US4172938A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Process for producing polyamides with lactam or urea solvent and CaCl2
Assignee: Teijin Ltd
•
Filing: 1977-06-13
•
Granted: 1979-10-30
•
Expires: 1997-06-13
Abstract
Abstract An aromatic polyamide having a high degree of polymerization is produced by polymerizing (A) a mixture of an aromatic diamine of the formula (1):
Inventors
- 👤 Hiroshi Mera
- 👤 Yasuo Nakagawa
- 👤 Masahiro Yamaguchi
- 👤 Mitsuyuki Ohno
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-01 19:55
CPC Classifications
C; C08; C08G; C08G69/00; C08G69/02; C08G69/08; C08G69/12; C08G69/26; C08G69/32; C08G69/36
Claims Analysis
Total Claims: 13
Claim 1
Independent Claim
319 words
A process for producing a fiber, film, fibroid or other shaped article forming aromatic polyamide having a logarithmic viscosity (ηinh/of) from about 4.3 to 8.8, comprising subjecting (A) a mixture of at least one aromatic diamine of the formula (1): H.sub.2 N--Ar.sub.1 --NH.sub.2 ( 1) and at least one aromatic dicarboxylic acid dihalide of the formula (2): XOC--Ar.sub.2 --COX (2), (b) a mixture of at least one of the aromatic diamines of the formula (1), at least one of the aromatic dicarboxylic acid dihalides of the formula (2) and at least one hydrogen halide salt of aromatic amino carboxylic acid halide of the formula (3): XH.H.sub.2 N--Ar.sub.3 --COX (3) or (C) at least one of the hydrogen halide salts of the aromatic amino carboxylic acid halides of the formula (3), wherein Ar 1 , Ar 2 and Ar 3 respectively represent, independently from each other, a divalent aromatic or heteroaromatic radical having two essentially coaxial or parallel, oppositely directed, chain extending bonds or a divalent heteroaromatic radical having two bonds extending from said radical with a maximum spacing from each other and X represents a halogen atom, to a condensation polymerization in a medium of at least one solvent selected from the group consisting of N-methyl-2-pyrrolidone containing calcium chloride in an amount of 1.5% or more but less than 5% based on the weight of the N-methyl-2-pyrrolidone, and dimethylacetamide, N-methylcaprolactam and tetramethylurea respectively containing calcium chloride in an amount of 1.5% to 8% based on the weight of the respective solvent compound, kneading said polymerization mixture, after the viscosity of said polymerization mixture reaches between 500 and 10,000 poises as determined by a falling-ball viscometer, until the logarithmic viscosity of the resultant polymer reaches from about 4.3 to 8.8, said logarithmic viscosity being determined by using a 5 g/dl solution of said polymer in 98.5% sulfuric acid at 30° C., and isolating the resultant polymer from the polymerization mixture.
Claim 2
Dependent Claim
319 words
A process for producing a fiber, film, fibroid or other shaped article forming aromatic polyamide having a logarithmic viscosity (ηinh/of) from about 4.3 to 8.8, comprising subjecting (A) a mixture of at least one aromatic diamine of the formula (1): H.sub.2 N--Ar.sub.1 --NH.sub.2 ( 1) and at least one aromatic dicarboxylic acid dihalide of the formula (2): XOC--Ar.sub.2 --COX (2), (b) a mixture of at least one of the aromatic diamines of the formula (1), at least one of the aromatic dicarboxylic acid dihalides of the formula (2) and at least one hydrogen halide salt of aromatic amino carboxylic acid halide of the formula (3): XH.H.sub.2 N--Ar.sub.3 --COX (3) or (C) at least one of the hydrogen halide salts of the aromatic amino carboxylic acid halides of the formula (3), wherein Ar 1 , Ar 2 and Ar 3 respectively represent, independently from each other, a divalent aromatic or heteroaromatic radical having two essentially coaxial or parallel, oppositely directed, chain extending bonds or a divalent heteroaromatic radical having two bonds extending from said radical with a maximum spacing from each other and X represents a halogen atom, to a condensation polymerization in a medium of at least one solvent selected from the group consisting of N-methyl-2-pyrrolidone containing calcium chloride in an amount of 1.5% or more but less than 5% based on the weight of the N-methyl-2-pyrrolidone, and dimethylacetamide, N-methylcaprolactam and tetramethylurea respectively containing calcium chloride in an amount of 1.5% to 8% based on the weight of the respective solvent compound, kneading said polymerization mixture, after the viscosity of said polymerization mixture reaches between 500 and 10,000 poises as determined by a falling-ball viscometer, until the logarithmic viscosity of the resultant polymer reaches from about 4.3 to 8.8, said logarithmic viscosity being determined by using a 5 g/dl solution of said polymer in 98.5% sulfuric acid at 30° C., and isolating the resultant polymer from the polymerization mixture.
