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US3723157A Expired / Lapsed US ⏱️ 0.0 years remaining

Production of resin impregnated fibrous graphite ribbons

Assignee: Celanese Corp
•
Filing: 1969-11-07
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Granted: 1973-03-27
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Expires: 1989-11-07
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Abstract

Abstract A process is provided wherein resin impregnated graphite ribbons may be efficiently produced which may be used in the manufacture of fiber reinforced composite structures. A plurality of multifilament bundles of a fibrous material capable of undergoing graphitization are continuously passed through a graphitization zone from which they are continuously conveyed to and through a coating zone in which they are impregnated with a thermosetting resin. Throughout the continuous process of the invention, the multifilament bundles are provided in an essentially parallel relationship in the form of a ribbon and are continuously passed in the direction of their length. The ribbon product of the invention is particularly suited for use in the formation of strong lightweight composites by filament winding, or other composite forming techniques.

Inventors

  • 👤 M Druin

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-31 07:26
CPC Classifications
D; D01; D01F; D01F11/00; D01F11/10; D01F11/14; B; B29; B29C; B29C70/00; B29C70/04; B29K; B29K2307/00; Y; Y10; Y10S; Y10S264/00; Y10S264/19

Claims Analysis

Total Claims: 23
Claim 1
Independent Claim 37 words
A process according to claim 1 wherein said plurality of multifilament bundles of a fibrous material capable of undergoing graphitization contain at least about 90 percent carbon by weight and exhibit an essentially amorphous X-ray diffraction pattern.
Claim 2
Dependent Claim 62 words
A process according to claim 1 wherein said multifilament bundles of a fibrous material capable of undergoing graphitization are derived from a fibrous material selected from the group consisting of an acrylonitrile Homopolymer and acrylonitrile copolymers which contain at least about 85 mol percent of acrylonitrile units and up to about 15 mol percent of one or more monovinyl units copolymerized therewith.
Claim 3
Dependent Claim 32 words
A process according to claim 1 wherein said multifilament bundles of fibrous material capable of undergoing graphitization are passed through said graphitization zone at a temperature of about 2,400* to 3,100* C.
Claim 4
Dependent Claim 18 words
A process according to claim 1 wherein said multifilament bundles are continuous multifilament yarns having essentially no twist.
Claim 5
Dependent Claim 23 words
A process according to claim 1 wherein said multifilament bundles are continuous multifilament yarns having a twist of about 0.1 to 5 tpi.
Claim 6
Dependent Claim 14 words
A process according to claim 1 wherein said thermosetting resin is an epoxy resin.
Claim 7
Dependent Claim 280 words
A process for the continuous production of a resin impregnated graphite ribbon for use in the manufacture of fiber reinforced composites comprising: a. continuously passing a plurality of substantially uniform multifilament bundles of a fibrous material capable of undergoing graphitization while in an adjoining essentially parallel relationship and in the form of a ribbon having a thickness corresponding to that of a single multifilament bundle with each bundle being under a substantially uniform tension through a graphitization zone at a temperature of about 2,000* to 3,100* C. and containing an inert atmosphere for a residence time sufficient to substantially convert said bundles to graphitic carbon while retaining their original fibrous configuration essentially intact, b. continuously feeding the resulting bundles of graphitic carbon from said graphitization zone to a coating zone, c. continuously passing said bundles of graphitic carbon through said coating zone while retaining said adjoining essentially parallel relationship of said bundles and said ribbon configuration having a thickness corresponding to that of a single multifilament bundle with each bundle being under a substantially uniform tension wherein said bundles are coated with a solventless system comprising an A-stage thermosetting resin, d. continuously feeding said coated ribbon from said coating zone to a heating zone while retaining said adjoining essentially parallel relationship of said bundles within said ribbon, e. continuously passing said coated ribbon through said heating zone wherein said A-stage thermosetting resin present on said ribbon is converted to B-stage thermosetting resin while retaining said adjoining essentially parallel relationship of said bundles within said ribbon, and f. continuously withdrawing said coated graphite ribbon from said heating zone while said thermosetting resin present on said ribbon is a B-stage thermosetting resin.
Claim 8
Dependent Claim 37 words
A process according to claim 8 wherein said plurality of multifilament bundles of a fibrous material capable of undergoing graphitization contain at least about 90 percent carbon by weight and exhibit an essentially amorphous X-ray diffraction pattern.
Claim 9
Dependent Claim 62 words
A process according to claim 9 wherein said multifilament bundles of a fibrous material capable of undergoing graphitization are derived from a fibrous material selected from the group consisting of an acrylonitrile homopolymer and acrylonitrile copolymers which contain at least about 85 mol percent of acrylonitrile units and up to about 15 mol percent of one or more monovinyl units copolymerized therewith.
Claim 10
Dependent Claim 32 words
A process according to claim 8 wherein said multifilament bundles of fibrous material capable of undergoing graphitization are passed through said graphitization zone at a temperature of about 2,400* to 3,100* C.
Claim 11
Dependent Claim 18 words
A process according to claim 9 wherein said multifilament bundles are continuous multifilament yarns having essentially no twist.
Claim 12
Dependent Claim 23 words
A process according to claim 9 wherein said multifilament bundles are continuous multifilament yarns having a twIst of about 0.3 to 1.0 tpi.
Claim 13
Dependent Claim 28 words
A process according to claim 9 wherein said solventless system comprising an A-stage thermosetting resin comprises an A-stage epoxy resin and a curing agent for said epoxy resin.
Claim 14
Dependent Claim 19 words
A process according to claim 14 wherein said epoxy resin is a condensation product of bisphenol A and epichlorohydrin.
Claim 15
Dependent Claim 336 words
