Patent US4024227A successfully refreshed from Google Patents.
US4024227A
Expired / Lapsed
US
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Process for producing carbon fibers having excellent properties
Assignee: Sumika Hercules Co Ltd
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Filing: 1975-10-30
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Granted: 1977-05-17
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Expires: 1995-10-30
Abstract
Abstract A process for producing a carbon fiber having high tensile strength and high modulus of elasticity which comprises heat-treating an acrylonitrile fiber impregnated with at least one compound selected from specific primary amines and/or quaternary ammonium salts so that an acrylic fiber which is partly insoluble in a concentrated aqueous solution of sodium thiocyanate is obtained; thermally stabilizing said partly insoluble acrylic fiber; and then carbonizing said thermally stabilized fiber.
Inventors
- 👤 Soichiro Kishimoto
- 👤 Saburo Okazaki
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-08 19:06
CPC Classifications
D; D01; D01F; D01F9/00; D01F9/08; D01F9/12; D01F9/14; D01F9/20; D01F9/21; D01F9/22
Claims Analysis
Total Claims: 13
Claim 1
Independent Claim
200 words
A process for producing a carbon fiber which comprises (a) impregnating a water-swollen acrylonitrile fiber containing at least 85 mol % acrylonitrile with 0.05 - 5%, based on the dry weight of the fiber, of at least one compound represented by the following general formula (I) or (II): r.sub.1 -nh.sub.2 (i) ##STR3## wherein R.sub.1 is a hydrocarbon group containing 7 - 16 carbon atoms; R.sub.2, R.sub.3, R.sub.4 and R.sub.5 are each a hydrocarbon group containing 1 - 16 carbon atoms, with at least one of R.sub.2, R.sub.3, R.sub.4 and R.sub.5 being a hydrocarbon group containing 7 - 16 carbon atoms; and X is a monovalent anion; (b) heat treating the fiber at a temperature of at least 150° C. for 0.1 second to 30 minutes so as to render the fiber to have 20 - 80 weight percent undissolved matter upon being immersed in a 60% aqueous sodium thiocyanate solution at 80° C. for 20 minutes; (c) thermally stabilizing the fiber by heating under tension in an oxidizing atmosphere at a temperature of from 150° C. to 400° C. and thereafter (d) carbonizing or carbonizing and then graphitizing under tension in a non-oxidizing atmosphere at a temperature above 800° C.
Claim 2
Dependent Claim
200 words
A process for producing a carbon fiber which comprises (a) impregnating a water-swollen acrylonitrile fiber containing at least 85 mol % acrylonitrile with 0.05 - 5%, based on the dry weight of the fiber, of at least one compound represented by the following general formula (I) or (II): r.sub.1 -nh.sub.2 (i) ##STR3## wherein R.sub.1 is a hydrocarbon group containing 7 - 16 carbon atoms; R.sub.2, R.sub.3, R.sub.4 and R.sub.5 are each a hydrocarbon group containing 1 - 16 carbon atoms, with at least one of R.sub.2, R.sub.3, R.sub.4 and R.sub.5 being a hydrocarbon group containing 7 - 16 carbon atoms; and X is a monovalent anion; (b) heat treating the fiber at a temperature of at least 150° C. for 0.1 second to 30 minutes so as to render the fiber to have 20 - 80 weight percent undissolved matter upon being immersed in a 60% aqueous sodium thiocyanate solution at 80° C. for 20 minutes; (c) thermally stabilizing the fiber by heating under tension in an oxidizing atmosphere at a temperature of from 150° C. to 400° C. and thereafter (d) carbonizing or carbonizing and then graphitizing under tension in a non-oxidizing atmosphere at a temperature above 800° C.
Claim 3
Dependent Claim
24 words
The process as claimed in claim 1 wherein the fiber is impregnated with 0.1 - 3% of the primary amines and/or quaternary ammonium salts.
Claim 4
Dependent Claim
21 words
The process as claimed in claim 1 wherein the heat treatment temperature in step (b) is 160° C. to 550° C.
Claim 5
Dependent Claim
21 words
The process as claimed in claim 1 wherein the heat treating time in step (b) is 0.2 second to 20 minutes.
Claim 6
Dependent Claim
31 words
The process as claimed in claim 1 wherein a condition in the temperature-time area shown by slanting lines in FIG. 2 is employed in heat treating the fiber in step (b).
Claim 7
Dependent Claim
24 words
The process as claimed in claim 1 wherein the water content of the acrylonitrile fiber in a water-swollen state is 20 to 200 percent.
Claim 8
Dependent Claim
25 words
The process as claimed in claim 1 wherein the primary amine is a compound selected from the group consisting of nonylamine, dodecylamine, tridecylamine and cetylamine.
Claim 9
Dependent Claim
37 words
The process as claimed in claim 1 wherein the quaternary ammonium salt is a compound selected from the group consisting of decyl trimethylammonium chloride, decyl triethylammonium chloride, undecyl trimethylammonium chloride, dodecyl trimethylammonium chloride and tridecyl trimethylammonium bromide.
Claim 10
Dependent Claim
32 words
The process as claimed in claim 1 wherein the water-swollen acrylonitrile fiber impregnated with at least one compound selected from said primary amines and/or quaternary ammonium salts is dried and then heat-treated.
Claim 11
Dependent Claim
13 words
The process as claimed in claim 1 wherein the oxidizing atmosphere is air.
Claim 12
Dependent Claim
45 words
The process as claimed in claim 1 wherein the thermally stabilized fiber is carbonized in a non-oxidizing atmosphere at a temperature of from 800° C to 2000° C. and then graphitized in a non-oxidizing atmosphere at a temperature of from 2000° C. to 3500° C.
Claim 13
Dependent Claim
13 words
The process as claimed in claim 1 wherein the non-oxidizing atmosphere is nitrogen.
References Cited (Backward Citations)
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1980-05-16 | 1980-11-15 | 1981-05-17 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1984-05-16 | 1984-11-15 | 1985-05-17 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1988-05-16 | 1988-11-15 | 1989-05-17 | $7700.00 | Window Closed / Lapsed |