Classifications

• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
  • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
  • H01B1/20—Conductive material dispersed in non-conductive organic material
  • H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B82—NANOTECHNOLOGY
  • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
  • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
  • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
  • C08J9/0066—Use of inorganic compounding ingredients
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
  • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
  • C08J9/0066—Use of inorganic compounding ingredients
  • C08J9/0071—Nanosized fillers, i.e. having at least one dimension below 100 nanometers
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
  • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
  • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
  • C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
  • C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
  • C08K3/00—Use of inorganic substances as compounding ingredients
  • C08K3/02—Elements
  • C08K3/04—Carbon
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
  • C08K3/00—Use of inorganic substances as compounding ingredients
  • C08K3/02—Elements
  • C08K3/04—Carbon
  • C08K3/041—Carbon nanotubes
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L101/00—Compositions of unspecified macromolecular compounds
  • C08L101/12—Compositions of unspecified macromolecular compounds characterised by physical features, e.g. anisotropy, viscosity or electrical conductivity
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
  • C08K2201/00—Specific properties of additives
  • C08K2201/001—Conductive additives
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
  • C08K9/00—Use of pretreated ingredients
  • C08K9/04—Ingredients treated with organic substances

Definitions

• the present invention relates to a highly conductive polymer mixture comprising a composite carbon material and to a polymer composition comprising a composite carbon material having excellent economic and conductivity.
• Thermoplastic resins are excellent in processability and formability, and are widely applied to various household goods, office automation equipment, electrical and electronic products, and the like. Moreover, according to the kind and the characteristic of the product in which such a thermoplastic resin is used, in addition to the said excellent workability and moldability, the attempt to add a special property to a thermoplastic resin and to use it as a high value-added material is continuously made.
• thermoplastic resins many attempts have been made to impart electrical conductivity to thermoplastic resins, and to use such electrically conductive thermoplastic resins for applications such as automobiles, various electrical devices, electronic assemblies, or cables to exhibit electromagnetic shielding performance.
• Such electrically conductive thermoplastic resins are typically prepared using an electrically conductive thermoplastic resin composition in which a thermoplastic resin is mixed with a conductive additive such as carbon black, carbon fiber, metal powder, metal coated inorganic powder or metal fiber.
• a conductive additive such as carbon black, carbon fiber, metal powder, metal coated inorganic powder or metal fiber.
• Korean Patent Inventive No. 706652 80 to 99 parts by weight of a thermoplastic resin; 0.1 to 10 parts by weight of carbon nanotubes; And it has been proposed an electrically conductive thermoplastic resin composition comprising 0.1 to 10 parts by weight of the organic nanoclay.
• a composition has been proposed comprising fibrils, D) from 0.2 to 10.0 parts by weight of at least one particulate carbon compound, preferably carbon black or graphite powder, E) from 0 to 50 parts by weight of at least one filler and / or reinforcing material.
• an object of the present invention is to provide a polymer composition having excellent dispersibility, high conductivity, and economical efficiency by complexing a surface-modified carbon nanotube and another carbon compound to improve dispersibility.
• the present invention provides a polymer composition having excellent impact mitigation properties.
• the present invention 100 parts by weight of thermoplastic resin to achieve the above object; 0.1 to 5.0 parts by weight of surface-modified carbon nanotubes based on 100 parts by weight of the thermoplastic resin; It provides a conductive resin composition comprising; and 1 to 20 parts by weight of the carbon compound with respect to 100 parts by weight of the thermoplastic resin.
• the present invention provides a conductive resin composition further comprises 0.01 to 5 parts by weight of the blowing agent relative to 100 parts by weight of the thermoplastic resin.
• the present invention is the surface-modified carbon nanotube is a conductive resin that is surface-modified to include 0.1 to 10 parts by weight of an element selected from the group consisting of oxygen, nitrogen and mixtures thereof with respect to 100 parts by weight of carbon nanotubes To provide a composition.
• the surface-modified carbon nanotubes of the present invention provides a conductive resin composition obtained by oxidation of a carbon nanotube surface by adding carboxylic acid, nitric acid, phosphoric acid or sulfuric acid to the carbon nanotubes.
