WO2015190881A1 - Procédé de production de graphite - Google Patents

Procédé de production de graphite Download PDF

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Publication number
WO2015190881A1
WO2015190881A1 PCT/KR2015/005959 KR2015005959W WO2015190881A1 WO 2015190881 A1 WO2015190881 A1 WO 2015190881A1 KR 2015005959 W KR2015005959 W KR 2015005959W WO 2015190881 A1 WO2015190881 A1 WO 2015190881A1
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Prior art keywords
organic
inorganic
graphite
source
inorganic complex
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Ceased
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PCT/KR2015/005959
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English (en)
Korean (ko)
Inventor
박기륜
김정규
백종갑
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SKC Co Ltd
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SKC Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/20—Graphite
    • C01B32/205—Preparation
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/20—Graphite

Definitions

  • TECHNICAL FIELD Embodiments relate to a method of preparing graphite. Specifically, it relates to a method for producing graphite powder or sheet.
  • BACKGROUND Graphite is important as an industrial material because of its excellent heat resistance, chemical resistance, high thermal conductivity, and high electric conductivity. Radiation optical elements such as heat-radiating materials, heat-resistant sealing materials, gaskets, and X-ray monochromators, fuel cell separators, and acoustics It is used as a vibration plate. In addition to the use of graphite alone, it is widely used as a heat dissipation material, an electronic device case, and an aircraft material by forming a composite with resin.
  • an artificial graphite method As a representative example of the manufacturing method of an artificial film-like graphite, there is a method called "expand (expanded) graphite method".
  • artificial graphite is prepared by immersing the natural graphite in a mixture of concentrated sulfuric acid and concentrated acetic acid and then heating it rapidly. After the acid is removed by washing, the artificial graphite is processed into a film by a high pressure press.
  • the film-like graphite produced in this way has problems such as weak strength, poor physical properties, and concern about the influence of residual acid.
  • polymer grind method a method in which a special polymer film is directly heat treated to graphite.
  • the polymer film used for this purpose include polyoxadiazole, polyimide, polyphenylenevinylene, polybenzoimidazole, polybenzoxazole, polythiazole, and polyamide film.
  • Polymer graphite method species Compared to the conventional expanded graphite method, it is a much simpler method, which does not induce impurities such as acid, and also has excellent characteristics of achieving excellent thermal conductivity and electrical conductivity close to single crystal graphite. 60-181129, Japanese Patent Laid-Open No.
  • the method of mixing additives such as carbon nanotubes can improve the tensile strength or the peeling strength in the thickness direction, but there is a limit in improving the flexibility.
  • the ablation temperature is high and sheeting is difficult.
  • SUMMARY Embodiments seek to provide a method for easily preparing graphite powder or sheets with improved thermal and mechanical properties. Specifically, the embodiment is to provide a method for producing a graphite powder or sheet excellent in both thermal conductivity and flexibility.
  • the embodiment uses a very inexpensive abyss particles as a seed (Seed) In order to provide a new graphite powder or sheet manufacturing method that can be heat-treated at low temperatures and low production costs.
  • Graphite manufacturing method comprises the steps of providing an inorganic source for forming graphite; Providing an organic source comprising polymeric resin particles; Mixing the inorganic source and the organic source to form an organic-inorganic complex; And heat treating the organic-inorganic complex.
  • an organic-inorganic complex for preparing graphite includes an organic source including graphite particles and polymer resin particles.
  • an organic-inorganic complex including an inorganic source and an organic source is formed, and the mixture is heat-treated to produce graphite.
  • the organic source comprises polymer resin particles.
  • the graphite production method according to the embodiment forms the organic-inorganic complex using the polymer resin particles, and heat-treat the organic-inorganic complex. Accordingly, the graphite sheet according to the embodiment can have improved flexibility, and can prevent wrinkles during the heat treatment process ; have.
  • the organic-inorganic complex may include pores. That is, since the graphite sheet is formed including the polymer resin particles, pores may be included between the polymer resin particles or between the polymer resin particles and the inorganic particles.
  • the pores may complete the thermal shock during the heat treatment of the organic-inorganic complex. Accordingly, the graphite sheet according to the embodiment has improved mechanical properties, and wrinkles in the heat treatment process can be prevented.
  • the graphite according to the embodiment may use a pendulum as the inorganic source.
  • the abyss can act as a seed (graphite) of the graphitization can significantly lower the temperature of the ablation.
