# US 2019/0378634 A1 · Masterbatches for Preparing Composite Materials with Enhanced Conductivity Properties, Process and Composite Materials Produced

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- Number: US 2019/0378634 A1
- Document ID: US20190378634A1
- Status: Published application
- Kind: A1
- Application number: 16/548,588
- Filed: 2019-08-22
- Published: 2019-12-12
- Earliest claimed: 2013-08-01
- Assignees: Total Research & Technology Feluy
- Applicants: Total Research & Technology Feluy
- Inventors: Dimitri Rousseaux; Olivier Lhost; Philippe Lodefier; Eddi Scandino
- Web page: https://patentgrep.com/patent/US20190378634A1

## CPC

- H01B 1/24: the conductive material comprising carbon-silicon compounds, carbon or silicon
- B29C 70/58: comprising fillers only {, e.g. particles, powder, beads, flakes, spheres (B29C70/025 takes precedence, agglomerating hollow spheres to produce synthetic foam B29C70/66; compounding ingredients per se C08K)}
- B29C 70/882: {partly or totally electrically conductive, e.g. for EMI shielding (conductive floors or floor coverings H05F3/025; EMI shielding in general H05K9/00)}
- B32B 27/06: as the main or only constituent of a layer, {which is} next to another layer of {the same or of} a {different material (next to a layer of a particular substance B32B9/045; next to a bituminous or tarry layer B32B11/046; next to a water setting substance layer B32B13/12; next to a metal layer B32B15/08; next to a glass layer B32B17/10; next to a layer formed of natural mineral fibres or particles B32B19/045; next to a wood layer B32B21/08; next to a cellulosic plastic layer B32B23/08; next to a natural or synthetic rubber layer B32B25/08)}
- B32B 27/302: {comprising aromatic vinyl (co)polymers, e.g. styrenic (co)polymers}
- C08J 3/203: {Solid polymers with solid and/or liquid additives}
- C08J 3/22: using masterbatch techniques
- C08J 3/226: {using a polymer as a carrier}
- C08K 7/24: inorganic
- C08L 25/06: Polystyrene
- C08L 51/04: grafted on to rubbers
- C08L 55/02: ABS [Acrylonitrile-Butadiene-Styrene] polymers
- H01B 3/442: {from aromatic vinyl compounds}
- B29K 2025/06: {PS, i.e. polystyrene}
- B29K 2105/16: Fillers
- B29K 2507/04: Carbon
- B32B 2307/206: Insulating
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- C08J 2309/00: Characterised by the use of homopolymers or copolymers of conjugated diene hydrocarbons
- C08J 2325/06: Polystyrene
- C08J 2325/10: with conjugated dienes
- C08J 2327/06: Homopolymers or copolymers of vinyl chloride
- C08J 2333/12: Homopolymers or copolymers of methyl methacrylate
- C08J 2351/04: grafted on to rubbers
- C08J 2355/02: Acrylonitrile-Butadiene-Styrene [ABS] polymers
- C08J 2367/02: Polyesters derived from dicarboxylic acids and dihydroxy compounds; (C08J2367/06 takes precedence)
- C08J 2369/00: Characterised by the use of polycarbonates; Derivatives of polycarbonates
- C08J 2371/12: Polyphenylene oxides
- C08J 2379/02: Polyamines
- C08J 2381/06: Polysulfones; Polyethersulfones
- C08J 2425/06: Polystyrene
- H01B: CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES (selection for magnetic properties H01F1/00; waveguides H01P {; printed circuits H05K})
- 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)
- B32B: LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- 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)
- C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09)
- C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06)
- 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
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES

## Abstract

The present invention relates to a masterbatch to for use in a process of preparing a composite material, the masterbatch comprising a blend of a first amorphous polymer with carbon nanotubes, and at least 5% by weight of carbon nanotubes based on the total weight of the masterbatch, preferably from 5% to 15%, wherein the masterbatch exhibit a high load melt flow index HLMI1 of less than 40 g/10 min determined at 200° C. under a load of 21.6 kg according to ISO1133 and the first amorphous polymer has a melt flow index MFI1 of at least 10 g/10 min determined at 200° C. under a load of 5 kg according to ISO1133H. The invention also relates to the process for preparing such masterbatch and to process of preparing a composite material using said masterbatch.

