WO2009000408A1 - Verfahren zur herstellung eines leitfähigen polymerverbundwerkstoffs - Google Patents

Verfahren zur herstellung eines leitfähigen polymerverbundwerkstoffs Download PDF

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Publication number
WO2009000408A1
WO2009000408A1 PCT/EP2008/004611 EP2008004611W WO2009000408A1 WO 2009000408 A1 WO2009000408 A1 WO 2009000408A1 EP 2008004611 W EP2008004611 W EP 2008004611W WO 2009000408 A1 WO2009000408 A1 WO 2009000408A1
Authority
WO
WIPO (PCT)
Prior art keywords
carbon nanotubes
polymer
cnt
screw extruder
extruder
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/EP2008/004611
Other languages
German (de)
English (en)
French (fr)
Inventor
Michael Bierdel
Sigurd Buchholz
Volker Michele
Leslaw Mleczko
Reiner Rudolf
Aurel Wolf
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Covestro Deutschland AG
Original Assignee
Bayer MaterialScience AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Family has litigation
First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=39683963&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=WO2009000408(A1) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by Bayer MaterialScience AG filed Critical Bayer MaterialScience AG
Priority to JP2010513705A priority Critical patent/JP2010530925A/ja
Priority to CN200880021617A priority patent/CN101687354A/zh
Priority to AT08759138T priority patent/ATE520515T1/de
Priority to EP08759138A priority patent/EP2160278B1/de
Publication of WO2009000408A1 publication Critical patent/WO2009000408A1/de
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00Making granules
    • B29B9/12Making granules characterised by structure or composition
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00Mixing; Kneading
    • B29B7/30Mixing; Kneading continuous, with mechanical mixing or kneading devices
    • B29B7/58Component parts, details or accessories; Auxiliary operations
    • B29B7/60Component parts, details or accessories; Auxiliary operations for feeding, e.g. end guides for the incoming material
    • B29B7/603Component parts, details or accessories; Auxiliary operations for feeding, e.g. end guides for the incoming material in measured doses, e.g. proportioning of several materials
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00Mixing; Kneading
    • B29B7/80Component parts, details or accessories; Auxiliary operations
    • B29B7/86Component parts, details or accessories; Auxiliary operations for working at sub- or superatmospheric pressure
    • BPERFORMING OPERATIONS; TRANSPORTING
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    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00Making granules
    • B29B9/02Making granules by dividing preformed material
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    • BPERFORMING OPERATIONS; TRANSPORTING
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    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/04Particle-shaped
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    • B29C48/03Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82BNANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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    • CCHEMISTRY; METALLURGY
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    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/005Reinforced macromolecular compounds with nanosized materials, e.g. nanoparticles, nanofibres, nanotubes, nanowires, nanorods or nanolayered materials
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
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    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
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    • B29C2948/92Measuring, controlling or regulating
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    • BPERFORMING OPERATIONS; TRANSPORTING
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    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
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    • BPERFORMING OPERATIONS; TRANSPORTING
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    • B29C2948/92819Location or phase of control
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C48/40Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
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    • B29KINDEXING 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
    • B29K2067/00Use of polyesters or derivatives thereof, as moulding material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29KINDEXING 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
    • B29K2067/00Use of polyesters or derivatives thereof, as moulding material
    • B29K2067/006PBT, i.e. polybutylene terephthalate
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29KINDEXING 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
    • B29K2069/00Use of PC, i.e. polycarbonates or derivatives thereof, as moulding material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29KINDEXING 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
    • B29K2071/00Use of polyethers, e.g. PEEK, i.e. polyether-etherketone or PEK, i.e. polyetherketone or derivatives thereof, as moulding material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29KINDEXING 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
    • B29K2075/00Use of PU, i.e. polyureas or polyurethanes or derivatives thereof, as moulding material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29KINDEXING 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
    • B29K2077/00Use of PA, i.e. polyamides, e.g. polyesteramides or derivatives thereof, as moulding material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29KINDEXING 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
    • B29K2079/00Use of polymers having nitrogen, with or without oxygen or carbon only, in the main chain, not provided for in groups B29K2061/00 - B29K2077/00, as moulding material
    • B29K2079/08PI, i.e. polyimides or derivatives thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29KINDEXING 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
