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US4079113A Expired / Lapsed US ⏱️ 0.0 years remaining

Method for the preparation of fibers or films from phenolic resins

Assignee: Mitsubishi Chemical Corp
•
Filing: 1976-03-18
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Granted: 1978-03-14
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Expires: 1996-03-18
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Abstract

Abstract Fibers or films with high mechanical strengths are produced from novolacs which are obtained by reaction of resols with phenols under neutral or acidic conditions.

Inventors

  • 👤 Tomiaki Kimura
  • 👤 Masamichi Watanabe
  • 👤 Yoichiro Yamakawa
  • 👤 Seiichi Mukai
  • 👤 Kunihiro Takenaka
  • 👤 Masahiro Kita

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-27 13:51
CPC Classifications
D; D01; D01F; D01F6/00; D01F6/58; D01F6/76; C; C08; C08G; C08G8/00; C08G8/04; D01F11/00; D01F11/04; D01F11/08

Claims Analysis

Total Claims: 16
Claim 1
Independent Claim 106 words
In a method for the preparation of a phenolic fiber or film which comprises subjecting a phenolic resin to a melt spinning or melt-forming treatment, and curing the resulting fiber or film by means of an aldehyde, the improvement which comprises: providing as said phenolic resin a novolac having a molecular weight ranging from 500 to 2000 which is obtained by reacting a resol prepared by reacting a phenol and an aldehyde in the presence of ammonia or a primary, secondary or tertiary amine as a catalyst with a phenol under neutral or acidic conditions, wherein said neutral or acidic conditions are attained with oxalic acid.
Claim 2
Dependent Claim 106 words
In a method for the preparation of a phenolic fiber or film which comprises subjecting a phenolic resin to a melt spinning or melt-forming treatment, and curing the resulting fiber or film by means of an aldehyde, the improvement which comprises: providing as said phenolic resin a novolac having a molecular weight ranging from 500 to 2000 which is obtained by reacting a resol prepared by reacting a phenol and an aldehyde in the presence of ammonia or a primary, secondary or tertiary amine as a catalyst with a phenol under neutral or acidic conditions, wherein said neutral or acidic conditions are attained with oxalic acid.
Claim 3
Dependent Claim 28 words
The method according to claim 1, wherein the amount of said ammonia or amine catalyst is in the range of 0.5 to 20 mole % to said phenol.
Claim 4
Dependent Claim 19 words
The method according to claim 1, wherein the interaction is effected at a temperature of 40° to 100° C.
Claim 5
Dependent Claim 12 words
The method according to claim 1, wherein the solution conditions are acid.
Claim 6
Dependent Claim 25 words
The method according to claim 1, wherein the reaction between said resol and said phenol is effected at a temperature of 70° to 120° C.
Claim 7
Dependent Claim 11 words
The method according to claim 1, wherein said aldehyde is formaldehyde.
Claim 8
Dependent Claim 29 words
The method according to claim 1, wherein said fiber or film is cured by heating said fiber or film with said aldehyde in the presence of an acid catalyst.
Claim 9
Dependent Claim 17 words
The method according to claim 7, wherein said acid catalyst for said curing reaction is hydrochloric acid.
Claim 10
Dependent Claim 45 words
The method according to claim 7, wherein said curing is effected by heating said fiber or film from 20° - 40° C to 80° - 130° over a period of 1 to 5 hours and maintained at the elevated temperature for 5 to 50 hours.
Claim 11
Dependent Claim 42 words
The method according to claim 1, wherein said curing by said aldehyde is effected in two stages wherein said fiber or film is first heated in the presence of an acid catalyst and then heated in the presence of a basic catalyst.
Claim 12
Dependent Claim 87 words
The method according to claim 10, wherein the first stage heating in the presence of said acid catalyst is conducted by raising the temperature of the fiber or film from 20° - 40° C to 80° - 130° C over a period of 0.5 to 4 hours and keeping the elevated temperature for 0.5 to 4 hours and the second stage heating in the presence of said basic catalyst is conducted by keeping the film or fiber at 70° to 120° C for 0.5 to 3 hours.
Claim 13
Dependent Claim 124 words
In a method for the preparation of a phenolic fiber or film which comprises subjecting a phenolic resin to a melt spinning or film-forming treatment and curing the resulting fiber or film by means of an aldehyde, the improvement which comprises: providing as said phenolic resin a mixture containing (1) a novolac having a molecular weight ranging from 500 to 2000 obtained by reacting a resol prepared by reacting a phenol and an aldehyde in the presence of ammonia or a primary, secondary or tertiary amine as a catalyst with a phenol under a neutral or acidic conditions, wherein said neutral or acidic conditions are attained with oxalic acid and (2) a polyamide in an amount of 0.5 to 40% by weight of novolac.
Claim 14
Dependent Claim 124 words
In a method for the preparation of a phenolic fiber or film which comprises subjecting a phenolic resin to a melt spinning or film-forming treatment and curing the resulting fiber or film by means of an aldehyde, the improvement which comprises: providing as said phenolic resin a mixture containing (1) a novolac having a molecular weight ranging from 500 to 2000 obtained by reacting a resol prepared by reacting a phenol and an aldehyde in the presence of ammonia or a primary, secondary or tertiary amine as a catalyst with a phenol under a neutral or acidic conditions, wherein said neutral or acidic conditions are attained with oxalic acid and (2) a polyamide in an amount of 0.5 to 40% by weight of novolac.
Claim 15
Dependent Claim 126 words
In a method for the preparation of a phenolic fiber or film which comprises subjecting a phenolic resin to a melt spinning or film-forming treatment and curing the resulting fiber or film by means of an aldehyde, the improvement which comprises: providing as said phenolic resin a novolac having a molecular weight ranging from 500 to 2000 obtained by reacting a resol prepared by reacting a phenol and an aldehyde in the presence of ammonia or a primary, secondary or tertiary amine as a catalyst with a phenol under neutral or acidic conditions, wherein said neutral or acidic conditions are attained with oxalic acid, and subjecting the cured fiber or film to a treatment which blocks phenolic hydroxyl groups of the novolac by esterification or etherification.
Claim 16
Dependent Claim 126 words
In a method for the preparation of a phenolic fiber or film which comprises subjecting a phenolic resin to a melt spinning or film-forming treatment and curing the resulting fiber or film by means of an aldehyde, the improvement which comprises: providing as said phenolic resin a novolac having a molecular weight ranging from 500 to 2000 obtained by reacting a resol prepared by reacting a phenol and an aldehyde in the presence of ammonia or a primary, secondary or tertiary amine as a catalyst with a phenol under neutral or acidic conditions, wherein said neutral or acidic conditions are attained with oxalic acid, and subjecting the cured fiber or film to a treatment which blocks phenolic hydroxyl groups of the novolac by esterification or etherification.

References Cited (Backward Citations)

US3650102A Cited
US3931386A Cited
US3928526A Cited
US3972959A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1981-03-13 1981-09-12 1982-03-14 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1985-03-13 1985-09-12 1986-03-14 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1989-03-13 1989-09-12 1990-03-14 $7700.00 Window Closed / Lapsed

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