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US5059273A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for preparing polyimide composites

Assignee: Fiberite Inc
•
Filing: 1989-10-26
•
Granted: 1991-10-22
•
Expires: 2009-10-26
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Abstract

Abstract Low void composites with high Tg polyimide matrices are prepared from stoichiometrically unbalanced precursors.

Inventors

  • 👤 Richard J. Boyce
  • 👤 Thomas P. Gannett

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-05 15:40
CPC Classifications
C; C08; C08J; C08J5/00; C08J5/04; C08G; C08G73/00; C08G73/06; C08G73/10; C08G73/1003; C08G73/1007; C08G73/101; C08G73/1014; C08G73/1028; C08J5/24; C08J5/241; C08J5/243; C08J2379/00; C08J2379/04; C08J2379/08; Y; Y10; Y10T; Y10T428/00; Y10T428/31504; Y10T428/31721

Claims Analysis

Total Claims: 5
Claim 1
Independent Claim 224 words
A process for preparing high quality fiber reinforced polyimide matrix composites having a void content of less than 1%, at moderate melt-consolidation pressures comprising a) forming a prepreg by combining fiber with a molecular weight limiting polyimide precursor solution of i) at least one aromatic diamine and a molar excess of at least one aromatic dianhydride or functional equivalent thereof; ii) at least one aromatic diamine and at least one aromatic dianhydride or functional equivalent thereof in stoichiometric proportions and an aromatic monoanhydride or functional equivalent thereof; or iii) at least one aromatic dianhydride or functional equivalent thereof and a molar excess of at least one aromatic diamine and an aromatic monoanhydride or functional equivalent thereof in amount sufficient to end-cap the molar excess of diamine; b) polymerizing the precursors and devolatilizing the product by heating until the volatiles are substantially removed; c) heating the devolatilized product to a temperature above the glass transition temperature until the melt viscosity of the polymer is sufficiently low to permit melt-consolidating without substantial degradation at a pressure of under 650 pounds per square inch; d) melt-consolidating the product to reduce void content below 1%; and e) heating the product until the glass transition temperature of the resulting product is equal to or greater than that of the polymer prepared from stoichiometric proportions of the same polyimide precursors.
Claim 2
Dependent Claim 224 words
A process for preparing high quality fiber reinforced polyimide matrix composites having a void content of less than 1%, at moderate melt-consolidation pressures comprising a) forming a prepreg by combining fiber with a molecular weight limiting polyimide precursor solution of i) at least one aromatic diamine and a molar excess of at least one aromatic dianhydride or functional equivalent thereof; ii) at least one aromatic diamine and at least one aromatic dianhydride or functional equivalent thereof in stoichiometric proportions and an aromatic monoanhydride or functional equivalent thereof; or iii) at least one aromatic dianhydride or functional equivalent thereof and a molar excess of at least one aromatic diamine and an aromatic monoanhydride or functional equivalent thereof in amount sufficient to end-cap the molar excess of diamine; b) polymerizing the precursors and devolatilizing the product by heating until the volatiles are substantially removed; c) heating the devolatilized product to a temperature above the glass transition temperature until the melt viscosity of the polymer is sufficiently low to permit melt-consolidating without substantial degradation at a pressure of under 650 pounds per square inch; d) melt-consolidating the product to reduce void content below 1%; and e) heating the product until the glass transition temperature of the resulting product is equal to or greater than that of the polymer prepared from stoichiometric proportions of the same polyimide precursors.
Claim 3
Dependent Claim 32 words
The process according to claim 1 wherein the polyimide precursor is selected from i) and consists essentially of a mixture of meta- and para-phenylene diamines and a molar excess of 2,2-bis(3', 4'-dicarboxyphenyl)hexafluoropropane.
Claim 4
Dependent Claim 36 words
The process according to claim 1 wherein the polyimide precursor is selected from iii) and consists essentially of pyromellitic diethylester diacid and a molar excess of 4,4'-[(1, 1'-biphenyl)-2,5-diylbis(oxy)]bisbenzeneamine, the excess amine being end-capped with phthalic anhydride.
Claim 5
Dependent Claim 22 words
The process according to claim 1 wherein a plurality of prepregs formed in step a) are stacked before proceeding with step b).

References Cited (Backward Citations)

GB1396331A Cited
US3745149A Cited
US4336175A Cited
US4358581A Cited
US4576857A Cited
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US4600617A Cited
US4645823A 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) 1994-10-21 1995-04-22 1995-10-22 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1998-10-21 1999-04-22 1999-10-22 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2002-10-21 2003-04-22 2003-10-22 $7700.00 Window Closed / Lapsed

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