    • B29K2081/00Use of polymers having sulfur, with or without nitrogen, oxygen or carbon only, in the main chain, as moulding material
    • B29K2081/04Polysulfides, e.g. PPS, i.e. polyphenylene sulfide or derivatives thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29KINDEXING 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
    • B29K2081/00Use of polymers having sulfur, with or without nitrogen, oxygen or carbon only, in the main chain, as moulding material
    • B29K2081/06PSU, i.e. polysulfones; PES, i.e. polyethersulfones or derivatives thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29KINDEXING 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
    • B29K2105/00Condition, form or state of moulded material or of the material to be shaped
    • B29K2105/0005Condition, form or state of moulded material or of the material to be shaped containing compounding ingredients
    • B29K2105/002Agents changing electric characteristics
    • B29K2105/0023Agents changing electric characteristics improving electric conduction
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29KINDEXING 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
    • B29K2105/00Condition, form or state of moulded material or of the material to be shaped
    • B29K2105/0005Condition, form or state of moulded material or of the material to be shaped containing compounding ingredients
    • B29K2105/0044Stabilisers, e.g. against oxydation, light or heat
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29KINDEXING 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
    • B29K2105/00Condition, form or state of moulded material or of the material to be shaped
    • B29K2105/0005Condition, form or state of moulded material or of the material to be shaped containing compounding ingredients
    • B29K2105/0047Agents changing thermal characteristics
    • B29K2105/005Heat sensitisers or absorbers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29KINDEXING 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
    • B29K2105/00Condition, form or state of moulded material or of the material to be shaped
    • B29K2105/06Condition, form or state of moulded material or of the material to be shaped containing reinforcements, fillers or inserts
    • B29K2105/16Fillers
    • B29K2105/162Nanoparticles

Definitions

  • the invention relates to a method for producing an electrically conductive polymer composite with reduced surface resistance based on thermoplastic polymers and carbon nanotubes, wherein a carbon nanotube-polymer melt mixture in a double-shaft
  • Screw extruder is dispersed and then extruded.
  • the carbon nanotubes are hereinafter abbreviated to "CNT”.
  • a comparable method is known in principle from WO 2005/014259 A1. Thereafter, a batch CNT polymer blend is mixed in a miniature twin screw extruder with co-rotating conical shafts and a reflux channel and extruded after multiple passes through the extruder.
  • the method is suitable only for the laboratory scale, the processed amounts are 4 - 15 grams.
  • An industrial scale (i.e., tons per hour) throughput is not possible, or at least extremely difficult, because the underlying apparatuses are not suitable for continuous operation in large scale operations.
  • the dispersion of the CNT takes place here essentially by hydrodynamic forces.
  • WO 2001/092381 A1 describes a process in which a CNT polymer mixture is produced, wherein the dispersion of the CNT in the polymer melt is effected by hydrodynamic forces.
  • the process may be carried out in an extruder, a rheometer or a fiber spinning apparatus.
  • the object of the invention is to disperse strongly entangled CNT agglomerates with a mean diameter of 0.5-2 mm, as obtained, for example, according to WO 2006/050903 A2 by catalytic vapor deposition, in a polymer melt and to separate the CNTs and to distribute it homogeneously in a polymer such that the CNTs form a three-dimensional, electrically conductive network in the polymer.
  • the process for the dispersion of multi-walled carbon nanotubes (abbreviated as MWNT) should be suitable.
  • the method should be readily modifiable (applicable) for industrial scale flow rates, ie scalable to large throughput on a ton scale.
  • CNT carbon nanotubes
  • the specific mechanical energy input in the screw extruder to a value in the range of 0.1 kWh / kg to 1 kWh / kg, preferably from 0.2 kWh / kg to 0.6 kWh / kg and the minimum residence time to one Value is set in the range of 6 s to 90 s, preferably 8 s to 30 s.
  • the process according to the invention has the advantage that it is possible to produce CNT polymer composites with CNTs homogeneously distributed in the polymer matrix and high electrical conductivity, high thermal conductivity and very good mechanical properties on an industrial scale in an economically efficient manner.
  • multi-walled carbon nanotubes are used in the new process.
  • the carbon nanotubes are particularly preferably used in the form of agglomerates, the agglomerates in particular having a mean diameter in the range of 0.5 to 2 mm.
  • a further preferred method is characterized in that the carbon nanotubes have an average diameter of 3 to 100 nm, preferably 3 to 80 nm.
  • the CNTs disclosed in WO 2006/050903 A2 are particularly preferably used in the novel process.
  • thermoplastic polymer used is preferably at least one of the series polycarbonate, polyamide, polyester, in particular polybutylene terephthalate and polyethylene terephthalate, polyethers, thermoplastic polyurethane, polyacetal, fluoropolymer, in particular polyvinylidene fluoride, polyethersulfones, polyolefin, in particular polyethylene and polypropylene, polyimide, polyacrylate, in particular poly (methyl ) methacrylate, polyphenylene oxide, Polyphenylensulf ⁇ d, polyether ketone, polyaryletherketone, styrene polymers, especially polystyrene, styrene copolymers, in particular styrene-acrylonitrile copolymer, acrylate rubber (ASA), Acrylnitrilbutadienstyrolblockcopolymere and polyvinyl chloride used.
