US3533741A - Process for the production of filamentary carbon - Google Patents

Process for the production of filamentary carbon Download PDF

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Publication number
US3533741A
US3533741A US729927A US3533741DA US3533741A US 3533741 A US3533741 A US 3533741A US 729927 A US729927 A US 729927A US 3533741D A US3533741D A US 3533741DA US 3533741 A US3533741 A US 3533741A
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United States
Prior art keywords
carbon
filamentary
filaments
temperature
filamentary material
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US729927A
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Francis James Higgins
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Akzo Nobel UK PLC
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Courtaulds PLC
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Assigned to COURTAULDS, PLC reassignment COURTAULDS, PLC CHANGE OF NAME (SEE DOCUMENT FOR DETAILS). EFFECTIVE MARCH 1, 1982. Assignors: COURTAULDS, LIMITED
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Classifications

    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/20Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
    • D01F9/24Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F9/26Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds from polyesters
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/16Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from products of vegetable origin or derivatives thereof, e.g. from cellulose acetate
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/20Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
    • D01F9/21Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F9/22Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/20Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
    • D01F9/24Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F9/28Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds from polyamides
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/32Apparatus therefor
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10STECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S264/00Plastic and nonmetallic article shaping or treating: processes
    • Y10S264/19Inorganic fiber

Definitions

  • This invention relates to a process for the production of filamentary carbon and in particular to a process for producing filamentary carbon which enables it to be handled during the production process and thereafter-with minimal damage.
  • Carbon filaments may be produced by subjecting organic filamentary material to a series of treatments under specific conditions of temperature and surrounding atmosphere.
  • the organic filamentary material may be subjected to heating at a temperature which may be in the range from 200 to 300 C. in an atmosphere of air, air enriched with oxygen or nitrogen.
  • the so-treated filamentary material may then be heated at a temperature in excess of 1000 C. in an inert atmosphere to produce carbon filaments which may be graphitised at a temperature in excess of 2000 C. also in an inert atmosphere.
  • Carbon filaments and especially graphite filaments have considerable tensile strength and elastic modulus values but at all stages in their production and especially in the early stages they require to be handled with care to avoid breakage of individual filaments in a bundle.
  • a process for the production of filamentary carbon comprises heating organic filamentary material at a temperature in the range from about 200 to 300 C. in an atmosphere of air, air enriched with oxygen or nitrogen, wrapping the so-treated filamentary material in a cloth made from carbon filaments or fibres, and heating the package so obtained at a temperature in excess of 1000 C. in an inert atmosphere to carbonise the filamentary material.
  • the first stage results in a filamentary product which can be bent during handling, and if a bent filamentary product is subsequently carbonised it exhibits corresponding kinks which are substantially impossible to remove. It is found that wrapping a bundle of filamentary material treated in the first stage of the process in carbon cloth protects the first stage filamentary material from bending, and the carbonised filaments produced therefrom do not show permanent kinks.
  • the second stage of treatment carried out while the filamentary material is wrapped in carbon cloth, it is heated in an inert atmosphere to a temperature in excess of 1000 C., and becomes carbonised.
  • Such carbonised filaments may be satisfactory for many purposes, but in order to develop the most valuable properties it may be desired to graphitise them.
  • This may be achieved by transferring the package to a high temperature furnace in which it is heated to a temperature in excess of 2000" C,, preferably in excess of 2500 C., in an inert atmosphere.
  • the package, after carbonisation or after graphitisation may be used entirely for despatching the filaments, when it may be handled with minimal damage to the filaments.
  • Carbon cloth may be made from continuous filaments or staple carbon fibres which may be produced in a manner similar to the filamentary carbon produced by the process of this invention, or by any other suitable method.
  • the cloths may be made of carbonised filaments or fibres or they may have been graphitised. Carbonised cloths may exhibit weight loss and dimensional change when heated above 2000 C. but such changes do not interfere with the process of the invention, and they are irreversible. Accordingly after the first treatment of the cloth in a graphitisation stage no further changes will occur on subsequent heating above 2000" C.
  • the filamentary carbon produced in the process of the invention may be made, for example, from cellulosic, polyamide or polyester materials or from substantially any other organic filamentary material, the structure of which includes a carbon to carbon backbone. It is however, preferred to use filamentary material consisting wholly and mainly of polyacrylonitrile.
  • the carbon cloth may have been produced in a similar manner from any of the above mentioned organic filamentary materials.
  • the invention is particularly suitable for the production of staple carbon filaments, for example those having a staple length up to about 10 feet.
  • a process for the production of filamentary carbon which comprises heating organic filamentary material at a temperature in the range from about 200 to 300 C. in an atmosphere of air, air enriched with oxygen, or nitrogen, wrapping the so-treated filamentary material in a cloth made from carbon filaments or fibres and heating the package so obtained at a temperature in excess of 1000 C. in an inert atmosphere to carbonise the filamentary material.
  • organic filamentary material is made from cellulosic, polyamide or polyester material.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Inorganic Fibers (AREA)

