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WO1999056870A1 - Matiere et procede d'occlusion de gaz - Google Patents

Matiere et procede d'occlusion de gaz Download PDF

Info

Publication number
WO1999056870A1
WO1999056870A1 PCT/JP1999/002326 JP9902326W WO9956870A1 WO 1999056870 A1 WO1999056870 A1 WO 1999056870A1 JP 9902326 W JP9902326 W JP 9902326W WO 9956870 A1 WO9956870 A1 WO 9956870A1
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WO
WIPO (PCT)
Prior art keywords
carbon
gas
gas storage
amorphous
metal
Prior art date
Application number
PCT/JP1999/002326
Other languages
English (en)
Japanese (ja)
Inventor
Chiharu Yamaguchi
Hisaji Matsui
Hitoshi Nishino
Katsuhiro Sasaki
Ryoichi Nishida
Ayumu Yasuda
Noboru Kawase
Original Assignee
Osaka Gas Company Limited
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
Application filed by Osaka Gas Company Limited filed Critical Osaka Gas Company Limited
Publication of WO1999056870A1 publication Critical patent/WO1999056870A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C11/00—Use of gas-solvents or gas-sorbents in vessels
    • 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
    • Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00—Capture or disposal of greenhouse gases
    • Y02C20/40—Capture or disposal of greenhouse gases of CO2