Claim 3
Dependent Claim
38 words
A process as claimed in claim 1, wherein said Ar 1 , Ar 2 and Ar 3 respectively represent, independently from each other, 1,4-phenylene, 4,4'-biphenylene, 1,5-naphthylene, 1,4-naphthylene 2,6-naphthylene, or ##STR12## wherein Y represents --NH--, --O-- or --S-- radical.
Claim 4
Dependent Claim
50 words
A process as claimed in claim 1, wherein (A) a mixture of 1,4-phenylene diamine and terephthalic acid, (B) a mixture of 1,4-phenylene diamine, terephthalic acid and hydrogen chloride salt of p-aminobenzoic acid chloride, or (C) the hydrogen chloride salt of p-aminobenzoic acid chloride alone is subjected to the condensation polymerization.
Claim 5
Dependent Claim
25 words
A process as claimed in claim 1, wherein said calcium chloride is contained in an amount of 1.5 to 5% in dimethylacetamide, N-methylcaprolactam or tetramethylurea.
Claim 6
Dependent Claim
23 words
A process as claimed in claim 1, wherein said calcium chloride is contained in an amount of 2 to 4% in said N-methyl-pyrrolidone.
Claim 7
Dependent Claim
26 words
A process as claimed in claim 4, wherein said calcium chloride is contained in an amount of 2 to 4% in said dimethylacetamide, N-methylcaprolactam or tetramethylurea.
Claim 8
Dependent Claim
29 words
A process as claimed in claim 1, wherein a solubility enhancing or polymerization rate regulating amount of an aromatic or heterocyclic tertiary amine is added to the polymerization mixture.
Claim 9
Dependent Claim
18 words
A process as claimed in claim 7, wherein said aromatic tertiary amine is dimethyl aniline or diethyl aniline.
Claim 10
Dependent Claim
14 words
A process as claimed in claim 7, wherein said heterocyclic tertiary amine is pyridine.
Claim 11
Dependent Claim
57 words
A process as claimed in claim 1, wherein said polymerization mixture is kneaded for 5 minutes or more under such a condition that the kneading operation for 5 minutes results in a width of the Mohr's pattern of 200μ or less while a shear stress of at least 1 g/cm 2 is applied to said polymerization mixture.
Claim 12
Dependent Claim
161 words
A process for producing a fiber-, film-, fibroid- or other shaped article-forming poly-p-phenylene terephthalamide having a logarithmic viscosity (ηinh) from about 4.3 to 8.8, comprising the steps of: stirring a condensation-polymerization mixture consisting of 1,4-phenylene diamine and terephthalic acid dihalide dissolved in a medium of at least one solvent selected from the group consisting of N-methyl-2-pyrrolidone containing calcium chloride in an amount of 1.5% or more but less than 5% based on the weight of the N-methyl-2-pyrrolidone, and dimethylacetamide, N-methyl-caprolactam and tetramethylurea respectively containing calcium chloride in an amount of 1.5% to 8% based on the weight of the respective solvent compound, and kneading said polymerization mixture, after the viscosity of said polymerization mixture reaches between 500 and 10,000 poises as determined by a falling-ball viscometer, until the logarithmic viscosity of the resultant polymer reaches from about 4.3 to 8.8, said logarithmic viscosity being determined by using a 0.5 g/dl solution of said polymer in 98.5% sulfuric acid at 30° C.
Claim 13
Dependent Claim
161 words
A process for producing a fiber-, film-, fibroid- or other shaped article-forming poly-p-phenylene terephthalamide having a logarithmic viscosity (ηinh) from about 4.3 to 8.8, comprising the steps of: stirring a condensation-polymerization mixture consisting of 1,4-phenylene diamine and terephthalic acid dihalide dissolved in a medium of at least one solvent selected from the group consisting of N-methyl-2-pyrrolidone containing calcium chloride in an amount of 1.5% or more but less than 5% based on the weight of the N-methyl-2-pyrrolidone, and dimethylacetamide, N-methyl-caprolactam and tetramethylurea respectively containing calcium chloride in an amount of 1.5% to 8% based on the weight of the respective solvent compound, and kneading said polymerization mixture, after the viscosity of said polymerization mixture reaches between 500 and 10,000 poises as determined by a falling-ball viscometer, until the logarithmic viscosity of the resultant polymer reaches from about 4.3 to 8.8, said logarithmic viscosity being determined by using a 0.5 g/dl solution of said polymer in 98.5% sulfuric acid at 30° C.
References Cited (Backward Citations)
US3063966A
Cited
US3966686A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1982-10-29 | 1983-04-30 | 1983-10-30 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1986-10-29 | 1987-04-30 | 1987-10-30 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1990-10-29 | 1991-04-30 | 1991-10-30 | $7700.00 | Window Closed / Lapsed |