WO2012148037A1 - Procédé de production de nanopores façonnés dans une grille de carbone - Google Patents

Procédé de production de nanopores façonnés dans une grille de carbone Download PDF

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Publication number
WO2012148037A1
WO2012148037A1 PCT/KR2011/003985 KR2011003985W WO2012148037A1 WO 2012148037 A1 WO2012148037 A1 WO 2012148037A1 KR 2011003985 W KR2011003985 W KR 2011003985W WO 2012148037 A1 WO2012148037 A1 WO 2012148037A1
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WIPO (PCT)
Prior art keywords
carbon
nanopore
lattice
alkali metal
precursor
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Ceased
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PCT/KR2011/003985
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English (en)
Korean (ko)
Inventor
김호
최창식
한기보
장정희
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Institute for Advanced Engineering
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Institute for Advanced Engineering
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Publication date
Application filed by Institute for Advanced Engineering filed Critical Institute for Advanced Engineering
Priority to JP2014508268A priority Critical patent/JP5784822B2/ja
Publication of WO2012148037A1 publication Critical patent/WO2012148037A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28078—Pore diameter
    • B01J20/2808—Pore diameter being less than 2 nm, i.e. micropores or nanopores
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
    • 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
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28023—Fibres or filaments
    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B1/00—Nanostructures formed by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
    • 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
    • C01B32/30—Active carbon
    • C01B32/354—After-treatment
    • C01B32/382—Making shaped products, e.g. fibres, spheres, membranes or foam
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