Definitions

  • the present invention relates to a gas storage material and a gas storage method or a gas storage method.
  • hydrogen storage alloys have been used as hydrogen storage materials, and zeolite, activated carbon, and the like have been used as methane storage materials.
  • the hydrogen storage alloy has a low hydrogen storage capacity per weight, and is powdered by repeated use, and therefore lacks durability. There are also problems with storage materials, such as insufficient storage capacity.
  • the present invention provides a lightweight, hydrogen-per-weight It has a large amount of occlusion, its structure is highly controlled, and it has excellent storage capacity for various gases at a pressure close to normal pressure in a cooling state and at a relatively low pressure at normal temperature, and has durability.
  • the main objective is to provide a novel gas storage material or gas storage material that is excellent in quality.
  • the present inventor has conducted research while paying attention to the current state of the technology as described above, and as a result, has developed amorphous carbon tubes (diameter of 1 O Onra or less), hollow onion-like carbon, and carbon nano particles.
  • Hydrogen, methane, helium, neon, xenon are amorphous carbon materials containing at least one kind of carbon, and carbon materials containing at least one kind of metal salt and metal. It has been found that it exhibits excellent properties as a gas storage material or a gas storage material such as crypton and carbon dioxide.
  • the present invention provides the following gas storage material and gas storage method:
  • a gas storage material consisting of amorphous carbon tube (diameter less than O Onm), amorphous onion-like carbon, and amorphous carbonaceous material containing at least one kind of carbon nanoparticle.
  • Amorphous carbon tube (diameter less than 10 Om), a gas occlusion material composed of amorphous carbonaceous material containing at least one kind of hollow onion-like carbon and carbon nanoparticle
  • a gas storage method characterized by storing gas under relatively low pressure or lower conditions.
  • Amorphous carbon material is iron, cobalt, nickel, copper, platinum, palladium, rubidium, strontium, cesium, sodium, manganese, nickel, aluminum Item 4.
  • the carbon material is synthesized by irradiating at least one kind of plasma and plasma, or subjecting the carbon material to heat treatment and irradiation treatment.
  • the carbonaceous material according to the present invention can be imparted with unique physical properties due to the amorphous structure, and exhibit excellent performance as a gas occluding material.
  • the amorphous carbon tube can be manufactured to have a straight shape, an opening at the tip is easy, and an amorphous structure.
  • Materials with or without characteristics are particularly suitable as gas storage materials or gas storage materials.
  • the term “amorphous structure” means not a graphitic structure consisting of a continuous carbon layer of regularly arranged carbon atoms but a structure consisting of a relatively irregular carbon layer. I do. From an image obtained by a transmission electron microscope, which is a typical analysis technique, it is clear that the amorphous carbon tube according to the present invention has a carbon layer length along the axis of the carbon tube. Can be specified to be less than twice the tube diameter.
  • hollow onion-like carbon and carbon nanoparticle can be controlled to have an amorphous structure suitable for gas occlusion.
  • the nanocarbon according to the present invention can be synthesized as follows, but the synthesis method is not limited to these methods.
  • the desired nanocarbon can be produced by subjecting it to at least one kind of irradiation treatment of electron beam irradiation, ion beam irradiation, and plasma irradiation, or by subjecting it to heat treatment and irradiation treatment. it can.
  • irradiation treatment of electron beam irradiation, ion beam irradiation, and plasma irradiation, or by subjecting it to heat treatment and irradiation treatment.
  • it can.
  • Material, carbon material entirely composed of at least one of -C3C-bond and 2c bond and / or at least part of at least one of poly and cumulene
  • the above-mentioned carbon material also includes a material containing at least one of a metal salt and a metal in combination.
  • Amorphous carbon tubes, hollow onion-like carbon, and carbon nanoparticle as products are used to determine the density of raw materials, heating conditions or irradiation conditions (pressure, temperature, irradiation energy, etc.). By adjusting, it is possible to separate them.
  • the wavelength is usually about 1,200 nin or less (more than Ri and rather is preferable about 150 to 1200 nm), the output 0. 1 ⁇ 10mJ / cm 2 of about (yo Ri favored properly is irradiated with a laser beam of about 0.5 ⁇ 5mJ / cm 2).
  • the type of laser light can be any of those commonly used, and is not particularly limited.
  • Nd YAG laser
  • Ti Sa laser
  • dye laser dye + SHG laser
  • Ar + laser Kr + laser and the like.
  • the acceleration voltage is about 1 to 2000 kV (more preferably about 10 to 10 to 17 torr (more preferably, about 10 to 3 to 10 to 5 torr)). Irradiation is preferably performed at about 50 to 1000 kV).
