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WO2003026792A1 - Charbon actif en fibre et procede de production - Google Patents

Charbon actif en fibre et procede de production Download PDF

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Publication number
WO2003026792A1
WO2003026792A1 PCT/JP2002/009919 JP0209919W WO03026792A1 WO 2003026792 A1 WO2003026792 A1 WO 2003026792A1 JP 0209919 W JP0209919 W JP 0209919W WO 03026792 A1 WO03026792 A1 WO 03026792A1
Authority
WO
WIPO (PCT)
Prior art keywords
activated carbon
value
carbon fiber
nitrogen
carbon fibers
Prior art date
Legal status (The legal status 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 status listed.)
Ceased
Application number
PCT/JP2002/009919
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English (en)
Japanese (ja)
Inventor
Toyoki Uyama
Tatsuo Katayama
Takeshi Maeda
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
AD'ALL Co Ltd
Osaka Gas Chemicals Co Ltd
Unitika Ltd
Original Assignee
AD'ALL Co Ltd
Osaka Gas Chemicals Co Ltd
Unitika Ltd
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 AD'ALL Co Ltd, Osaka Gas Chemicals Co Ltd, Unitika Ltd filed Critical AD'ALL Co Ltd
Priority to JP2003530419A priority Critical patent/JPWO2003026792A1/ja
Publication of WO2003026792A1 publication Critical patent/WO2003026792A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • 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

