Method for making polyetherimide

Claim 2

A process for making polyetherimide in a continuous manner which comprising (1) feeding molten aromatic bis(ether anhydride) and molten organic diamine into an extruder to produce a plural phase viscous melt, (2) conveying the plural phase liquid mixture of (1) to a mixing stage which effects a high degree of contact between the molten aromatic bis(ether anhydride) and molten organic diamine to produce a substantially uniform viscous melt as a result of intense kneading of the ingredients of the mixture, (3) conveying the resulting viscous melt of (2) to a mass transfer stage, where water of reaction is separated from the surface of the partially polymerized polyetherimide melt, (4) thereafter conveying the resulting melt to high shear and intensive mixing at a temperature in the range of from 250° C. to 350° C. and a pressure of from 1 to 5 atmospheres, and (5) separating high molecular weight polyetherimide therefrom along with the removal of final water of reaction,

Claim 3

A process in accordance with claim 1, where the polyetherimide resulting from the continuous steady state polymerization of the aromatic bis(ether anhydride) and organic diamine has an intrinsic viscosity in chloroform of at least 0.4.

Claim 4

A process in accordance with claim 1, where the polyetherimide consists essentially of chemically combined units of the formula ##STR10## where R is a member selected from ##STR11## and divalent organic radicals of the general formula, ##STR12## X is a member selected from the class consisting of divalent radicals of the formula, ##STR13## y is an integer from 1 to 5; and R 1 is a divalent organic radical selected from the class consisting of aromatic hydrocarbon radicals having from 6 to about 20 carbon atoms and halogenated derivatives thereof, alkylene radicals having from 2 to about 20 carbon atoms, cycloalkylene radicals having from 3 to about 20 carbon atoms, from C 2 to about C 8 alkylene terminated polydiorganosiloxanes and divalent radicals of the general formula, ##STR14## Q is a member selected from the class consisting of --O--,--S--,C.sub.x H.sub.2 x, x is an integer from 1 to 5 and n is 0 or 1.

Claim 5

A method in accordance with claim 1, where the aromatic bis(ether anhydride) has the formula, ##STR15## where R is a member selected from ##STR16## and divalent organic radicals of the general formula, ##STR17## X is a member selected from the class consisting of divalent radicals of the formula, ##STR18## and y is an integer from 1 to 5.

Claim 6

A method in accordance with claim 1, where the aromatic bis(ether anhydride) is a mixture of ##STR19## and up to 30 mole percent of benzophenone dianhydride, where R is a member selected from ##STR20## and divalent organic radicals of the general formula, ##STR21## X is a member selected from the class consisting of divalent radicals of the formula, ##STR22## and y is an integer from 1 to 5.

Claim 7

A method in accordance with claim 1, where the organic diamine has the formula, H.sub.2 N--R.sup.1 --NH.sub.2, where R 1 is a divalent organic radical selected from the class consisting of aromatic hydrocarbon radicals having from 6 to about 20 carbon atoms and halogenated derivatives thereof, alkylene radicals having from 2 to about 20 carbon atoms, cycloalkylene radicals having from 3 to about 20 carbon atoms, from C 2 to about C 8 alkylene terminated polydiorganosiloxanes and divalent radicals of the general formula, ##STR23## Q is a member selected from the class consisting of --O--,--S--,C.sub.x H.sub.2 x, x is an integer from 1 to 5 and n is 0 or 1.

Claim 8

A method in accordance with claim 1, where there is utilized an effective amount of a chain stopper.

Claim 9

A continuous polymerization process in accordance with claim 1, where there is utilized a ratio of from about 1.0 to 1.5 mole of organic diamine per mole aromatic bis(ether anhydride) in the feed mixture.

Claim 10

A continuous polymerization process in accordance with claim 1, where the extruder is operated during the mixing of the molten feed mixture of aromatic bis(ether anhydride) and organic diamine to provide a mixing factor of from 1 to 100,000.