• the surface-modified carbon nanotubes of the present invention using a oxidizing agent selected from oxygen, air, ozone, hydrogen peroxide, nitric acid, nitro compounds and mixtures thereof, at a pressure of 50 to 400 atm and a temperature of 100 to 600 ° C. It provides a conductive resin composition obtained by oxidizing the carbon nanotube surface in the counting or supercritical water conditions.
• a oxidizing agent selected from oxygen, air, ozone, hydrogen peroxide, nitric acid, nitro compounds and mixtures thereof, at a pressure of 50 to 400 atm and a temperature of 100 to 600 ° C.
• the surface-modified carbon nanotubes of the present invention using a oxidizing agent selected from oxygen, air, ozone, hydrogen peroxide, nitric acid, nitro compounds and mixtures thereof, at a pressure of 50 to 400 atm and a temperature of 100 to 600 ° C.
• a oxidizing agent selected from oxygen, air, ozone, hydrogen peroxide, nitric acid, nitro compounds and mixtures thereof, at a pressure of 50 to 400 atm and a temperature of 100 to 600 ° C.
• the carbon nanotube surface is oxidized under counting or supercritical conditions, followed by carboxyl, carboxyl salt, amine, amine salt, tetravalent-amine, phosphate group, phosphate, sulfate group, sulfate, alcohol, thiol, ester, amide, epoxide
• a functional compound having at least one functional group selected from the group consisting of side, aldehyde, ketone, and mixtures thereof is injected into a surface reforming reaction tank at a pressure of 50 to 400 atm and a temperature of 100 to 600 ° C. to provide a conductive resin composition obtained by surface treatment. .
• the thermoplastic resin is a polyacetal resin, acrylic resin, polycarbonate resin, styrene resin, polyester resin, vinyl resin, polyphenylene ether resin, polyolefin resin, acrylonitrile-butadiene-styrene copolymer Resin, polyarylate resin, polyamide resin, polyamideimide resin, polyarylsulfone resin, polyetherimide resin, polyethersulfone resin, polyphenylene sulfide resin, fluorine resin, polyimide resin, polyetherketone resin, Polybenzoxazole resin, polyoxadiazole resin, polybenzothiazole resin, polybenzimidazole resin, polypyridine resin, polytriazole resin, polypyrrolidine resin, polydibenzofuran resin, polysulfone resin, polyurea resin, One resin, two or more copolymers selected from the group consisting of polyphosphazene resins and liquid crystal polymer resins It provides a resin or a mixture of two
• the present invention provides a conductive resin composition containing carbon black, graphite or carbon fiber as the carbon compound.
• the present invention provides a conductive resin composition having an average particle diameter of 0.001 ⁇ m ⁇ 300 ⁇ m.
• the present invention provides a molding prepared by extruding the conductive resin composition.
• the present invention provides a plastic molding capable of flexibly varying the surface resistance of the molding, electromagnetic shielding, electrostatic dispersion and antistatic.
• the present invention by using a composite material of carbon nanotubes and a carbon compound modified in a thermoplastic resin, by using a surface-modified carbon nanotubes to improve dispersibility, an effect of increasing conductivity and a large amount of expensive carbon nanotubes is achieved.
• the functionalities of carbon blacks, carbon black, graphite, and carbon fibers, which can support them are used together with surface-modified carbon nanotubes. It is intended to extend the applicability of the conductive composition by providing synergy to provide functionality and economy.
• the present invention is intended to expand the applicability of the conductive composition exhibiting impact relaxation (buffering) with the addition of an excellent blowing agent and an excellent conductivity.
• the present invention 100 parts by weight of thermoplastic resin; 0.1 to 5.0 parts by weight of surface-modified carbon nanotubes based on 100 parts by weight of the thermoplastic resin; It provides a conductive resin composition comprising; and 1 to 20 parts by weight of the carbon compound with respect to 100 parts by weight of the thermoplastic resin.
• the present invention also relates to a conductive resin composition further comprising 0.01 to 5 parts by weight of the blowing agent based on 100 parts by weight of the thermoplastic resin.
