US4567247A — Process for forming thermally stable thermotropic…

Claim 1

Independent Claim 299 words

In a process for the formation within a polymerization zone of a polyester which is capable of forming an anisotropic melt phase and which optionally may include amide linkages through a polymerization reaction of ester-forming and optionally also amide-forming monomers to form a polymer having recurring moieties selected from the group consisting of the following where in each instance Ar may be the same or different and comprises at least one aromatic ring: (a) ##STR11## and (b) a mixture of ##STR12## where Z is NH or NR where R is an alkyl group of 1 to 6 carbon atoms or an aryl group; the improvement of providing in the polymerization zone during the polymerization reaction an approximately 0.25 to 4 percent molar excess of an aromatic monomer selected from the group consisting of the following where in each instance Ar may be the same or different and comprises at least one aromatic ring: (c) HO--Ar--OH, and/or an esterified derivative thereof, (d) H 2 N--Ar--NH 2 , and/or an amidated derivative thereof, (e) HO--Ar--NH 2 , and/or an esterified and/or an amidated derivative thereof, and (f) mixtures of the foregoing, which during the polymerization reaction imparts units to the interior of the polymer chains selected from the group consisting of: (g) dioxyaryl units, (h) diaminoaryl units, (i) oxyaminoaryl units, and (j) mixtures of the foregoing, and causes the polymer chains to end in groups selected from group consisting of: (k) hydroxyl end groups and/or an esterified derivative thereof, (l) amino end groups and/or an amidated derivative thereof, and (m) mixtures of the foregoing, wherein the polymer chains achieve a predetermined average chain length through the depletion of other monomers present in the polymerization zone to yield a polyester product which is substantially incapable of additional chain growth upon subsequent heating.

Claim 2

Dependent Claim 299 words

In a process for the formation within a polymerization zone of a polyester which is capable of forming an anisotropic melt phase and which optionally may include amide linkages through a polymerization reaction of ester-forming and optionally also amide-forming monomers to form a polymer having recurring moieties selected from the group consisting of the following where in each instance Ar may be the same or different and comprises at least one aromatic ring: (a) ##STR11## and (b) a mixture of ##STR12## where Z is NH or NR where R is an alkyl group of 1 to 6 carbon atoms or an aryl group; the improvement of providing in the polymerization zone during the polymerization reaction an approximately 0.25 to 4 percent molar excess of an aromatic monomer selected from the group consisting of the following where in each instance Ar may be the same or different and comprises at least one aromatic ring: (c) HO--Ar--OH, and/or an esterified derivative thereof, (d) H 2 N--Ar--NH 2 , and/or an amidated derivative thereof, (e) HO--Ar--NH 2 , and/or an esterified and/or an amidated derivative thereof, and (f) mixtures of the foregoing, which during the polymerization reaction imparts units to the interior of the polymer chains selected from the group consisting of: (g) dioxyaryl units, (h) diaminoaryl units, (i) oxyaminoaryl units, and (j) mixtures of the foregoing, and causes the polymer chains to end in groups selected from group consisting of: (k) hydroxyl end groups and/or an esterified derivative thereof, (l) amino end groups and/or an amidated derivative thereof, and (m) mixtures of the foregoing, wherein the polymer chains achieve a predetermined average chain length through the depletion of other monomers present in the polymerization zone to yield a polyester product which is substantially incapable of additional chain growth upon subsequent heating.

Claim 3

Dependent Claim 17 words

A process in accordance with claim 1 wherein said polymerization reaction is carried out in the melt.

Claim 4

Dependent Claim 22 words

A process in accordance with claim 1 wherein said polymerization reaction is carried out while the monomers are suspended as a slurry.

Claim 5

Dependent Claim 43 words

A process in accordance with claim 1 wherein any monomer present in the polymerization zone which would otherwise include a hydroxyl group and/or an amine group is provided as a lower acyl ester and/or amide of about 2 to about 4 carbon atoms.

