Method for producing hollow fiber carbon membrane

• US 9,731,250 B2
• Filed: 02/26/2014
• Issued: 08/15/2017
• Est. Priority Date: 02/27/2013
• Status: Active Grant

• Current Assignee: NOK Corporation
• Original Assignee: NOK Corporation
• Inventors: Yamamoto, Hirokazu, Ikawa, Yusuke, Koda, Yutaka
• Primary Examiner(s): Menon, Krishnan S
• Application Number:
  US14/769,062
• Publication Number:
  US 20160008770A1
• Time in Patent Office: 1,266 Days
• Field of Search: None
• CPC Class Codes: B01D 2323/081 Heating
• CPC Class Codes: B01D 2323/082 Cooling
• CPC Class Codes: B01D 69/08 Hollow fibre membranes manufacture of hollow fibres D01D5/24, D01F1/08
• CPC Class Codes: B01D 69/087 Details relating to the spinning process
• CPC Class Codes: B01D 71/601 Polyethylenimine
• CPC Class Codes: D01D 5/06 Wet spinning methods D01D5/0046 takes precedence
• CPC Class Codes: D01D 5/24 with a hollow structure; Spinnerette packs therefor D01D5/38 takes precedence; producing tubes of plastic material B29D; addition of agents forming hollow filaments D01F1/08
• CPC Class Codes: D01D 5/34 Core-skin structure; Spinnerette packs therefor
• CPC Class Codes: D01F 9/24 from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
• CPC Class Codes: D10B 2331/06 polyethers
• CPC Class Codes: D10B 2401/10 porous

Abstract

Disclosed is a method for producing a hollow fiber carbon membrane using a hollow fiber carbon membrane-forming material by means of a dry method or dry-wet method comprising a spinning step, a drying step, an infusibilization step, and a carbonization step as basic steps; wherein in the infusibilization step, heat treatment is performed at least two times at different temperatures, with the second temperature being higher than the first temperature. It is preferable that the second heat treatment is performed directly after the first treatment is performed, without once cooling to room temperature. The obtained hollow fiber carbon membrane has improved permeability, without reducing its separation coefficient.

Claims

1. A method for producing a hollow fiber carbon membrane using a hollow fiber carbon membrane-forming material by means of a dry method or dry-wet method comprising a spinning step, a drying step, an infusibilization step, and a carbonization step as basic steps;

wherein in the infusibilization step, heat treatment is performed at least two times at different temperatures, with the second temperature being higher than the first temperature;

in the spinning step, spinning is performed using a water-soluble organic polyamine aqueous solution having a concentration of 10 to 30 wt. % as a core liquid.

2. The method for producing a hollow fiber carbon membrane according to claim 1, wherein in the infusibilization step, after the first heat treatment is performed, the temperature is changed directly to the second heating temperature without once being cooled to room temperature, and the second heat treatment is performed.

3. The method for producing a hollow fiber carbon membrane according to claim 1, wherein in the infusibilization step, after the first heat treatment is performed at a heating temperature of 150 to 280°

C., the second heat treatment is performed at a heating temperature of 200 to 350°

C., which is higher than the first heating temperature.

4. The method for producing a hollow fiber carbon membrane according to claim 1, wherein the hollow fiber carbon membrane-forming material is a polyphenylene oxide-based polymer.

5. The method for producing a hollow fiber carbon membrane according to claim 1, wherein the water-soluble organic polyamine is an alkylenediamine, polyethylene polyamine, aminoalkyl group-containing amine, ether group-containing amine, or water-soluble organic amine-based polymer having a weight average molecular weight Mw of 200 to 5,000.

6. The method for producing a hollow fiber carbon membrane according to claim 2, wherein in the infusibilization step, after the first heat treatment is performed at a heating temperature of 150 to 280°

C., the second heat treatment is performed at a heating temperature of 200 to 350°

C., which is higher than the first heating temperature.