Patent US4649038A successfully refreshed from Google Patents.
US4649038A
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Cyanogen polymers and pyropolymers and fibers thereof
Assignee: Temple University
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Filing: 1985-09-17
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Granted: 1987-03-10
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Expires: 2005-09-17
Abstract
Abstract A novel polycyanogen (MW at least 500) is made by electrochemical polymerization of cyanogen in solution. Fiber and pyrolyzed forms of this polymer and methods of making same are also described.
Inventors
- 👤 Mortimer M. Labes
- 👤 Jiann H. Chen
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-01 16:20
CPC Classifications
D; D01; D01F; D01F9/00; D01F9/08; D01F9/12; D01F9/14; D01F9/20; C; C08; C08G; C08G73/00; D01F6/00; D01F6/02; D01F6/18
Claims Analysis
Total Claims: 28
Claim 1
Independent Claim
62 words
A method for electrochemically synthesizing a poly(cyanogen) comprising the steps of: (1) preparing a solution of C 2 N 2 and a soluble stable electrolyte in a polar organic solvent; (2) passing an electric current through said solution between an inert cathode and an inert anode, said current adapted to initiate polymerization in said solution and to deposit poly(cyanogen) on said anode.
Claim 2
Independent Claim
62 words
A method for electrochemically synthesizing a poly(cyanogen) comprising the steps of: (1) preparing a solution of C 2 N 2 and a soluble stable electrolyte in a polar organic solvent; (2) passing an electric current through said solution between an inert cathode and an inert anode, said current adapted to initiate polymerization in said solution and to deposit poly(cyanogen) on said anode.
Claim 3
Dependent Claim
16 words
A method, as recited in claim 1, wherein said anodic deposit is purified by solvent precipitation.
Claim 4
Dependent Claim
30 words
A method, as recited in claim 2, wherein a high molecular weight fraction of said deposit is precipitated from a solution of said deposit in tetrahydrofuran by adding petroleum ether.
Claim 5
Dependent Claim
26 words
The method of claim 1 wherein said electrolyte is R 4 NBF 4 where R is selected from the group of C 1 -C 10 alkyls.
Claim 6
Dependent Claim
17 words
The method of claim 4 wherein said electrolyte is a mixture of at least two different salts.
Claim 7
Dependent Claim
10 words
The method of claim 4 wherein said solvent is acetonitrile.
Claim 8
Dependent Claim
61 words
The method of claim 1 further including the step of: (3) pyrolyzing said anodic deposit at a temperature above 400° C. for a time sufficient to produce a pyropolymer characterized by a carbon-nitrogen ratio above 1.2, a room temperature conductivity of greater than 10 -1 ohm -1 cm -1 , and an activation energy for conduction of less than 0.03 ev.
Claim 9
Dependent Claim
11 words
A polycyanogen fiber spun from a polycyanogen comprised of ##STR6## units.
Claim 10
Dependent Claim
11 words
A polycyanogen fiber spun from a polycyanogen comprised of ##STR6## units.
Claim 11
Dependent Claim
20 words
A polycyanogen fiber as recited in claim 8, which has been pyrolyzed and which has a carbon-to-nitrogen ratio above 1.2.
Claim 12
Dependent Claim
20 words
A polycyanogen fiber as recited in claim 8, which has been pyrolyzed and which has a carbon-to-nitrogen ratio above 5:1.
Claim 13
Dependent Claim
20 words
A polycyanogen fiber as recited in claim 8, which has been pyrolyzed and which has a carbon-to-nitrogen ratio of 10:1.
Claim 14
Dependent Claim
20 words
A polycyanogen fiber as recited in claim 8, which has been pyrolyzed and which has a carbon-to-nitrogen ratio above 10:1.
Claim 15
Dependent Claim
24 words
A polycyanogen fiber as recited in claim 8, which has been pyrolyzed and which has a resistivity of less than 9×10 -5 ohms meter.
Claim 16
Dependent Claim
85 words
Method of making a polycyanogen fiber comprising: (a) preparing a solution of C 2 N 2 in a soluble stable electrolyte in a polar organic solvent; (b) passing an electric current through said solution between an inert cathode and an inert anode, said current adapted to initiate polymerization in said solution; (c) allowing poly(cyanogen) formed thereby to deposit on said anode; (d) forming a concentrated solution of said poly(cyanogen) in an organic solvent therefor; (e) and spinning a fiber of said polycyanogen from said solution.
Claim 17
Dependent Claim
85 words
Method of making a polycyanogen fiber comprising: (a) preparing a solution of C 2 N 2 in a soluble stable electrolyte in a polar organic solvent; (b) passing an electric current through said solution between an inert cathode and an inert anode, said current adapted to initiate polymerization in said solution; (c) allowing poly(cyanogen) formed thereby to deposit on said anode; (d) forming a concentrated solution of said poly(cyanogen) in an organic solvent therefor; (e) and spinning a fiber of said polycyanogen from said solution.
Claim 18
Dependent Claim
35 words
A method of forming a pyrolyzed polycyanogen fiber comprising forming a polycyanogen fiber, as recited in claim 14 and heating said fiber in an inert atmosphere or in vacuo to a temperature above 700° C.
Claim 19
Dependent Claim
24 words
A method of forming a pyrolyzed polycyanogen, as recited in claim 15 wherein said polycyanogen fiber is heated to a temperature above 1,000° C.
Claim 20
Dependent Claim
24 words
A method of forming a pyrolyzed polycyanogen, as recited in claim 15 wherein said polycyanogen fiber is heated to a temperature above 1,500° C.
Claim 21
Dependent Claim
25 words
A method of forming a pyrolyzed polycyanogen, as recited in claim 15 wherein in step (d) of claim 14 said polycyanogen is dissolved in tetrahydrofuran.
Claim 22
Dependent Claim
39 words
A polymer of cyanogen comprised of ##STR7## units, having a molecular weight of at least 500, IR absorption peaks at 2220-2240 cm -1 and 1500-1600 cm -1 and C13 NMR peaks at 112-117 and 157-161 PPM in deuterated DMSO.
Claim 23
Dependent Claim
39 words
A polymer of cyanogen comprised of ##STR7## units, having a molecular weight of at least 500, IR absorption peaks at 2220-2240 cm -1 and 1500-1600 cm -1 and C13 NMR peaks at 112-117 and 157-161 PPM in deuterated DMSO.
Claim 24
Dependent Claim
15 words
A polymer as recited in claim 19 wherein said molecular weight is at least 1000.
Claim 25
Dependent Claim
13 words
A product formed by pyrolysis of a polymer as recited in claim 19.
Claim 26
Dependent Claim
20 words
A product as recited in claim 21 having a conductivity of greater than 10 -1 ohms -1 cm -1 .
Claim 27
Dependent Claim
18 words
A product as recited in claim 21 having a conductivity greater than 1 ohm -1 cm -1 .
Claim 28
Dependent Claim
18 words
A polymer as recited in claim 21 having an activation energy for conduction of less than 0/03 eV.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1990-03-09 | 1990-09-08 | 1991-03-10 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1994-03-09 | 1994-09-08 | 1995-03-10 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1998-03-09 | 1998-09-08 | 1999-03-10 | $7700.00 | Window Closed / Lapsed |