Description

United States Patent Oflice Patented Oct. 13, 1970 3,533,741 PROCESS FOR THE PRODUCTION OF FILAMENTARY CARBON Francis James Higgins, Kenilworth, Warwickshire, England, assignor to Courtaulds Limited, London, England, a British company No Drawing. Filed May 17, 1968, Ser. No. 729,927 Claims priority, application Great Britain, May 26, 1967, 24,605/ 67 Int. Cl. C01b 31/07 US. Cl. 23-2091 8 Claims ABSTRACT OF THE DISCLOSURE A process for the production of filamentary carbon which comprises heating organic filamentary material, for example of cellulosic, polyamide, polyester or polyacrylonitrile material, at a temperature inthe range from about 200 to 300 C. in an atmosphere of air, air enriched with oxygen, or nitrogen, wrapping the so-treated filamentary material in a cloth made from carbon filaments or fibres and heating the package so obtained at a temperature in excess of 1000 C. in an inert atmosphere to carbonise the filamentary material. The package of carbonised filamentary material wrapped in carbon cloth may be subjected to a further heat treatment at a temperature in excess of 2000 C. in an inert atmosphere.
This invention relates to a process for the production of filamentary carbon and in particular to a process for producing filamentary carbon which enables it to be handled during the production process and thereafter-with minimal damage.
Carbon filaments may be produced by subjecting organic filamentary material to a series of treatments under specific conditions of temperature and surrounding atmosphere. Thus, in a first stage, the organic filamentary material may be subjected to heating at a temperature which may be in the range from 200 to 300 C. in an atmosphere of air, air enriched with oxygen or nitrogen. The so-treated filamentary material may then be heated at a temperature in excess of 1000 C. in an inert atmosphere to produce carbon filaments which may be graphitised at a temperature in excess of 2000 C. also in an inert atmosphere. Carbon filaments and especially graphite filaments have considerable tensile strength and elastic modulus values but at all stages in their production and especially in the early stages they require to be handled with care to avoid breakage of individual filaments in a bundle.
According to the invention a process for the production of filamentary carbon comprises heating organic filamentary material at a temperature in the range from about 200 to 300 C. in an atmosphere of air, air enriched with oxygen or nitrogen, wrapping the so-treated filamentary material in a cloth made from carbon filaments or fibres, and heating the package so obtained at a temperature in excess of 1000 C. in an inert atmosphere to carbonise the filamentary material.
During the process of manufacture of filamentary carbon the first stage results in a filamentary product which can be bent during handling, and if a bent filamentary product is subsequently carbonised it exhibits corresponding kinks which are substantially impossible to remove. It is found that wrapping a bundle of filamentary material treated in the first stage of the process in carbon cloth protects the first stage filamentary material from bending, and the carbonised filaments produced therefrom do not show permanent kinks. In the second stage of treatment, carried out while the filamentary material is wrapped in carbon cloth, it is heated in an inert atmosphere to a temperature in excess of 1000 C., and becomes carbonised. Such carbonised filaments may be satisfactory for many purposes, but in order to develop the most valuable properties it may be desired to graphitise them. This may be achieved by transferring the package to a high temperature furnace in which it is heated to a temperature in excess of 2000" C,, preferably in excess of 2500 C., in an inert atmosphere. The package, after carbonisation or after graphitisation may be used entirely for despatching the filaments, when it may be handled with minimal damage to the filaments.
Carbon cloth may be made from continuous filaments or staple carbon fibres which may be produced in a manner similar to the filamentary carbon produced by the process of this invention, or by any other suitable method. The cloths may be made of carbonised filaments or fibres or they may have been graphitised. Carbonised cloths may exhibit weight loss and dimensional change when heated above 2000 C. but such changes do not interfere with the process of the invention, and they are irreversible. Accordingly after the first treatment of the cloth in a graphitisation stage no further changes will occur on subsequent heating above 2000" C.
The filamentary carbon produced in the process of the invention may be made, for example, from cellulosic, polyamide or polyester materials or from substantially any other organic filamentary material, the structure of which includes a carbon to carbon backbone. It is however, preferred to use filamentary material consisting wholly and mainly of polyacrylonitrile. The carbon cloth may have been produced in a similar manner from any of the above mentioned organic filamentary materials. The invention is particularly suitable for the production of staple carbon filaments, for example those having a staple length up to about 10 feet.
What is claimed is:
1. A process for the production of filamentary carbon which comprises heating organic filamentary material at a temperature in the range from about 200 to 300 C. in an atmosphere of air, air enriched with oxygen, or nitrogen, wrapping the so-treated filamentary material in a cloth made from carbon filaments or fibres and heating the package so obtained at a temperature in excess of 1000 C. in an inert atmosphere to carbonise the filamentary material.
2. The process as claimed in claim 1 in which the organic filamentary material is made from cellulosic, polyamide or polyester material.
3. The process as claimed in claim 1 in which the organic filamentary material comprises filaments consisting wholly or mainly of polyacrylonitrile.
4. The process as claimed in claim 1 in which the cloth made from carbon filaments or fibres is produced from filaments or fibres of cellulosic, polyamide, polyester or polyacrylic materials.
5. The process as claimed in claim 1 in which the cloth made from carbon filaments or fibres has been produced by heating organic filamentary material at a temperature in the range from about 200 to 300 C. in an atmosphere of air, air enriched with oxygen or nitrogen and subse- 3 quently heating the product at a temperature in excess of 1000 C. to carbonise the filaments or fibres.
6. The process as claimed in claim 1 in which the package of carbonised filamentary material wrapped in carbon cloth is further heated to a temperature in excess of 2000 C. in an inert atmosphere.
7. The process as claimed in claim 6 in which the further heating is carried out at a temperature in excess of 25 00 C. in an inert atmosphere.
8. The process as claimed in claim 1 in which the organic filamentary material is in the form of filaments of staple length up to 10 feet.
References Cited UNITED STATES PATENTS 12/1961 Soltes 23-209.1 X 9/1962 Abbott 252421 11/1966 Tsunoda 23-209.1 3/1967 Davila 23-2092 X 4/1967 Hogg et a1. 23209.1
US. Cl. X.R.
US729927A 1967-05-26 1968-05-17 Process for the production of filamentary carbon Expired - Lifetime US3533741A (en)

