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US3923950A Expired / Lapsed US ⏱️ 0.0 years remaining

Production of stabilized acrylic fibers and films

Assignee: Celanese Corp
•
Filing: 1971-11-18
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Granted: 1975-12-02
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Expires: 1991-11-18
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Abstract

Abstract An improved process is provided for the production of stabilized acrylic fibers and films. An organic antioxidant is incorporated in a solution of an acrylic polymer prior to forming an acrylic fibrous material or film from the same, and the resulting acrylic fibrous material or film having a minor quantity of the organic antioxidant incorporated therein is heated in an oxygencontaining atmosphere until a stabilized fibrous material or film is formed. The organic antioxidant advantageously serves to moderate the oxidative portion of the stabilization reaction and enables the cyclization portion thereof to proceed in the absence of substantial polymer chain degradation. The resulting stabilized fibrous material or film is flexible and non-burning, and may be utilized as a fire resistant fiber, fabric or film, or optionally carbonized or carbonized and graphitized to form a carbonaceous fibrous material or film.

Inventors

  • 👤 Klaus Hannes Gump
  • 👤 Dagobert Englebert Stuetz

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-26 03:57
CPC Classifications
D; D01; D01F; D01F1/00; D01F1/02; D01F1/10; D01F6/00; D01F6/02; D01F6/18; D01F9/00; D01F9/08; D01F9/12; D01F9/14; D01F9/20; D01F9/21; D01F9/22; D01F9/225; D06; D06M; D06M11/00; D06M11/32; D06M11/34; Y; Y10; Y10S; Y10S264/00; Y10S264/19