Claim 11

A process for the continuous steady state polymerization of polyetherimides comprising (1) separately metering into an extruder an aromatic bis(ether anhydride) melt and an organic diamine melt in a preselected proportion to produce a plural phase molten blend under an inert atmosphere in the feed stage of the extruder, said feed stage being provided with melt conveying elements, (2) conveying the blend from said feed stage to a mixing stage of said extruder where viscous heating is accomplished and the components of said blend are partially polymerized, (3) conveying said liquid, partially polymerized polyetherimide to a mass transfer stage of said extruder, melt pool acceleration being accomplished in said mass transfer stage, and water of reaction being removed in said stage, (4) conveying said partially polymerized polyetherimide from said mass transfer stage to a second mixing stage of said extruder, melt pool deceleration and further polymerization of said polyetherimide being accomplished in said second stage, (5) conveying said further polymerized polyetherimide from said second mixing stage to an advanced polymerization stage where complete polymerization of said polyetherimide is accomplished with extended residence time, and (6) removing a high polymer polyetherimide from said advanced polymerization stage with removal of final water of reaction.

Claim 12

A process for the continuous steady state polymerization of polyetherimides comprising (1) separately metering into an extruder an aromatic bis(ether anhydride) melt and an organic diamine melt in a preselected proportion to produce a plural phase molten blend under an inert atmosphere in the feed stage of the extruder, said feed stage being provided with melt conveying elements, (2) conveying the blend from said feed stage to a mixing stage of said extruder where viscous heating is accomplished and the components of said blend are partially polymerized, (3) conveying said liquid, partially polymerized polyetherimide to a mass transfer stage of said extruder, melt pool acceleration being accomplished in said mass transfer stage, and water of reaction being removed in said stage, (4) conveying said partially polymerized polyetherimide from said mass transfer stage to a second mixing stage of said extruder, melt pool deceleration and further polymerization of said polyetherimide being accomplished in said second stage, (5) conveying said further polymerized polyetherimide from said second mixing stage to an advanced polymerization stage where complete polymerization of said polyetherimide is accomplished with extended residence time, and (6) removing a high polymer polyetherimide from said advanced polymerization stage with removal of final water of reaction.

Claim 13

The process of claim 10 wherein from 60 to 70% of the water of reaction is removed in said mass transfer stage and from 30 to 40% of said water of reaction is removed upon removal of the high polymer from said advanced polymerization stage.

Claim 14

The process of claim 10 wherein the elements in said first mixing stage of said extruder are zero and forward conveying kneading blocks.

Claim 15

The process of claim 12 wherein the temperature in said first mixing stage is raised to from 200° to 350° C. at a pressure of 2 to 6 atmospheres.

Claim 16

The process of claim 13 wherein the temperature is maintained at from 250° to 350° C. at the pressure is maintained at from 2 to 3 atmospheres.

Claim 17

The process of claim 10 wherein the elements in said mass transfer stage are open and medium pitch, forward conveying elements.

Claim 18

The process of claim 15 wherein the temperature in said mass transfer stage is maintained at from 250° to 325° C. at atmospheric pressure.

Claim 19

The process of claim 16 wherein the temperature is maintained at from 300° to 325° C.

Claim 20

The process of claim 10 wherein the elements in said second mixing stage are tight pitch forward conveying elements.

Claim 21

The process of claim 18 wherein the temperature in said second mixing stage is maintained at from 250° to 350° C. and the pressure is maintained at from 1 to 2 atmospheres.

Claim 22

The process of claim 19 wherein the temperature is maintained at from 300° to 350° C.

Claim 23

The process of claim 10 wherein the elements in said advanced polymerization stage of said extruder are tight pitch, forward conveying elements and said stage is provided with a restricted exit.

Claim 24

The process of claim 21 wherein the temperature in said advanced polymerization stage is maintained at from 300° to 400° C. and the pressure is maintained at from 1 to 50 atmospheres.

Claim 25

The process of claim 22 wherein the temperature is from 325° to 400° C. and the pressure is from 1 to 25 atmospheres.

Claim 26

The process of claim 10 wherein said extruder has two screws, said screws being co-rotating and intermeshing.

Claim 27

The process of claim 10 wherein the temperature of said first melt and said second melt are approximately 210° C.

Claim 28

The process of claim 10 wherein the said second mixing stage and said advanced polymerization stage are combined into a single process stage.

Claim 29

The process of claim 26 wherein the temperature and pressure in the combined said final stage are 250°-400° C. and 1-25 atmospheres.