# US 11,306,206 B2 · Vacuum-assisted co-extrusion of flexible fibres and the moldable thermoplastic composites produced

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- Number: US 11,306,206 B2
- Document ID: US11306206B2
- Status: Granted
- Kind: B2
- Application number: 16/320,567
- Filed: 2017-07-25
- Published: 2019-05-30
- Granted: 2022-04-19
- Earliest claimed: 2016-07-27
- Assignees: FPInnovations
- Applicants: FPInnovations
- Inventors: Wadood Yasser Hamad; Shunxing Su; Norman Roberts; Otman Oulanti; Michelle Agnes Ricard; Chuanwei Miao
- Web page: https://patentgrep.com/patent/US11306206B2

## CPC

- C08L 97/02: Lignocellulosic material, e.g. wood, straw or bagasse {(manufacture of articles made from lignocellulosic material by dry processes B27N)}
- B29B 7/483: {the other mixing parts being discs perpendicular to the screw axis}
- B29B 7/488: {Parts, e.g. casings, sealings; Accessories, e.g. flow controlling or throttling devices (discharging B29B7/582; feeding B29B7/60)}
- B29B 7/489: {Screws (B29B7/482 takes precedence)}
- B29B 7/726: {Measuring properties of mixture, e.g. temperature or density (B29B7/724 takes precedence)}
- B29B 7/728: {Measuring data of the driving system, e.g. torque, speed, power, vibration (B29B7/724 takes precedence)}
- B29B 7/823: {Temperature control}
- B29B 7/826: {Apparatus therefor}
- B29B 7/86: for working at sub- or superatmospheric pressure {(B01F33/70 takes precedence)}
- B29B 7/92: Wood chips or wood fibres
- B29C 48/00: Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor (extrusion blow-moulding B29C49/04)
- B29C 48/022: {characterised by the choice of material}
- B29C 48/144: {at the plasticising zone}
- B29C 48/18: the components being layers
- B29C 70/44: using isostatic pressure, e.g. pressure difference-moulding, vacuum bag-moulding, autoclave-moulding or expanding rubber-moulding
- C08J 3/203: {Solid polymers with solid and/or liquid additives}
- C08J 3/2053: {the additives only being premixed with a liquid phase}
- C08J 3/212: {and solid additives}
- C08L 23/06: Polyethylene
- C08L 23/12: Polypropene
- C08L 55/02: ABS [Acrylonitrile-Butadiene-Styrene] polymers
- C08L 67/04: Polyesters derived from hydroxycarboxylic acids, e.g. lactones (C08L67/06 takes precedence)
- B29B 9/06: in the form of filamentary material, e.g. combined with extrusion
- B29B 9/14: fibre-reinforced
- B29C 48/14: characterised by the particular extruding conditions, e.g. in a modified atmosphere or by using vibration
- B29C 48/54: with additional forward-feeding elements
- B29C 48/55: having reverse-feeding elements
- B29C 48/57: provided with kneading disc-like elements, e.g. with oval-shaped elements
- B29C 48/875: for achieving a non-uniform temperature distribution, e.g. using barrels having both cooling and heating zones
- B29C 2791/006: Using vacuum
- B29K 2001/00: Use of cellulose, modified cellulose or cellulose derivatives, e.g. viscose, as moulding material
- B29K 2101/12: Thermoplastic materials
- B29K 2311/14: Wood, e.g. woodboard or fibreboard
- C08J 2323/06: Polyethene
- C08J 2323/12: Polypropene
- C08J 2367/04: Polyesters derived from hydroxy carboxylic acids, e.g. lactones (C08J2367/06 takes precedence)
- C08L 2205/03: containing three or more polymers in a blend
- C08L 2205/08: containing additives to improve the compatibility between two polymers
- C08L 2205/16: Fibres; Fibrils
- C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06)
- B29B: PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- 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)
- 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)
- B29K: INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR {MOULDS, } REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS

## Abstract

A composite and method for producing the composite by incorporating wood or wood pulp fibres with a suitable thermoplastic polymer and coupling agent are described. Homogeneous, void-free transparent/translucent thermoplastic materials in the form of pellets, films or three-dimensional moldable products are produced. The wood pulp fibres can be discrete natural fibres, and flexible assemblies of nano to micro elements, e.g., assemblies of aggregated carbon nanotubes. It is also possible to use our vacuum-assisted co-extrusion process to produce hybrid composites comprising the wood pulp fibre and a further rigid fibre, like glass or carbon fibres, and a flexible fibre or fibrillar network, like cellulose fibres or cellulose filaments. The thermoplastic resin can be, but not limited to, polyolefins, like polypropylene or polyethylene, or polyesters, like polylactic acid, or co-polymers, like acrylonitrile-butadiene-styrene terpolymer.

