US3657082A - Treatment of fibrous materials - Google Patents

Treatment of fibrous materials Download PDF

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Publication number
US3657082A
US3657082A US787558A US3657082DA US3657082A US 3657082 A US3657082 A US 3657082A US 787558 A US787558 A US 787558A US 3657082D A US3657082D A US 3657082DA US 3657082 A US3657082 A US 3657082A
Authority
US
United States
Prior art keywords
carbon fibers
treatment
fibers
fibrous materials
order
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
US787558A
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English (en)
Inventor
Henry Wells
William James Colclough
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
UK Atomic Energy Authority
Original Assignee
UK Atomic Energy Authority
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by UK Atomic Energy Authority filed Critical UK Atomic Energy Authority
Application granted granted Critical
Publication of US3657082A publication Critical patent/US3657082A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • D01F11/00Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/10Chemical after-treatment of artificial filaments or the like during manufacture of carbon
    • D01F11/12Chemical after-treatment of artificial filaments or the like during manufacture of carbon with inorganic substances ; Intercalation
    • D01F11/121Halogen, halogenic acids or their salts
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/06Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
    • 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
    • D01F11/00Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/10Chemical after-treatment of artificial filaments or the like during manufacture of carbon
    • D01F11/12Chemical after-treatment of artificial filaments or the like during manufacture of carbon with inorganic substances ; Intercalation
    • D01F11/122Oxygen, oxygen-generating compounds
    • 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
    • D01F11/00Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/10Chemical after-treatment of artificial filaments or the like during manufacture of carbon
    • D01F11/16Chemical after-treatment of artificial filaments or the like during manufacture of carbon by physicochemical methods

Definitions

  • ABSTRACT In order to improve the surface characteristics of carbon fibers, e.g. their adhesion to a resin matrix, they are treated by immersion in an aqueous oxidising agent, e.g. a hypochlorite.
  • an aqueous oxidising agent e.g. a hypochlorite.
  • the present invention relates to the treatment of fibrous material and more particularly to the treatment of carbon or graphite fibers.
  • carbon fibers may be made by taking fibers of an organic material, such as polyacrylonitrile, and subjecting them to high temperatures. Very often the heat treatment is effected in several steps in different atmospheres and the final temperature may be in the range l,500 to 2,600 C so that the fibers may be at least partially graphitized.
  • the term carbon fibers is used inclusively hereinafter.
  • These carbon fibers may have many uses, but one use is to reinforce a matrix, more particularly a matrix of plastics material, in order to produce a reinforced or laminated material in rather a similar way to that in which glass fiber is used to reinforce plastics material.
  • One difficulty that has been found is that poor adhesion may occur between the carbon fibers and the matrix which leads to reduced mechanical strength of the composite.
  • carbon fibers are surface treated by immersion in an aqueous oxidizing agent.
  • the aqueous oxidizing agent is a hypochlorite solution containing available chlorine.
  • hypochlorite solution One very desirable way of obtaining the hypochlorite solution is to generate it by electrolysis of a chloride solution using the carbon fibers as one electrode.
  • the fibers were then placed in a bath containing 5 percent by weight of sodium chloride and 0.25 percent by weight of sodium hydroxide in water.
  • the fibers were connected to the anode and were at the same time subjected to ultrasonic agitation at 13 kHz.
  • a copper cathode was also inserted in the bath and current was passed between the cathode and anode at a current density of 2 amps per square inch of carbon fiber surface and at a voltage of 12 volts. After treatments for 5 minutes in this bath (which generated free chlorine) the carbon fibers were removed, rinsed in water and dried.
  • the carbon fibers were then incorporated into an epoxide resin matrix in the proportion of 55 percent by volume and the resulting composite was tested in a 3 point bend test on a 1 inch beam.
  • the interlaminar shear strength of the composite was 6,275 p.s.i. which compares with a strength of 2,000 to 3,000 p.s.i. for a similar laminate made from untreated fibers.
  • a method of surface treating carbon fibers comprising generating a hypochlorite solution containing available chlorine by electrolysis of an aqueous chloride solution using carbon fibers as the anode.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
  • Electrodes For Compound Or Non-Metal Manufacture (AREA)
  • Inorganic Fibers (AREA)
US787558A 1968-01-03 1968-12-27 Treatment of fibrous materials Expired - Lifetime US3657082A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB52568 1968-01-03

Publications (1)

Publication Number Publication Date
US3657082A true US3657082A (en) 1972-04-18

Family

ID=9705900

Family Applications (1)

Application Number Title Priority Date Filing Date
US787558A Expired - Lifetime US3657082A (en) 1968-01-03 1968-12-27 Treatment of fibrous materials

Country Status (5)