• thermoplastic resin used in the present invention is polyacetal resin, acrylic resin, polycarbonate resin, styrene resin, polyester resin, vinyl resin, polyphenylene ether resin, polyolefin resin, acrylonitrile-butadiene-styrene copolymer resin , Polyarylate resin, polyamide resin, polyamideimide resin, polyarylsulfone resin, polyetherimide resin, polyethersulfone resin, polyphenylene sulfide resin, fluorine resin, polyimide resin, polyetherketone resin, poly Benzoxazole resin, polyoxadiazole resin, polybenzothiazole resin, polybenzimidazole resin, polypyridine resin, polytriazole resin, polypyrrolidine resin, polydibenzofuran resin, polysulfone resin, polyurea resin, poly One resin, two or more copolymers selected from the group consisting of phosphazene resins and liquid crystal polymer resins Resins or mixtures of two or more may
• the surface-modified carbon nanotubes of the present invention may be used as 0.1 to 5.0 parts by weight of surface-modified carbon nanotubes based on 100 parts by weight of the thermoplastic resin.
• the surface modified carbon nanotubes of the present invention can make excellent balance between mechanical properties and electrical conductivity. If the surface-modified carbon nanotubes are used at less than 0.1 part by weight, the effect of improving conductivity is insignificant. If the surface-modified carbon nanotubes are used in excess of 5.0 parts by weight, the mechanical properties of the thermoplastic resin may be deteriorated. This results in expensive raw material waste.
• Carbon nanotubes of the present invention is composed of a single-walled, double walled, thin multi-walled, multi-walled, bundled and mixtures thereof Any form selected from the group is possible.
• the surface-modified carbon nanotubes of the present invention is preferably surface-modified to include 0.1 to 10 parts by weight of a material selected from the group consisting of oxygen, nitrogen and mixtures thereof with respect to 100 parts by weight of carbon nanotubes.
• the surface-modified carbon nanotubes through the oxidation have a significantly higher dispersibility in mixing with the resin and affect the conductivity. In addition, mixing with not only the resin but also other carbon materials or carbon compounds is facilitated.
• the surface-modified carbon nanotubes of the present invention include a method of causing oxidation of a surface by adding an acid, a method of oxidizing a surface of a carbon nanotube by reactivity of water under high temperature and high pressure.
• the surface-modified carbon nanotube of the present invention is oxygen, air, ozone, hydrogen peroxide, nitric acid, nitro compounds And oxidizing the surface of the carbon nanotubes under subcritical water or supercritical water conditions at a pressure of 50 to 400 atm and a temperature of 100 to 600 ° C. using an oxidant selected from a mixture thereof.
• Environmentally friendly surface modified carbon nanotubes can be obtained using oxidants that are not harmful in subcritical or supercritical conditions and are easy to handle and treat in wastewater.
• the surface modification of the subcritical water or supercritical water condition is that the oxidant is easily introduced to increase the surface modification effect of the carbon nanotubes, thereby increasing the dispersibility.
• the surface-modified carbon nanotubes are subcritical water or supercritical water at a pressure of 50 to 400 atm and a temperature of 100 to 600 ° C. using an oxidant selected from oxygen, air, ozone, hydrogen peroxide, nitric acid, nitro compounds, and mixtures thereof.
• the carbon nanotube surface is oxidized under counting conditions, followed by carboxyl, carboxyl salt, amine, amine salt, tetra-amine, phosphate group, phosphate, sulfate group, sulfate, alcohol, thiol, ester, amide, epoxide, aldehyde
• functional compounds having at least one functional group selected from the group consisting of ketones and mixtures thereof may be obtained by injecting a surface treatment reactor at a pressure of 50 to 400 atm and a temperature of 100 to 600 ° C.
• the surface-modified carbon nanotubes may be obtained by adding carboxylic acid, nitric acid, phosphoric acid, or sulfuric acid to the carbon nanotubes by oxidation of the surface of the carbon nanotubes. Oxidation can be provided.
• the carbon compound used in the present invention may be included as 1 to 20 parts by weight of the carbon compound based on 100 parts by weight of the thermoplastic resin. If the carbon compound is less than 1 part by weight, there is no effect of economical supplementation due to the addition of the carbon compound, and if it exceeds 20 parts by weight, there is no synergistic effect of the excess amount or conductivity.