  • ASA acrylate rubber
  • the invention further provides a carbon nanotube polymer composite material obtained from the process according to the invention.
  • the invention also provides the use of the obtained by the novel carbon nanotube polymer composite material for the production of moldings.
  • Fig. 1 is a process diagram of a system for carrying out the method
  • Fig. 2 is a schematic longitudinal sectional view of the system used in the Fig. 1
  • FIG. 3 shows a measuring arrangement for determining the surface electrical resistance of the CNT
  • Fig. 1 consists in the core of a twin-screw extruder 1 with a
  • additives e.g., antioxidants, UV stabilizers, mold release agents
  • CNT optionally, additives (e.g., antioxidants, UV stabilizers, mold release agents), CNT, optionally
  • Polymer 2 are conveyed via metering screws 8-11 into the feed hopper 2 of the extruder 1.
  • the melt strands emerging from the nozzle plate 3 are cooled in a water bath 6 and solidified and then comminuted with a granulator 7.
  • the twin-screw extruder 1 (see FIG. 2) has, inter alia, a housing consisting of ten parts, in which two worm shafts (not shown) rotating in the same direction and meshing with one another are arranged.
  • the components to be compounded including the CNT agglomerates are fed to the extruder 1 via the feed hopper 2 arranged on the housing part 12.
  • a feed zone which preferably consists of threaded elements with a pitch of 2 times the screw shaft diameter (short: 2 D) to 0.9 D.
  • the threaded elements promote the CNT agglomerates together with the other constituents of the carbon nanotube polymer composite to the melting zone 14, 15, and intensify the CNT agglomerates by frictional forces between the solid polymer granules and the likewise solid phase CNT powder mixed and predispersed.
  • the melting zone which preferably consists of Knetblöcken; Alternatively, depending on the polymer, it is also possible to use a combination of kneading blocks and tooth mixing elements.
  • the melting zone 14, 15 the polymeric constituents are melted and the predispersed CNT and additives are further dispersed and mixed intensively with the remaining composite components.
  • the heating temperature of the extruder housing in the region of the melting zone 14, 15 is set to a value which is greater than the melting temperature of the polymer (in the case of semicrystalline thermoplastics) or the glass transition temperature (in the case of amorphous thermoplastics).
  • a post-dispersion zone is provided downstream of the melting zone 14, 15 between the conveying elements of the screw shafts. She shows kneading and mixing elements, which cause a frequent rearrangement of the melt streams and a broad residence time distribution. In this way, a particularly homogeneous distribution of CNT is achieved in the polymer melt. Very good results were achieved with tooth mixing elements. Furthermore, for mixing the CNT and screw mixing elements, eccentric discs, sudforderimplantation etc. can be used. Alternatively, several Nachdispergierzonen can be connected in series to intensify the fine dispersion.
  • the combination of predispersion in the solid phase, the main dispersion during the melting of the polymer (s) and the downstream fine dispersion, which takes place in the liquid phase, is important for achieving the most uniform possible CNT distribution in the polymer.
  • the removal of volatile substances takes place in a degassing zone in the housing part 20 via a degassing opening 4, which is connected to a suction device (not shown).
  • the degassing zone consists of threaded elements with a pitch of at least 1 D.
  • the last housing part 21 contains a pressure build-up zone, at the end of which the compounded and degassed product exits the extruder.
  • the pressure buildup zone 21 has threaded elements with a pitch between 0.5 D and 1, 5 D.
  • the CNT polymer composite granules obtained can then be further processed using all known thermoplastic processing methods.
  • moldings can be produced by injection molding.
  • two LeitsilberstMail 23, 24 are applied, whose length B coincides with their distance L, so that a square area sq (Square) is defined.
  • the electrodes of a resistance measuring device 25 are pressed onto the Leitsilberstsammlung 23, 24 and read the resistance value at the meter 25.
  • voltages up to 3xlO 7 ohms / sq 9 volts were used for resistors and from 3xlO 7 ohms / sq
  • Example 1 The incorporation of multi-walled carbon nanotubes (commercial product: Baytubes® C 150P (CNT produced by catalytic vapor deposition according to WO 2006/050903 A2), Manufacturer: Bayer MaterialScience AG) in polycarbonate (PC) (commercial product: Makrolon® 2800, manufacturer Bayer MaterialScience AG) is carried out on a ZSK 26Mc twin-screw extruder (Coperion Werner & Pfleiderer).
