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Hollow fiber composite film used for separating carbinol/ dimethyl carbonate mixture and preparation method and application thereof

A dimethyl carbonate and fiber composite technology, applied in the field of membrane separation, can solve the problems of complex and difficult operation, high equipment requirements, poor safety, etc., and achieve the effect of simple operation, large permeation flux, and high selectivity

Inactive Publication Date: 2013-02-13
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above separation methods all have relatively large shortcomings and deficiencies, such as complicated and difficult operation, high equipment requirements, high energy consumption, poor safety, etc. In contrast, membrane separation technology has the advantages of convenient operation, compact equipment, It has the advantages of safe working environment, energy saving, etc., and the most important thing is that it can break through the azeotropic equilibrium of methanol and dimethyl carbonate

Method used

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  • Hollow fiber composite film used for separating carbinol/ dimethyl carbonate mixture and preparation method and application thereof
  • Hollow fiber composite film used for separating carbinol/ dimethyl carbonate mixture and preparation method and application thereof
  • Hollow fiber composite film used for separating carbinol/ dimethyl carbonate mixture and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Preparation of polyacrylonitrile (PAN) hollow fiber ultrafiltration membranes. Use polyacrylonitrile as the membrane material, methylpyrrolidone (NMP) as the solvent, and polyvinylpyrrolidone (PVP) as the additive to prepare the casting solution (the mass ratio of PAN, NMP, and PVP is 15:81:4), stirring and dissolving at 60°C To a homogeneous transparent solution, the hollow fiber membrane is spun. After the casting solution was left to defoam, the casting solution was placed in N 2 Extruded from the spinneret under pressure, N 2 The pressure is 0.25MPa; the core liquid is water, and the material liquid extruded from the spinning head enters the gel water tank to precipitate the gel, and the gel temperature is 20°C; it is then rinsed and finally collected in the collection tank. In order to remove the residual solvent in the membrane, the spun hollow fiber membrane needs to be soaked in deionized water for 48 hours, and then dried in a dust-free laboratory.

[0029] ...

Embodiment 2~5

[0031] Weigh an appropriate amount of perfluorosulfonic acid (PFSA) and deionized water into a conical flask, stir at 95°C for 6 h to fully dissolve perfluorosulfonic acid, and prepare a 4% perfluorosulfonic acid solution. Prepare 4% polyvinyl alcohol (PVA) solution in the same way. Weigh different PFSA solutions and PVA solutions respectively to prepare coating solutions with mass ratios of PFSA and PVA of 0:10, 3:7, 5:5, and 7:3, and stir for 2 hours to make the solutions evenly mixed. Put the coating liquid on the polyacrylonitrile (PAN) membrane prepared in Example 1 after standing for defoaming, and apply the film for 30 seconds each time. After drying, apply the reverse coating for the second time to obtain the PFSA-PVA / PAN hollow fiber composite membrane . Put the dried PFSA-PVA / PAN composite film into a vacuum oven for heat treatment at 100°C for 1h.

[0032] The prepared PFSA-PVA / PAN composite membrane membrane filament is made into a membrane module 3; figure 1 In...

Embodiment 6~9

[0045] In Example 1, the mass ratio of PFSA to PVA is 5:5, and the coating solution is left to defoam and then coated on the bottom film polyacrylonitrile (PAN) film treated with isopropanol and cyclohexane. 30s, after drying, apply the second time in reverse. Put the dried composite membrane into a vacuum oven for heat treatment at 100°C for 1 h. Measure the separation factor and permeation flux of the prepared composite membrane with a performance evaluation device. The feed liquid is an azeotropic system of methanol and dimethyl carbonate, that is, the mass fraction of methanol is 70wt.%. The separation performance at different operating temperatures See Table 2.

[0046] Table 2 Separation performance at different operating temperatures

[0047] Example Operating temperature / ℃ separation factor Permeation flux (g m -2 h -1 ) 6 30 5.98 88.12 7 40 7.70 101.42 8 50 10.62 130.26 9 60 8.8 235.64 ...

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Abstract

The invention discloses a hollow fiber composite film used for separating carbinol / dimethyl carbonate mixture and preparation method and application thereof. The method includes the following steps: (1) respectively preparing 1-10wt. % water solutions of polyving akohol (PVA) and perfluor sulfonic acid (PFSA), mixing the water solutions according to any ratio to prepare PFSA-PVA film coating liquid, statically placing the liquid, conducting defoaming, coating the PFSA-PVA film coating liquid on a polyacrylonitrile (PAN) hollow fiber ultrafiltration film, conducting airing in dust-free environment, statically placing the film and conducting secondary coating and airing with each coating time being 30s; and (2) conducting vacuum drying on the composite film prepared in the step (1) with heat processing temperature as 80-170 DEG C and the heat processing time as 1-3h. The prepared hollow fiber composite film is penetrated by the carbinol first, can be used for separating the carbinol / dimethyl carbonate mixture, and has the advantages of being low in energy consumption, free of pollution, simple in operation and the like.

Description

technical field [0001] The invention belongs to the technical field of membrane separation, and in particular relates to a hollow fiber composite membrane used for separating methanol / dimethyl carbonate mixture and its preparation method and application. Background technique [0002] Dimethyl carbonate (DMC) is a colorless transparent liquid that is miscible with ethanol, ether, etc. in any ratio. Its molecular structure contains -CO, -COOCH 3 、-CH 3 And many other functional groups, the chemical properties are very active, as an organic synthesis intermediate, it can react with phenol, alcohol, amine, hydrazine, and ester compounds to synthesize many compounds with special properties. It is an environmentally friendly green chemical that has attracted widespread attention at home and abroad in recent years. product. [0003] The product obtained by general rectification in the production process of DMC is methanol (CH 3 OH) and the binary azeotrope formed by DMC must un...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/42B01D67/00B01D69/12B01D71/38B01D71/06B01D61/36B01D69/08C07C31/04C07C29/76C07C68/08C07C69/96D01D5/24D01F6/54D01F1/10
Inventor 郎万中牛海燕郭亚军褚联峰
Owner SHANGHAI NORMAL UNIVERSITY