WO2017199966A1 - Procédé de production de fibres de carbone, fibres de carbone, et électrode destinée à des condensateurs électriques à double couche - Google Patents

Procédé de production de fibres de carbone, fibres de carbone, et électrode destinée à des condensateurs électriques à double couche Download PDF

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WO2017199966A1
WO2017199966A1 PCT/JP2017/018391 JP2017018391W WO2017199966A1 WO 2017199966 A1 WO2017199966 A1 WO 2017199966A1 JP 2017018391 W JP2017018391 W JP 2017018391W WO 2017199966 A1 WO2017199966 A1 WO 2017199966A1
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Prior art keywords
coal
carbon fiber
solvent
carbon fibers
ashless coal
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PCT/JP2017/018391
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English (en)
Japanese (ja)
Inventor
眞基 濱口
祥平 和田
聡則 井上
昌宏 豊田
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株式会社神戸製鋼所
国立大学法人大分大学
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Priority to KR1020187033029A priority Critical patent/KR102118943B1/ko
Priority to CN201780030160.2A priority patent/CN109154108A/zh
Publication of WO2017199966A1 publication Critical patent/WO2017199966A1/fr

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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/04—Dry spinning methods
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/32—Carbon-based
    • H01G11/40—Fibres
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13—Energy storage using capacitors

