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Asymmetric polyimide film for separating methyl cyclopentadiene and cyclopentadiene

A technology of methylcyclopentadiene and polyimide membrane, which is applied in the fields of semi-permeable membrane separation, membrane purification/separation, membrane technology, etc., and can solve the problem of complex vacuum distillation process, complex process flow and large equipment investment etc. to achieve the effect of good selective permeability, high separation rate and simple equipment

Inactive Publication Date: 2013-06-05
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, after the MCPD mixed raw material is completely depolymerized, the dimerization reaction is carried out, which increases energy consumption, and the vacuum distillation process is complicated, and the vacuum system (vacuum degree: -0.1~-0.01 MPa) has high requirements for equipment.
[0007] Traditional MCPD and CPD separation processes mostly include depolymerization and rectification processes. Since MCPD is easily polymerized into dimers at room temperature, traditional separation technologies have disadvantages such as complex process flow, large equipment investment, and high energy consumption.

Method used

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  • Asymmetric polyimide film for separating methyl cyclopentadiene and cyclopentadiene
  • Asymmetric polyimide film for separating methyl cyclopentadiene and cyclopentadiene
  • Asymmetric polyimide film for separating methyl cyclopentadiene and cyclopentadiene

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Experimental program
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Effect test

Embodiment 1

[0035] Dissolve an appropriate amount of dried 4,4-diaminodiphenyl ether (ODA) in N, N-dimethylacetamide (DMAc), stir to fully dissolve the ODA, and add an appropriate amount of bisphenol-A diether in three batches Dianhydride (BPADA), N 2Stir under protection, slowly add equimolar equivalents of acetic anhydride and triethylamine dropwise, and raise the temperature to 60 °C for chemical imidization, then pour the mixture quickly into stirring ethanol to precipitate a polymer, wash with deionized water Afterwards, place in a vacuum oven to prepare polyimide solids.

[0036] The above-mentioned polyimide solid is dissolved in N-methylpyrrolidone (NMP) according to a certain mass ratio, N 2 Add acetone with a mass ratio of 15% under protection, oscillate to dissolve, filter the casting solution through a stainless steel wire mesh to remove impurities, let it stand to remove air bubbles, and evenly drool on a glass plate, control different solvent volatilization times, scrape to...

Embodiment 2

[0041] Take the polyimide solids prepared by different amounts of example 1 according to the polyimide solid content as 16%, 17%, 18%, and 20%, and dissolve them in N-methylpyrrolidone (NMP), N 2 Add acetone with a mass ratio of 15% under protection, oscillate to dissolve, filter the casting film solution through stainless steel wire mesh to remove impurities, let it stand to remove air bubbles, and evenly drool on a glass plate. The solvent volatilization time is 60s, scrape to form a film, and place Precipitate in a deionized hydrogel bath at 20 ℃, soak in deionized water and glycerin to replace the solvent, prepare polyimide asymmetric membranes with different solid contents, and use a membrane pervaporation performance evaluation device to measure its separation performance. Liquid is C 5 Fractional distillation products (the mass ratio of methylcyclopentadiene to cyclopentadiene after thermal depolymerization is about 80:20), and the through-test material is analyzed by t...

Embodiment 3

[0045] Take by weighing the polyimide solid prepared by an appropriate amount of example one, dissolve in N-methylpyrrolidone (NMP), N 2 Add acetone with a mass ratio of 15% under protection, oscillate to dissolve, filter the casting film solution through stainless steel wire mesh to remove impurities, let it stand to remove air bubbles, and evenly drool on a glass plate. The solvent volatilization time is 60s, scrape to form a film, and place Phase inversion precipitation in different gel media at 20 ℃, respectively soaked in deionized water and glycerin to replace the solvent, prepared polyimide asymmetric membranes formed under different gel media conditions, and measured their properties using a membrane pervaporation performance evaluation device Separation performance, feed liquid is C 5 Fractional distillation products (the mass ratio of methylcyclopentadiene to cyclopentadiene after thermal depolymerization is about 80:20), and the through-test material is analyzed by ...

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Abstract

The invention discloses an asymmetric polyimide pervaporation film for separating methyl cyclopentadiene and cyclopentadiene homologs. The repeating unit of the asymmetric polyimide film is condensed from a bisphenol A structure and a phenylate structure, and the asymmetric polyimide film is in a multilayer asymmetric structure with a compact skin layer and a regular porous spongy layer. The asymmetric film is preferentially permeable to cyclopentadiene, and can separate methyl cyclopentadiene and cyclopentadiene homologs and purify methyl cyclopentadiene. The cyclopentadiene separation factor of the asymmetric polyimide film prepared under the optimum conditions can reach 2.1, and the permeation flux is 1003 g / m<2>.h, and thus, the asymmetric polyimide film can be used for purifying and producing 95% methyl cyclopentadiene. The film separation method for purifying methyl cyclopentadiene has the advantages of simple equipment, high separation efficiency, low energy consumption, no pollution and the like. The film preparation technique is simple; and the film has the advantages of low material price, high cyclopentadiene selectivity and high permeation flux.

Description

technical field [0001] The invention relates to the preparation of an asymmetric polyimide pervaporation membrane, which is used to separate methylcyclopentadiene (MCPD) and cyclopentadiene (CPD), and the raw material solution is C 5 Fractional distillation separates the product, and the mass ratio of methylcyclopentadiene to cyclopentadiene is 80:20. Background technique [0002] Methylcyclopentadiene is a high-end fine chemical raw material, mainly used in the synthesis of gasoline anti-shock agent methylcyclopentadiene tricarbonyl manganese (MMT), special binder methylnadic anhydride (MNA), polyolefin Catalysts, high-energy fuels, new product flame retardants, etc., due to the presence of methyl groups in the molecule, their chemical products are superior to cyclopentadiene in performance and use. In industry, the direct source of methylcyclopentadiene is very limited, and it is usually synthesized by gas-phase methylation of cyclopentadiene, or by pyrolysis of petroleum...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/64B01D67/00B01D61/36C07C7/144C07C13/15
Inventor 陈金庆李青松陈冰
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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