride modified zeolite filled silicon rubber compound film

A silicon rubber composite membrane and zeolite technology, applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc., can solve the problems of separation performance degradation, filled membrane defects and increased pores, and achieve low production cost and excellent production process simple effect

Inactive Publication Date: 2012-07-25
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Increasing the filling amount of zeolite will easily cause the increase of defects and pores in the filled membrane, thus reducing the separation performance

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-methylpyrrolidone to make a solution with a concentration of 15wt%, stir evenly at 70°C, filter, defoam, and scrape the film directly on one side of the 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.

[0021] 2) Disperse 5g of all-silicon MFI zeolite in 25g of cyclohexane, add 0.75g of dodecyltrichlorosilane, stir magnetically at 25°C for 6h, filter, wash with cyclohexane, and dry at 120°C .

[0022] 3) Dissolve 5.4g of silane-modified zeolite, 9g of PDMS with a viscosity of 50000Pa·s, 1.2g of tetraethyl orthosilicate crosslinking agent, and 0.5g of catalyst dibutyltin dilaurate in 30g of n-hexane to prepare a solution , stir evenly, scrape the film on the PVDF porous bottom film, and dry it at room temperature to complete the ...

Embodiment 2

[0025] 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.

[0026] 2) Disperse 5 g of MFI zeolite with a silicon-aluminum ratio of 100 in 40 g of toluene, add 0.75 g of octyltrimethoxysilane, stir magnetically at 40°C for 24 hours, filter, wash with toluene, and dry at 200°C.

[0027] 3) Dissolve 1.8g of silane-modified zeolite, 9g of PDMS with a viscosity of 10000Pa·s, 1.2g of tetraethyl orthosilicate crosslinking agent, and 0.5g of catalyst dibutyltin dilaurate in 30g of tetrahydrofuran to prepare a solution. Stir evenly, scrape the film on the PVDF porous bottom film, and dry it at room temper...

Embodiment 3

[0030] 1) Dissolve 6g of PVDF in 27.3g of triethyl phosphate to make a solution with a concentration of 18wt%, stir evenly at 70°C, filter, defoam, and scrape the film directly on one side of the 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.

[0031] 2) Disperse 5 g of MFI zeolite with a silicon-aluminum ratio of 200 in 50 g of n-heptane, add 1.25 g of ethyl orthosilicate, stir magnetically at 80°C for 8 hours, filter and wash with n-heptane, drying.

[0032] 3) Dissolve 2.7g of silane-modified zeolite, 9g of PDMS with a viscosity of 50000Pa·s, 1.2g of octyltrimethoxysilane crosslinking agent, and 0.5g of catalyst dibutyltin dilaurate in 30g of n-heptane to prepare Form a solution, stir evenly, scrape the film on the PVDF porous bottom film, and dry it at room tempera...

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Abstract

The invention relates to a method for preparing a silicone rubber composite membrane filled with silane-modified zeolite and pertains to the technical field of the separation of pervaporation membrane. The method includes the steps that of scraping a polyester non-woven fabric layer by using polyvinylidene fluoride (PVDF) solution, and a PVDF porous basement membrane is obtained by applying the immersion precipitation phase inversion process; after MFI-type zeolite is modified by various alkoxy silanes or chlorosilanes, a membrane liquid which contains MFI-type zeolite, polydimethylsiloxane (PDMS), a crossing linking agent and a catalyst is prepared; the scraping is carried out on the PVDF porous basement membrane, and the scrapped membrane is air-dried at room temperature to ensure that the crossing linking is complete. The prior PDMS membrane which is not filled with zeolite has poorer performance of separating the ethanol water, and has separately lower separation factor and permeation flux. The silicone rubber composite membrane filled with silane modified zeolite obtained in the method has excellent ethanol permselective performance. When the mass ratio of silane modified zeolite to PDMS ranges from 50 to 100, the separation factor Alpha is equal to 19.9, and the permeation flux J is equal to 66.3g / m2h((EtOH) is equal to 5wt percent, 40 DEG C).

Description

technical field [0001] The invention relates to a preparation method of a silane-modified zeolite-filled silicon rubber composite membrane, which belongs to the field of pervaporation membrane separation. Background technique [0002] Pervaporation technology is an emerging membrane separation technology, which has significant advantages such as high separation efficiency, simple equipment, convenient operation, and low energy consumption. It is especially suitable for the separation of near-boiling point and constant-boiling point mixture systems. or near-boiling point mixture system has been widely valued by people. [0003] Polydimethylsiloxane has both the characteristics of organic polymers and inorganic materials. It is a typical polymer material with preferential permeability to alcohol. It has excellent resistance to ozone and corona discharge, and also has good Gas permeability, hydrophobicity, surface tension, chemical and physiological inertness, etc. are also on...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D71/34B01D71/70B01D69/12
Inventor 李继定展侠陈剑黄军其
Owner TSINGHUA UNIV