  • a graphite manufacturing method may include providing an inorganic source for forming graphite; Providing an organic source comprising polymeric resin particles; Mixing the inorganic source and the oil-valued source to form an organic-inorganic complex; and heat-treating the organic-inorganic complex.
  • the graphite manufacturing method according to the embodiment may be provided in the form of graphite powder or sheet.
  • the method for producing graphite powder omits the compression process after preparing the graphite sheet, or pulverizes it after preparing the graphite sheet.
  • the raw materials can be manufactured by heat treatment in a powder state without undergoing sheeting or filming, and those skilled in the art can easily infer the method.
  • the forming of the organic-inorganic complex may include preparing a slurry including the organic source, the inorganic source, a binder, and a solvent; Casing the slurry; And it may include the step of removing the solvent contained in the slurry.
  • an organic-inorganic mixed body is formed.
  • the organic-inorganic complex may include other additives such as an organic source, an inorganic source, a binder and a solvent, and a dispersant, as necessary.
  • the organic-inorganic complex may have a film or sheet shape.
  • the organic-inorganic complex may have a plate shape or a scroll shape. That is, the organic-inorganic complex may be an organic-inorganic composite sheet.
  • the thickness of the organic-inorganic complex There is no limitation on the thickness of the organic-inorganic complex. For example, it may be several mm to several mm. In more detail, the thickness of the organic-inorganic complex may be about 5 to about 1000. In more detail, the thickness of the organic-inorganic complex may be about 10 to about. In more detail, the thickness of the organic-inorganic complex may be about 20 to about 300.
  • the organic-inorganic complex may have various shapes in addition to the film or sheet shape. For example, it may be in the form of a powder or agglomerated powder.
  • the inorganic source is a raw material for forming the graphite sheet according to the embodiment.
  • the inorganic source may be an inorganic material containing carbon.
  • the inorganic source may be an inorganic material that can be converted into graphite by heat treatment.
  • the inorganic source may include an inorganic material having an abyss or having a graphite structure.
  • the inorganic source may include a bead, such as a natural nob, impression graphite, or expandable graphite.
  • the inorganic source may include carbon nanotubes, carbon nanofibers, and the like having a graphite structure.
  • the expandable nib may be treated with an insert such as sulfuric acid, which may be expanded by heat.
  • the expandable abyss may be expanded several to several thousand times by the heat applied.
  • the inorganic source may be provided in the form of particles. That is, the inorganic source may be in powder form.
  • the inorganic source may include a plate-shaped, polyhedral or spherical-shaped inorganic particles.
  • the average particle diameter of the inorganic particles contained in the inorganic source is not limited.
  • the average particle diameter (D50) of the inorganic particles is from about 0.1 kPa to about 1,000, more specifically from about 0.1 l / mi to about 500 / kPa, more specifically from about 0.1 im to about 300, more specifically May be from about 1 to about 300 / m. More specifically, the average particle diameter of the inorganic particles is about: m to about 200; may be m.
  • the size of the inorganic particles is too large, the dispersion degree of the inorganic particles may be reduced in the process of forming the complex.
  • the size of the inorganic particles is too small, in the process of forming the complex, it is difficult to control the inorganic particles, the particle size of the graphite particles after heat treatment may be small, the thermal conductivity may be lowered.
  • the content of the inorganic source is about 10 to 100 parts by weight of the organic source
  • the amount may be greater than or equal to, more specifically, greater than or equal to 30 parts by weight, more specifically, greater than or equal to 50 parts by weight, more specifically, greater than or equal to 100 parts by weight.
  • the content of the inorganic source may be 900 parts by weight or less based on 100 parts by weight of the organic source.
  • Organic Source includes polymer resin particles that can be converted into graphite by heat treatment.
  • the organic source may comprise aromatic polymer particles.
  • the organic source may be composed of the polymer resin particles.
  • the polymer resin may be polyimide, polyamide, polyacrylonitrile, polyethylene terephthalate, polybutylene terephthalate, polypropylene, polyethylene, polyethylene naphthalate, polyoxadiazole, polybenzothiazole, polybenzobisthiazole , Polybenzoxazole, polybenzobisoxazole, polypyrimerimide, aromatic polyamide, polyphenylene benzoimitazor, polyphenylene benzobisimitazor, polythiazole and polyparaphenylenevinylene It may include one or more selected from the group consisting of, and may be a homopolymer or a copolymer.
  • the organic source may not only be a raw material converted into graphite by heat treatment, but may also perform a binder function to prevent the inorganic source from falling off.