Definitions

  • the present invention relates to a novel activated carbon fiber and a method for producing the same.
  • Activated carbon fibers have different characteristics from granular or powdered activated carbon in not only their appearance but also their pore structure. 'Activated carbon fibers with such characteristics are widely used for various applications including adsorbents.
  • activated carbon fibers are fibrous as the name implies, they generally have a larger exposed surface per unit weight than granular or powdered activated carbon. For this reason, it exhibits characteristics that it is easier to make contact with the object to be processed and that the pressure loss during passage of the object fluid can be reduced.
  • Activated carbon fiber has a large specific surface area and has many micropores, so it is very effective for removing the smell of powder.
  • the substance causing the moldy odor is a macromolecule, it is difficult to be trapped in the micropores of the activated carbon fiber and is not suitable for the activated carbon fiber.
  • a main object of the present invention is to provide an activated carbon fiber which is excellent in both the performance of removing and adsorbing trihalomethanes and the performance of removing and adsorbing substances causing moldy odor.
  • an activated carbon fiber having a specific microstructure can achieve the above object, and have completed the present invention.
  • the present invention relates to the following activated carbon fiber and a method for producing the same.
  • V (0.1) is greater than 200 c c / g
  • V (0.1) / V (0.2) The value of V (0.1) / V (0.2) is 0.92 to 0.99,
  • V (0.2) / V (0.8) is 0.80 to 0.95
  • a method for producing activated carbon fibers for adsorption of trihalomethanes and moldy odor-causing substances comprising: (1) 0.01 to 5% by weight of at least one metal component of vanadium, platinum and iron as an activated carbon precursor.
  • V (0.1) is 200 cc / g or more
  • V (0.2) is 0.92 to 0.99
  • V (0.2) ZV (0.8) is 0.80 to 0.95 and
  • the activated carbon fiber has a relative pressure PZP in the nitrogen adsorption isotherm at 77.4 K. V (P / Po)
  • V (0.1) The value of V (0.1) is 200 c cZg or more,
  • V (0.1) / V (0.2) The value of V (0.1) / V (0.2) is 0.92 to 0.99,
  • V (0.2) ZV (0.8) is 0.80 to 0.95 and
  • V (0.8) / V (1.0) is 0.80 to 0.90
  • a method for removing trioctanemethane and fungi-causing substances by passing water to be treated through a tubular body filled with activated carbon fibers according to the above item 1.
  • micropore refers to a pore having a pore diameter of less than 20 A
  • mesopore refers to a pore having a pore diameter of 20 to 500 A
  • macropore refers to a fine pore.
  • the activated carbon fiber of the present invention has a nitrogen adsorption isotherm at 77.4 K at a relative pressure PZP. V (P / Po)
  • V (0.1) (hereinafter referred to as “a value”) is 200 c cZg or more
  • V (0.1) ZV (0.2) (hereinafter referred to as “b value”) is 0.92 to 0.99
  • V (0.2) ZV (0.8) (hereinafter referred to as “c value”) is 0.80 to 0.95 and
  • V (0.8) ZV (1.0) (hereinafter referred to as “d value”) is 0.80 to 0.90
  • the nitrogen adsorption isotherm is created as follows. Cool the activated carbon fiber to 77.4 K (boiling point of nitrogen), introduce nitrogen gas, and measure the adsorption amount of nitrogen gas V [cc / g] by the volumetric method. At this time, the pressure P [mmHg] of the nitrogen gas to be introduced is gradually increased to the saturated vapor pressure P of the nitrogen gas. The value divided by [mmHg] is the relative pressure PZP.
  • the nitrogen adsorption isotherm is created by plotting the amount of adsorption with respect to each relative pressure. In this nitrogen adsorption isotherm, let the amount of nitrogen gas adsorbed at each relative pressure (PZPo) be V (P / Po).
  • the nitrogen gas adsorption amount when the relative pressure is 0.1 is expressed as V (0.1).
  • the nitrogen adsorption isotherm can be obtained by taking the relative pressure (P / P.) On the horizontal axis and the nitrogen gas adsorption amount V (P / Po) on the vertical axis.
  • a commercially available automatic gas adsorption amount measuring device can be used.
  • trade name “AUTOSORB-6” manufactured by QUANT CHROME) or the like can be preferably used.
  • the value a is set to 200 cc / g or more, preferably 220 cc / g or more. If the a value is less than 200 ccZg, it may generally be difficult to effectively adsorb and remove the substance to be adsorbed.
  • the b value is 0.92 to 0.99, preferably 0.95 to 0.99. If the b value is less than 0.92, the number of micropores and mesopores having a pore diameter close to the pore diameter of the micropores becomes excessive, so that the desired adsorption performance may not be obtained. is there. On the other hand, if the b value exceeds 0.99, the number of micropores and mesopores having a pore diameter close to that of the micropores becomes too small, so that the adsorption performance may be reduced.
  • the c value is set to 0.80 to 95, preferably 0.85 to 0.95. If the c value is less than 0.80, the mesopores having a pore diameter of about 20 to 100 A are excessive, and the effect of the present invention may not be obtained. If the c value exceeds 0.95, the number of mesopores in the vicinity of the pore diameter of 20 to 100 A becomes too small, so that the effect as the water purification material of the present invention may not be obtained.
  • the d value is 0.80 to 0.90, preferably 0.82 to 0.90. If the d value is less than 0.80, the macropores and the mesopores having a pore diameter close to the macropore diameter become excessive, so that the desired adsorption performance may not be obtained. You. If the d-value exceeds 0, 90, the macropores and the mesopores having a pore diameter close to the macropore diameter become too small, so that the performance as the material for water purification and purification etc. of the present invention is reduced. The power may not be exerted.
  • the activated carbon fiber of the present invention can be suitably used for conventional activated carbon fiber applications.
  • it can be suitably used as a material for adsorbing and removing trihalomethanes and fungi-causing substances. Therefore, it can be used as a material for water purification and gas purification.