  • the raw material under reduced pressure Ju members (usually 10. ⁇ 10- 7 torr about, yo Ri and rather is preferable 10-1 to 10-about 5 torr) was placed in Irradiation is performed at a wavelength of about 0.01 to 100 angstroms (more preferably, about 0.1 to 10 angstroms).
  • the arrangement feedstock Metsu ⁇ Choi members (usually 10. ⁇ 10- 4 torr about, rather then preferred Ri yo is 10-1 ⁇ 10-3 about torr) in Then, using an ionized He ion or Ar ion, an acceleration voltage of about 100 V to 10 kV (more preferably, about 200 V to lkV) and an ion current of about 0.01 to 100 mA / cm 2 (more preferably, Irradiation is performed under conditions of about 0.1 to 10 mA / cm 2 ).
  • a raw material is placed in an inert gas atmosphere or a reducing gas atmosphere and brought into contact with a high-energy plasma fluid to produce a desired product.
  • An electromagnetic excitation source is used to generate the plasma fluid.
  • Conditions for plasma generation can be appropriately selected according to the type of gas, gas pressure, excitation voltage, excitation current, excitation power supply frequency, electrode shape, and the like.
  • gases are difficult to form a plasma state due to their characteristics. Even in such a case, it is possible to form a plasma state by increasing the input amount of the excitation electromagnetic field.
  • the gas used in the present invention include an inert gas such as Ar, He, Kr, and N 2 . Among these gases, Ar, He, etc. are more preferable.
  • the gas pressure needs to be selected in relation to the input excitation electromagnetic quantity. That is, as the gas pressure increases, the number of gas molecules increases and the energy required to excite each gas molecule also increases, so that a large amount of excitation electromagnetic is required. For example, it is possible to generate plasma even under a gas pressure of 10 atmospheres or more, but a large power supply is required, and equipment costs are significantly increased.
  • the gas pressure when the gas pressure is low, plasma is generated with a relatively small input excitation electromagnetic quantity. However, when the pressure is too low, a sufficient amount of plasma cannot be obtained.
  • the gas pressure during plasma generation 1 0- 2 Torr to arbitrarily favored and the call to the atmospheric pressure or less.
  • the electromagnetism may be either direct current or alternating current, and the material and shape of the electrode are selected according to the type of electromagnet to be applied.
  • alternating current a low frequency of about 50 to 60 Hz, a low frequency of about 10 to 10 kHz, or a high frequency of about 10 MHz to several GHz is usually used.
  • industrial high frequencies 13-56 ⁇ , 40MHz, 915MHz, 2.45GHz, etc. are commonly used.
  • the electrode material stainless steel, aluminum and its alloys, ordinary steel, etc. are usually used, and the shape is capacitive coupling type, parallel plate type, holo-force type, coil type, etc. Is selected from
  • At the time of treating the carbon raw material at least one of the above-described irradiation treatments and a heat treatment may be used in combination.
  • the carbonaceous material when the surface of the nanocarbon as described above is subjected to metal coating by a method such as vapor deposition, sputtering, and plating, the carbonaceous material is more excellent. Exhibits gas storage or gas storage capacity.
  • carbonaceous materials the above-mentioned metal-containing carbonaceous materials and metal-coated carbonaceous materials are collectively referred to as carbonaceous materials unless otherwise required.
  • the present invention can employ the following method.
  • carbon materials containing -C ⁇ C- or 2C2 synthesized by the reactive anodic electrolytic reduction method Can contain a trace amount of metal eluted from the anode during synthesis. Therefore, by subjecting such a carbon material to a heat treatment and a heat treatment or an irradiation treatment under conditions in which the contained metal component does not evaporate, the metal dispersion operation is not performed, and the metal dispersion operation is not performed. The resulting carbonaceous material is obtained.
  • the carbonaceous material according to the method of the present invention exerts an extremely excellent gas occlusion or storage ability for the following reasons.
  • a porous carbon material such as activated carbon and activated carbon fiber has a large specific surface area and has a property of adsorbing gas well on its surface.
  • carbon nanotubes can physically adsorb gas at high density inside the tube due to the capillary phenomenon, and can store gas at high density also in the space outside the tube created by the tubes. From this, it was pointed out that in a carbon nanotube, the gas storage capacity may be proportional to the controlled space in the nano order, that is, the specific surface area of the inner and outer surfaces of the tube.
  • the single-walled carbon nanotubes reported to date have difficulty in synthesis, structural control, opening of the tube tip, etc., as well as low density when filling the gas container and low expansion and contraction of the nanotube itself. There was a problem in durability due to low elasticity.