Definitions

  • the present invention relates to a method for producing carbon lattice nano-pores having a surface area of at least 2,500 m 2 / g by developing fine pores of 3 nm or less in a carbon matrix material having pores.
  • carbon lattice materials having pores that are widely used include activated carbon (AC), activated carbon fiber (ACF), and the like.
  • AC activated carbon
  • ACF activated carbon fiber
  • the carbon lattice material has a surface area of 1,000 to 1,500 m 2 / g.
  • the size of the pores of 1 to 10 is broadly distributed from 5 nm range, there is the structure of the pore is a complex form, the size of the pore adsorption and desorption than the activated carbon fiber present at least 90% 3 nm or less, only There is a drawback that it is slow.
  • the structure, size and size distribution of pores of carbon lattice materials when adsorbing and desorbing hydrocarbons such as volatile organic compounds (VOCs) by carbon lattice materials are determined by adsorption amount and adsorption / desorption rate .
  • the carbon lattice material has a larger adsorption amount because the surface area increases as the number of micropores increases, and as the pore structure is simple and the pore size distribution is narrower, the adsorption / desorption rate is faster.
  • the adsorption capacity is increased and at the same time, it is possible to secure a long-life adsorbent which is easy to repeatedly regenerate and desorb, and the recovery of the adsorbed material by repeated adsorption / There is an effect that it becomes easy.
  • FIG. 1 shows a conventional method of developing nano-sized micro pores on the surface of a carbon lattice having pores such as activated carbon and activated carbon fibers.
  • the conventional micro pore manufacturing method includes a step (S10) of preparing a precursor using activated carbon as a starting material and a fibrous material as an activated carbon fiber, (S30) in which the carbon material formed in the stabilization process is carbonized in an oxygen-free condition at a temperature of 1,000 to 1,500 DEG C to form primary pores; ) And an activation process (S40) for further developing the first formed pores by injecting CO 2 or steam in an oxygen-free condition at a temperature of 800 to 1,200 ° C.
  • a final process (S 50) the surface area Activated carbon or activated carbon fibers having a level of 1,500 m 2 / g are produced.
  • Conventional methods utilize means for increasing the temperature by forming oxygen functional groups and controlling the density.
  • the higher the temperature the greater the loss of oxidation of the carbon body, and the temperature at the surface of the carbon lattice is not uniformly distributed, so that the formed oxygen functional group is also difficult to uniformly form on the surface of the carbon lattice.
  • the porosity must be partially oxidized only at the site of the oxygen functional group.
  • the pores are not developed and simply pyrolyzed, resulting in the reduction of the weight of the carbon body.
  • the method of injecting CO 2 or steam has an advantage in adjusting the partial oxidation rate, but it can be performed only at a high temperature of 800 ° C or more because of low oxidizing power, And the economical efficiency is lowered.
  • the object of the present invention is to solve the problems of the prior art, namely, 1 low concentration and non-uniformity of oxygen functional groups in the stabilization process, and In order to solve the problem of temperature and long process time, surface treatment and surface modification are carried out in conjunction with the development of micropores of less than 3 nm on a carbon matrix material with pores to obtain a surface area of 2,500 m 2 / g or more of carbon nanotubes.
  • the present invention provides a method for producing a carbon lattice-like nano-pore, comprising the steps of: preparing a precursor as a starting material of a carbon lattice material; A carbonization step of carbonizing the carbon body formed in the stabilization step to form primary pores by carbonization under anaerobic conditions, and a step of forming a primary oxygen-functional group on the surface of the carbon lattice in a highly homogeneous manner A surface treatment process in which ozone is contacted to perform a surface treatment; and a step of immersing the carbon body subjected to the surface treatment in an aqueous solution of an alkali metal to bring the alkali metal into contact with the oxygen functional group formed by the ozone contact in the surface treatment process , And the surface of the carbon body subjected to the surface treatment in an oxygen-free atmosphere is heated to 800 DEG C or lower Comprises a surface modification step of the developed micropores and characters perform surface modification by inducing
  • the surface treatment may be carried out at a room temperature with ozone in a weight ratio of 0.2-0.7 g to the weight of 1 g of the carbon body.
  • the surface modification process can immerse the surface-treated carbon body in an aqueous solution of alkali metal having a concentration of 1 to 5M for 1 hour or more.
  • alkali metal having a concentration of 1 to 5M for 1 hour or more.
  • Na or K is preferably used as the alkali metal.
  • the carbon lattice-phase nano pore manufacturing method of the present invention is characterized in that after completion of the surface modification process, the carbon material subjected to the surface modification treatment is cooled to an ordinary temperature under anoxic condition and then immersed in a sulfuric acid solution having a concentration of 5M or more for 1 hour or more And then washing with distilled water to neutralize the pH to 5 to 7, followed by drying at about 150 ° C in an air atmosphere, so that activated carbon or activated carbon fiber can be produced.
  • the precursor is preferably oxidized at a temperature ranging from 200 to 300 ° C.
  • the carbon material is preferably carbonized at a temperature ranging from 900 to 1000 ° C.
  • the carbon lattice material may include activated carbon, and the precursor of the activated carbon preferably includes a wood-based material.
  • the carbon lattice material may include activated carbon fibers, and the precursor of the activated carbon fibers may include a fibrous material.
  • the carbon lattice material produced by the conventional method has a surface area of 1,000 to 1,500 m 2 / g, but when the surface treatment according to the present invention is performed in conjunction with the surface modification, the surface area of the carbon lattice material And more than 2,500 m 2 / g.
  • the conventional carbonization temperature is lowered from 1,000 to 1,500 ° C. to 900 to 1,000 ° C. and the conventional activation temperature is reduced from 700 to 800 ° C. at 800 to 1,200 ° C.
  • the conventional surface area of 1,000 to 1,500 m 2 / g to 2,500 m 2 / g or more.
  • the number of regeneration times in conventional regeneration conditions in which activated carbon or low-quality activated carbon fiber is desorbed at 120 DEG C after adsorbing hydrocarbons such as toluene to the destruction point is 70% of the initial adsorption amount at the conventional four- ,
  • the active and activated carbon fibers prepared according to the present invention retained more than 90% of the initial adsorption amount even when the number of regeneration was repeated 50 times or more.
  • the nanocomposite carbonaceous adsorbent produced by the present invention can be produced at a lower temperature than the conventional method and can be used as a hydrocarbon treatment and recovery filter having high efficiency and long life Effect.
  • FIG. 1 is a process diagram showing a conventional method of manufacturing a carbon nanotube with a lattice structure.
  • FIG. 2 is a process diagram of a method for manufacturing a carbon lattice-like nano-pores according to a preferred embodiment of the present invention.
  • FIG. 2 shows a process for producing a carbon nanotube with carbon nanotubes according to a preferred embodiment of the present invention.
  • the carbon lattice-phase nanopore production method of the present invention is a method of developing nano-sized micropores in a carbon matrix material having pores.
  • carbon lattice materials having pores include activated carbon (AC), activated carbon fiber (ACF), and the like.
  • Surface treatment (ST) and surface treatment Surface modification (Surface Activation, SA) can be linked to develop nano-sized pores to increase surface area and speed up adsorption and desorption. By increasing the surface area as described above, the amount of adsorbed to hydrocarbons in the air or in the water is increased, and the adsorption / desorption rate is rapidly exhibited, thereby improving the regeneration and recovery efficiency.
  • the method for preparing a carbon lattice-like nano-pores according to the present invention includes a step (S100) of preparing a precursor as a starting material.
  • a step (S100) of preparing a precursor as a starting material When the carbon lattice material of the present invention is activated carbon, a wood-based material is used as the precursor, and when the carbon lattice material is activated carbon fiber, a fiber-based material is used as the precursor.
  • the carbon lattice-phase nano-pore structure of the present invention may further comprise a stabilization step (S200) of oxidizing the precursor by bringing the precursor into contact with air at a temperature of 200 to 300 ° C (S200)
  • the contact of ozone in the surface treatment process is carried out for the purpose of forming a highly homogeneous oxygen functional group on the surface of the carbon lattice on the carbon body having unfilled pores for producing a carbon body,
  • the surface treatment is performed by the pre-treatment concept.
  • ozone can be contacted with 1 g of carbon body at room temperature and ozone in a weight ratio of 0.2 to 0.7 g or less.
  • the surface treated carbon body is immersed in an aqueous solution of alkali metal of 1 to 5M concentration for 1 hour or more (at room temperature in 1-5 M solution), wherein the alkali metal is Na or K desirable.
  • the surface of the carbon body is immersed in an aqueous solution of an alkali metal, and the carbon body is dried in an air atmosphere at a temperature of 100 to 200 ° C. and maintained at an oxygen-free condition and a temperature of 600 to 800 ° C. for 1 hour or more.
  • the substrate was cooled to room temperature under anaerobic conditions, immersed in a sulfuric acid solution having a concentration of 5M or less for 1 hour or more, washed with distilled water to neutralize the pH to 5 to 7, (S700) at about 150 < 0 > C.
  • activated carbon or activated carbon fiber having a large surface area at a surface area of 2,500 m 2 / g can be produced.
  • Table 1 shows the detailed characteristics of the activated carbon fibers produced by the production method of the present invention in conjunction with the surface treatment and the surface modification as described above and the conventional activated carbon fibers having no pores.
  • the number of regeneration times is reduced to 70% or less of the initial adsorption amount at the conventional four times level, It can be confirmed that the carbon fiber retains more than 90% of the initial adsorption amount even when the number of regeneration is repeated 50 times or more.
  • the present invention is not limited to the above-described embodiments, the present invention can provide a nano- It will be understood by those of ordinary skill in the art that various changes in form and details may be made therein without departing from the spirit and scope of the present invention.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