Definitions

  • the present invention relates to a carbon fiber manufacturing method, carbon fiber, and electrode for an electric double layer capacitor.
  • Carbon fiber is widely used as a reinforcing material for structural materials such as resin, concrete and ceramic.
  • carbon fiber is also used as, for example, a heat insulating material, activated carbon raw material, conductive material, heat transfer material, and the like.
  • a method for producing carbon fiber a method of electrospinning pitch or resin derived from petroleum or coal is known (see Japanese Patent Application Laid-Open No. 2011-157668 and International Publication No. 2011/070893).
  • porous carbon fibers having fine pores are useful as adsorbents and electrodes.
  • a method for producing such a porous carbon fiber a method called so-called activation in which the surface of the carbon fiber is eroded by treatment with high-temperature steam or strong alkali, or the pitch or resin of the carbon fiber raw material such as MgO is used.
  • the above-described method requires a special treatment or material such as a surface treatment or a template substance, which raises a problem that the manufacturing cost of the porous carbon fiber increases.
  • the present invention provides a carbon fiber production method capable of producing porous carbon fibers in a relatively simple process, a carbon fiber obtained in a relatively simple process, and an electric double layer capacitor using the same. It is an object to provide a working electrode.
  • the invention made to solve the above problems includes a step of obtaining ashless coal by solvent extraction treatment of coal, a step of electrospinning ashless coal obtained in the ashless coal acquisition step together with a solvent, and the electric field And a step of carbonizing the filament obtained in the spinning step.
  • the carbon fiber manufacturing method uses ashless coal as a raw material, and electrospinning ashless coal together with a solvent and then carbonizing to obtain porous carbon fibers in which fine pores are formed by volatilization of the solvent. be able to. That is, according to the carbon fiber manufacturing method, porous carbon fibers can be manufactured by a relatively simple process of carbonization after electrospinning.
  • the carbonization may be performed by heating the filament to 700 ° C. or more and 1200 ° C. or less. By performing carbonization in this way, porous carbon fibers can be obtained easily and reliably.
  • Another invention made to solve the above problems is a carbon fiber made from coal, having a specific surface area of 300 m 2 / g to 3000 m 2 / g, an average diameter of 0.5 ⁇ m to 5 ⁇ m, oxygen Content is 0.4 mass% or more, It is characterized by the above-mentioned.
  • the carbon fiber has a specific surface area and an average diameter in the above ranges, and the oxygen content is 0.4% by mass or more. Therefore, after the ashless coal is electrospun together with a solvent, the ashless coal is used as a raw material. Obtained by carbonization. Therefore, the carbon fiber can be produced by a relatively simple process and can be effectively used as a porous material having many fine pores.
  • Still another invention made to solve the above problems is an electrode for an electric double layer capacitor using the carbon fiber.
  • the electric double layer capacitor electrode is excellent in manufacturing cost because the carbon fiber is used.
  • Specific surface area means a value measured according to JIS-Z8830 (2013).
  • Oxygen content means the content of oxygen atoms including not only oxygen molecules but also atoms bonded to other atoms, and is specifically measured according to JIS-M8813 (2004). Mean value.
  • the carbon fiber production method can produce porous carbon fiber by a relatively simple process. Further, the carbon fiber is obtained by a relatively simple process, and the electric double layer capacitor electrode using the carbon fiber is excellent in manufacturing cost.
  • the carbon fiber production method includes ashless coal acquisition step S1 for obtaining ashless coal by solvent extraction treatment of coal and ashless coal obtained in ashless coal acquisition step S1 together with a solvent.
  • An electrospinning process S2 for electrospinning and a carbonization process S3 for carbonizing the filament obtained in the electrospinning process S2 are mainly provided.
  • ashless coal acquisition process In the ashless coal acquisition step S1, raw material coal is subjected to solvent extraction treatment to obtain ashless coal. Specifically, the slurry obtained by mixing the raw coal and the solvent is heated to a temperature equal to or higher than the pyrolysis temperature of the raw coal, the soluble component of the pyrolyzed raw coal is extracted into the solvent, and the insoluble component at this pyrolysis temperature is extracted. Ashless coal is obtained by separating from the slurry.
  • the “ashless coal” is a modified coal obtained by modifying coal, and has an ash content of 5% by mass or less, preferably 3% by mass or less, more preferably 1% by mass or less. “Ash” means a value measured in accordance with JIS-M8812 (2004).
  • coal used as raw material for ashless coal examples include anthracite coal, bituminous coal, subbituminous coal, lignite, etc., in descending order of degree of coalification. Of these, bituminous coal or subbituminous coal having a moderate degree of coalification is preferred.
  • the solvent is not particularly limited as long as it has a property of dissolving the raw material coal.
  • monocyclic aromatic compounds such as benzene, toluene and xylene, bicyclic rings such as naphthalene, methylnaphthalene, dimethylnaphthalene and trimethylnaphthalene.
  • Aromatic compounds, tricyclic aromatic compounds such as anthracene, and the like can be used.
  • the bicyclic aromatic compound includes naphthalenes having an aliphatic chain, biphenyls having a long aliphatic chain, and the like.
  • a bicyclic aromatic compound which is a coal derivative purified from a coal dry distillation product is preferable.
  • the bicyclic aromatic compound of the coal derivative is stable even in a heated state and has an excellent affinity with coal. Therefore, by using such a bicyclic aromatic compound as a solvent, the ratio of coal components extracted into the solvent can be increased, and the solvent can be easily recovered and reused by a method such as distillation. .
  • the lower limit of the slurry heating temperature is preferably 300 ° C, more preferably 350 ° C, and even more preferably 380 ° C.
  • the upper limit of the heating temperature of the slurry is preferably 450 ° C, more preferably 420 ° C. If the heating temperature of the slurry is less than the above lower limit, the bonds between the molecules constituting the coal cannot be sufficiently weakened. For example, when low grade coal is used as the raw coal, There is a possibility that the solidification temperature cannot be increased, and the yield may be low and uneconomical.