  • the organic source is provided in the form of particles. That is, the organic source may be in powder form.
  • the organic source may include plate-shaped, polyhedral or spherical organic particles.
  • the average particle diameter of the polymer resin particles contained in the organic source There is no limitation on the average particle diameter of the polymer resin particles contained in the organic source. All. For example, it may have a size of several hundred nanometers to several tens of millimeters, but embodiments are not limited thereto. In other words, commercially available polymer water particles may be used as the polymer resin particles.
  • the average particle diameter (D50, based on the primary particles) of the polymer resin particles may be about ⁇ ⁇ to about 1,000, about ⁇ mi to about 500 / im, about 0.1 ⁇ to about 200; can be m.
  • the average particle diameter of the organic particles may be about 1 / m to about 100.
  • the size of the organic particles is too large, the dispersion degree of the organic particles may be reduced in the process of forming the complex. In addition, if the size of the organic particles is too small, it is difficult to control the inorganic particles in the process of forming the complex.
  • the organic source may be mixed with the inorganic source in a molten state of organic particles. That is, after the organic source and the inorganic source are mixed with each other, the organic source may be melted by heat, and an organic-inorganic complex in the form of a chip may be formed.
  • the organic-inorganic mixture of the chip form may be extruded into a sheet-like organic-inorganic mixture through an extruder or the like.
  • Organic Binder The organic-inorganic complex may further include an organic binder.
  • the organic binder may perform a function of mechanically coupling the organic source and the inorganic source to each other.
  • the organic binder may be converted into graphite by heat treatment, and may be removed during the debinder process, the drying process and the carbonization process.
  • the organic binder examples include polyvinyl resins such as polyvinyl alcohol; Polyvinyl acetal resins such as polyvinyl butyral; Acrylic resins; Polyurethane resins; Rubber-based resins such as ethylene-propylene-diene monomer (EPDM, ethylene-propylene-diene monomer), silicon, butadiene; Or these mixtures etc. are mentioned. More specifically, polyvinyl butyral resin may be used as the organic binder.
  • the organic The binder may be included in an amount of about 200 parts by weight or less based on 100 parts by weight of the organic source, more specifically 100 parts by weight or less, and more specifically 50 parts by weight or less. In more detail, the organic binder may be included in about 30 parts by weight or less based on 100 parts by weight of the organic source.
  • the slurry may be prepared by uniformly mixing the organic source, the inorganic source, the binder, and the solvent. The slurry is then cast in sheet or film form. Thereafter, the solvent is removed through a drying process, and an organic-inorganic complex may be formed.
  • the drying process may proceed at a temperature between about 8 CTC and about 20 CTC.
  • the drying process may proceed for about 30 seconds to about 2 hours.
  • an alcohol such as ethanol or an organic solvent such as toluene may be used.
  • the solvent may be used in an amount such that the slurry has an appropriate viscosity and can be easily casted.
  • the solvent may be included in about 20wt% to about 70wt% based on the weight of the slurry.
  • the slurry may further include an additive such as a dispersant or an antifoaming agent to improve dispersibility and processability.
  • an additive such as a dispersant or an antifoaming agent to improve dispersibility and processability.
  • the organic source includes polymer resin particles
  • pores may be formed between the polymer resin particles.
  • the organic-inorganic complex may include pores. The pores may be formed while the solvent is dried and removed.
  • pores may be formed between the additive polymer resin particles and the inorganic particles.
  • pores may be formed between the inorganic particles.
  • the pore size and porosity of the organic-inorganic complex may be variously controlled by the content of the polymer resin particles, the diameter of the polymer resin particles, the content of the inorganic particles and the diameter of the inorganic particles.
  • the porosity of the organic-inorganic complex may be about lvol% to about 30vol%. In more detail, the porosity of the organic-inorganic complex may be about 2 vol% to about 20 vol%. More specifically, the porosity of the organic-inorganic complex may be about 3 vol% to about 10 vol%.
  • the organic-inorganic complex may be prepared in sheet or film form.
  • rectangular, circular, elliptical or indefinite plates can be made in the form of scrolls.
  • the thickness of the organic-inorganic complex may be about ⁇ to about 1000 zm. In more detail, the thickness of the organic-inorganic complex may be about 5 / kPa to about 500 / im. In more detail, the thickness of the organic-inorganic complex may be about 10 to about 200 ⁇ n.
  • the organic-inorganic complex is subjected to a heat treatment process that undergoes a carbonization process and a derivatization process. Accordingly, the organic source is carbonized and a carbonaceous sheet is formed. Thereafter, the carbonaceous sheet is subjected to a graphitization process to form a graphite sheet.
