US4436894A — Novel wholly aromatic copolyester, process for pr…

Claim 1

Independent Claim 145 words

A wholly aromatic copolyester composed mainly of isophthalic acid units and hydroquinone units, the total proportion of said isophthalic acid units and hydroquinone units being at least about 80 mole% based on the entire units, said wholly aromatic copolyester having a terminal carboxyl group concentration, measured by dissolving the wholly aromatic copolyester in a mixed solvent of phenol and tetrachloroethane in a weight ratio of 4:6 and titrating the resulting solution with a benzyl alcohol solution of sodium hydroxide using bromocresol green as an indicator, of not more than about 90 eq/10 6 g and a reduced viscosity, determined at 35° C. in a mixed solvent of phenol and tetrachloroethane in a weight ratio of 4:6 in a concentration of 1.2 g/dl of at least about 0.6 and being substantially linear and melt-shapable and substantially free from a halogen atom bonded to the molecular chain.

Claim 2

Dependent Claim 145 words

A wholly aromatic copolyester composed mainly of isophthalic acid units and hydroquinone units, the total proportion of said isophthalic acid units and hydroquinone units being at least about 80 mole% based on the entire units, said wholly aromatic copolyester having a terminal carboxyl group concentration, measured by dissolving the wholly aromatic copolyester in a mixed solvent of phenol and tetrachloroethane in a weight ratio of 4:6 and titrating the resulting solution with a benzyl alcohol solution of sodium hydroxide using bromocresol green as an indicator, of not more than about 90 eq/10 6 g and a reduced viscosity, determined at 35° C. in a mixed solvent of phenol and tetrachloroethane in a weight ratio of 4:6 in a concentration of 1.2 g/dl of at least about 0.6 and being substantially linear and melt-shapable and substantially free from a halogen atom bonded to the molecular chain.

Claim 3

Dependent Claim 30 words

The wholly aromatic copolyester of claim 1 wherein the total proportion of the isophthalic acid units and hydroquinone units is about 85 to about 95 mole% of the entire units.

Claim 4

Dependent Claim 192 words

The wholly aromatic copolyester of claim 1 or 2 which is composed substantially of the isophthalic acid units and hydroquinone units and at least one type of units selected from the group consisting of bisphenol units of the following formula ##STR19## wherein X is --O--, >C═O or ##STR20## in which R 1 and R 2 are identical or different and each represents a hydrogen atom, a methyl group, an ethyl group or a phenyl group, or R 1 and R 2 taken, together with the carbon atom to which they are bonded, may form a cyclohexane ring, substituted hydroquinone units of the following formula ##STR21## wherein R 3 represents a tertiary alkyl group having 4 to 9 carbon atoms or a phenyl group which may be substituted by a tertiary butyl group, substituted or unsubstituted resorcinol units of the following formula ##STR22## wherein R 4 represents a hydrogen atom, a tertiary alkyl group having 4 to 9 carbon atoms, or a phenyl group which may be substituted by a tertiary butyl group, and hydroxybenzoic acid units of the following formula ##STR23## wherein --O-- and --CO-- are meta or para to each other.

Claim 5

Dependent Claim 31 words

The wholly aromatic copolyester of claim 3 which consists substantially of isophthalic acid units, hydroquinone units, and the bisphenol units of formula (1) and/or the substituted hydroquinone units of formula (2).

Claim 6

Dependent Claim 23 words

The wholly aromatic copolyester of claim 1 which has a terminal carboxyl group concentration of about 5 to about 70 eq./10 6 g.

Claim 7

Dependent Claim 18 words

The wholly aromatic copolyester of claim 1 which has a reduced viscosity of about 0.7 to about 210.

Claim 8

Dependent Claim 40 words

The wholly aromatic copolyester of claim 1 wherein a halogen atom bonded to the molecular chain is a halogen atom at the terminal of the molecular chain, or a halogen atom bonded to the aromatic ring in the molecular chain.

Claim 9

Dependent Claim 31 words

The wholly aromatic copolyester of claim 1 which has a flow index, at a shear rate of about 50 to about 500 sec -1 of 0.7 to 0.9 on an average.

Claim 10

Dependent Claim 136 words

A process for producing the wholly aromatic copolyester defined in claim 1 or a wholly aromatic copolyester having a reduced viscosity of less than about 0.6, which comprises polycondensing under heat in the presence of a polycondensation catalyst a reaction mixture consisting of a major proportion of a diaryl ester of isophthalic acid and hydroquinone and a minor proportion of at least one other component selected from diaryl esters of aromatic dicarboxylic acids other than isophthalic acid, aromatic dihydroxy compounds other than hydroquinone and aryl hydroxybenzoates while intermittently or continuously removing the hydroxyaryl compound formed, and after the reduced viscosity of the polymer formed in the reaction system has reached about 0.2, performing the polycondensation at a temperature lower than the crystalline melting point of the polymer while maintaining the reaction system in a molten condition.