• the carbon compound may be used as long as the carbon compound includes carbon black, graphite or carbon fiber, and is not limited thereto.
• the carbon compound may have an average particle diameter of 0.001 to 0.5 ⁇ m, and graphite may have an average particle diameter of 1 to 300 ⁇ m in powder form.
• the carbon fiber is also preferably a fine fiber having an average particle diameter of 0.01 to 0.1 mu m.
• the present invention may be used by mixing a carbon composite material with a conductive additive such as metal powder, metal coated inorganic powder, or metal fiber, and more preferably, lead (Pb), aluminum ( Al) metal powder can be used.
• a conductive additive such as metal powder, metal coated inorganic powder, or metal fiber, and more preferably, lead (Pb), aluminum ( Al) metal powder can be used.
• the present invention may further comprise 0.01 to 5 parts by weight of the blowing agent with respect to 100 parts by weight of the thermoplastic resin
• the blowing agent is a component that can improve the conductivity, azodicarboxyamide, azobistetrazoldiaminoguanidine, azo Selected from bistetrazoleguanidine, 5-phenyltetrazole, bistetrazoleguanidine, bistetrazole piperazine, bistetrazolediammonium, N, N-dinitrosopentamethylenetetramine, hydrazodicarboxyamide and mixtures thereof Can be appropriately selected according to the thermoplastic resin.
• the foaming agent in 0.01 to 5 parts by weight, the dispersibility is good together with the surface-modified carbon nanotubes and the carbon compound, it is possible to excellently improve the conductivity and at the same time forming a good foam (foam) without trouble.
• the present invention can be prepared by a known method by mixing the respective conductive resin compositions.
• the mixing of each of these components can be made into pellets by conventional extrusion, which can be used for various purposes, and the prepared pellets can be made into moldings to suit the purpose of sheets, films and the like.
• the present invention provides a plastic molding capable of flexibly varying the surface resistance of the molding, electromagnetic shielding, electrostatic dispersion and antistatic.
• the present invention is a conductive paint, electrostatic dispersion material, electrostatic dispersion paint, conductive material, electromagnetic wave shielding material, electromagnetic wave absorbing material, electromagnetic wave shielding paint, electromagnetic wave absorbing paint, solar cell material, dye-sensitized battery (DSSC) electrode material, electric device, electronic device , Semiconductor device, optoelectronic device, notebook component material, computer component material, mobile phone component material, PDA (PDA) component material, game machine component material, housing material, transparent electrode material, opaque electrode material, field emission display ( Field emission display (FED) materials, back light unit (BLU) materials, liquid crystal display (LCD) materials, plasma display panel (PDP) materials, light emitting diodes (LED) ) Materials, touch panel materials, billboard materials, billboard materials, display materials, heating elements, radiators, plating materials, catalysts, promoters, oxidants, reducing agents, automotive parts materials, ship parts Materials, aircraft component materials, electronic envelope materials, protective tape materials, adhesive materials, tray materials, clean room materials, transportation
• the conductive resin composition including the composite carbon material of the present invention has excellent conductivity by using a surface-modified carbon nanotube and a carbon compound such as graphite, carbon black, and carbon fiber together as a composite material, and a small amount.
• the use of carbon nanotubes has an economic effect of showing high conductivity.
• the resin composition further includes a foaming agent and has good foaming property, and exhibits excellent buffering effect due to excellent foaming, and has an excellent impact relaxation effect with conductivity.
• the conductive resin composition of the present invention has the effect of showing high conductivity even when using a small amount of expensive carbon nanotubes.
• the carbon nanotubes of the present invention by using the surface-modified carbon nanotubes in subcritical water or supercritical water conditions to exclude the use of acids to facilitate the surface modification under environmentally friendly conditions and improve the dispersibility with the resin There is.
• the conductive resin including the composite carbon material of the present invention is produced by the pellets has the effect of extending the applicability according to the application.