  • the upper limit of the slurry heating time is preferably 120 minutes, more preferably 60 minutes, and even more preferably 30 minutes.
  • the lower limit of the slurry heating time is preferably 10 minutes.
  • the cooling temperature of the slurry is preferably 300 ° C. or higher and 370 ° C. or lower.
  • the cooling temperature of the slurry exceeds the above upper limit, the thermal decomposition reaction may not be sufficiently suppressed.
  • the cooling temperature of the slurry is less than the lower limit, the solvent dissolving power is reduced, and re-precipitation of the extracted coal component occurs, which may reduce the recovery rate of ashless coal.
  • the pressure at the time of heat extraction of the slurry depends on the heating temperature and the vapor pressure of the solvent used, it can be, for example, 1 MPa or more and 2 MPa or less.
  • the pressure at the time of heat extraction is lower than the vapor pressure of the solvent, the solvent is volatilized and the soluble component of coal cannot be confined in the liquid phase, and the soluble component cannot be extracted.
  • the pressure at the time of heating extraction is too high, the cost of the equipment, the operating cost, etc. increase.
  • the method for separating the insoluble component from the slurry is not particularly limited, and a known separation method such as a filtration method, a centrifugal separation method, a gravity sedimentation method, or a combination of these two methods can be employed.
  • a combination of a centrifugal separation method and a filtration method that can continuously operate a fluid is suitable for a large amount of processing at low cost, and can reliably remove insoluble components is preferable.
  • the extraction rate (yield) of ashless coal from coal is, for example, 20% by mass to 60% by mass in the case of bituminous coal or sub-bituminous coal, although it depends on the quality of the raw coal.
  • oxygen content of ashless coal As a minimum of oxygen content of ashless coal, 1 mass% is preferred, 1.5 mass% is more preferred, and 2 mass% is still more preferred. On the other hand, as an upper limit of oxygen content of ashless coal, 5 mass% is preferable, 4 mass% is more preferable, and 3.5 mass% is further more preferable.
  • the oxygen content of ashless coal is less than the above lower limit, it is not possible to sufficiently suppress crystal development in electrospinning due to an increase in aromatic compounds, and the resulting carbon fiber is insufficiently porous There is a risk.
  • the oxygen content of ashless coal exceeds the above upper limit, the mass reduction rate during carbonization is large, and the carbon fiber production cost may increase due to a decrease in the carbon fiber yield.
  • electrospinning step S2 electrospinning is performed using the mixed solution of ashless coal and a solvent (solution of ashless coal) obtained in the ashless coal acquisition step S1 as a raw material liquid.
  • the ashless coal extraction solvent used in the ashless coal acquisition step S1 may be used as it is. That is, it is good to use for electrospinning the solvent which isolate
  • solid ashless coal may be separated from the solvent from which insoluble components have been separated in the ashless coal acquisition step S1, and the solvent may be mixed with the separated ashless coal.
  • this solvent the same solvents that can be used for extraction of ashless coal can be used.
  • a general distillation method, evaporation method (for example, spray drying method) or the like can be used.
  • the lower limit of the boiling point of the solvent used in the mixed solution is preferably 50 ° C, more preferably 100 ° C.
  • an upper limit of the boiling point of a solvent 150 degreeC is preferable and 130 degreeC is more preferable.
  • the carbon fiber can be made porous. Examples of such a solvent include pyridine and tetrahydrofuran.
  • the lower limit of the content of ashless coal in the mixed solution is preferably 3% by mass, more preferably 5% by mass, and even more preferably 10% by mass.
  • an upper limit of the content rate of ashless coal in the said liquid mixture 50 mass% is preferable and 40 mass% is more preferable.
  • Electrospinning is a known method for obtaining a filament by spinning a raw material liquid with electric charge repulsion while spinning the raw material liquid in an electric field. Specifically, a nozzle for jetting the raw material liquid and a drum-shaped collector facing the nozzle are used as a pair of electrodes, and a high voltage is applied to the raw material liquid by these electrodes, so that A filamentous body having a skeleton of carbon derived from ashless coal contained in the raw material liquid is formed.
  • the voltage is 1 kV to 50 kV
  • the raw material liquid flow rate is 0.1 ml / h to 2 ml / h
  • the distance between the nozzle and the collector is 1 cm to 50 cm
  • the nozzle diameter is 0.1 mm or more. It can be 1 mm or less.
  • the filament is made porous by volatilizing the solvent at the time of ejection from the nozzle and laminating molecules constituting ashless coal randomly.
  • the filamentous body when the filamentous body is formed on the collector, it contains a part of the solvent that has not volatilized after ejection together with the carbon skeleton. This solvent is removed by the next carbonization step S3.
  • porous carbon fibers are obtained by heating and carbonizing (graphitizing) the filament containing the solvent obtained in the electrospinning step S2.
  • the filamentous body is inserted into an arbitrary heating device such as an electric furnace and the inside is replaced with a non-oxidizing gas
  • the filament is heated to a constant temperature while blowing the non-oxidizing gas into the heating device.
  • heating temperature in a carbonization process 700 ° C is preferred and 800 ° C is more preferred.
  • an upper limit of heating temperature 1200 degreeC is preferable and 1000 degreeC is more preferable.
  • carbonization may become inadequate.
  • the heating temperature exceeds the above upper limit, the production cost may increase from the viewpoint of improving the heat resistance of the equipment and fuel consumption.
  • the heating time including the temperature increase in the carbonization step is preferably 15 minutes or more and 10 hours or less. Moreover, as a temperature increase rate, 1 degreeC / min or more and 5 degrees C / min or less are preferable.
  • the non-oxidizing gas is not particularly limited as long as it can suppress the oxidation of the carbon material, but nitrogen gas is preferable from the economical viewpoint.