Cette invention concerne un procédé de production de nanopores façonnés dans une grille de carbone, comprenant : une étape de préparation d'un précurseur en tant que matière première ; une étape de stabilisation à laquelle le précurseur est oxydé par mise en contact avec l'air ; une étape de carbonisation à laquelle la forme de carbone formée à l'étape de stabilisation, est carbonisée dans une atmosphère sans oxygène de façon à former des pores primaires ; une étape de traitement de surface, à laquelle la forme de carbone dans laquelle les pores primaires ont été formés est soumise à un traitement de surface par mise en contact avec de l'ozone ; une étape de trempage, à laquelle la forme de carbone ayant subi le traitement de surface est trempée dans une solution aqueuse d'un métal alcalin ; et une étape de modification de la surface, à laquelle une modification de la surface est réalisée par oxydation et réduction du métal alcalin dans une atmosphère sans oxygène tandis que la température est portée à un niveau inférieur ou égal à 800°C. Suite à l'exécution de la modification de surface, le procédé de l'invention comprend en outre une étape de refroidissement à température ambiante dans une atmosphère sans oxygène, suivie d'une étape de trempage d'au moins une heure dans une solution d'acide sulfurique inférieure à 5M, d'une étape de nettoyage dans de l'eau distillée et d'une étape de séchage à l'air, à une température d'environ 150°C.
PCT/KR2011/003985 2011-04-28 2011-05-31 Procédé de production de nanopores façonnés dans une grille de carbone Ceased WO2012148037A1 (fr)

