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Ionic liquid functionalized PVA catalytic composite membrane and preparation method thereof

A technology of ionic liquid and composite membrane, applied in the field of materials science, can solve the problems of large amount of ionic liquid, easy to be corroded, difficult to recycle, etc., and achieve the effects of low price, high conversion rate, and easy control

Active Publication Date: 2019-05-21
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional method of immobilized ionic liquid can solve the problem of large amount of ionic liquid and difficult recovery to a certain extent, but it is easy to be corroded and peeled off during the esterification reaction

Method used

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  • Ionic liquid functionalized PVA catalytic composite membrane and preparation method thereof
  • Ionic liquid functionalized PVA catalytic composite membrane and preparation method thereof
  • Ionic liquid functionalized PVA catalytic composite membrane and preparation method thereof

Examples

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Embodiment example 1

[0029] (1) First take by weighing 3g of PVA solid powder (the degree of polymerization is 1750), add in the container that deionized water is housed, stir continuously at 90 ℃ to obtain the PVA solution that the mass fraction is 3%; Then, take by weighing 50g of PVA Put the solution in a beaker, add the crosslinking agent glutaraldehyde (0.05% of the PVA mass), stir evenly, filter out the insoluble impurities and let stand for defoaming to obtain the separation layer casting liquid, adjust the height of the scraper to 100 μm, and the scraping speed 50m·min -1 , carefully coat the casting solution on the substrate, and dry it at room temperature for 2 days to obtain a separation membrane;

[0030](2) get 30g mass fraction and be the PVA solution of 3%, add strongly acidic ionic liquid monomer 1-vinyl-3-sulfonic acid butylimidazole hydrochloride (the mol ratio of ILs and PVA is 0.1), place in 60 In a constant temperature water bath at ℃, under the protection of nitrogen, first ...

Embodiment example 2

[0034] (1) First take by weighing 5g of PVA solid powder (the degree of polymerization is 2050), add in the container that deionized water is housed, stir continuously at 95 ℃ to obtain the PVA solution that the mass fraction is 5%; Then, take by weighing 50g of PVA Solution, add cross-linking agent glutaraldehyde (0.1% of the mass of PVA), stir evenly, filter out insoluble impurities, stand for defoaming to obtain the separation layer casting solution, adjust the height of the scraper to 100 μm, and the scraping speed to 10m min -1 , carefully coat the casting solution on the substrate, and dry it at room temperature for 3 days to obtain a separation membrane;

[0035] (2) get 30g mass fraction and be the PVA solution of 5%, add strongly acidic ionic liquid monomer 1-vinyl-3-sulfonic acid propylimidazolium bisulfate (the mol ratio of ILs and PVA is 0.2), place in 75 In a constant temperature water bath at ℃, under the protection of nitrogen, first purging for 30min, then addi...

Embodiment example 3

[0039] (1) First weigh 10g of PVA solid powder (the degree of polymerization is 1750), add it into a container with deionized water, and continuously stir at 100°C to obtain a PVA solution with a mass fraction of 10%; then, weigh 30g of PVA Solution, add cross-linking agent maleic acid (0.1% of PVA quality), stir at room temperature, leave standstill defoaming after filtering out insoluble impurity to obtain separation layer cast film liquid, adjust scraper height to be 200 μ m, scrape film speed to be 5m. min -1 , carefully coat the casting solution on the substrate, dry it at room temperature for 2 days, and finally obtain a separation membrane with high separation performance;

[0040] (2) get 30g mass fraction and be the PVA solution of 8%, add strongly acidic ionic liquid monomer 1-ene butyl-3-sulfonic acid butylimidazole trifluoromethanesulfonate (the mol ratio of ILs and PVA is 0.3 ), placed in a constant temperature water bath at 80°C, under the protection of argon, f...

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Abstract

The invention relates to an ionic liquid functionalized PVA catalytic composite membrane and a preparation method thereof. The ionic liquid functionalized PVA catalytic composite membrane is of a double-layer structure; a separating layer adopts a polyvinyl alcohol (PVA) membrane cross-linked by a cross linker; and a catalyst layer adopts an acid ionic liquid functionalized PVA membrane. The specific preparation method comprises the steps of using the cross linker to cross-link the PVA membrane in the separating layer, grafting and polymerizing double bond containing strong-acid ionic liquid (ILs) with the PVA through free radical polymerization under the protection of inert gas in the catalyst layer; and using a solvent evaporation method to prepare the catalytic composite membrane with the double-layer structure. The ionic liquid functionalized PVA catalytic composite membrane provided by the invention has the advantages that a strong-acid ionic liquid is grafted and copolymerized ona PVA molecular chain by using a chemical grafting method, so that each unit on a polymer chain contains an acid site, and therefore, the catalytic activity and catalytic stability of the PVA membrane are greatly improved, and higher catalytic performance is shown in esterification reaction; and meanwhile, as the ionic liquid is immobilized on the PVA membrane in the form of a chemical bond, a problem that the ionic liquid is easy to lose is preferably solved.

Description

technical field [0001] The invention belongs to the field of material science and the field of membrane separation technology, and in particular relates to an ionic liquid functionalized PVA catalytic composite membrane for promoting esterification reaction and a preparation method thereof. Background technique [0002] Esters are an important fine chemical product, widely used in petrochemical, pharmaceutical, paint, fragrance, plasticizer and other chemical industries, and will also be used as biodiesel instead of petrochemical diesel. Esterification is a traditional process for directly synthesizing carboxylic acid esters. This process usually uses strong liquid acids such as concentrated sulfuric acid as esterification catalysts, which easily causes equipment corrosion, difficult disposal of reaction waste liquid, difficult separation of products, and high overall production costs. Difficult separation and recycle of catalysts for esterification reactions are key issues ...

Claims

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Application Information

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IPC IPC(8): B01J31/06
Inventor 李卫星张莉邢卫红
Owner NANJING UNIV OF TECH