  • the manufacturing method of the said carbon fiber may be provided with the oxidation process process which lightly oxidizes a filament before carbonization process S3.
  • this oxidation treatment for example, heating in an atmosphere containing oxygen of 300 ° C. or lower, treatment with an oxidizing agent, or the like can be used.
  • the carbon fiber is made of coal, has a specific surface area of 300 m 2 / g to 3000 m 2 / g, an average diameter of 0.5 ⁇ m to 5 ⁇ m, and an oxygen content of 0.4% by mass or more.
  • the said carbon fiber can be obtained with the manufacturing method of the said carbon fiber mentioned above.
  • the carbon fiber has a small proportion of polycyclic aromatic compounds because the oxygen content is not less than the above lower limit. Therefore, in the carbon fiber, since the planarity of the molecule of the compound contained is low and the ring size is small, the molecule is difficult to orient. That is, since the molecules are randomly stacked during electrospinning as described above, the carbon fiber is excellent in porosity.
  • the lower limit of the specific surface area of the carbon fiber 350m 2 / g are preferred, 400m 2 / g is more preferable.
  • the upper limit of the specific surface area is preferably 2500 m 2 / g, and more preferably 1000 m 2 / g.
  • the lower limit of the average diameter of the carbon fiber is preferably 0.8 ⁇ m.
  • the upper limit of the average diameter is preferably 1.5 ⁇ m.
  • the lower limit of the oxygen content of the carbon fiber is preferably 0.5% by mass.
  • the upper limit of the oxygen content is not particularly limited, but is, for example, 5% by mass.
  • the oxygen content is less than the above lower limit, the carbon fiber becomes difficult to be porous due to the increase of the aromatic compound, and the suitability as an adsorbent may be lowered.
  • the oxygen content exceeds the above upper limit, it may be difficult to produce carbon fibers.
  • the electric double layer capacitor electrode is formed using the carbon fiber. Specifically, the electrode for the electric double layer capacitor is obtained by mixing the carbon fiber with a binding aid and laminating the fibers so that the fibers are entangled with each other.
  • the carbon fiber manufacturing method uses ashless coal as a raw material, and electrospinning ashless coal together with a solvent and then carbonizing to obtain porous carbon fibers in which fine pores are formed by volatilization of the solvent. be able to. That is, according to the carbon fiber manufacturing method, porous carbon fibers can be manufactured by a relatively simple process of carbonization after electrospinning.
  • the carbon fiber can be produced by a relatively simple process and can be effectively used as a porous material having many fine pores. Furthermore, since the said electrode for electric double layer capacitors uses the said carbon fiber, it is excellent in manufacturing cost.
  • the method for producing the carbon fiber is not limited to the above embodiment.
  • the carbon fiber manufacturing method may include steps other than those described above as necessary. Specifically, within a range that does not adversely affect each step, there may be a step such as a step of pulverizing raw coal, a step of removing foreign matters, or the like between or before and after each step.
  • Examples 1 and 2 > 1 kg of bituminous coal pulverized to 1 mm or less as raw material coal was mixed with 5 kg of methylnaphthalene, charged in an autoclave, held at 400 ° C. for 1 hour in a nitrogen atmosphere, and then cooled to obtain a pyrolyzate. Next, this pyrolyzate was filtered, and the obtained filtrate was distilled under reduced pressure to separate soluble components, thereby obtaining solid ashless coal.
  • Table 1 shows the elemental analysis values of the ashless coal. The oxygen content was calculated from the difference from the content of other elements.
  • the resulting ashless coal was mixed with pyridine to obtain an ashless coal solution having a concentration of 35.9% by mass.
  • electrospinning was performed at a voltage of 14 to 18 kV, a flow rate of 0.7 to 0.9 ml / h, a distance between the nozzle and the collector (inter-spinning distance) of 15 cm, and an inner diameter of the nozzle of 0.48 mm.
  • a filamentous body was formed on the aluminum foil.
  • electrospinning was performed by changing the yarn conditions.
  • the filament was peeled from the aluminum foil, it was heated to 900 ° C. at a heating rate of 3.3 ° C./min to carbonize to obtain carbon fibers having an average diameter of 1 ⁇ m.
  • Powdered activated carbon having a diameter of 50 ⁇ m or less was obtained by using coconut shell as a raw material and making it porous by a steam activation method.
  • the specific surface area was measured using “BELSORP-max” manufactured by Microtrac Bell.
  • the capacitance is obtained by creating an electrode for an electric double layer capacitor using carbon fiber or activated carbon, and measuring the charge / discharge characteristics in a 1 M H 2 SO 4 electrolyte in a capacitor using this electrode, The capacitance at 100 mA / g was determined.
  • the carbon fibers of Examples 1 and 2 which were carbonized after electrospinning ashless coal with a solvent using ashless coal as a raw material, had a large specific surface area compared to the comparative example and were sufficiently porous. You can see that In Example 1, as can be seen from FIG. 2, the diameter of the micropores is approximately 10 nm or less. Furthermore, the average fiber diameter determined from FIG. 3 was 1.1 ⁇ m. Further, the carbon fibers of Examples 1 and 2 are excellent in capacitance as compared with the carbon fiber of the comparative example and the activated carbon of the reference example.
  • the carbon fiber of the comparative example uses a coal-based pitch with a high ratio of aromatic compounds, and therefore, by condensing while forming an orientation in which molecules are stacked in parallel in electrospinning, a structure with high crystallinity and no development of pores It is speculated that it became.
  • the activated carbon of the reference example is larger in specific surface area than the carbon fibers of Examples 1 and 2, but has a small capacitance. This is thought to be due to the difference in pore structure.
  • the carbon fiber obtained by the carbon fiber production method and the carbon fiber can produce porous carbon fiber by a relatively simple process, they can be suitably used as an adsorbent or an electrode raw material.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
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  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Inorganic Fibers (AREA)
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  • Electric Double-Layer Capacitors Or The Like (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)