  • the material of the present invention may be used as it is instead of a known adsorbent in a water purifier or the like.
  • the present invention also includes a method for removing trihalomethanes and moldy odor-causing substances using the activated carbon fibers.
  • the tubular body filled with the activated carbon fiber of the present invention by passing water to be treated through the tubular body filled with the activated carbon fiber of the present invention, trihalomethines and fungal odor-causing substances in the water to be treated can be adsorbed and removed.
  • the amount of water passed, the amount of the material of the present invention, and the like may be in accordance with known methods and conditions.
  • the activated carbon fiber of the present invention may be produced by any method as long as it has the above-mentioned a to d values.
  • the following production method is preferable.
  • the activated carbon fiber of the present invention in a method for producing an activated carbon fiber by melt-spinning, infusibilizing, and activating the activated carbon precursor, at least one metal component of vanadium, platinum, and iron is used as the activated carbon precursor. According to the method characterized by using a pitch containing 1 to 5% by weight, the activated carbon fiber of the present invention can be obtained more reliably.
  • the metal component is at least one of vanadium, platinum and iron.
  • the type of metal to be combined, the ratio thereof, and the like may be appropriately set according to the use of the activated carbon fiber, the purpose of use, and the like.
  • the content of the metal component is adjusted so as to be 0.01 to 5% by weight, preferably 0.1 to 2% by weight in the activated carbon precursor. If the content of the metal component is less than 0.01% by weight, activated carbon fibers having the above a-values-d cannot be obtained due to weakening of the action of the metal during the activation reaction. There is. Conversely, if it exceeds 5% by weight, Since the metal component condenses and forms in the charcoal, the physical strength of the activated carbon fiber is remarkably reduced, which may make it impractical as a water purification material.
  • the content of the metal component is not a content as a metal compound but a content in terms of a metal element, and is a value measured by an ICP emission spectrometry.
  • the activated carbon precursor can be prepared, for example, by mixing a compound containing the metal component (metal compound) and pitch.
  • the pitch is not particularly limited as long as it can be activated carbon by infusibilization, carbonization, and the like, and can be mixed with a metal compound.
  • any of petroleum pitch, coal pitch, synthetic pitch and the like can be used.
  • the optical properties may be either isotropic or anisotropic.
  • an activated carbon precursor containing pitch and a metal component may be obtained by mixing and stirring a coal tar, which is a raw material for pitch, and a metal compound in a solvent, and then performing distillation under reduced pressure. it can.
  • the metal compound is not particularly limited as long as these metal components are contained, and any of an inorganic compound and an organic compound can be used.
  • the inorganic compound for example, inorganic salts such as chloride, nitrate, and acetate are used. Specifically, iron chloride, iron nitrate, iron acetate and the like can be exemplified.
  • the organic compound an organic metal complex of the above metal component and acetylacetone / cyclopentene is used. Specifically, iron trisacetyl acetatonate, iron acetyl acetatonate, trissix pen penis genil iron and the like can be exemplified.
  • the method of mixing the metal compound and the pitch is not limited as long as they can be uniformly mixed.
  • the metal compound and the pitch may be mixed as they are, or both may be mixed in an appropriate solvent.
  • the solvent is not particularly limited as long as it can dissolve both the metal compound and the pitch.
  • Pitch to be used is selected from known solvents such as quinoline, benzene, dichloromethane, toluene, xylene, tetrahydrofuran, methanol, and ethanol. And the type of the metal compound may be appropriately selected.
  • quinoline or the like can be used.
  • the amount of the solvent used is not particularly limited as long as a uniform activated carbon precursor can be obtained, and may be appropriately set according to the type of the solvent, the metal compound, and the like to be used.
  • the obtained activated carbon precursor After spinning the obtained activated carbon precursor, it is subjected to infusibilization treatment and / or carbonization treatment and then to activation treatment, whereby the activated carbon fiber of the present invention can be obtained.
  • the spinning method, the infusibilization treatment, the carbonization treatment and the activation treatment are preferably carried out by the following methods.
  • the spinning method can be performed according to a known melt spinning method.
  • the melting temperature and the spinning temperature are generally set to a temperature equal to or higher than the softening point of the activated carbon precursor, and preferably set to a temperature higher by 30 to 100 ° C. than the softening point.
  • the molten activated carbon precursor is sent to the nozzle of a spinning machine, and is discharged from a nozzle surface having many pores while forming fibers in an atmosphere controlled at a spinning temperature or lower.
  • the activated carbon precursor is heated from a temperature below its melting point to about 400 ° C at a rate of 0.1 to 10 ° CZ in an inert gas atmosphere or an oxygen-containing gas atmosphere. Can be implemented.
  • the activated carbon precursor is heated to about 800 to 1200 ° C. at a temperature increasing rate of 5 to 10 ° C.Z under an inert gas atmosphere such as nitrogen gas and argon gas. It can be implemented by maintaining the maximum temperature at that time for a maximum of about 10 minutes.
  • the activation treatment is an activated carbon precursor that has been subjected to infusibilizing treatment and Z or carbonization treatment in a gas atmosphere in which water vapor, carbon dioxide, oxygen, a mixed gas thereof, and these gases are diluted with an inert gas such as nitrogen. Is held at a temperature of about 800 to 1200 ° C. for about 5 to 120 minutes.