Claim 11

Dependent Claim 137 words

A process for producing the wholly aromatic copolyester defined in claim 1 or a wholly aromatic copolyester having a reduced viscosity of less than about 0.6, which comprises polycondensing under heat in the presence of a polycondensation catalyst a reaction mixture consisting of a major proportion of isophthalic acid, hydroquinone and a diaryl carbonate and a minor proportion of at least one other component selected from aromatic dicarboxylic acids other than isophthalic acid, aromatic dihydroxy compounds other than hydroquinone, hydroxybenzoic acid and aryl hydroxybenzoates while intermittently or continuously removing the hydroxyaryl compound and carbon dioxide formed, and after the reduced viscosity of the polymer formed in the reaction system has reached about 0.2, performing the polycondensation at a temperature lower than the crystalline melting point of the polymer while maintaining the reaction system in a molten conditions.

Claim 12

Dependent Claim 31 words

The process of claim 9 or 10 wherein when the reduced viscosity of the polymer formed in the reaction system has reached about 0.08, the reaction system is under reduced pressure.

Claim 13

Dependent Claim 42 words

The process of claim 9 or 10 wherein at least until the reduced viscosity of the polymer formed in the reaction system reaches about 0.15, the polycondensation is carried out at a temperature higher than the crystalline melting point of the polymer.

Claim 14

Dependent Claim 70 words

A process for producing the wholly aromatic copolyester defined in claim 1 whose reduced viscosity has been enhanced, which comprises polymerizing the wholly aromatic copolyester defined in claim 1 or a wholly aromatic copolyester having a reduced viscosity of less than about 0.6 in the solid phase at a temperature of from 250° C. to 300° C. under reduced pressure or while passing an inert gas into the reaction system.

Claim 15

Dependent Claim 151 words

A film prepared by melt shaping from a wholly aromatic copolyester composed mainly of isophthalic acid units and hydroquinone units, said wholly aromatic copolyester comprising at least about 80 mol%, based on the entire units, of the isophthalic acid units and hydroquinone units, said copolyester having a terminal carboxyl group concentration, measured by dissolving the wholly aromatic copolyester in a mixed solvent of phenol and tetrachloroethane in a weight ratio of 4:6 and titrating the resulting solution with a benzyl alcohol solution of sodium hydroxide using bromocresol green as an indicator, of not more than about 90 eq per 10 6 g and a reduced viscosity, determined at 35° C. in a mixed solvent of phenol and tetrachloroethane in a weight ratio of 4:6 in a concentration of 1.2 g/dl, of at least about 0.6 and being substantially linear and substantially free from a halogen atom bonded to the molecular chain.

Claim 16

Dependent Claim 151 words

A film prepared by melt shaping from a wholly aromatic copolyester composed mainly of isophthalic acid units and hydroquinone units, said wholly aromatic copolyester comprising at least about 80 mol%, based on the entire units, of the isophthalic acid units and hydroquinone units, said copolyester having a terminal carboxyl group concentration, measured by dissolving the wholly aromatic copolyester in a mixed solvent of phenol and tetrachloroethane in a weight ratio of 4:6 and titrating the resulting solution with a benzyl alcohol solution of sodium hydroxide using bromocresol green as an indicator, of not more than about 90 eq per 10 6 g and a reduced viscosity, determined at 35° C. in a mixed solvent of phenol and tetrachloroethane in a weight ratio of 4:6 in a concentration of 1.2 g/dl, of at least about 0.6 and being substantially linear and substantially free from a halogen atom bonded to the molecular chain.

Claim 17

Dependent Claim 8 words

The film of claim 14 which is unstretched.

Claim 18

Dependent Claim 8 words

The film of claim 14 which is stretched.

Claim 19

Dependent Claim 9 words

The film of claim 16 which is biaxially stretched.

Claim 20

Dependent Claim 45 words

The film of (claims 14, 15, 16 or 17) which has within its plane two perpendicularly crossing directions each of which has a Young's modulus of at least about 70 kg/mm 2 and a strength of at least about 7 kg/mm 2 at 25° C.

Claim 21

Dependent Claim 93 words

The film of claim 14, 16, or 17 which has a coefficient of linear expansion, defined by the following formula, of not more than about 8×10 5 mm/mm/°C. ##EQU5## wherein L 260 is the film length (mm) attained when a film sample having a length of about 100 mm and a width of about 5 mm at 25° C. is heated at 260° C. under no tension, and L 25 is the film length (mm) attained when the film used in the measurement of L 260 is allowed to cool to 25° C.

Claim 22

Dependent Claim 95 words

The film of (claims 14, 15, 16 or 17) which has a heat shrinkage (%), defined by the following formula, of not more than about 5%: ##EQU6## wherein l 25 is the length (cm) of the film at 25° C., and l 260 is the film length (cm) attained when the film sample used for the measurement of l 25 is heated at 260° C. for 60 seconds under no tension and then allowed to cool to 25° C. The film of claim 20 which has a heat shrinkage of not more than about 1%.

Claim 23

Dependent Claim 16 words

The film of claim 20 which has a heat shrinkage of not more than about 1%.

Claim 24

Dependent Claim 17 words

The film of claim 14 which has an elongation at 25° C. of at least about 20%.

Claim 25

Dependent Claim 28 words

The film of claim 22 which has an elongation at 25° C. of at least about 20% when heat-treated at 260° C. for 60 seconds under no tension.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1987-03-13	1987-09-12	1988-03-13	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	1991-03-13	1991-09-12	1992-03-13	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	1995-03-13	1995-09-12	1996-03-13	$7700.00	Window Closed / Lapsed

Novel wholly aromatic copolyester, process for production thereof, and film melt-shaped therefrom

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