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GB24605/67A GB1218180A (en) 1967-05-26 1967-05-26 Carbon filaments

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3716332A (en) * 1970-07-27 1973-02-13 Ducommun Inc Carbonization of wool
US3888958A (en) * 1970-03-21 1975-06-10 Bergwerksverband Gmbh Process for making shaped pieces from low temperature coke of low bulk weight
US4351816A (en) * 1980-12-17 1982-09-28 Union Carbide Corporation Method for producing a mesophase pitch derived carbon yarn and fiber
US4571317A (en) * 1976-02-25 1986-02-18 United Technologies Corporation Process for producing binderless carbon or graphite articles
US4856179A (en) * 1983-04-21 1989-08-15 Hoechst Celanese Corp. Method of making an electrical device made of partially pyrolyzed polymer

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3619033A1 (en) * 1986-06-06 1987-12-10 Bayer Ag METHOD FOR PRODUCING FLOCK

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3011981A (en) * 1958-04-21 1961-12-05 Soltes William Timot Electrically conducting fibrous carbon
US3053775A (en) * 1959-11-12 1962-09-11 Carbon Wool Corp Method for carbonizing fibers
US3285696A (en) * 1960-08-25 1966-11-15 Tokai Denkyoku Seizo Kabushiki Method for the preparation of flexible carbon fibre
US3308943A (en) * 1963-08-05 1967-03-14 Davila Eugene Method of packaging purified graphite and the package formed thereby
US3313596A (en) * 1963-07-26 1967-04-11 Great Lakes Carbon Corp Carbonization of fibrous rayon

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3011981A (en) * 1958-04-21 1961-12-05 Soltes William Timot Electrically conducting fibrous carbon
US3053775A (en) * 1959-11-12 1962-09-11 Carbon Wool Corp Method for carbonizing fibers
US3285696A (en) * 1960-08-25 1966-11-15 Tokai Denkyoku Seizo Kabushiki Method for the preparation of flexible carbon fibre
US3313596A (en) * 1963-07-26 1967-04-11 Great Lakes Carbon Corp Carbonization of fibrous rayon
US3308943A (en) * 1963-08-05 1967-03-14 Davila Eugene Method of packaging purified graphite and the package formed thereby

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3888958A (en) * 1970-03-21 1975-06-10 Bergwerksverband Gmbh Process for making shaped pieces from low temperature coke of low bulk weight
US3716332A (en) * 1970-07-27 1973-02-13 Ducommun Inc Carbonization of wool
US4571317A (en) * 1976-02-25 1986-02-18 United Technologies Corporation Process for producing binderless carbon or graphite articles
US4351816A (en) * 1980-12-17 1982-09-28 Union Carbide Corporation Method for producing a mesophase pitch derived carbon yarn and fiber
US4856179A (en) * 1983-04-21 1989-08-15 Hoechst Celanese Corp. Method of making an electrical device made of partially pyrolyzed polymer

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Publication number Publication date
GB1218180A (en) 1971-01-06

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Effective date: 19820520