Claims Analysis

Total Claims: 14
Claim 1
Independent Claim 279 words
AN IMPROVED PROCESS FOR THE PRODUCTION OF STABILIZED ACRYLIC FIBERS AND FILMS WHICH ARE CAPABLE OF UBDERGOING CARBONIZATION COMPRISING: A. PROVIDING A SOLUTION OF (1) AN ACRYLIC POLYMER SELECTED FROM THE GROUP CONSISTING OF AN ACRYLONITRILE HOMOPOLYLMER AND ACRYLONITRILE COPOLYMERS CONTAINING AT LEAST ABOUT 85 MOL PERCENT OF ACRYLONITRILE UNITS AND UP TO ABOUT 15 MOL PERCENT OF ONE OR MORE MONOVINYL UNITS COPOLYMERIZED THEREWIYH, (2) ABOUT 1 TO 20 PERCENT OF WEIGHT BASED UPON THE WEIGHT OF SAID ACRYLIC POLYMER OF AN ORANIC ANTIOXIDANT HAVING A MELTING POINT OF AT LEAST 200*C. CAPABLE OF MODERATING THE OXIDATIVE CROSS-LINKING REACTION OF ADJOINING ACRYLIC MOLECULES SELECTED FROM THE GROUP CONSISTING OF A NITROGEN-FREE PHENOLIC ANTIOXIDANT, AN AMINOPHENOL ANTIOXIDANT, A NON-PHENOLIC AROMATIC AMINE ANTIOXIDANT, A QUINONE ANTIOXIDANT, A SULFUR-CONTAINING ANTIOXIDANT, AND MIXTURES OF THE FOREGOING, AND (3) A SOLVENT FOR SAID ACRYLIC POLYMER AND SAID ORGANIC ANTIOXIDANT SELECTED FROM THE GROUP CONSISTING OF N, NDIMETHYLFORMAMIDE, N,N-DIMETHYLACETAMIDE, DIMETHYL SULFOXIDE, BUTYROLACTON, AND N-METHYL-2-PYRROLIDINONE, WITH SAID SOLUTION PRIOR TO STEP (B) BEING HEATED FOR INSULFFICIENT DURATION TO ACCOMPLISH A SUBSTANTIAL DEGREE OF CYCLIZATION OF PENDANT NITRILE GROUPS WHTHIN SAID ACRYLIC POLYMER WHILE DISSOLVED IN SAID SOLVENT. B. FORMING FROM SAID SOLUTION BY EXTRUSION THROUGH A SHAPED ORIFICE AN ACRYLIC FIBROUS MATERIAL OR FILM HAVING INCORPORATED THEREIN ABOUT 1 TO 10 PERCENT BY WEIGHT BASED UPON THE WEIGHT OF SAID ACRYLIC POLYMER OF SAID ORGANIC ANTIOXIDANT, AND C. HEATING SAID RESULTING ACRYLIC FIBROUS MATERIAL OR FILM IN AN OXYGEN-CONTANING ATMOSPHERE AT A TEMPERATURE OF ABOUT 200* TO 360*C. UNTIL A STABILIZED FIBROUS MATERIAL OF FILM IS FORMED WHICH RETAINS ITS ORGINAL CONFIGURATION SUBSTANTIALLY INTACT AND WHICH IS NON-BURNING WHEN SUBJECTED TO AN ORDINARY MATCH FLAME.
Claim 2
Dependent Claim 279 words
AN IMPROVED PROCESS FOR THE PRODUCTION OF STABILIZED ACRYLIC FIBERS AND FILMS WHICH ARE CAPABLE OF UBDERGOING CARBONIZATION COMPRISING: A. PROVIDING A SOLUTION OF (1) AN ACRYLIC POLYMER SELECTED FROM THE GROUP CONSISTING OF AN ACRYLONITRILE HOMOPOLYLMER AND ACRYLONITRILE COPOLYMERS CONTAINING AT LEAST ABOUT 85 MOL PERCENT OF ACRYLONITRILE UNITS AND UP TO ABOUT 15 MOL PERCENT OF ONE OR MORE MONOVINYL UNITS COPOLYMERIZED THEREWIYH, (2) ABOUT 1 TO 20 PERCENT OF WEIGHT BASED UPON THE WEIGHT OF SAID ACRYLIC POLYMER OF AN ORANIC ANTIOXIDANT HAVING A MELTING POINT OF AT LEAST 200*C. CAPABLE OF MODERATING THE OXIDATIVE CROSS-LINKING REACTION OF ADJOINING ACRYLIC MOLECULES SELECTED FROM THE GROUP CONSISTING OF A NITROGEN-FREE PHENOLIC ANTIOXIDANT, AN AMINOPHENOL ANTIOXIDANT, A NON-PHENOLIC AROMATIC AMINE ANTIOXIDANT, A QUINONE ANTIOXIDANT, A SULFUR-CONTAINING ANTIOXIDANT, AND MIXTURES OF THE FOREGOING, AND (3) A SOLVENT FOR SAID ACRYLIC POLYMER AND SAID ORGANIC ANTIOXIDANT SELECTED FROM THE GROUP CONSISTING OF N, NDIMETHYLFORMAMIDE, N,N-DIMETHYLACETAMIDE, DIMETHYL SULFOXIDE, BUTYROLACTON, AND N-METHYL-2-PYRROLIDINONE, WITH SAID SOLUTION PRIOR TO STEP (B) BEING HEATED FOR INSULFFICIENT DURATION TO ACCOMPLISH A SUBSTANTIAL DEGREE OF CYCLIZATION OF PENDANT NITRILE GROUPS WHTHIN SAID ACRYLIC POLYMER WHILE DISSOLVED IN SAID SOLVENT. B. FORMING FROM SAID SOLUTION BY EXTRUSION THROUGH A SHAPED ORIFICE AN ACRYLIC FIBROUS MATERIAL OR FILM HAVING INCORPORATED THEREIN ABOUT 1 TO 10 PERCENT BY WEIGHT BASED UPON THE WEIGHT OF SAID ACRYLIC POLYMER OF SAID ORGANIC ANTIOXIDANT, AND C. HEATING SAID RESULTING ACRYLIC FIBROUS MATERIAL OR FILM IN AN OXYGEN-CONTANING ATMOSPHERE AT A TEMPERATURE OF ABOUT 200* TO 360*C. UNTIL A STABILIZED FIBROUS MATERIAL OF FILM IS FORMED WHICH RETAINS ITS ORGINAL CONFIGURATION SUBSTANTIALLY INTACT AND WHICH IS NON-BURNING WHEN SUBJECTED TO AN ORDINARY MATCH FLAME.
Claim 3
Dependent Claim 38 words
An improved process according to claim 1 wherein said resulting acrylic fibrous material or film contains said organic antioxidant in a concentration of about 5 to 10 percent by weight immediately prior to heating in said oxygen-containing atmosphere.
Claim 4
Dependent Claim 16 words
An improved process according to claim 1 wherein said organic antioxidant is a nitrogen-free phenolic antioxidant.
Claim 5
Dependent Claim 15 words
An improved process according to claim 1 wherein said organic antioxidant is an aminophenol antioxidant.
Claim 6
Dependent Claim 17 words
An improved process according to claim 1 wherein said organic antioxidant is a non-phenolic aromatic amine antioxidant.
Claim 7
