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Carbon nanotube filling composite membrane with alcohol penetration priority and preparation method thereof

A carbon nanotube technology that preferentially penetrates alcohol and is applied in semipermeable membrane separation, chemical instruments and methods, membrane technology, etc., and can solve problems such as dissolution, small intermolecular forces, and decreased selectivity.

Inactive Publication Date: 2013-07-31
TSINGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although polydimethylsiloxane has a large free volume and good permeability, due to the small intermolecular force, the mechanical properties of film formation alone are poor, and it is easy to swell or even dissolve when it is applied to the separation of systems with high organic content, resulting in Decreased selectivity, not up to industrial requirements

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1) Mix polyvinylidene fluoride and triethyl phosphate at a mass ratio of 3:17 at 70°C, filter and stand for defoaming, then use water as a gel bath, and use the immersion phase inversion method to coat the polyester nonwoven Scratch the film on the cloth to obtain a polyvinylidene fluoride porous base film supported by non-woven fabric, and let it dry naturally with a thickness of 30 μm.

[0025] 2) Mix 0.4g, 0.8g, and 1.2g of single-walled carbon nanotubes with 9g of polydimethylsiloxane with a viscosity of 50,000mPa·s, stir and ultrasonically disperse evenly, and then add 0.75g of phenyltrimethoxysilane, Dissolve 0.3g of dibutyltin dilaurate in 30g of toluene, stir evenly, scrape the film on the polyvinylidene fluoride porous bottom film, dry at room temperature for 12h, then dry in an oven at 80°C for 5h, and select a layer thickness of 30μm.

[0026] The pervaporation performance of the zeolite-filled composite membrane was measured for a 5% ethanol aqueous solution...

Embodiment 2

[0032] 1) Mix polyvinylidene fluoride and N,N-dimethylformamide at a mass ratio of 3:17 at 70°C, filter and stand for defoaming, then use water as a gel bath, and use the immersion phase inversion method Scrape the film on the polyester non-woven fabric to obtain a polyvinylidene fluoride porous base film supported by the non-woven fabric, and let it dry naturally with a thickness of 50 μm.

[0033] 2) Mix 0.4g, 0.8g, 1.2g, 2g of multi-walled carbon nanotubes with 9g of polydimethylsiloxane with a viscosity of 50000mPa·s, stir and ultrasonically disperse evenly, then add 0.75g of phenyltrimethoxysilane in sequence 1. Dissolve 0.3g of dibutyltin dilaurate in 30g of toluene, stir evenly, scrape the film on the polyvinylidene fluoride porous bottom film, dry at room temperature for 12h, then dry in an oven at 80°C for 5h, and select a layer thickness of 30μm.

[0034] Under the conditions of operating temperature 40°C-70°C and absolute pressure behind the membrane of 200Pa, the c...

Embodiment 3

[0045] 1) Mix polyvinylidene fluoride and N,N-dimethylacetamide at a mass ratio of 3:17 at 70°C, filter and stand for defoaming, then use water as a gel bath, and use the immersion phase inversion method Scrape the film on the polyester non-woven fabric to obtain a polyvinylidene fluoride porous base film supported by the non-woven fabric, and let it dry naturally with a thickness of 40 μm.

[0046] 2) Disperse 1g of hydroxylated multi-walled carbon nanotubes passed through a 100-mesh sieve in 10g of n-heptane, stir for 1h, ultrasonicate for 30min, then magnetically stir for 1h, add 0.8g of dodecyltrichlorosilane, and heat at 70°C Reflux for 12 hours, filter, wash the filter cake with n-heptane for 3-5 times, and vacuum dry at 110° C. for 6 hours to obtain modified hydroxylated multi-walled carbon nanotubes.

[0047] 3) Mix 0.4g, 0.8g, 1.2g, 2g of modified hydroxylated multi-walled carbon nanotubes with 9g of polydimethylsiloxane with a viscosity of 50000mPa·s, stir and ultras...

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PUM

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Abstract

The invention discloses a carbon nanotube filling composite membrane with alcohol penetration priority in the field of penetration vaporization membrane separation technology and preparation method thereof. The preparation method of the composite membrane comprises the following steps: casting polyvinylidene fluoride on a polyester non-woven fabric, scraping membrane by an immersion phase inversion method for obtaining a supporting layer; And then stirring the carbon nanotube and the polydimethylsiloxane by ultrasound for uniform dispersion, adding cross-linking agent and catalyst for reacting and forming a membrane casting solution, casting onto the bottom membrane and obtaining a separating layer. The membrane obtained by the method has the advantages of improved mechanical strength, penetration throughtput and selectivity, especially substantially increased hydroxylate multi-wall carbon nanotube hydrophobicity after trichlorosilane modification, improved polydimethylsiloxane compatibility and separating factor. The invention has the advantages of reliable and stable method, simple preparation technology, enhanced mechanical performance of pure polydimethylsiloxane membrane, improved penetration throughput and separating factor, and good industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of pervaporation membrane separation, and in particular relates to a composite membrane filled with carbon nanotubes and an alcohol-preferred permeation membrane and a preparation method thereof. Background technique [0002] After the oil crisis broke out in the 1970s, coupled with the deteriorating human living environment, the development and utilization of biomass green new energy represented by ethanol has gradually become a worldwide research hotspot. The technology of coupling biological fermentation and pervaporation to produce ethanol has attracted extensive attention because of its low consumption, high efficiency and non-toxicity to cells. Pervaporation is the use of dense polymer membranes to separate components in liquid mixtures based on the difference in their dissolution and diffusion rates. The process has the remarkable advantages of high single-stage separation efficiency, simple equipmen...

Claims

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Application Information

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IPC IPC(8): B01D71/70B01D69/12B01D61/36
Inventor 李继定夏阳韩小龙王涛吴珍余立新
Owner TSINGHUA UNIV
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