  • the activated carbon precursor to be subjected to the carbonization treatment or the activation treatment preferably contains 5% by weight or more of oxygen atoms.
  • oxygen atoms are contained in an amount of 5% by weight or more, when the oxygen atoms are desorbed in the carbonization or activation reaction, the metal components interact with each other. The effect of appropriately perforating mesopores having a pore diameter close to the pore diameter of the pores is obtained.
  • the content of oxygen atoms can be appropriately adjusted under infusibilizing conditions such as infusibilizing temperature and infusibilizing time.
  • the nitrogen gas of the activated carbon fiber thus obtained is used.
  • the nitrogen gas adsorption amount at relative pressure P / P Q is defined as V (P / Po)
  • V (0.1) is greater than 200 c c / g
  • V (0.1) / V (0.2) The value of V (0.1) / V (0.2) is 0.92 to 0.99,
  • V (0.2) / V (0.8) is 0.80 to 0.95
  • V (0.8) / V (1.0) is 0.80 to 0.90
  • the method for measuring the nitrogen gas adsorption amount may be the same as described above.
  • the present invention also includes a method for selecting activated carbon fibers for adsorbing trihalomethanes and fungi-causing substances. That is, a method for selecting activated carbon fibers for adsorbing trioctanes and moldy odor causing substances,
  • V (0.1) is greater than 200 c c / g
  • V (0.1) / V (0.2) The value of V (0.1) / V (0.2) is 0.92 to 0.99,
  • V (0.2) / V (0.8) is 0.80 to 0.95
  • V (0.8) / V (1.0) is 0.80 to 0.90
  • the present invention encompasses a method characterized by selecting an activated carbon fiber that satisfies all conditions.
  • This selection method can be applied to all activated carbon fibers, including activated carbon fibers produced by a method other than the above-mentioned production method.
  • the method for measuring the nitrogen gas adsorption amount may be the same as described above.
  • Activated carbon fibers satisfying all of the above conditions (a) and (b) exhibit an excellent effect as a material for adsorbing trihalomenes and fungal odor-causing substances.
  • the size of the molecules of trihalomethanes is not so large that they cannot penetrate into the pores of Miku like the substances that cause moldy odor.
  • the activated carbon fiber of the present invention exerts an excellent effect as an adsorbent capable of removing virtually all of low molecular substances represented by a odor of lime, macromolecules such as trichloromethanes, and substances causing a moldy odor. be able to. That is, the activated carbon fiber of the present invention having such characteristics is useful as an activated carbon fiber for adsorbing trioctane compounds and fungi-causing substances, and specifically, a water purification material and a gas purification material. Etc. can be suitably used.
  • Figure 1 shows the nitrogen adsorption isotherms of the iron-containing activated carbon fiber of Example 1, the platinum-containing activated carbon fiber of Example 2, the metal-free activated carbon fiber of Comparative Example 1, and the iron-containing activated carbon fiber of Comparative Example 3. It is a figure showing a line.
  • the amount of nitrogen gas adsorbed on the activated carbon fiber was measured using "AUTOSORB-6" (trade name, manufactured by QUANTCHROME).
  • the spun pitch fibers are heated in the air from room temperature at a heating rate of 1 to 10 and held at the maximum temperature of 364 ° C for 4 minutes, and the infusibilizing treatment is performed over a total infusibilizing time of 65 minutes. Was done.
  • the infusibilized pitch fiber was exposed to saturated steam at 850 ° C. for 60 minutes in a nitrogen atmosphere to perform an activation treatment to obtain an iron-containing activated carbon fiber.
  • Table 1 shows a to d values of the obtained activated carbon fibers.
  • Figure 1 shows the nitrogen adsorption isotherm.
  • a coal tar pitch was obtained in the same manner as in Example 1, except that 5.7 g of acetyl acetonato platinum was used instead of 6 g of acetyl acetonato iron.
  • the platinum content of this pitch was 2.60% by weight.
  • the spun pitch fibers were heated from room temperature in the air at a rate of temperature increase of 2 ° C / min, and kept at 375 for 15 minutes for infusibility treatment.
  • the infusibilized pitch fiber was exposed to saturated steam at 850 for 35 minutes in a nitrogen atmosphere to perform an activation treatment to produce a platinum-containing activated carbon fiber.
  • Table 1 shows a to d values of the obtained activated carbon fibers.
  • Figure 1 shows the nitrogen adsorption isotherm.
  • Activated carbon fibers were produced in the same manner as in Example 1, except that no metal compound was mixed and the activation treatment time was 30 minutes.
  • Table 1 shows a to d values of the obtained activated carbon fibers.
  • Figure 1 shows the nitrogen adsorption isotherm.
  • Activated iron-containing carbon fibers were produced in the same manner as in Example 1 except that the maximum temperature in the infusibilization treatment was changed to 26.4 t :. At this time, the oxygen atom content in the activated carbon precursor was 2.55%.
  • Table 1 shows a to d values of the obtained activated carbon fibers.
  • Figure 1 shows the nitrogen adsorption isotherm. Tatami mat
  • JI SS-320 1 Acrylic container was filled with 8.4 g of a milled sample based on the “Test method for household water purifiers (continuous method)” so as to be 48 mm (diameter) ⁇ 30 mm (height). Then, raw water having a 2-methylisoborneol concentration of 5.5 ppt was passed at a flow rate of 3 L / min. Outlet concentration C and initial concentration C at this time. The flow rate at which the ratio CZCQ became 0.2 was defined as the filtration capacity.
  • the above analyzer was performed by the purge trap method using the trade name “GCMS-QP 5050” (manufactured by Shimadzu Corporation). Table 2
  • the activated carbon fiber of the present invention can exert excellent effects not only on the adsorption and removal performance of trioctane methanes but also on the adsorption and removal performance of the fungi-causing substance.
  • Comparative Example 2 it was difficult to carry out a filtration ability test due to the remarkable powdering.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Fibers (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

