US4470944A
Expired / Lapsed
US
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Process for producing an aromatic polyimide film
Assignee: Toray Industries Inc
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Filing: 1983-02-03
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Granted: 1984-09-11
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Expires: 2003-02-03
Abstract
Abstract The present invention relates to a process for producing an of aromatic polyimide film comprising (A) casting on a support a dope containing an amide-type polar solvent and 10-45 weight percent of a polyamic acid having more than 0.4 dl/g an inherent viscosity of more than 0.4 dl/g, (B) concentrating the polymer content to be at least higher than that of the initial dope while simultaneously raising the ring closure ratio above 30%, (C) removing the solvent from the film by extraction in an aqueous medium so as to lower the solvent content of the film below 10% and (D) then heating the film to a temperature of more than 200° C. The process of the present invention is useful for the production of aromatic polyimide film having a reduced rate of solvent decomposition and improved productivity. The aromatic polyimide film produced by the process of the present invention is superior in thermal as well as mechanical properties and is highly useful as an electric insulation material and also as a base for flexible printed circuits, magnetic tape, etc.
Inventors
- 👤 Toshiyuki Asakura
- 👤 Masanori Mizouchi
- 👤 Hiroaki Kobayashi
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-01 10:31
CPC Classifications
C; C08; C08J; C08J5/00; C08J5/18; B; B05; B05D; B05D5/00; B05D5/12; C08J2379/00; C08J2379/04; C08J2379/08; H; H05; H05K; H05K1/00; H05K1/02; H05K1/03; H05K1/0313; H05K1/032; H05K1/0346; H05K3/00; H05K3/02; H05K3/022; Y; Y10; Y10T; Y10T428/00; Y10T428/31504; Y10T428/31721
Claims Analysis
Total Claims: 19
Claim 1
Independent Claim
103 words
A process for producing an aromatic polyimide film comprising the steps of: (A) casting on a support a dope containing an amide-type polar solvent and 10-45 weight percent of a polyamic acid having an inherent viscosity of more than 0.4 dl/g, (B) concentrating the polymer content to be at least higher than that of the initial dope while simultaneously raising the ring closure ratio above 30%, (C) removing the solvent from the film by extraction in an aqueous medium so as to lower the solvent content of the film below 10% and (D) then heating the film to a temperature above 200° C.
Claim 2
Dependent Claim
103 words
A process for producing an aromatic polyimide film comprising the steps of: (A) casting on a support a dope containing an amide-type polar solvent and 10-45 weight percent of a polyamic acid having an inherent viscosity of more than 0.4 dl/g, (B) concentrating the polymer content to be at least higher than that of the initial dope while simultaneously raising the ring closure ratio above 30%, (C) removing the solvent from the film by extraction in an aqueous medium so as to lower the solvent content of the film below 10% and (D) then heating the film to a temperature above 200° C.
Claim 3
Dependent Claim
26 words
A process for producing an aromatic polyimide film as claimed in claim 1, wherein the inherent viscosity of said polyamic acid is less than 5.0 dl/g.
Claim 4
Dependent Claim
66 words
A process for producing an aromatic polyimide film as claimed in claim 1, wherein said polyamic acid has a recurring structural unit of the following general formula: ##STR5## where R 1 is a quadrivalent organic group with 6-25 carbon atoms and contains at least one aromatic ring; and R 2 is a divalent organic group with 6-25 carbon atoms and contains at least one aromatic ring.
Claim 5
Dependent Claim
68 words
A process for production of aromatic polyimide film as claimed in claim 1, wherein said polyamic acid has a recurring structural unit of the following general formula. ##STR6## where R 1 is a quadrivalent organic group with 6-25 in carbon number and containing at least one aromatic ring, and R 2 is a divalent organic group with 6-25 in carbon number and containing at least one aromatic ring.
Claim 6
Dependent Claim
26 words
A process for producing an aromatic polyimide film as claimed in claim 1, wherein said polyamic acid is derived from pyromellitic acid dianhydride and 4,4'-diaminodiphenyl ether.
Claim 7
Dependent Claim
28 words
A process for producing an aromatic polyimide film as claimed in claim 1, wherein the concentration of said polymer in step (B) is more than 50 weight percent.
Claim 8
Dependent Claim
34 words
A process for producing an aromatic polyimide film as claimed in claim 1, wherein said support comprises at least one member selected from the group consisting of a glass support and a metal support.
Claim 9
Dependent Claim
33 words
A process for producing an aromatic polyimide film as claimed in claim 1, wherein said amide-type polar solvent comprises at least one member selected from the group consisting of N,N'-dimethyl acetamide and N-methyl-2-pyrrolidone.
Claim 10
Dependent Claim
27 words
A process for producing an aromatic polyimide film as claimed in claim 1, wherein said dope has a solution viscosity of 100-20,000 poises at the casting temperature.
Claim 11
Dependent Claim
24 words
A process for producing an aromatic polyimide film as claimed in claim 1, wherein said polymer's ring closure ratio in step (B) is 35-90%.
Claim 12
Dependent Claim
42 words
A process for producing an aromatic polyimide film as claimed in claim 1, wherein the concentration of said dope and the ring closure ratio in step (B) are effected by heating the dope to a temperature in the range of 40°-250° C.
Claim 13
Dependent Claim
45 words
A process for producing an aromatic polyimide film as claimed in claim 1, wherein said aqueous medium is one selected from the group consisting of water and a mixture of water and said amide-type solvent said mixture containing more than 50 weight percent of water.
Claim 14
Dependent Claim
32 words
A process for producing an aromatic polyimide film as claimed in claim 1, wherein step (C) is carried out with the temperature of said aqueous medium in the range of 5°-90° C.
Claim 15
Dependent Claim
27 words
A process for producing an aromatic polyimide film as claimed in claim 1, wherein the heating temperature in step (D) is in the range of 230°-700° C.
Claim 16
Dependent Claim
67 words
A process for producing an aromatic polyimide film as claimed in claim 1, wherein said aromatic polyimide has a recurring structural unit represented by the following general formula: ##STR7## where R 1 is a quadrivalent organic group with 6-25 carbon atoms and contains at least one aromatic ring; and R 2 is a divalent organic group with 6-25 carbon atoms and contains at least one aromatic ring.
Claim 17
Dependent Claim
23 words
A process for producing an aromatic polyimide film as claimed in claim 1, wherein the ring closure in step (B) is done chemically.
Claim 18
Dependent Claim
27 words
A process for producing an aromatic polyimide film as claimed in claim 16, wherein acetic anhydride and a tertiary amine are used for said chemical ring closure.
Claim 19
Dependent Claim
19 words
A process for producing an aromatic polyimide film as claimed in claim 17, wherein the tertiary amine is pyridine.
References Cited (Backward Citations)
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Cited
GB903271A
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GB903272A
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US3179614A
Cited
GB1155541A
Cited
JPS48100460A
Cited
US4073837A
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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) | 1987-09-11 | 1988-03-12 | 1988-09-11 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1991-09-11 | 1992-03-12 | 1992-09-11 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1995-09-11 | 1996-03-12 | 1996-09-11 | $7700.00 | Window Closed / Lapsed |