## Claims

### Claim at position 1

-15. (canceled)

### Claim 16

A process for preparing a composite material comprising a polymer composition and carbon nanotubes, characterized in that said polymer composition comprises a mixture of a first and a second amorphous polymer and the composite material comprises from 0.05 to 1.95% by weight of carbon nanotubes based on the total weight of the composite material as determined according to ISO 11358, and in that the composite material has a surface resistivity of at most 1×104 Ohm/sq, said process comprising the steps of:
b. providing a masterbatch comprising a first amorphous polymer and at least 5%, and preferably from 5% to 15%, by weight of carbon nanotubes based on the total weight of the masterbatch as determined according to ISO 11358, and wherein the first amorphous polymer has a melt flow index MFI1 of at least 10 g/10 min determined at 200° C. under a load of 5 kg according to ISO1133H, wherein the first amorphous polymer is selected from the group consisting of polystyrene, modified-polystyrene, acrylonitrile-butadiene-styrene, polycarbonate, styrene acrylonitrile, poly(methyl methacrylate), poly(vinyl chloride), polybutadiene, polybutylene terephthalate, poly(p-phenylene oxide), polysulfone, polyethersulfone, polyethylenimine, polyphenylsulfone, acrylonitrile styrene acrylate and any combination thereof, wherein the masterbatch comprises at least 80% by weight of the first amorphous polymer, and wherein the masterbatch comprises a surface resistivity of at most 1×102 Ohm/sq as determined according to CEI 60167;
c. providing a second amorphous polymer having a glass transition temperature Tg2;
d. blending together the masterbatch and the second amorphous polymer by extrusion in an extruder at a barrel temperature ranging from Tg2+100° C. to Tg2+200° C., preferably ranging from Tg2+120° C. to Tg2+180° C.,
the glass transition temperature being determined according to according to ISO 11357-2:2013.

### Claim 17 (depends on 16)

The process according to claim 16 wherein the masterbatch comprises a blend of the first amorphous polymer with carbon nanotubes, at least 5% by weight of carbon nanotubes based on the total weight of the masterbatch as determined according to ISO 11358, and having a high load melt flow index HLMI1 of less than 40 g/10 min determined at 200° C. under a load of 21.6 kg according to ISO1133, the masterbatch being characterized in that the first amorphous polymer has a melt flow index MFI1 of at least 10 g/10 min determined at 200° C. under a load of 5 kg according to ISO1133H.

### Claim 18 (depends on 16)

The process according to claim 16 characterized in that the process includes, before (b), a process of preparing the masterbatch comprising:
a1 providing carbon nanotubes;
a2. providing an first amorphous polymer, said first amorphous polymer having a glass transition temperature Tg1, and a melt flow index MFI1 of at least 10 g/10 min determined at 200° C. under a load of 5 kg according to ISO1133H;
a3. blending together said carbon nanotubes and said first amorphous polymer by extrusion in an extruder at a barrel temperature ranging from Tg1 to Tg1+80° C., preferably Tg1+5° C. to Tg1+50 ° C., the glass transition temperature being determined according to ISO 11357-2:2013.

### Claim 21 (depends on 16)

The process according to claim 16, the first amorphous polymer having a melt flow index MFI1 and second amorphous polymer having a melt flow index MFI2, the process being characterized in that it further comprises the step of selecting the first and second amorphous polymer so that MFI1 has a value of at least twice the value of MFI2.

### Claim 22 (depends on 16)

The process according to claim 16 characterized in that said composite material comprises from 0.05 to 0.95% by weight of carbon nanotubes based on the total weight of the composite material as determined according to ISO 11358.

### Claim 23 (depends on 16)

The process according to claim 16, wherein the first amorphous polymer further comprises 0.01 to 4.0 by weight of one or more additive based on the total weight of the masterbatch, the one or more additive being selected from waxes, tristearin, zinc stearate, calcium stearate, magnesium stearate, erucyl amide, oleic acid amide, ethylene-acrilyc acid copolymer, ethylene vinyl acetate copolymer and cetyl trimethyl ammonium bromide.