  • PC polycarbonate
  • ZSK 26Mc twin-screw extruder Coperion Werner & Pfleiderer
  • experiments 1 and 2 both the polymer granules and the CNT are metered into the extruder via the main intake or hopper 2.
  • experiments 3 and 4 comparativative experiments
  • the polymer is metered into the main intake 2 and the CNT is fed via a side feeder (dashed line in FIG. 2 in housing part 16) of the polymer melt.
  • the melt temperature is measured with a commercially available temperature sensor directly in the emerging at the nozzle plate 3 melt strand.
  • the number and diameter of incompletely dispersed CNT agglomerates contained in the carbon nanotube polymer composite are measured by a light microscope on a 5 cm long strand of the CNT polymer composite.
  • multi-walled carbon nanotubes commercial product: Baytubes® C 150P (CNT produced by catalytic vapor deposition according to WO 2006/050903 A2), manufacturer Bayer MaterialScience AG
  • PC polycarbonate
  • Makrolon® 2800 commercial product: Makrolon® 2800, manufacturer Bayer MaterialScience AG
  • the polymer granules and the CNT are metered through the main throat 2 of the extruder.
  • the granules obtained are then injection-molded into test specimens and measured their electrical surface resistance as shown in Fig. 3.
  • On the circular plates (specimens) produced by means of injection molding technology two LeitsilberstMail were applied, whose length B is equal to their distance L to each other.
  • the electrodes of a resistance measuring device were pressed onto the conductive silver strips and the resistance value was read off on the measuring device.
  • the measuring voltage used for resistors up to 3xlO was 7 ohms / sq 9 volts, and from 3xl0 7 ohms / sq to 100 volts.
  • the surface resistance of the pure Makrolon® 2800 is 10 16 ohms / sq according to the manufacturer's data sheet.
  • the minimum residence time was determined as follows:
  • multi-walled carbon nanotubes commercial product: Baytubes® C 150P (CNT produced by catalytic vapor deposition according to WO 2006/050903 A2), manufacturer Bayer Technology Services
  • PC polycarbonate
  • Makrolon® 2800 commercial product: Makrolon® 2800, manufacturer Bayer MaterialScience AG
  • the polymer granules and the CNT are metered through the main throat 2 of the extruder.
  • the granules obtained are then injection-molded into test specimens and measured their electrical surface resistance as shown in Fig. 3.
  • multiwalled carbon nanotubes commercial product: Baytubes® C 150P (CNT produced by catalytic vapor deposition according to WO 2006/050903 A2), manufacturer: Bayer MaterialScience AG
  • PBT polybutylene terephthalate
  • Pocan® B 1600, manufacturer Lanxess Germany GmbH is carried out by the process according to the invention on a ZSK 26Mc twin-screw extruder (Coperion Werner & Pfleiderer).
  • the polymer granules and the CNT are metered through the main throat 2 of the extruder.
  • the granules obtained are then injection-molded into test specimens and measured their electrical surface resistance as shown in Fig. 3.
  • the surface resistance of the pure Pocan® B 1600 is, according to Campus Database> 10 15 ohms / sq.
  • Example 5 (Variation of CNT content) The incorporation of multi-walled carbon nanotubes (commercial product: Baytubes® C 150P (CNT produced by catalytic vapor deposition according to WO 2006/050903 A2), manufacturer: Bayer MaterialScience AG) in polyamide 6 (PA 6) (commercial product: Durethan® B 29, manufacturer Lanxess Germany GmbH) takes place according to the method according to the invention on a ZSK 26Mc twin-screw extruder (Coperion Werner & Pfleiderer).
  • PA 6 polyamide 6
  • the polymer granules and the CNT are metered through the main throat 2 of the extruder.
  • the granules obtained are then injection-molded into test specimens and measured their electrical surface resistance as shown in Fig. 3.
  • the surface resistance of the pure Durethan® B 30, which is comparable to the Durethan® B 29 used, is 10 13 ohms / sq according to Campus Database.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Nanotechnology (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Composite Materials (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Extrusion Moulding Of Plastics Or The Like (AREA)
  • Conductive Materials (AREA)
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JP2010513705A JP2010530925A (ja) 2007-06-23 2008-06-10 導電性ポリマー複合材料の製造方法
CN200880021617A CN101687354A (zh) 2007-06-23 2008-06-10 用于生产导电聚合物复合材料的方法
AT08759138T ATE520515T1 (de) 2007-06-23 2008-06-10 Verfahren zur herstellung eines leitfähigen polymerverbundwerkstoffs
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ATE520515T1 (de) 2011-09-15
KR20100023887A (ko) 2010-03-04
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