Process for preparing carbon fibers from low polydispersity polyacrylonitrile

Patent metadata

Field	Value
Publication number	US-12258683-B2
Application number	US-202017607488-A
Country	US
Kind code	B2
Filing date	May 1, 2020
Priority date	May 2, 2019
Publication date	Mar 25, 2025
Grant date	Mar 25, 2025

Abstract

The present disclosure relates to a process for producing one or more carbon fiber precursor fibers, particularly by spinning a polymer solution, wherein the polymer has a polydispersity (PDI) of less than or equal to 2, in a coagulation bath with a jet stretch of about 5 to about 60. The one or more carbon fiber precursor fibers produced may be used for producing carbon fiber, typically carbon fiber used in manufacturing composite materials.

First claim

What is claimed is:

1. A process for producing one or more carbon fiber precursor fibers, the process comprising: spinning a polymer solution comprising a polyacrylonitrile (PAN) polymer having a polydispersity (PDI) of less than or equal to 2 in a coagulation bath with a jet stretch of about 15 to about 60, thereby producing one or more coagulated carbon fiber precursor fibers, wherein spinning of the polymer solution is conducted by air qap spinning with a spinneret having more than 1000 capillaries, the concentration of PAN polymer in the polymer solution is at least 10 wt %, based on total weight of the solution, the coagulation bath comprises 20 wt % to 85 wt % of one or more solvents with the balance being non-solvent and the temperature of the coagulation bath is from 0° C. to 20° C., and the cross-sectional diameter of the coagulated carbon fiber precursor fiber exiting the coagulation bath is less than 55 μ.

2. The process according to claim 1 , wherein the jet stretch is from about 35 to about 50.

3. The process according to claim 1 , wherein the polydispersity (PDI) of the PAN polymer is less than or equal to 1.7.

4. The process according to claim 1 , the polymer comprises repeating units derived from and one or more co-monomers selected from the group consisting of methacrylic acid (MAA), acrylic acid (AA), itaconic acid (ITA), vinyl-based esters, typically, methacrylate (MA), methyl methacrylate (MMA), vinyl acetate (VA), ethyl acrylate (EA), butyl acrylate (BA), ethyl methacrylate (EMA); and other vinyl derivatives, and mixtures thereof.

5. The process according to claim 1 , wherein the coagulation bath comprises 75 wt % to 85 wt % of one or more solvents.

6. The process according to claim 5 , wherein the one or more solvents is selected from the group consisting of dimethyl sulfoxide (DMSO), dimethyl formamide (DMF), dimethyl acetamide (DMAc), ethylene carbonate (EC), zinc chloride (ZnCl2)/water and sodium thiocyanate (NaSCN)/water.

7. The process according to claim 1 , wherein a vertical air gap from 1 to 50 mm is provided between the spinneret and the coagulation bath.

8. The process according to claim 1 , wherein the polymer has a molecular weight (M w ) of at least 60,000 g/mol.

9. The process according to claim 1 , wherein the polymer is synthesized by controlled/living radical polymerization using a Reversible Addition/Fragmentation Chain Transfer (RAFT) agent.

10. A process for producing carbon fibers, the process comprising:
1) Producing the coagulated carbon fiber precursor fibers according to the process of claim 1 ;
2) drawing the coagulated carbon fiber precursor fibers produced in step 1) through one or more draw and wash baths, thereby forming drawn carbon fiber precursor fibers that are substantially free of solvent; and
3) oxidizing the drawn carbon fiber precursor fibers of step 2) to form stabilized carbon fiber precursor fibers and then carbonizing the stabilized carbon fiber precursor fiber, thereby producing carbon fibers.

Assignees

• Cytec Ind Inc

Inventors

• Moskowitz Jeremy
• Taylor Thomas
• Tucker Amy
• Gladden Eric
• Harmon Billy

Classifications

• D01F9/225

  from stabilised polyacrylonitriles · CPC title

• D01D5/14

  with flowing liquid {or gaseous} stretching media {, e.g. solution-blowing} · CPC title

• C01B32/05

  Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30 · CPC title

• D01F9/22

  from polyacrylonitriles · CPC title

• D01F6/38

  comprising unsaturated nitriles as the major constituent · CPC title