## Claims

### Claim 1

A composite comprising:
31 to 97.9 wt. % of a thermoplastic resin;
0.1 to 10 wt. % of a compatibilizer comprising a maleic anhydride content greater than 40 mg KOH/g and less than 50 mg KOH/g, and molecular weight between 8 000 and 10 000; and
2 to 63 wt. % of wood pulp fibres and/or a filamentous material, wherein the composite comprises less than 0.5 wt. % of water, wherein said wood pulp fibres are tube-like and conformable, wherein the composite comprises a Melt Flow Rate of 10 to 22 g/10 min measured at 230° C. / 2.16 kg according to ASTM D1238, and wherein the composite has a tensile strength at yield of from 29.7 to 51.2 MPa.

### Claim 2 (depends on 1)

The composite of claim 1, wherein said composite comprises between 40% wt. % to 63% of wood pulp fibres and/or filamentous material.

### Claim 3 (depends on 1)

The composite of claim 1, wherein the thermoplastic is a polyolefin, a polyester or a co-polymer resin.

### Claim 4 (depends on 1)

The composite of claim 1, wherein the polyolefin is a polypropylene or a polyethylene.

### Claim 5 (depends on 1)

The composite of claim 1, wherein the polyester is a polylactic acid.

### Claim 6 (depends on 1)

The composite of claim 1, wherein the copolymer is an acrylonitrile-butadienestyrene terpolymer.

### Claim 7 (depends on 1)

The composite of claim 1, wherein the thermoplastic resin is 55 to 90 wt. % of the composite.

### Claim 8 (depends on 1)

The composite of claim 1 further comprising 10 to 20 wt. % glass fibres.

### Claim 9 (depends on 1)

The composite of claim 1, wherein the filamentous material is selected from the group consisting of cellulose filaments and carbon nanofibres.

### Claim 10 (depends on 1)

A method for producing a composite as defined in claim 1 comprising:
providing an aqueous suspension of tube-like and conformable wood pulp fibres and cellulose filamentous material or providing tube-like and conformable dry wood pulp fibres and dry pulp filamentous material;
providing a compatibilizer comprising a maleic anhydride content greater than 40 mg KOH/g and less than 50 mg KOH/g, and molecular weight between 8 000 and 10 000;
mixing the wood pulp fibres aqueous suspension or the dry wood pulp fibers and dry pulp filamentous material, with the compatibilizer to produce a grafted fibre suitable for thermoplastic blending;
providing a thermoplastic resin in a vacuum assisted co-extruder and co-extruding the thermoplastic resin and the grafted fibre at controlled temperature to produce the composite, said composite comprising up to 63 wt. % of wood pulp fibres and/or filamentous material.

### Claim 11 (depends on 10)

The method of claim 10, wherein the cellulose filamentous material is selected from the group consisting of cellulose filaments and carbon nanofibres.

### Claim 12 (depends on 10)

The method of claim 10, wherein the aqueous suspension of wood pulp fibre and filamentous material comprises from 30 to 40 wt. % solids.

### Claim 13 (depends on 10)

The method of claim 10, further comprising providing glass fibres with the aqueous suspension of wood pulp fibre and cellulose filamentous material or with the dry wood pulp fibers and dry filamentous material.

### Claim 14 (depends on 10)

The method of claim 10, wherein the thermoplastic is a polyolefin, a polyester or a co-polymer.

### Claim 15 (depends on 10)

The method of claim 10, wherein the copolymer is an acrylonitrile-butadienestyrene terpolymer.

### Claim 16 (depends on 13)

The method of claim 13, wherein the polyolefin is a propylene or a polyethylene.

### Claim 17 (depends on 13)

The method of claim 13, wherein the polyester is a polylactic acid.

### Claim 18 (depends on 10)

The method of claim 10, wherein the dry pulp filamentous material is selected from the group consisting of cellulose filaments, clay platelets and carbon nanofibres.