Country Link
US (1) US3657082A (fr)
CH (1) CH511768A (fr)
DE (1) DE1817581B2 (fr)
FR (1) FR1600656A (fr)
GB (1) GB1257022A (fr)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3859187A (en) * 1972-09-25 1975-01-07 Celanese Corp Electrolytic process for the surface modification of high modulus carbon fibers
US4472541A (en) * 1982-10-01 1984-09-18 The Bendix Corporation Secondary matrix reinforcement using carbon microfibers
US4637925A (en) * 1984-06-22 1987-01-20 Toray Industries, Inc. Ultrahigh strength carbon fibers
US4927462A (en) * 1988-12-23 1990-05-22 Associated Universities, Inc. Oxidation of carbon fiber surfaces for use as reinforcement in high-temperature cementitious material systems
US5017274A (en) * 1987-02-25 1991-05-21 Aquanautics Corporation Method and systems for extracting oxygen employing electrocatalysts
US5271917A (en) * 1989-09-15 1993-12-21 The United States Of America As Represented By The Secretary Of The Air Force Activation of carbon fiber surfaces by means of catalytic oxidation
US20090092831A1 (en) * 2006-04-28 2009-04-09 Toho Tenax Europe Gmbh Carbon Fiber
CN112522729A (zh) * 2020-12-01 2021-03-19 宁波八益集团有限公司 一种次氯酸生产系统及其高稳定性次氯酸生产方法

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3671411A (en) * 1970-03-03 1972-06-20 Us Air Force Treatment of carbon or graphite fibers and yarns for use in fiber reinforced composites
IT1210610B (it) * 1981-08-07 1989-09-14 Sorin Biomedica Spa Procedimento per l attivazione di una punta di pirocarbone per elettrodi di stimolatori cardiaci
US4411880A (en) 1982-05-17 1983-10-25 Celanese Corporation Process for disposing of carbon fibers

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1062431A (en) * 1911-09-25 1913-05-20 Jean Billiter Method of purifying carbon for carbon filaments.
US2439442A (en) * 1943-02-06 1948-04-13 Cabot Godfrey L Inc Process of making hydrophilic carbon black
US2702260A (en) * 1949-11-17 1955-02-15 Massa Frank Apparatus and method for the generation and use of sound waves in liquids for the high-speed wetting of substances immersed in the liquid
US3323869A (en) * 1963-12-19 1967-06-06 Dow Chemical Co Process for producing expanded graphite
US3441488A (en) * 1964-09-03 1969-04-29 Atomic Energy Commission Electrolytic desalination of saline water by a differential redox method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1062431A (en) * 1911-09-25 1913-05-20 Jean Billiter Method of purifying carbon for carbon filaments.
US2439442A (en) * 1943-02-06 1948-04-13 Cabot Godfrey L Inc Process of making hydrophilic carbon black
US2702260A (en) * 1949-11-17 1955-02-15 Massa Frank Apparatus and method for the generation and use of sound waves in liquids for the high-speed wetting of substances immersed in the liquid
US3323869A (en) * 1963-12-19 1967-06-06 Dow Chemical Co Process for producing expanded graphite
US3441488A (en) * 1964-09-03 1969-04-29 Atomic Energy Commission Electrolytic desalination of saline water by a differential redox method

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3859187A (en) * 1972-09-25 1975-01-07 Celanese Corp Electrolytic process for the surface modification of high modulus carbon fibers
US4472541A (en) * 1982-10-01 1984-09-18 The Bendix Corporation Secondary matrix reinforcement using carbon microfibers
US4637925A (en) * 1984-06-22 1987-01-20 Toray Industries, Inc. Ultrahigh strength carbon fibers
USRE33537E (en) * 1984-06-22 1991-02-12 Toray Industries, Inc. Ultrahigh strength carbon fibers
US5017274A (en) * 1987-02-25 1991-05-21 Aquanautics Corporation Method and systems for extracting oxygen employing electrocatalysts
US4927462A (en) * 1988-12-23 1990-05-22 Associated Universities, Inc. Oxidation of carbon fiber surfaces for use as reinforcement in high-temperature cementitious material systems
US5271917A (en) * 1989-09-15 1993-12-21 The United States Of America As Represented By The Secretary Of The Air Force Activation of carbon fiber surfaces by means of catalytic oxidation
US20090092831A1 (en) * 2006-04-28 2009-04-09 Toho Tenax Europe Gmbh Carbon Fiber
US8834997B2 (en) * 2006-04-28 2014-09-16 Toho Tenax Europe Gmbh Carbon fiber
CN112522729A (zh) * 2020-12-01 2021-03-19 宁波八益集团有限公司 一种次氯酸生产系统及其高稳定性次氯酸生产方法

Also Published As

Publication number Publication date
DE1817581B2 (de) 1975-10-23
CH511768A (de) 1971-08-31
DE1817581A1 (de) 1969-10-16
FR1600656A (fr) 1970-07-27
GB1257022A (fr) 1971-12-15

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