  • Carbonization Process may be performed by heating the organic-inorganic complex in an inert gas. In the case of including an expandable nibble as an inorganic source, expansion of the expandable nib may be performed by a separate expansion process or in a carbonization process.
  • the temperature of the carbonization process may be about 40C C or more. In more detail, the temperature of the carbonization process may be about 60C C or higher. The temperature of the carbonization process may be more than 400 ° C, less than 2oocrc. More specifically, the carbonization process is about
  • the temperature range is 80 ° C. to 1600 ° C., more specifically iooo ° c to i4 (about 30 minutes to about 4 hours in the temperature range of xrc.
  • the organic source included in the organic-inorganic complex may be carbonized.
  • the organic source in the organic-inorganic complex is burnt And carbonaceous sheet is formed.
  • the organic-inorganic complex may be sandwiched by two alumina plates or graphite plates, or may be subjected to a carbonization process after laminating the organic-inorganic complex and the alumina plate or a lamellar plate in alternating numbers of several hundreds.
  • the organic-inorganic complex when it is in the form of a scroll, it may be wound around a cylindrical seam and then subjected to the carbonization process described above.
  • the cylindrical shim may be a graphite shim, and may be heat-treated after winding the sheet in which the polymer film and the organic-inorganic complex are laminated in a roll form.
  • the organic-inorganic complex wound around the cylindrical seam may be subjected to a carbonization process, and the organic-inorganic complex, that is, the carbonaceous sheet may be removed from one side of the organic-inorganic complex, and the other may be subjected to a carbonization process.
  • the carbonization process can also be carried out while winding up.
  • the carbonization process and the derivatization process may be performed in different reaction stages.
  • the carbonization process may include a binder removal process to burn out the binder (burn out).
  • a separate debinder process there may be a separate debinder process.
  • Decalcification Process The carbonaceous sheet is heat treated in an inert gas and graphitized to form a graphite sheet.
  • the temperature of the derivatization process may be about 200 CTC or more. In more detail, the temperature of the derivatization process may be about 240 C C or more.
  • the derivatization process may proceed for about 30 minutes to about 4 hours at a temperature of about 240CTC to 300CTC.
  • the carbonaceous sheet may be sandwiched by two sheets of graphite plates, or after several to several hundred sheets of carbonaceous sheets and graphite plates are alternately laminated, the carbonizing sheet may be subjected to the graphitization process.
  • the carbonaceous sheet when the carbonaceous sheet is in the form of a roll, the carbonaceous sheet is cylindrical. It can be wound on the shim and then subjected to the decalcification process. The cylindrical seam is graphite Can be done.
  • the derivatization process may be carried out in the other semi-unggi to take out the carbonaceous sheet, or may be carried out continuously in the same reactor.
  • Compression Process The graphite sheet formed through the decalcification process is compressed, and the graphite sheet according to the present embodiment may be manufactured.
  • the graphite sheet in the foamed state immediately after the graphitization process may be compressed to produce a graphite sheet having improved flexibility (flex resistance).
  • the graphite particles (deposited layer) which have undergone the above-mentioned decalcification process may be greatly inclined with respect to the horizontal direction of the sheet.
  • the highly deformed layer may reduce the thermal conductivity in the horizontal direction and reduce the flex resistance.
  • the graphite sheet according to the present embodiment may have improved thermal conductivity and flex resistance.
  • the graphite sheet in the foamed state can be compressed by a metal roller such as a ceramic roller, a copper roller or a stainless steel, a polyurethane roller, a rubber roller or the like.
  • the graphite sheet in the foamed state can be compressed by the press device.
  • the pressure applied to the graphite sheet in the foamed state may be about 2 to about 2000 kg / cm.
  • the pressure of the rolling process may be about 20 to 1000 kg / cm.
  • the pressure of the rolling process may be about 50 to about 500 kg / cm.
  • the graphite sheet formed according to this embodiment may have improved thermal diffusivity and thermal conductivity.
  • the graphite sheet according to the present embodiment is improved Softness (flexibility) and density.
  • the thickness of the graphite sheet according to the present embodiment may be about 5 / to about 500. In more detail, the thickness of the graphite sheet according to the present embodiment may be about 5 kPa to about 400 1.
  • the density of the graphite sheet according to the present embodiment may be about a7g / cm 3 or more. In more detail, the density of the graphite sheet according to the present embodiment may be about 0.3 Sg / an 3 to about 2.5 g / atf.
