US4414383A
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High molecular weight polybenzimidazole preparation with phosphorus containing polymerization catalyst
Assignee: Celanese Corp
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Filing: 1982-05-24
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Granted: 1983-11-08
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Expires: 2002-05-24
Abstract
Abstract This invention provides a single stage melt polymerization process for the production of an improved type of high molecular weight polybenzimidazole, which involves the use of a phosphorus-containing polymerization catalyst. The process provides poly-2,2'-(m-phenylene)-5,5'-bibenzimidazole of improved color and plugging value, and is further characterized by an inherent viscosity of at least about 0.7 dl/g, and a weight average molecular weight of at least about 100,000.
Inventors
- 👤 Anthony B. Conciatori
- 👤 Eui W. Choe
- 👤 Henry K. Hall, Jr.
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-05 13:12
CPC Classifications
C; C08; C08G; C08G73/00; C08G73/06; C08G73/18
Claims Analysis
Total Claims: 21
Claim 1
Independent Claim
111 words
A single stage melt polymerization process for the production of high molecular weight polybenzimidazole which comprises preparing a mixture of (1) at least one aromatic tetraamine containing two groups of amine substituents, said amine substituents in each group being in an ortho position relative to each other, and (2) at least one dicarboxylic acid; and heating the mixture above its melting temperature in contact with a phosphorus-containing polymerization catalyst corresponding to the formula: ##STR13## where R is a radical selected from organic, halide and hydrogen substituents, with the proviso that not more than one R is hydrogen; and Y is an oxygen atom, and n is the integer zero or one.
Claim 2
Dependent Claim
111 words
A single stage melt polymerization process for the production of high molecular weight polybenzimidazole which comprises preparing a mixture of (1) at least one aromatic tetraamine containing two groups of amine substituents, said amine substituents in each group being in an ortho position relative to each other, and (2) at least one dicarboxylic acid; and heating the mixture above its melting temperature in contact with a phosphorus-containing polymerization catalyst corresponding to the formula: ##STR13## where R is a radical selected from organic, halide and hydrogen substituents, with the proviso that not more than one R is hydrogen; and Y is an oxygen atom, and n is the integer zero or one.
Claim 3
Dependent Claim
45 words
A process in accordance with claim 1 wherein the high molecular weight polybenzimidazole exhibits an inherent viscosity of at least about 0.7 dl/g when measured at a concentration of 0.4 g of said polybenzimidazole in 100 ml of 97 percent sulfuric acid at 25° C.
Claim 4
Dependent Claim
34 words
A process in accordance with claim 1 wherein the melt polymerization reaction is conducted at a temperature of at least about 340° C., and for a reaction period of at least about 3 hours.
Claim 5
Dependent Claim
18 words
A process in accordance with claim 1 wherein the melt polymerization reaction is conducted under an inert atmosphere.
Claim 6
Dependent Claim
29 words
A process in accordance with claim 1 wherein the polymerization catalyst is present in a quantity between about 0.01-5 weight percent, based on the weight of the monomeric reactants.
Claim 7
Dependent Claim
18 words
A process in accordance with claim 1 wherein the monomeric dicarboxylic acid reactant is an aromatic dicarboxylic acid.
Claim 8
Dependent Claim
15 words
A process in accordance with claim 1 wherein the monomeric aromatic tetraamine reactant is 3,3',4,4'-tetraaminobiphenyl.
Claim 9
Dependent Claim
16 words
A process in accordance with claim 1 wherein said monomeric dicarboxylic acid reactant is isophthalic acid.
Claim 10
Dependent Claim
15 words
A process in accordance with claim 1 wherein the polymerization catalyst is an organophosphine compound.
Claim 11
Dependent Claim
15 words
A process in accordance with claim 1 wherein the polymerization catalyst is an organophosphite compound.
Claim 12
Dependent Claim
15 words
A process in accordance with claim 1 wherein the polymerization catalyst is an organophosphate compound.
Claim 13
Dependent Claim
13 words
A process in accordance with claim 1 wherein the polymerization catalyst is triphenylphosphite.
Claim 14
Dependent Claim
13 words
A process in accordance with claim 1 wherein the polymerization catalyst is phenyldichlorophosphine.
Claim 15
Dependent Claim
18 words
A process in accordance with claim 1 wherein the polymerization catalyst is a mixture comprising triphenylphosphite and phenyldichlorophosphine.
Claim 16
Dependent Claim
14 words
A process in accordance with claim 1 wherein the polymerization catalyst is diphenylphosphine oxide.
Claim 17
Dependent Claim
13 words
A process in accordance with claim 1 wherein the polymerization catalyst is di(methoxy)phenylphosphine.
Claim 18
Dependent Claim
13 words
A process in accordance with claim 1 wherein the polymerization catalyst is tri(p-methoxyphenyl)phosphine.
Claim 19
Dependent Claim
14 words
A process in accordance with claim 1 wherein the polymerization catalyst is o-phenylenephosphochloridite: ##STR14##
Claim 20
Dependent Claim
132 words
A single stage melt polymerization process for the production of high molecular weight polybenzimidazole which comprises heating a mixture of 3,3',4,4'-tetraaminobiphenyl and isophthalic acid at a melting temperature of at least about 340° C. in contact with a phosphorus-containing polymerization catalyst corresponding to the formula: ##STR15## wherein R is a radical selected from organic, halide and hydrogen substituents, with the proviso that not more than one R is hydrogen; and Y is an oxygen atom, and n is the integer zero or one; wherein the polybenzimidazole exhibits an inherent viscosity of at least about 0.7 dl/g when measured at a concentration of 0.4 g of said polybenzimidazole in 100 ml of 97 percent sulfuric acid at 25° C., and the polybenzimidazole has a weight average molecular weight of at least about 100,000.
Claim 21
Dependent Claim
132 words
A single stage melt polymerization process for the production of high molecular weight polybenzimidazole which comprises heating a mixture of 3,3',4,4'-tetraaminobiphenyl and isophthalic acid at a melting temperature of at least about 340° C. in contact with a phosphorus-containing polymerization catalyst corresponding to the formula: ##STR15## wherein R is a radical selected from organic, halide and hydrogen substituents, with the proviso that not more than one R is hydrogen; and Y is an oxygen atom, and n is the integer zero or one; wherein the polybenzimidazole exhibits an inherent viscosity of at least about 0.7 dl/g when measured at a concentration of 0.4 g of said polybenzimidazole in 100 ml of 97 percent sulfuric acid at 25° C., and the polybenzimidazole has a weight average molecular weight of at least about 100,000.
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) | 1986-11-07 | 1987-05-09 | 1987-11-08 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1990-11-07 | 1991-05-09 | 1991-11-08 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1994-11-07 | 1995-05-09 | 1995-11-08 | $7700.00 | Window Closed / Lapsed |