  • the amorphous force tubing according to the present invention is straight, has no entanglement between tubes, is capable of achieving high density, and has a multilayer and non-multilayer structure. Due to its crystalline structure, it has excellent elasticity and elasticity, so it absorbs the expansion and contraction of the tube due to physical adsorption of gas into the tube (hollow part) and exhibits high durability It has the feature of In other words, there is almost no problem in the graphitic structural material that the material is damaged by the expansion due to the adsorption of hydrogen between the layers and the durability is reduced.
  • the tip of the amorphous carbon tube according to the present invention has a specific flat structure and has a large strain, which is advantageous for opening the tip.
  • the hollow onion-like carbon, force-bon nanoparticle, and the like according to the present invention have a hollow nano-order controlled space, and are most suitable for absorbing gas molecules inside and outside. With structure.
  • these nanocarbons have a three-dimensional structure, and are not compatible with gas. Very large contact area. Since these nanocarbons have an amorphous structure, they have excellent elasticity and elasticity, and have remarkably high durability as a gas storage material.
  • the force contained in the nanocarbon or the metal coated on the surface thereof is iron, copper, nickel, copper, platinum, palladium, norrebedium. , Strontium, cesium, vanadium, manganese, nickel, aluminum, silver, lithium, sodium, magnesium, hydrogen storage alloy and metal complex, etc. it can.
  • the metal complex is not particularly limited, but examples thereof include a porphyrin complex and a Schiff base complex.
  • an amorphous carbonaceous material whose size, pore diameter, crystallinity, specific surface area, etc. are controlled is used as a gas storage material or a gas storage material, a pressure close to normal pressure in a cooled state At room temperature, various gases can be stably stored, durable, and efficiently stored and stored under relatively low pressure conditions at normal temperature.
  • the present invention is used, for example, as an energy source.
  • Neon, helium, and xenon which are extremely useful for the efficient storage, transportation, and use of hydrogen and methane (for example, automotive fuel for vehicles). It is also very useful for separating, transporting and storing rare gases such as non- and cryptones or carbon dioxide.
  • Reference Example 1 - C ⁇ C - or o containing samples to, under high vacuum of 10- 6 torr, the temperature 800 ° C, and irradiated with electron beam at an acceleration voltage 100k V.
  • TEM transmission electron microscope
  • amorphous carbon tube was immersed in dilute hydrochloric acid to dissolve the tip, whereby the tip was opened to obtain a gas storage material.
  • Example 2 After an onion-like carbon fiber containing magnesium fine particles was produced by the same operation as in Example 2, the temperature of the sample holder was raised to 800 ° C. and held for 10 minutes. As a result, the encapsulated magnesium particles were melted, then vaporized and disappeared, and hollow onion-like carbon was obtained as a final product.
  • (CH 3) 3 Si- ( C ⁇ C) 3 2 - was synthesized Si (CH 3) 3. That is, 10 wt% of commercially available 1,4-bis (trimethylsilyl) -1,3-butadiyne ⁇ (CH 3 ) 3 Si- (C ⁇ C) 2 -Si (CH 3 ) 3 ⁇
  • One drop of 1N aqueous K 2 CO 3 solution was added to 50 ml of a 50% methanol solution, and the mixture was stirred to hydrolyze the silyl group to give trimethylsilylbutadiyne ((CH 3 ) 3 Si -(C3C) 4 -H ⁇ was separated by column.
  • the amorphous carbon tube synthesized in Example 4 was graphitized at 2800 ° C to develop a graphite structure having a controlled structure.
  • Example 4 - was synthesized (C ⁇ C) 3 2 -H, and dispersing fine particles of metal magnesium (particle diameter of 1mm or less), irradiated with an electron beam, in the following manner under reduced pressure did.
  • the amorphous carbon tube produced in Example 1 was used as a gas occluding material without opening the tip.
  • the amorphous carbon tube produced in Example 4 was used as a gas occluding material without opening the tip.
  • the material was placed in an argon atmosphere (0.1 torr) and plasma-excited under the conditions of a power of 400 W and an R f frequency of 13.56 MHz.
  • the carbonaceous material having -C3C-structure on the PTFE phenol obtained in Reference Example 1 was subjected to X-ray irradiation. That is, against the material held in the 800 ° C under a reduced pressure (5 X 10- 4 torr), and irradiated X-rays (Cu K. i) 1 minute.
  • the obtained amorphous carbon tube was immersed in dilute hydrochloric acid to dissolve the tip, thereby opening the tip to obtain a gas storage material.
  • the carbonaceous materials obtained in Examples 1 to 8 can be used for other gases (such as methane, hydrogen, neon, xenon, krypton, and carbon dioxide). It was confirmed that the same excellent gas occlusion effect as for hydrogen was exhibited.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Hydrogen, Water And Hydrids (AREA)