  • This embodiment can provide a graphite sheet having improved mechanical performance and thermal properties.
  • Example 1 50 parts by weight of polyimide particles (Evonik, P84 NT), 30 parts by weight of impression graphite particles (GK, NGR25), 50 parts by weight of polyvinyl butyral and 350 parts by weight of a mixture of toluene and ethanol Mixed to make a slurry.
  • the slurry was coated on a PET film to a thickness of 0.1 mm, dried at a temperature of 100 ° C for 30 minutes, A composite sheet of thickness was formed.
  • the composite sheet was heated to a temperature of 10 ° C./minute up to a temperature of 1200 ° C. in a nitrogen atmosphere, and maintained at 120 ° C. for 2 hours to prepare a carbonaceous sheet by carbonization.
  • the carbonaceous sheet was heated to a temperature of 10 ° C./min up to a temperature of 250CTC in an argon atmosphere and then maintained at 250 ° C. for 4 hours to prepare an uncompressed graphite sheet.
  • Example 2 The same procedure as in Example 1 was carried out, except that 50 parts by weight of the impression agglomerate particles (GK, NGR25) were used in place of the 30 parts by weight of the impression particles, thereby compressing a thickness of about 60.
  • Graphite sheets were prepared.
  • Example 3 The same procedure as in Example 1 was carried out except that 70 parts by weight of impression graphite particles (GK, NGR25) were used in place of 30 parts by weight of impression graphite particles, thereby compressing the thickness to about 60.
  • Graphite sheets were prepared.
  • Example 4 A compressed graphite sheet having a thickness of about 60 was prepared by performing the same process as in Example 1, except that polyacrylonitrile particles (Aldrich, 181315-100G) were used instead of the polyimide particles of Example 1. It was. Results The relative thermal conductivity of the graphite sheets prepared in Examples 1 to 4 was measured, and the results are shown in Table 1 below.
  • Relative thermal conductivity was evaluated by heat-sensitive stickers. After attaching a commercially available natural graphite sheet (Graphtech, eGraftech) and the graphite sheets of Examples 1 to 4 to a heat-sensitive sticker having a length of 10 cm, the end of the sheet and the graphite sheet were heated to change the temperature at the other end ( Blue to yellow) was visually observed.
  • the heat conduction time of Table 1 shows the relative heat conduction time when the temperature change time of the heat-sensitive sticker on which the natural graphite sheet is attached is 100.
  • the graphite manufacturing method according to the embodiment was able to easily produce a thick graphite sheet compared to the conventional polymer graphite method, it was confirmed that the flexibility can be used commercially. It is assumed that pores are formed in the organic-inorganic composite by using organic particles and / or abyss particles, thereby facilitating the discharge of cracked gas and providing flexibility by the pores. In addition, even if the graphite particles serve as the seed and use the organic particles, it is estimated that sufficient graphitization proceeds.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

Le présent mode de réalisation concerne un procédé de production de graphite comprenant les étapes consistant à prendre une source inorganique pour former du graphite; à prendre une source organique qui comprend des particules de résine polymère; à former un mélange organique-inorganique par mélange de la source inorganique et de la source organique; et à soumettre le mélange organique-inorganique à un traitement thermique. Le procédé de production selon le présent mode de réalisation permet de produire une poudre ou une feuille de graphite ayant une performance mécanique et des propriétés thermiques améliorées.
PCT/KR2015/005959 2014-06-13 2015-06-12 Procédé de production de graphite Ceased WO2015190881A1 (fr)

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KR1020140071954A KR101473432B1 (ko) 2014-06-13 2014-06-13 그라파이트의 제조방법

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KR101997120B1 (ko) * 2016-03-18 2019-07-05 (주)시엔케이 전기전도성 카본페이퍼의 제작방법.
KR102158039B1 (ko) * 2018-08-23 2020-09-21 한국화학연구원 폐 pet를 활용한 흑연의 제조방법
KR102081783B1 (ko) * 2019-04-03 2020-02-27 (주)시엔케이 전기전도성 카본페이퍼의 제작방법
KR102458823B1 (ko) * 2020-09-21 2022-10-25 조인셋 주식회사 고순도 천연 그라파이트 시트와 그 제조 방법 및 복합 그라파이트 시트

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JP2007320775A (ja) * 2005-07-28 2007-12-13 Kaneka Corp グラファイトフィルムおよびグラファイトフィルムの製造方法
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