La présente invention concerne un charbon actif en fibre se prêtant particulièrement à l'élimination par adsorption de composés trihalométanés et de substances sources de mauvaises odeurs. La caractéristique de ces fibres est de donner à 77,4 K un isotherme d'adsorption V(P/P0) de l'azote gazeux, 'P/P0' exprimant la pression relative, (a) d'au moins 200 cm3 pour V(0.1), (b) de 0,92 cm3 à 0,99 cm3 à pour V(0.1)/V(0.1), (c) de 0,80 cm3 à 0,95 cm3 à pour V(0.2)/V(0.8), et (d) de 0,80 cm3 à 0,90 cm3 à pour V(0.8)/V(1.0).
PCT/JP2002/009919 2001-09-26 2002-09-26 Charbon actif en fibre et procede de production Ceased WO2003026792A1 (fr)

Priority Applications (1)

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JP2003530419A JPWO2003026792A1 (ja) 2001-09-26 2002-09-26 活性炭素繊維及びその製造方法

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JP2001-294225 2001-09-26
JP2001294225 2001-09-26

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020218370A1 (fr) * 2019-04-26 2020-10-29 株式会社クラレ Matière carbonée, son procédé de production, filtre pour purification d'eau et purificateur d'eau
US20210261441A1 (en) * 2018-06-19 2021-08-26 Ad'all Co., Ltd. Activated carbon
EP3812349A4 (fr) * 2018-06-19 2022-02-09 Ad'All Co., Ltd. Charbon actif

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03265510A (ja) * 1990-03-13 1991-11-26 Osaka Gas Co Ltd 金属含有活性炭の製造方法
JPH10328563A (ja) * 1997-05-30 1998-12-15 Adall:Kk 有害ガス除去用素材およびその製造方法
JPH11240708A (ja) * 1998-02-27 1999-09-07 Adooru:Kk 繊維状活性炭
JPH11240707A (ja) * 1998-02-27 1999-09-07 Adooru:Kk 活性炭

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03265510A (ja) * 1990-03-13 1991-11-26 Osaka Gas Co Ltd 金属含有活性炭の製造方法
JPH10328563A (ja) * 1997-05-30 1998-12-15 Adall:Kk 有害ガス除去用素材およびその製造方法
JPH11240708A (ja) * 1998-02-27 1999-09-07 Adooru:Kk 繊維状活性炭
JPH11240707A (ja) * 1998-02-27 1999-09-07 Adooru:Kk 活性炭

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20210261441A1 (en) * 2018-06-19 2021-08-26 Ad'all Co., Ltd. Activated carbon
EP3812348A4 (fr) * 2018-06-19 2022-02-09 Ad'All Co., Ltd. Charbon actif
EP3812349A4 (fr) * 2018-06-19 2022-02-09 Ad'All Co., Ltd. Charbon actif
US11873235B2 (en) 2018-06-19 2024-01-16 Ad'all Co., Ltd. Activated carbon
US12258284B2 (en) 2018-06-19 2025-03-25 Ad'all Co., Ltd. Activated carbon
WO2020218370A1 (fr) * 2019-04-26 2020-10-29 株式会社クラレ Matière carbonée, son procédé de production, filtre pour purification d'eau et purificateur d'eau
JP6829796B1 (ja) * 2019-04-26 2021-02-10 株式会社クラレ 炭素質材料及びその製造方法、並びに浄水用フィルター及び浄水器
US12258276B2 (en) 2019-04-26 2025-03-25 Kuraray Co., Ltd. Carbonaceous material, method for producing same, filter for water purification and water purifier

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