Claim 6

Dependent Claim 35 words

A process in accordance with claim 1 wherein any monomer present in the reaction zone which would otherwise include a hydroxyl group and/or an amine group is provided as an acetate ester and/or an acetamide.

Claim 7

Dependent Claim 25 words

A process in accordance with claim 1 wherein said aromatic monomer which is provided in said molar excess is HO--Ar--OH, or an esterified derivative thereof.

Claim 8

Dependent Claim 29 words

A process in accordance with claim 1 wherein said aromatic monomer which is provided in said molar excess is H 2 N--Ar--NH 2 , or an amidated derivative thereof.

Claim 9

Dependent Claim 29 words

A process in accordance with claim 1 wherein said aromatic monomer which is provided in said molar excess is HO--Ar--NH 2 , and/or an esterified and/or amidated derivative thereof.

Claim 10

Dependent Claim 34 words

A process in accordance with claim 1 wherein said aromatic monomer which is provided in said molar excess is provided in the polymerization zone in a molar excess of approximately 0.5 to 4 percent.

Claim 11

Dependent Claim 36 words

A process in accordance with claim 1 wherein said polyester product exhibits an inherent viscosity of approximately 0.8 to 10.0 dl./g. when dissolved in a concentration of 0.1 percent by weight in pentafluorophenol at 60° C.

Claim 12

Dependent Claim 130 words

A process in accordance with claim 1 wherein said polyester product consists essentially of moieties I and II which optionally may include substitution of at least some of the hydrogen atoms present upon an aromatic ring wherein: I is ##STR13## and II is ##STR14## with said optional substitution if present being selected from the group consisting of an alkyl group of 1 to 4 carbon atoms, an alkoxy group of 1 to 4 carbon atoms, halogen, phenyl, and mixtures of the foregoing, and wherein said polyester comprises approximately 10 to 90 mole percent of moiety I, and approximately 10 to 90 mole percent of moiety II, and which additionally incorporates an approximately 0.25 to 4 percent of said units derived from said aromatic monomer which is provided in molar excess.

Claim 13

Dependent Claim 215 words

A process in accordance with claim 1 wherein said product consists essentially of moieties I, II, and optionally III, which optionally may include substitution of at least some of the hydrogen atoms present upon an aromatic ring wherein: I is ##STR15## II is ##STR16## where Ar comprises at least one aromatic ring and where Z is NH or NR where R is an alkyl group of 1 to 6 carbon atoms or an aryl group, and III is ##STR17## wherein at least some of the hydrogen atoms present upon the rings optionally may be replaced by substitution selected from the group consisting of an alkyl group of 1 to 4 carbon atoms, an alkoxy group of 1 to 4 carbon atoms, halogen, phenyl, and mixtures thereof, and wherein moiety I is present in a concentration of approximately 10 to 90 mole percent, moiety II is present in a concentration of approximately 5 to 45 mole percent, and moiety III is present in a concentration of approximately 0 to 45 mole percent, with the total concentrations of moieties I and III being within the range of approximately 55 to 95 mole percent, and which additionally incorporates an approximately 0.25 to 4 percent of said units derived from said aromatic monomer which is provided in molar excess.

Claim 14

Dependent Claim 30 words

A polyester formed in accordance with the process of claim 1 which is capable of forming an anisotropic melt phase, and is substantially incapable of further chain growth upon heating.