A process for the continuous production of a resin impregnated graphite ribbon for use in the manufacture of fiber reinforced composites comprising: a. continuously passing while in an adjoining essentially parallel relationship and in the form of a ribbon having a thickness corresponding to that of a single multifilament bundle a plurality of substantially uniform multifilament bundles of a stabilized acrylic fibrous material with each bundle being under a substantially uniform tension having a temperature within the range of about 20* to 500* C. which is non-burning when subjected to an ordinary match flame and derived from an acrylic fibrous material selected from the group consisting of an acrylonitrile homopolymer and acrylonitrile copolymers which contain at least about 85 mol percent of one or more monovinyl units copolymerized therewith through a carbonization heating zone provided with an inert atmosphere in which said bundles of stabilized acrylic fibrous material are raised within a period of about 3 seconds to about 10 minutes to a temperature within the range of about 900* C. to about 1,600* C. wherein a carbonized ribbon is formed, b. continuously passing said carbonized ribbon through a graphitization heating zone provided with an inert atmosphere while retaining said adjoining parallel relationship of said bundles within said ribbon with each bundle being under a substantially uniform tension in which said carbonized ribbon is heated at a temperature within the range of about 2,000* to 3,100* C. for a residence time sufficient to substantially convert said bundles to graphitic carbon, c. continuously feeding the resulting bundles of graphitic carbon from said graphitization heating zone to a coating zone, d. continuously passing said bundles of graphitic carbon through said coating zone while retaining said adjoining essentially parallel relationship of said bundles and said ribbon configuration having a thickness corresponding to that of a single multifilament bundle with each bundle being under a substantially uniform tension wherein said ribbon is impregnated with a thermosetting resin, and e. withdrawing the resulting resin impregnated graphite ribbon from said coating zone.
Claim 16
Dependent Claim 18 words
A process according to claim 16 wherein said multifilament bundles are continuous multifilament yarns having essentially no twist.
Claim 17
Dependent Claim 23 words
A process according to claim 16 wherein said multifilament bundles are continuous multifilament yarns having a twist of about 0.1 to 5 tpi.
Claim 18
Dependent Claim 21 words
A process according to claim 16 wherein said multifilament bundles of stabilized acrylic fibrous material are derived from an acrylonitrile homopolymer.
Claim 19
Dependent Claim 39 words
A process according to claim 16 wherein said carbonized ribbon is continuously passed through a graphitization heating zone at about 2,400* to 3,100* C. for a residence time sufficient to convert said bundles forming the same to graphitic carbon.
Claim 20
Dependent Claim 428 words
A process for the continuous production of a resin impregnated graphite ribbon for use in the manufacture of fiber reinforced composites comprising: a. continuously passing while in an adjoining essentially parallel relationship and in the form of a ribbon having a thickness corresponding to that of a single multifilament bundle a plurality of substantially uniform multifilament bundles of a stabilized acrylic fibrous material with each bundle being under a substantially uniform tension having a temperature within the range of about 20* to 500* C. Which is non-burning when subjected to an ordinary match flame and derived from an acrylic fibrous material selected from the group consisting of an acrylonitrile homopolymer and acrylonitrile copolymers which contain at least about 85 mol percent of acrylonitrile units and up to about 15 mol percent of one or more monovinyl units copolymerized therewith through a carbonization heating zone provided with an inert atmosphere in which said bundles of stabilized acrylic fibrous material are raised within a period of about 3 seconds to about 10 minutes to a temperature within the range of about 900* C. to about 1,600* C. wherein a carbonized ribbon is formed, b. continuously passing said carbonized ribbon through a graphitization heating zone provided with an inert atmosphere while retaining said adjoining parallel relationship of said bundles within said ribbon with each bundle being under a substantially uniform tension in which said carbonized ribbon is heated at a temperature within the range of about 2,400* to 3,100* C. for a residence time sufficient to substantially convert said bundles to graphitic carbon, c. continuously feeding the resulting bundles of graphitic carbon from said graphitization heating zone to a coating zone, d. continuously passing said bundles of graphitic carbon through said coating zone while retaining said adjoining essentially parallel relationship of said bundles and said ribbon configuration having a thickness corresponding to that of a single multifilament bundle with each bundle being under a substantially uniform tension wherein said ribbon is coated with a solventless system comprising an A-stage thermosetting resin, e. continuously feeding said coated ribbon from said coating zone to a heating zone while retaining said adjoining essentially parallel relationship of said bundles within said ribbon, f. continuously passing said coating ribbon through said heating zone wherein said A-stage thermosetting resin present on said ribbon is converted to B-stage thermosetting resin while retaining said adjoining essentially parallel relationship of said bundles within said ribbon, and g. continuously withdrawing said coated graphite ribbon from said heating zone while said thermosetting resin present on said ribbon is a B-stage thermosetting resin.
Claim 21
Dependent Claim 18 words
A process according to claim 21 wherein said stabilized acrylic fibrous material is derived from an acrylonitrile homopolymer.
Claim 22
Dependent Claim 28 words
A process according to claim 21 wherein said solventless system comprising an A-stage thermosetting resin comprises an A-stage epoxy resin and a curing agent for said epoxy resin.
Claim 23
Dependent Claim 20 words
A process according to claim 22 wherein said A-stage epoxy resin is a condensation product of bisphenol A and epichlorohydrin.

References Cited (Backward Citations)

US3235323A Cited
US3108018A Cited
US3214324A Cited
US3323941A Cited
US3367812A Cited
US3412062A Cited
US3552923A Cited
US3471322A Cited
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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) 1976-03-26 1976-09-25 1977-03-27 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1980-03-26 1980-09-25 1981-03-27 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1984-03-26 1984-09-25 1985-03-27 $7700.00 Window Closed / Lapsed

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