Organic-inorganic hybrid membrane for pervaporation separation of methanol/methyl acetate azeotropic system and preparation method thereof

A technology of methyl acetate and pervaporation, applied in the preparation of organic compounds, carboxylate esters, organic chemistry, etc., to achieve the effects of low density, good toughness, good mechanical properties and stability

Inactive Publication Date: 2011-12-07
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The primary technical problem to be solved by the present invention is to provide an organic-inorganic hybrid system for pervaporation separation of methanol / methyl acetate azeotropic system with high mechanical strength, good stability and good separation performance in view of the existing background technology. membrane

Method used

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  • Organic-inorganic hybrid membrane for pervaporation separation of methanol/methyl acetate azeotropic system and preparation method thereof
  • Organic-inorganic hybrid membrane for pervaporation separation of methanol/methyl acetate azeotropic system and preparation method thereof
  • Organic-inorganic hybrid membrane for pervaporation separation of methanol/methyl acetate azeotropic system and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Add 3.5g of PVA (polymerization degree 1750, the same below), 1.5g of PVP (K90), 0.1282g of 4A molecular sieve and 44.8718g of dimethyl sulfoxide (the total weight of the solution is 50g) into the flask. Heat and stir in a constant temperature water bath at 95° C. for 4 hours to completely dissolve PVA and PVP and uniformly disperse 4A molecular sieves to obtain a PVA / PVP / 4A molecular sieve blend. 4A molecular sieve accounts for 2.5wt% of the total amount of PVA / PVP / 4A molecular sieve. Weigh 0.5g DAS and dissolve it in 49.5g dimethyl sulfoxide under dark conditions and stir to dissolve it, then add an equal amount of PVA / PVP / 4A molecular sieve blend to this solution, and stir evenly in the dark to obtain cast Membrane fluid. Filter the casting solution, let it sit for defoaming, scrape the film on clean glass, and dry it at a constant temperature of 80°C under dark conditions. Place the dried film under a straight-tube high-pressure mercury lamp (short-wave UVC, cente...

Embodiment 2

[0038] Change the content of 4A molecular sieve so that 4A molecular sieve accounts for 1.5wt% of the total amount of PVA / PVP / 4A molecular sieve. All the other conditions are with embodiment 1. Use this membrane to separate the methanol / methyl acetate azeotrope by pervaporation. The raw material side is kept at normal pressure, the permeate side is vacuumed, the temperature of the feed liquid is 45°C, and the retentate is returned to the feed liquid tank. The test is carried out after 3 hours of permeation reaches stability. , the permeate flux of the membrane is 24g / (m 2 h), the separation coefficient is 28.5.

Embodiment 3

[0040] Change the content of 4A molecular sieve so that 4A molecular sieve accounts for 3.5wt% of the total amount of PVA / PVP / 4A molecular sieve. All the other conditions are with embodiment 1. Use this membrane to separate the methanol / methyl acetate azeotrope by pervaporation. The raw material side is kept at normal pressure, the permeate side is vacuumed, the temperature of the feed liquid is 45°C, and the retentate is returned to the feed liquid tank. The test is carried out after 3 hours of permeation reaches stability. , the permeate flux of the membrane is 45.1g / (m 2 · h), the separation coefficient is 15.4.

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Abstract

The invention discloses an organic-inorganic hydrid film used for pervaporation separation of a methanol / methyl acetate azeotropic system and a preparation method thereof. The preparation method comprises the following processes of: (1) heating and stirring polyvinyl alcohol (PVA), polyvinylpyrrolidone (PVP), a 4A molecular sieve and a solvent of dimethyl sulfoxide according to proportions in a constant-temperature water bath to obtain a PVA / PVP / 4A molecular sieve mixing solution; and (2) weighing DAS (Dialdehyde Starch) according to a proportion, dissolving into the dimethyl sulfoxide, stirring in a dark place and dissolving, then adding the equivalent PVA / PVP / 4A molecular sieve mixing solution obtained in the step (1) to the solution, and uniformly stirring to obtain a casting film solution. The casting film solution is filtered and defoamed, and then the film is scraped from glass and dried. The dried film is placed below a high-pressure mercury lamp and irradiated for 30-60 min toensure that coupling reaction is completed so as to obtain a 4A molecular sieve-filled DAS-crosslinking polyvinyl alcohol / polyvinylpyrrolidone organic-inorganic hydrid film. The organic-inorganic hydrid film has favorable mechanical strength and chemical stability and a higher pervaporation separation coefficient and can effectively break azeotropic components and has better separation degree than the traditional method.

Description

technical field [0001] The invention belongs to polymer membrane separation technology, in particular to an organic-inorganic hybrid membrane used for pervaporation separation of methanol / methyl acetate azeotropic system and a preparation method thereof. Background technique [0002] Methyl acetate is widely used in industries such as textiles, spices, and medicine. It is an intermediate of organic raw materials and can be used to synthesize acetic acid, acid anhydride, methyl acrylate, vinyl acetate, and acetamide. The main production method of methyl acetate---direct esterification method and methanol carbonylation method all use methanol as raw material, and methyl alcohol and methyl acetate can form azeotrope (methanol content is about 18wt%), so from methyl acetate Methanol removal is an important process for product purification. In addition, in the production of vinylon, the waste liquid of polyvinyl acetate alcoholysis to produce polyvinyl alcohol contains a large a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/38C07C29/82C07C31/04C07C67/54C07C69/14
Inventor 肖通虎徐小莉
Owner NINGBO UNIV
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