Claim 15

Dependent Claim 173 words

In a process for the formation within a polymerization zone of a polyester which is capable of forming an anisotropic melt phase through a polymerization reaction of ester-forming monomers to form a polymer which consists essentially of moieties I and II wherein: I is ##STR18## and II is ##STR19## wherein said polyester comprises approximately 25 to 45 mole percent of moiety I, and approximately 55 to 75 mole percent of moiety II; the improvement of providing in the polymerization zone during said polymerization reaction an approximately 0.25 to 4 percent molar excess of an aromatic monomer of the formula: HO--Ar--OH, and/or an esterified derivative thereof, which during the polymerization reaction imparts dioxyaryl units to the interior of the polymer chains and causes the polymer chains to end in hydroxy end groups and/or an esterified derivative thereof, wherein the polymer chains achieve a predetermined average chain length through the depletion of other monomers present in the polymerization zone to yield a polyester product which is substantially incapable of additional chain growth upon subsequent heating.

Claim 16

Dependent Claim 173 words

In a process for the formation within a polymerization zone of a polyester which is capable of forming an anisotropic melt phase through a polymerization reaction of ester-forming monomers to form a polymer which consists essentially of moieties I and II wherein: I is ##STR18## and II is ##STR19## wherein said polyester comprises approximately 25 to 45 mole percent of moiety I, and approximately 55 to 75 mole percent of moiety II; the improvement of providing in the polymerization zone during said polymerization reaction an approximately 0.25 to 4 percent molar excess of an aromatic monomer of the formula: HO--Ar--OH, and/or an esterified derivative thereof, which during the polymerization reaction imparts dioxyaryl units to the interior of the polymer chains and causes the polymer chains to end in hydroxy end groups and/or an esterified derivative thereof, wherein the polymer chains achieve a predetermined average chain length through the depletion of other monomers present in the polymerization zone to yield a polyester product which is substantially incapable of additional chain growth upon subsequent heating.

Claim 17

Dependent Claim 17 words

A process in accordance with claim 14 wherein said polymerization reaction is carried out in the melt.

Claim 18

Dependent Claim 39 words

A process in accordance with claim 14 wherein the oxy portions of the ester-forming monomers which form moieties I and II are provided in said polymerization zone as lower acyl esters of about 2 to about 4 carbon atoms.

Claim 19

Dependent Claim 30 words

A process in accordance with claim 14 wherein the oxy portions of the ester-forming monomers which form moieties I and II are provided in said polymerization zone as acetate esters.

Claim 20

Dependent Claim 25 words

A process in accordance with claim 14 wherein the aromatic monomer which is provided in a molar excess is 2,6-dihydroxynaphthalene and/or an esterified derivative thereof.

Claim 21

Dependent Claim 25 words

A process in accordance with claim 14 wherein the aromatic monomer which is provided in a molar excess is p,p'-biphenol and/or an esterified derivative thereof.

Claim 22

Dependent Claim 37 words

A process in accordance with claim 14 wherein the aromatic monomer which is provided in said molar excess is provided in said polymerization zone as a lower acryl ester of about 2 to about 4 carbon atoms.

Claim 23

Dependent Claim 28 words

A process in accordance with claim 14 wherein the aromatic monomer which is provided in said molar excess is provided in said polymerization zone as an acetate ester.

Claim 24

Dependent Claim 34 words

A process in accordance with claim 14 wherein the aromatic monomer which is provided in said molar excess is provided in the polymerization zone in a molar excess of approximately 0.5 to 4 percent.

Claim 25

Dependent Claim 36 words

A process in accordance with claim 14 wherein said polyester product exhibits an inherent viscosity of approximately 0.8 to 10.0 dl./g. when dissolved in a concentration of 0.1 percent by weight in pentafluorophenol at 60° C.

Claim 26

Dependent Claim 30 words

A polyester formed in accordance with the process of claim 14 which is capable of forming an anisotropic melt phase, and is substantially incapable of further chain growth upon heating.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1989-01-27	1989-07-29	1990-01-28	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	1993-01-27	1993-07-29	1994-01-28	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	1997-01-27	1997-07-29	1998-01-28	$7700.00	Window Closed / Lapsed

Process for forming thermally stable thermotropic liquid crystalline polyesters of predetermined chain length utilizing aromatic hydroxyl monomer and/or aromatic amine monomer

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