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JP2014508268A JP5784822B2 (ja) 2011-04-28 2011-05-31 カーボンマトリックスナノ気孔の製造方法

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KR10-2011-0039867 2011-04-28
KR1020110039867A KR101315112B1 (ko) 2011-04-28 2011-04-28 탄소격자상 나노기공 제조방법

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KR101383127B1 (ko) * 2012-03-29 2014-04-09 고등기술연구원연구조합 표면처리와 표면개질을 연계한 탄소격자상 나노기공 제조방법
KR101419868B1 (ko) * 2013-04-22 2014-07-16 고등기술연구원연구조합 탄소체의 나노기공 제조방법
KR102599131B1 (ko) 2023-02-23 2023-11-07 고등기술연구원연구조합 자원순환형 고도활성화를 이용한 리그노셀룰로오스 바이오매스 활용 고비표면적 활성탄소 제조방법
KR102879820B1 (ko) 2023-04-13 2025-11-03 고등기술연구원연구조합 석유계 잔사물을 활용한 자원순환형 활성탄소 제조방법

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US5997613A (en) * 1988-10-25 1999-12-07 Osaka Gas Company Limited Gas phase adsorption process utilizing oxidized pitch-based activated carbon fibers
KR20030095694A (ko) * 2002-06-14 2003-12-24 한국화학연구원 나노섬유를 이용한 활성탄소섬유의 제조방법
US20070155847A1 (en) * 2005-12-29 2007-07-05 Miller Douglas J High surface area activated carbon foam
US7256156B2 (en) * 2002-02-25 2007-08-14 Gentex Corporation Reactive-adsorptive protective materials and methods for use

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JPH07100635B2 (ja) * 1987-03-30 1995-11-01 ぺんてる株式会社 活性炭成形物の製造方法
JP3446339B2 (ja) * 1994-10-18 2003-09-16 三菱化学株式会社 活性炭の製造方法
JP3930131B2 (ja) * 1997-12-26 2007-06-13 松下エコシステムズ株式会社 アルデヒド類除去剤
JP2004099742A (ja) 2002-09-10 2004-04-02 At Kk 炭化装置
JP4844942B2 (ja) * 2005-11-29 2011-12-28 東海カーボン株式会社 親水性多孔質炭素材料及びその製造方法
JP5599186B2 (ja) * 2009-12-28 2014-10-01 Ｊｘ日鉱日石エネルギー株式会社 電気二重層キャパシタ電極用活性炭およびその製造方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5997613A (en) * 1988-10-25 1999-12-07 Osaka Gas Company Limited Gas phase adsorption process utilizing oxidized pitch-based activated carbon fibers
US7256156B2 (en) * 2002-02-25 2007-08-14 Gentex Corporation Reactive-adsorptive protective materials and methods for use
KR20030095694A (ko) * 2002-06-14 2003-12-24 한국화학연구원 나노섬유를 이용한 활성탄소섬유의 제조방법
US20070155847A1 (en) * 2005-12-29 2007-07-05 Miller Douglas J High surface area activated carbon foam

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JP2014516904A (ja) 2014-07-17
JP5784822B2 (ja) 2015-09-24
KR101315112B1 (ko) 2013-10-08

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