Abstract

La présente invention concerne une matière d'occlusion de gaz comprenant un carbone amorphe contenant au moins un des composants cités ci-après: des tubes de carbone amorphe, des carbones de type oignon creux ou des nanoparticules de carbone. L'invention concerne également un procédé d'occlusion de gaz dans lequel est utilisée la matière d'occlusion de gaz précitée.
PCT/JP1999/002326 1998-05-01 1999-04-30 Matiere et procede d'occlusion de gaz WO1999056870A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP10/122148 1998-05-01
JP12214898 1998-05-01

Publications (1)

Publication Number Publication Date
WO1999056870A1 true WO1999056870A1 (fr) 1999-11-11

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Family Applications (1)

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PCT/JP1999/002326 WO1999056870A1 (fr) 1998-05-01 1999-04-30 Matiere et procede d'occlusion de gaz

Country Status (1)

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WO (1) WO1999056870A1 (fr)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000040509A1 (fr) * 1998-12-28 2000-07-13 Osaka Gas Company Limited Tube de carbone amorphe de l'ordre du nanometre et son procede de fabrication
JP2002228097A (ja) * 2000-11-22 2002-08-14 Air Products & Chemicals Inc 水素ガスの可逆的収着方法及び貯蔵方法
WO2003014018A1 (fr) * 2001-08-06 2003-02-20 Osaka Gas Company Limited Matiere carbonee, matiere d'occlusion de gaz renfermant ladite matiere carbonee et procede de stockage de gaz a l'aide de cette matiere d'occlusion de gaz
JP2004261739A (ja) * 2003-03-03 2004-09-24 Toyota Motor Corp 水素吸蔵複合材料
KR20160044707A (ko) * 2014-10-15 2016-04-26 건국대학교 산학협력단 이산화탄소 포집 및 저장 물질 및 이를 이용한 이산화탄소 포집 및 저장 방법

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0663396A (ja) * 1992-08-18 1994-03-08 Osaka Gas Co Ltd 吸蔵材
JPH06227806A (ja) * 1992-12-22 1994-08-16 Nec Corp 異物質内包カーボンナノチューブとその製造方法
JPH08325195A (ja) * 1995-05-31 1996-12-10 Nec Corp 金属被覆カーボンナノチューブおよびその製造方法
JPH1072201A (ja) * 1996-08-30 1998-03-17 Toyota Motor Corp 水素貯蔵方法
JPH11502494A (ja) * 1994-12-08 1999-03-02 ハイピリオン カタリシス インターナショナル インコーポレイテッド 官能基化されたナノチューブ
JPH11116219A (ja) * 1997-10-15 1999-04-27 Matsushita Electric Ind Co Ltd 水素貯蔵体とその製法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0663396A (ja) * 1992-08-18 1994-03-08 Osaka Gas Co Ltd 吸蔵材
JPH06227806A (ja) * 1992-12-22 1994-08-16 Nec Corp 異物質内包カーボンナノチューブとその製造方法
JPH11502494A (ja) * 1994-12-08 1999-03-02 ハイピリオン カタリシス インターナショナル インコーポレイテッド 官能基化されたナノチューブ
JPH08325195A (ja) * 1995-05-31 1996-12-10 Nec Corp 金属被覆カーボンナノチューブおよびその製造方法
JPH1072201A (ja) * 1996-08-30 1998-03-17 Toyota Motor Corp 水素貯蔵方法
JPH11116219A (ja) * 1997-10-15 1999-04-27 Matsushita Electric Ind Co Ltd 水素貯蔵体とその製法

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000040509A1 (fr) * 1998-12-28 2000-07-13 Osaka Gas Company Limited Tube de carbone amorphe de l'ordre du nanometre et son procede de fabrication
JP3355442B2 (ja) 1998-12-28 2002-12-09 大阪瓦斯株式会社 アモルファスナノスケールカーボンチューブおよびその製造方法
US6960334B1 (en) 1998-12-28 2005-11-01 Osaka Gas Company Limited Amorphous nano-scale carbon tube and production method therefor
JP2002228097A (ja) * 2000-11-22 2002-08-14 Air Products & Chemicals Inc 水素ガスの可逆的収着方法及び貯蔵方法
WO2003014018A1 (fr) * 2001-08-06 2003-02-20 Osaka Gas Company Limited Matiere carbonee, matiere d'occlusion de gaz renfermant ladite matiere carbonee et procede de stockage de gaz a l'aide de cette matiere d'occlusion de gaz
JP2004261739A (ja) * 2003-03-03 2004-09-24 Toyota Motor Corp 水素吸蔵複合材料
KR20160044707A (ko) * 2014-10-15 2016-04-26 건국대학교 산학협력단 이산화탄소 포집 및 저장 물질 및 이를 이용한 이산화탄소 포집 및 저장 방법
KR101913328B1 (ko) 2014-10-15 2018-10-30 건국대학교 산학협력단 이산화탄소 포집 및 저장 물질 및 이를 이용한 이산화탄소 포집 및 저장 방법

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