# US 2008/0185751 A1 · Polybenzimidazole-polyetherketoneketone blends and miscible blends

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- Number: US 2008/0185751 A1
- Document ID: US20080185751A1
- Status: Published application
- Kind: A1
- Application number: 11/671,169
- Filed: 2007-02-05
- Published: 2008-08-07
- Earliest claimed: 2007-02-05
- Assignees: PBI Performance Products, Inc.
- Inventors: Bobby G. Dawkins; Michael Gruender; Gregory S. Copeland; Tim Hsu
- Web page: https://patentgrep.com/patent/US20080185751A1

## CPC

- C08L 79/04: Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- B29C 48/40: using two or more parallel screws {or at least two parallel non-intermeshing screws}, e.g. twin screw extruders
- B29C 48/625: characterised by the ratio of the threaded length of the screw to its outside diameter [L/D ratio]
- B29C 48/793: upstream of the plasticising zone, e.g. heating in the hopper
- B29C 48/802: {Heating}
- B29C 48/832: {Heating}
- B29C 48/865: {Heating}
- B29C 48/875: for achieving a non-uniform temperature distribution, e.g. using barrels having both cooling and heating zones
- B29C 48/92: Measuring, controlling or regulating
- C08G 65/4012: {Other compound (II) containing a ketone group, e.g. X-Ar-C(=O)-Ar-X for polyetherketones}
- C08G 73/22: Polybenzoxazoles
- C08J 3/005: {Processes for mixing polymers}
- C08L 65/00: Compositions of macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain (C08L7/00 - C08L57/00, C08L61/00 take precedence); Compositions of derivatives of such polymers
- C08L 71/00: Compositions of polyethers obtained by reactions forming an ether link in the main chain (of polyacetals C08L59/00; of epoxy resins C08L63/00; of polythioether-ethers C08L81/02; of polyether-sulfones C08L81/06); Compositions of derivatives of such polymers
- B29C 48/022: {characterised by the choice of material}
- B29C 48/09: Articles with cross-sections having partially or fully enclosed cavities, e.g. pipes or channels
- B29C 48/83: {Heating or cooling the cylinders}
- C08G 2261/3442: Polyetherketones
- C08G 2650/40: containing ketone groups, e.g. polyarylethylketones, PEEK or PEK
- C08J 2365/00: Characterised by the use of macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain (C08J2307/00 - C08J2357/00, C08J2361/00 take precedence); Derivatives of such polymers
- C08J 2371/00: Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J 2379/04: Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06)
- B29C: SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING (making preforms B29B11/00; making laminated products by combining previously unconnected layers which become one product whose layers will remain together B32B37/00 - B32B41/00)
- C08G: MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08J: WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H (working, e.g. shaping, of plastics B29)

## Abstract

A process for producing a solution blend of a polybenzimidazole (PBI) and a polyetherketoneketone (PEKK). The PBI is mixed with sulfuric acid at a temperature between 40° C. and 80° C. for 30 minutes to 2 hours to produce a PBI solution then cooled to room temperature to form a cooled PBI solution. Then PEKK is added to the cooled PBI solution to form a mixture and that mixture is stirred from 30 minutes to 2 hours at room temperature to form a stirred mixture. The stirred mixture is poured into an excess of water being stirred swiftly to form an aqueous mixture. The aqueous mixture is filtered to produce a blend. The blend is washed with water and dried. The resulting blend can yield a blend in all proportion from 1/99 PBI/PEKK to 99/1 PBI/PEKK.

## Claims

### Claim 1

A process for producing a solution blend of a polybenzimidazole (PBI) and a polyetherketoneketone (PEKK) which comprises the steps of:
providing a polybenzimidazole (PBI) and a polyetherketoneketone (PEKK);
mixing said PBI with sulfuric acid at a temperature between 40° C. and 80° C. for 30 minutes to 2 hours to produce a PBI solution;
cooling said PBI solution to room temperature to form a cooled PBI solution;
adding said PEKK to said cooled PBI solution to form a mixture;
stirring said mixture from 30 minutes to 2 hours at room temperature to form a stirred mixture;
pouring said stirred mixture into an excess of water being stirred swiftly to form an aqueous mixture;
filtering said aqueous mixture to remove the water and sulfuric acid to produce a blend;
washing said blend with water; and
drying said blend to yield a blend in all proportion from 1/99 PBI/PEKK to 99/1 PBI/PEKK.

### Claim 2 (depends on 1)

The process for producing a blend of a polybenzimidazole (PBI) and a polyetherketoneketone (PEKK) according to claim 1 where sulfuric acid has a concentration of between 85% and 110%.

### Claim 3 (depends on 1)

The process for producing a blend of a polybenzimidazole (PBI) and a polyetherketoneketone (PEKK) according to claim 1 further comprising the steps of:
neutralizing said blend in a base to produce a neutralized blend;
washing said neutralized blend in water to produce a washed blend; and
drying said washed blend to yield a blend in all proportion from 1/99 PBI/PEKK to 99/1 PBI/PEKK.