Dependent Claim 15 words
An improved process according to claim 1 wherein said organic antioxidant is a quinone antioxidant.
Claim 8
Dependent Claim 15 words
An improved process according to claim 1 wherein said organic antioxidant is a sulfur-containing antioxidant.
Claim 9
Dependent Claim 21 words
An improved process according to claim 1 wherein said oxygen-containing atmosphere is provided at a temperature of about 240* to 360*C.
Claim 10
Dependent Claim 245 words
An improved process for the production of stabilized acrylic fibers and films which are capable of undergoing carbonization comprising: a. providing a solution of (1) an acrylic polymer selected from the group consisting of an acrylonitrile homopolymer and acrylonitrile copolymers containing at least about 85 mol percent of acrylonitrile units and up to about 15 mol percent of one or more monovinyl units copolymerized therewith, (2) about 1 to 20 percent by weight based upon the weight of said acrylic polymer of an organic antioxidant selected from the group consisting of tetrachlorohydroquinone, chloranil, chloranilic acid, and mixtures of the foregoing, and (3) a solvent for said acrylic polymer and said organic antioxidant selected from the group consisting of N,N-dimethylformamide, N, N-dimethylacetamide, dimethyl sulfoxide, butyrolactone, and N-methyl-2-pyrrolidinone, with said solution prior to step (b) being heated for insufficient duration to accomplish a substantial degree of cyclization of pendant nitrile groups within said acrylic polymer while dissolved in said solvent, b. extruding said solution through a shaped orifice to form an acrylic fibrous material or film having incorporated therein about 1 to 10 percent by weight based upon the weight of said acrylic polymer of said organic antioxidant, and c. heating said resulting acrylic fibrous material or film in an oxygen-containing atmosphere at a temperature of about 200* to 360*C. until a stabilized fibrous material or fiLm is formed which retains its original configuration essentially intact and which is non-burning when subjected to an ordinary match flame.
Claim 11
Dependent Claim 245 words
An improved process for the production of stabilized acrylic fibers and films which are capable of undergoing carbonization comprising: a. providing a solution of (1) an acrylic polymer selected from the group consisting of an acrylonitrile homopolymer and acrylonitrile copolymers containing at least about 85 mol percent of acrylonitrile units and up to about 15 mol percent of one or more monovinyl units copolymerized therewith, (2) about 1 to 20 percent by weight based upon the weight of said acrylic polymer of an organic antioxidant selected from the group consisting of tetrachlorohydroquinone, chloranil, chloranilic acid, and mixtures of the foregoing, and (3) a solvent for said acrylic polymer and said organic antioxidant selected from the group consisting of N,N-dimethylformamide, N, N-dimethylacetamide, dimethyl sulfoxide, butyrolactone, and N-methyl-2-pyrrolidinone, with said solution prior to step (b) being heated for insufficient duration to accomplish a substantial degree of cyclization of pendant nitrile groups within said acrylic polymer while dissolved in said solvent, b. extruding said solution through a shaped orifice to form an acrylic fibrous material or film having incorporated therein about 1 to 10 percent by weight based upon the weight of said acrylic polymer of said organic antioxidant, and c. heating said resulting acrylic fibrous material or film in an oxygen-containing atmosphere at a temperature of about 200* to 360*C. until a stabilized fibrous material or fiLm is formed which retains its original configuration essentially intact and which is non-burning when subjected to an ordinary match flame.
Claim 12
Dependent Claim 23 words
An improved process according to claim 9 wherein an acrylic fibrous material is formed from said solution having incorporated therein said organic antioxidant.
Claim 13
Dependent Claim 13 words
An improved process according to claim 9 wherein said organic antioxidant is tetrachlorohydroquinone.
Claim 14
Dependent Claim 21 words
An improved process according to claim 9 wherein said oxygen-containing atmosphere is provided at a temperature of about 240* to 360*C.

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1978-12-01 1979-06-02 1979-12-02 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1982-12-01 1983-06-02 1983-12-02 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1986-12-01 1987-06-02 1987-12-02 $7700.00 Window Closed / Lapsed

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