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Method for preparing polydimethylsiloxane (PDMS)/polyvinylidene fluoride (PVDF) composite hollow fiber film

A fiber membrane and hollow technology, applied in the field of pervaporation membrane separation, can solve the problems of large footprint of membrane modules, difficulty in industrial application, low mechanical strength, etc., and achieve low production cost, not easy to be polluted, and good mechanical strength.

Inactive Publication Date: 2012-11-21
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Polyether copolyamide (PEBA) is an important polymer material. The separation effect of a polymer membrane with a thickness of 100 μm on binary systems (acetone-water, butanol-water, ethanol-water) is: separation factor alpha 丙酮 =4.2, α 丁醇 = 8.2 and α 乙醇 =2.4, the corresponding total permeation flux is 27.4gm -2 h -1 、65.3gm -2 h -1 and 37.2gm -2 h -1 (Liu, FF; Liu, L; Feng, XS. Separation of acetone-butanol-ethanol (ABE) from dilute aqueous solution by pervaporation [J]. Sep. Purif. Technol. 2005, 42(3): 273-282) ; The disadvantages of inorganic membranes due to the high price of materials and poor stability of liquid membranes limit their industrial application
[0006] The above-mentioned membrane is basically a flat membrane, its mechanical strength is not high, and the membrane area per unit volume is small, and the membrane module occupies a large area, which is not easy for industrial application

Method used

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  • Method for preparing polydimethylsiloxane (PDMS)/polyvinylidene fluoride (PVDF) composite hollow fiber film
  • Method for preparing polydimethylsiloxane (PDMS)/polyvinylidene fluoride (PVDF) composite hollow fiber film
  • Method for preparing polydimethylsiloxane (PDMS)/polyvinylidene fluoride (PVDF) composite hollow fiber film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Dissolve 10g of polydimethylsiloxane (PDMS) in 100g of n-hexane, add 0.6g of cross-linking agent ethyl orthosilicate, mix and stir at room temperature for 0.5 hours, then add 0.1g of catalyst dibutyltin dilaurate, add n-hexane alkane until the concentration of polydimethylsiloxane in the mixed solution is 5 wt%, and after sealing, stir at room temperature for 8 hours, and the obtained solution is centrifuged and defoamed to make a film-making solution. Rinse the polyvinylidene fluoride (PVDF) hollow fiber membrane with distilled water until neutral, dry it at room temperature, and use it as the base membrane. The treated basement membrane is immersed in the membrane-forming solution for 2 to 3 seconds, taken out, and dried at room temperature. The coating was repeated 3 times, and then placed in a vacuum oven at 110°C for 10 hours to be vacuum-dried until completely cross-linked to obtain a PDMS / PVDF composite hollow fiber membrane. The outer layer of the obtained comp...

Embodiment 2

[0019] Dissolve 10g of polydimethylsiloxane in 50g of n-hexane, add 1.0g of crosslinking agent ethyl orthosilicate, mix and stir at room temperature for 1 hour, then add 0.5g of catalyst dibutyltin dilaurate, add n-hexane to mix The concentration of polydimethylsiloxane in the liquid is 15 wt%, and after sealing, it is stirred at room temperature for 12 hours, and the obtained solution is centrifuged and defoamed to prepare a film-forming liquid. Rinse the PVDF hollow fiber membrane with distilled water until neutral, dry it at room temperature, and use it as the base membrane. The treated basement membrane is immersed in the membrane-forming solution for 2 to 3 seconds, taken out, and dried at room temperature. The coating was repeated 3 times, and then placed in a vacuum oven at 30°C for 10 hours to be vacuum-dried until completely cross-linked to obtain a PDMS / PVDF composite hollow fiber membrane. The outer layer of the obtained composite hollow fiber membrane is a dense P...

Embodiment 3

[0024] Dissolve 20g of polydimethylsiloxane in 50g of n-hexane, add 1.6g of crosslinking agent ethyl orthosilicate, mix and stir at room temperature for 2 hours, then add 0.6g of catalyst dibutyltin dilaurate, add n-hexane until mixed The concentration of polydimethylsiloxane in the liquid is 30 wt%, and after being sealed, it is stirred at room temperature for 16 hours, and the obtained solution is centrifuged and defoamed to make a film-forming liquid. Rinse the PVDF hollow fiber membrane with distilled water until neutral, dry it at room temperature, and use it as the base membrane. The treated basement membrane is immersed in the membrane-forming solution for 2 to 3 seconds, taken out, and dried at room temperature. The coating was repeated twice, and then placed in a vacuum oven at 80°C for 10 hours to be vacuum-dried until completely cross-linked to obtain a PDMS / PVDF composite hollow fiber membrane. The outer layer of the obtained composite hollow fiber membrane is a d...

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Abstract

The invention discloses a method for preparing a polydimethylsiloxane (PDMS) / polyvinylidene fluoride (PVDF) composite hollow fiber film, which comprises the following steps: (1) dissolving polydimethylsiloxane in normal hexane, adding a crosslinking agent, mixing, stirring for 0.5 to 2 hours, adding a catalyst, supplementing normal hexane till the polydimethylsiloxane mass percentage concentration of the mixed solution is 5 to 30 percent, stirring at room temperature for 8 to 16 hours, centrifuging, defoaming and preparing film solution, wherein the crosslinking agent is tetraethoxysilane, the mass ratio of the crosslinking and the polydimethylsiloxane is 0.06-0.1:1, the catalyst is dibutyltin dilaurate, and the mass ratio of the catalyst to the polydimethylsiloxane is 0.01-0.05:1; and (2) immersing a dried neutral polyvinylidene fluoride hollow fiber base film in the film-making solution for 2 to 3 seconds, taking the base film out, drying the base film at room temperature, repeatingthe film immersing and drying operation for 2 to 3 times, and drying under vacuum at 30 to 110 DEG C till complete crosslinking. In the invention, the process is simple; and the obtained hollow fiberfilm has an excellent separation effect on low-concentration ketone / butanol / ethanol solution.

Description

technical field [0001] The invention relates to a preparation method of a PDMS / PVDF (polydimethylsiloxane / polyvinylidene fluoride) composite hollow fiber membrane used for pervaporation preferentially permeating organic matter, and belongs to the field of pervaporation membrane separation. Background technique [0002] As early as 1861, Pasteur had discovered that bacteria could produce butanol. By 1945, 2 / 3 of butanol in the United States was produced by biological fermentation. However, in the 1960s, due to the high price of fermentation raw materials, low product concentration, high product recovery costs, and under the impact of the petrochemical industry, the bio-butanol industry developed slowly. Until the oil crisis in 1973, the oil shortage and the soaring oil price made bio-butanol get people's attention again. [0003] In addition to butanol, the fermentation broth produced by Clostridium acetobutylicum contains acetone and a small amount of ethanol (commonly kno...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D71/70B01D67/00B01D69/08B01D69/10
Inventor 陈雄吴坚平张林杨立荣
Owner ZHEJIANG UNIV
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