Maps modified silica filled pim-1 composite film and preparation method thereof

A PIM-1, silica technology, applied in chemical instruments and methods, separation/purification of hydroxyl compounds, membranes, etc., can solve the problems of high cost of carbon nanotubes and limited improvement of separation efficiency, and improve pervaporation performance. , high separation ability, the effect of improving hydrophobicity

Active Publication Date: 2020-12-11
SANMING UNIV
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Problems solved by technology

Patent CN103877874A discloses a preparation method of polydimethylsiloxane-carbon nanotube composite membrane, its composite membrane and a method for separating and purifying butanol, by adding carbon nanotubes to polydimethylsiloxane, although To a certain extent, the permeation flux and separation factor in the process of separating butanol are improved, but the separation efficiency is limited, and the cost of carbon nanotubes is high

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  • Maps modified silica filled pim-1 composite film and preparation method thereof
  • Maps modified silica filled pim-1 composite film and preparation method thereof
  • Maps modified silica filled pim-1 composite film and preparation method thereof

Examples

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preparation example Construction

[0025] A method for preparing a MAPS-modified silica-filled PIM-1 composite membrane provided in an embodiment of the present invention comprises the following steps:

[0026] S1, PIM-1 preparation: 5,5',6,6'-tetrahydroxy-3,3,3',3'-tetramethyl-1,1'-spirobiindole, Nitrile, catalyst and the first solvent are mixed, heated and stirred at 140-165°C for 30-60 minutes under the condition of inert gas, and the crude product is obtained, and the crude product is dissolved in the second solvent, stirred for 5-15 minutes, filtered, washed and dried Obtain PIM-1, wherein, catalyst comprises K 2 CO 3 .

[0027] S2, Preparation of modified silica: Disperse nano fumed silica and γ-(methacryloyloxy)propyltrimethoxysilane in the third solvent, stir magnetically for 50-80 minutes, and then ultrasonically treat for 20-40 minutes , to obtain a modified silica solution.

[0028] S3, pour the modified silicon dioxide solution into the PIM-1 solution with a mass fraction of 8-12%, and mix to ob...

Embodiment 1

[0043] A kind of MAPS modified silica filled PIM-1 composite membrane provided in this embodiment is prepared according to the following method:

[0044] (1) Pretreatment of the support layer: place the CA microfiltration membrane in deionized water for 2 hours before use.

[0045] (2) Preparation of PIM-1: 8.3g K 2 CO 3 , 6.8g 5,5',6,6'-tetrahydroxy-3,3,3',3'-tetramethyl-1,1'-spirobiindole, 4g tetrafluoroterephthalonitrile, 15mL Add toluene and 30mL of N,N-dimethylacetamide into a 500mL three-necked flask. Heat and stir at 155°C, and stir with nitrogen gas. The crude product was collected after 40 min. The crude product was dissolved in a chloroform / methanol mixture, stirred for 10 min, and the precipitate was obtained by filtration, and the solvent and salt in the precipitated product were washed away with deionized water. Then the product was placed in a vacuum oven at 100° C. for 12 hours to obtain the final product of PIM-1.

[0046] (3) Preparation of PIM-1 solutio...

Embodiment 2

[0053] The PIM-1 composite membrane filled with MAPS modified silica provided in this example is different from Example 1 in that the amount of modified silica added is 4%.

[0054] The PIM-1 composite membrane that present embodiment makes measures pervaporation performance at 40 ℃ of 5% n-butanol aqueous solution, and its permeation flux is 509g m -2 h -1 , the separation factor is 15.8.

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Abstract

The invention provides an MAPS-modified silica-filled PIM-1 composite membrane and a preparation method thereof and relates to the technical field of pervaporation membranes. The preparation method ofthe composite membrane comprises the following steps: modifying nano-fumed silica with MAPS (gamma-methylallyloxopropyltrimethoxysilane), then taking modified silica particles as filling agents, adding in a soluble intrinsic micro-porous polymer (PIM-1) matrix and taking a cellulose acetate (CA) micro-filtration membrane as a supporting layer to prepare the plate pervaporation composite membrane.The composite membrane can effectively separate and purify an n-butanol solution, is strong in hydrophobic property and good in pervaporation property and has high N-butanol separation capacity whilethe high permeation flux can be ensured.

Description

technical field [0001] The invention relates to the technical field of pervaporation membranes, and in particular to a MAPS modified silicon dioxide filled PIM-1 composite membrane and a preparation method thereof. Background technique [0002] With the aggravation of the energy crisis and the increasingly serious environmental pollution, the development of clean energy has attracted increasing attention. n-butanol is an important chemical raw material, and it is expected to become a new generation of biofuel. The production of n-butanol by fermentation of renewable biomass has attracted more and more attention. N-butanol can be added to gasoline in a very high proportion, which greatly improves the combustion efficiency of gasoline. At the same time, the combustion of n-butanol will only produce carbon dioxide and water, and will not pollute the environment. Because the fermentation product butanol has a toxic inhibitory effect on the fermentation strains, the efficiency o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D69/12B01D69/10B01D69/02B01D61/36B01D67/00C07C29/76C07C31/12
CPCB01D61/362B01D67/0079B01D69/02B01D69/10B01D69/12B01D2325/38C07C29/76C07C31/12
Inventor 兰永强彭平肖旺钏苏志忠李奇勇
Owner SANMING UNIV
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