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Polyamic acids dope composition, preparation method of hollow fiber using the same and hollow fiber prepared therefrom

Inactive Publication Date: 2009-11-19
IUCF HYU (IND UNIV COOP FOUNDATION HANYANG UNIV)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Benefits of technology

[0027]Therefore, it is one object of the present invention to provide a dope solution composition suitable for use in preparing hollow fibers made of high free volume polymers by imidizing polyamic acid hollow fibers to obtain polyimide hollow fibers and subjecting the polyimide hollow fibers to thermal rearrangement via thermal treatment.
[0029]It is another object of the present invention to provide hollow fibers that have microcavities, increased polymer backbone strength and high fractional free volumes, thus exhibiting superior gas permeability and selectivity.

Problems solved by technology

On the other hand, gas separation using the membrane process has a relatively short history.
However, polymeric materials having membrane performance available commercially for use in gas separation (in the case of air separation, oxygen permeability is 1 Barrer or higher, and oxygen / nitrogen selectivity is 6.0 or higher) are limited to only a few types.
This is because there is considerable limitation in improving polymeric structures, and great compatibility between permeability and selectivity makes it difficult to obtain separation and permeation capabilities beyond a predetermined upper limit.
Furthermore, conventional polymeric membrane materials have a limitation of permeation and separation properties and disadvantages in that they undergo decomposition and aging upon a long-term exposure to high pressure and high temperature processes or to gas mixtures containing hydrocarbon, aromatic and polar solvents, thus causing a considerable decrease in inherent membrane performance.
Due to these problems, in spite of their high economic value, gas separation processes are utilized in considerably limited applications to date.

Method used

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  • Polyamic acids dope composition, preparation method of hollow fiber using the same and hollow fiber prepared therefrom
  • Polyamic acids dope composition, preparation method of hollow fiber using the same and hollow fiber prepared therefrom
  • Polyamic acids dope composition, preparation method of hollow fiber using the same and hollow fiber prepared therefrom

Examples

Experimental program
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Effect test

example 1

[0121]As depicted in Reaction Scheme 3 below, a hollow fiber comprising polybenzoxazole represented by Formula 41 are prepared from the polyhydroxyamic acid-containing dope solution.

[0122](1) Preparation of Polyhydroxyamic Acid

[0123]36.6 g (0.1 mol) of 2,2′-bis(3-amino-4-hydroxyphenyl)hexafluoropropane and 44.4 g (0.1 mol) of 4,4′-(hexafluoroisopropylidene)diphthalic anhydride were added to 189 g (70 wt %) of N-methylpyrrolidone (NMP) and were allowed to react at 15° C. for 4 hours to prepare a pale yellow viscous polyamic acid.

[0124](2) Preparation of Dope Solution

[0125]Without removing the solvent, 5% by weight of tetrahydrofurane as an additive was added to the NMP containing polyamic acid and then mixed to prepare a homogeneous dope solution.

[0126](3) Preparation of Hollow Fiber

[0127]The dope solution thus prepared was defoamed at ambient temperature under reduced pressure for 24 hours, and foreign materials were removed using a glass filter (pore diameter: 60 μm). Subsequently,...

example 2

[0129]A hollow fiber comprising polybenzothiazole represented by the following Formula 42 was prepared from the polythiolamic acid-containing dope solution through the following reactions.

[0130]A hollow fiber thermally rearranged into polybenzothiazole represented by Formula 42 was prepared in the same manner as in Example 1, except that 20.8 g (0.1 mol) of 2,5-diamino-1,4-benzenedithiol dihydrochloride and 44.4 g (0.1 mol) of 4,4′-(hexafluoroisopropylidene)diphthalic anhydride as starting materials were reacted to prepare thiol group (—SH)-containing polyamic acid.

[0131]The hollow fiber thus prepared had a weight average molecular weight of 14,500 Da. As a result of FT-IR analysis, characteristic bands of polybenzothiazole at 1,484 cm−1 (C—S) and 1,404 cm−1 (C—S) which were not detected in polyimide were confirmed.

example 3

[0132]A hollow fiber comprising polybenzopyrrolone represented by Formula 43 was prepared from the polyaminoamic acid-containing dope solution through the following reactions.

[0133]A hollow fiber thermally rearranged into polybenzopyrrolone represented by Formula 43 was prepared in the same manner as in Example 1, except that 21.4 g (0.1 mol) of 3,3′-diaminobenzidine as a starting material was reacted with 44.4 g (0.1 mol) of 4,4′-(hexafluoroisopropylidene)diphthalic anhydride to prepare an amine group (—NH2)-containing polyamic acid.

[0134]The prepared hollow fiber had a weight average molecular weight of 18,000 Da. As a result of FT-IR analysis, characteristic bands of polybenzopyrrolone at 1,758 cm−1 (C═O) and 1,625 cm−1 (C═N) which were not detected in polyimide were confirmed.

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Abstract

Disclosed herein are a polyamic acid dope solution composition, a method for preparing a hollow fiber using the composition and a hollow fiber prepared by the method. More specifically, disclosed are a method for preparing a hollow fiber, comprising preparing a polyamic acid dope solution composition comprising polyhydroxyamic acid, polythiolamic acid or polyaminoamic acid, spinning the composition to prepare a hollow fiber, and imidizing and thermally rearranging the hollow fiber, and the hollow fiber prepared by the method.In accordance with the method, a hollow fiber made of a high free volume polymer membrane can be prepared by spinning the dope solution composition to prepare a hollow fiber and thermally rearranging the hollow fiber via thermal treatment. The hollow fiber thus prepared exhibits excellent gas permeability and selectivity, thus being suitable for use as a gas separation membrane.

Description

CROSS-REFERENCE TO RELATED APPLICATION[0001]This application claims priority to and the benefit of Korean Patent Application No. 10-2008-0046115 filed in the Korean Intellectual Property Office on May 19, 2008, the entire contents of which are incorporated herein by reference.BACKGROUND OF THE INVENTION[0002](a) Field of the Invention[0003]The present invention relates to a polyamic acid dope solution composition, a method for preparing a hollow fiber using the same and a hollow fiber prepared by the method. More specifically, the present invention relates to a dope solution composition to prepare hollow fibers that have well-connected microcavities and are thus applicable to gas separation membranes for separating various types of gases via thermal rearrangement, a method for preparing hollow fibers from the composition and hollow fibers prepared by the method.[0004](b) Description of the Related Art[0005]Separation membranes must satisfy the requirements of superior thermal, chemi...

Claims

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Application Information

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IPC IPC(8): C08L5/08C08G63/685C08L5/02C08G73/10C08G16/00C08K3/00C08K5/05
CPCB01D69/08D01F6/74B01D71/64C08G73/1039C08G73/1042C08G73/1046C08G73/105C08G73/1053C08G73/1067C08G73/1071C08G73/22C08G75/32C08L79/04C08L79/08C08L81/00C08L2205/05D01D5/06D01D5/24D01D10/02B01D69/087B01D53/22B01D63/021B01D2256/12B01D2256/16B01D2256/18B01D2256/22B01D2257/102B01D2257/702B01D2325/02Y02C20/20Y10T428/2938Y10T428/2969Y10T428/2975C08L79/02B01D71/00
Inventor LEE, YOUNG-MOOHAN, SANG-HOONJUNG, CHUL-HOPARK, HO-BUM
Owner IUCF HYU (IND UNIV COOP FOUNDATION HANYANG UNIV)
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