Abstract

La présente invention concerne un procédé de production de fibres de carbone, comprenant : une étape d'obtention d'un charbon sans cendres au moyen d'une extraction par solvant d'un charbon ; une étape de filage électrostatique du charbon sans cendres obtenu dans l'étape d'acquisition de charbon sans cendres conjointement avec un solvant ; et une étape de carbonisation des fibres obtenues dans l'étape de filage électrostatique, de préférence une étape de chauffage des fibres à une température allant de 700 °C à 1200 °C (inclus). Les fibres de carbone ainsi obtenues possèdent une surface spécifique allant de 300 m2/g à 3000 m2/g (inclus), un diamètre moyen allant de 0,5 μm à 5 μm (inclus) et une teneur en oxygène de 0,4 % en masse ou plus, et sont appropriées en tant qu'électrode destinée à des condensateurs électriques à double couche.
PCT/JP2017/018391 2016-05-19 2017-05-16 Procédé de production de fibres de carbone, fibres de carbone, et électrode destinée à des condensateurs électriques à double couche WO2017199966A1 (fr)

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KR1020187033029A KR102118943B1 (ko) 2016-05-19 2017-05-16 탄소 섬유의 제조 방법, 탄소 섬유 및 전기 이중층 캐패시터용 전극
CN201780030160.2A CN109154108A (zh) 2016-05-19 2017-05-16 碳纤维的制造方法、碳纤维和双电层电容器用电极

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JP2016-100345 2016-05-19
JP2016100345A JP6571043B2 (ja) 2016-05-19 2016-05-19 炭素繊維の製造方法、炭素繊維及び電気二重層キャパシタ用電極

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KR102069839B1 (ko) * 2017-12-13 2020-01-23 한국에너지기술연구원 슈퍼커패시터 전극 용 활성탄, 이를 포함하는 슈퍼커패시터 용 전극, 및 상기 활성탄의 제조방법
KR102585145B1 (ko) * 2021-09-16 2023-10-05 경상국립대학교산학협력단 표면활성화된 탄소섬유 전극, 이의 제조방법, 플렉시블 섬유형 슈퍼커패시터 및 플렉시블 섬유형 슈퍼커패시터의 제조 방법

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