• MWCNT solution was prepared in a pretreatment tank by mixing 12 g of Multi Wall Carbon Nano Tube (hereinafter referred to as MWCNT) (HANWHA NANOTECH, product name: CM95) with 988 g of distilled water and a circulation pump. Before the MWCNT solution is introduced into the preheater at a flow rate of 30 g / min through a high pressure injection pump, the oxygen in the gaseous state compressed to 245 atm to 252 atm is mixed with the MWCNT solution at a flow rate of 0.8 g / min at the front end of the heat exchanger The mixed solution was added to a preheating tank preheated to 200 to 260 ° C. through a heat exchanger.
• MWCNT Multi Wall Carbon Nano Tube
• the preheated mixed solution is injected into a surface reforming reactor in a subcritical water state of 350 ° C. and 230 atm to 250 atm, and the surface modified product is transferred to a heat exchanger, and then first cooled to 200 ° C., and then again through a cooling device. After cooling to a temperature of about 25 °C to obtain a surface-modified continuously 11.8g multilayer carbon nanotubes.
• the carbon nanotubes of Preparation Example 1 were used in the same manner as in Example 6 except that 10g of carbon nanotubes of Preparation Example 3 and 50g of carbon fibers having an average particle diameter of 0.1 ⁇ m were used instead of 50g of carbon black.
• the carbon nanotubes of Preparation Example 1 were used in the same manner as in Example 7, except that 5g of the carbon nanotubes of Preparation Example 5 and 90g of carbon fibers having an average particle diameter of 10.0 ⁇ m were used instead of 90g of carbon black.
• Comparative Example 1 The same procedure was followed as in Comparative Example 1 except that 650 kg of low density polyethylene (LDPE830; HCC) and 350 g of carbon black (VXC500; CABOT) were added to a hopper of a rotating twin screw extruder.
• LDPE830; HCC low density polyethylene
• VXC500 carbon black
• Comparative Example 1 The same procedure was followed as in Comparative Example 1 except that 750 g of low density polyethylene (LDPE830; HCC) and 250 g of carbon fiber having an average particle diameter of 0.1 ⁇ m were added to a hopper of a rotating twin screw extruder.
• LDPE830 low density polyethylene
• HCC low density polyethylene
• carbon fiber having an average particle diameter of 0.1 ⁇ m were added to a hopper of a rotating twin screw extruder.
• Example 2 The same procedure as in Example 2 was carried out except that 5 g of unmodified carbon nanotubes (MWCNT) were used instead of the surface modified carbon nanotubes.
• MWCNT unmodified carbon nanotubes
• Example 3 The same procedure as in Example 3 was carried out except that 10 g of unmodified carbon nanotubes (MWCNT) were used instead of the surface modified carbon nanotubes.
• MWCNT unmodified carbon nanotubes
• Example 6 Same as Example 6, except that 968 g of low density polyethylene (LDPE 830; HCC), 30 g of unmodified carbon nanotube (MWCNT), and 2 g of azodicarboxyamide were added to the hopper of the rotating twin screw extruder. It was carried out.
• LDPE 830; HCC low density polyethylene
• MWCNT unmodified carbon nanotube
• azodicarboxyamide 2 g
• Example 6 The same procedure as in Example 6 was conducted except that 5 g of unmodified carbon nanotubes (MWCNT) were used.
• MWCNT unmodified carbon nanotubes
• Example 7 The same procedure as in Example 7 was carried out except that 5 g of unmodified carbon nanotubes (MWCNT) were used.
• MWCNT unmodified carbon nanotubes
• Example 8 The same procedure as in Example 8 was conducted except that 10 g of unmodified carbon nanotubes (MWCNT) were used.
• MWCNT unmodified carbon nanotubes
• Example 9 The same procedure as in Example 9 was carried out except that 5 g of unmodified carbon nanotubes (MWCNT) were used.
• MWCNT unmodified carbon nanotubes
• Example 6 The same procedure as in Example 6 was carried out except that low density polyethylene (LDPE 830; HCC) was adjusted to 940 g without using azodicarboxyamide.
• LDPE 830; HCC low density polyethylene

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• 2009
  • 2009-11-24 WO PCT/KR2009/006909 patent/WO2010059008A2/ko active Application Filing
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