### Claim 4

A process for producing a solution blend of a polybenzimidazole (PBI) and a polyetherketoneketone (PEKK) which comprises the steps of:
providing a polybenzimidazole (PBI) and a polyetherketoneketone (PEKK);
providing a strong acid which is selected from a group consisting of: sulfuric acid, methane sulfonic acid, trifluoromethane sulfonic acid, trifluoroacetic acid, dichloroacetic acid, formic acid and combinations thereof;
mixing said PBI and PEKK with said strong acid at a temperature between 40° C. and 80° C. for 30 minutes to 2 hours to produce a mixture;
cooling said mixture to room temperature;
dropping said mixture into a bath where said bath is selected from the group of water or a water methanol blend;
stirring swiftly said mixture and said bath to form an aqueous mixture;
filtering said aqueous mixture to remove the water and strong acid to produce a blend;
washing said blend with water; and
drying said blend to yield a blend in all proportion from 1/99 PBI/PEKK to 99/1 PBI/PEKK.

### Claim 5 (depends on 1)

The process for producing a blend of a polybenzimidazole (PBI) and a polyetherketoneketone (PEKK) according to claim 1 where said process is performed at atmospheric pressure.

### Claim 6 (depends on 5)

The process for producing a blend of a polybenzimidazole (PBI) and a polyetherketoneketone (PEKK) according to claim 5 where said process is absent of added pressure.

### Claim 7 (depends on 1)

The process for producing a blend of a polybenzimidazole (PBI) and a polyetherketoneketone (PEKK) according to claim 1 where the step of being swiftly stirred is done in a Waring blender.

### Claim 8 (depends on 3)

The process for producing a blend of a polybenzimidazole (PBI) and a polyetherketoneketone (PEKK) according to claim 3 where said base is ammonium hydroxide.

### Claim 9 (depends on 3)

The process for producing a blend of a polybenzimidazole (PBI) and a polyetherketoneketone (PEKK) according to claim 3 where said drying step is performed at a temperature from 90° C. to 180° C.

### Claim 10 (depends on 9)

The process for producing a blend of a polybenzimidazole (PBI) and a polyetherketoneketone (PEKK) according to claim 9 where said drying step is performed from 4 to 12 hours.

### Claim 11 (depends on 10)

The process for producing a blend of a polybenzimidazole (PBI) and a polyetherketoneketone (PEKK) according to claim 10 where said drying step is performed in a vacuum.

### Claim 12 (depends on 1)

The process for producing a blend of a polybenzimidazole (PBI) and a polyetherketoneketone (PEKK) according to claim 1 where said blend is a miscible blend of a polybenzimidazole (PBI) and a polyetherketoneketone (PEKK) where said blend is miscible in all proportions from 50/50 to 90/10 (PBI/PEKK).

### Claim 13 (depends on 12)

The process for producing said miscible blend of a polybenzimidazole (PBI) and a polyetherketoneketone (PEKK) according to claim 12 where said blend has a glass transition temperature, Tg, of greater than 400° C.

### Claim 14 (depends on 1)

A miscible blend of a polybenzimidazole (PBI) and a polyetherketoneketone (PEKK) made by the process of claim 1 where said blend is miscible in all proportions from 50/50 to 90/10 (PBI/PEKK) having a glass transition temperature, Tg, of greater than 400° C.

### Claim 15 (depends on 1)

A miscible blend of a polybenzimidazole (PBI) and a polyetherketoneketone (PEKK) made by the process of claim 1 where said blend has from 50/50 to 90/10 (PBI/PEKK) where said blend has a weight loss of less than 20% at 600° C.

### Claim 16 (depends on 1)

A miscible blend of a polybenzimidazole (PBI) and a polyetherketoneketone (PEKK) made by the process of claim 1 where said blend has from 50/50 to 90/10 (PBI/PEKK) where said blend has a weight loss of 30% or less at 800° C.

### Claim 17

A process for producing a melt blend of a polybenzimidazole (PBI) and a polyetherketoneketone (PEKK) which comprises the steps of:
providing a polybenzimidazole (PBI) and a polyetherketoneketone (PEKK);
providing an extruder with a plurality of heating zones;
pre-dry-mixing said PBI with said PEKK to obtain a dry mix;
feeding said dry mix to said extruder;
setting said heating zones in the range 240° C. to 410° C.;
melting said dry mix blend as it passes through said extruder; and
obtaining said melt blend of PBI/PEKK in all proportion from 1/99 PBI/PEKK to 80/20 PBI/PEKK.

### Claim 18 (depends on 18)

The process for producing a melt blend of a polybenzimidazole (PBI) and a polyetherketoneketone (PEKK) according to claim 18 where said extruder is a screw extruder where said screw is run in a range of 30 to 160 rpm.

### Claim 19 (depends on 18)

A miscible blend of a polybenzimidazole (PBI) and a polyetherketoneketone (PEKK) made by the process of claim 18 where said blend has from 60/40 to 80/20 (PBI/PEKK) where said blend has a weight loss of less than 20% at 600° C.

### Claim 20 (depends on 18)

A miscible blend of a polybenzimidazole (PBI) and a polyetherketoneketone (PEKK) made by the process of claim 18 where said blend has from 60/40 to 80/20 (PBI/PEKK) where said blend has a glass transition temperature, Tg, of greater than 400° C.
