JPH05294607A - Production of metal-containing activated carbon - Google Patents
Production of metal-containing activated carbonInfo
- Publication number
- JPH05294607A JPH05294607A JP4094118A JP9411892A JPH05294607A JP H05294607 A JPH05294607 A JP H05294607A JP 4094118 A JP4094118 A JP 4094118A JP 9411892 A JP9411892 A JP 9411892A JP H05294607 A JPH05294607 A JP H05294607A
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- Prior art keywords
- softening point
- metal
- activated carbon
- pitch
- raw material
- Prior art date
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Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、金属含有活性炭の製造
方法に関する。TECHNICAL FIELD The present invention relates to a method for producing metal-containing activated carbon.
【０００２】[0002]
【従来の技術及びその課題】従来の活性炭は、主として
炭素を水蒸気存在下に焼成（賦活）して製造される。こ
のような方法によれば、主としてミクロポア（口径：
０．８〜２ｎｍ）及びサブミクロポア（口径：０．８ｎ
ｍ未満）の発達した活性炭が製造され、メソポア（口
径：２〜５０ｎｍ）及びマクロポア（口径：５０ｎｍ以
上）の比率は合計でも１０％に満たないものであった。
そのような活性炭は、比表面積が非常に大きく吸着能力
に優れている半面、活性炭に吸着される物質の大きさは
活性炭のポアの大きさによって制限されるので、従来の
活性炭は、２ｎｍ以下の口径内に入り得る小分子の吸着
には適していたが、より大きな分子を効率的に吸着する
ことはできなかった（図１参照）。2. Description of the Related Art Conventional activated carbon is manufactured mainly by burning (activating) carbon in the presence of steam. According to such a method, the micropore (caliber:
0.8-2 nm) and sub-micropore (caliber: 0.8n)
Activated carbon with developed (less than m) was produced, and the ratio of mesopores (bore diameter: 2 to 50 nm) and macropores (bore diameter: 50 nm or more) was less than 10% in total.
While such activated carbon has a very large specific surface area and excellent adsorption capacity, the size of the substance adsorbed on the activated carbon is limited by the size of the pores of the activated carbon. It was suitable for adsorbing small molecules that could enter the aperture, but could not adsorb larger molecules efficiently (see Figure 1).
【０００３】活性炭のポアの口径を大きくし、中分子以
上の物質を吸着する試みは従来から成されていたが、未
だ満足のいく結果は得られていない。Although attempts have been made so far to increase the pore size of activated carbon to adsorb substances having a medium or higher molecular weight, satisfactory results have not yet been obtained.
【０００４】本発明の目的は、活性炭のポアの大きさを
コントロールし、従来品では吸着することが難しかった
中分子及び大分子を選択的に吸着し得る活性炭の製造方
法を提供することにある。An object of the present invention is to provide a method for producing activated carbon capable of controlling the size of the pores of activated carbon and selectively adsorbing medium and large molecules which were difficult to be adsorbed by conventional products. ..
【０００５】[0005]
【課題を解決するための手段】本発明者は、上記目的を
達成するため鋭意検討を重ねた結果、低軟化点ピッチと
金属化合物を混合してなる低軟化点焼成原料を炭素化処
理及び賦活処理すること或いは低軟化点ピッチとイッテ
ルビウム化合物及び／又はイットリウム化合物を混合し
てなる焼成原料を紡糸ピッチと混合し、得られた高軟化
点焼成原料を不融化処理、炭素化処理及び水蒸気賦活処
理することによりメソポア（口径：２〜５０ｎｍ）ある
いはマクロポア（口径：５０ｎｍ以上）を有する活性炭
が得られることを見出した。Means for Solving the Problems As a result of intensive studies to achieve the above object, the present inventor has conducted a carbonization treatment and activation of a low softening point firing raw material obtained by mixing a low softening point pitch and a metal compound. Treating or mixing a low-softening point pitch with a ytterbium compound and / or a yttrium compound, and mixing the firing raw material with the spinning pitch, and the obtained high-softening-point firing raw material is infusibilized, carbonized and steam activated. It was found that by doing so, activated carbon having mesopores (caliber: 2 to 50 nm) or macropores (caliber: 50 nm or more) can be obtained.
【０００６】即ち、本発明は、低軟化点ピッチと金属化
合物を混合してなる低軟化点焼成原料を炭素化処理及び
賦活処理することを特徴とする金属含有活性炭の製造方
法（以下、第１方法という）を提供するものである。That is, the present invention is a method for producing a metal-containing activated carbon characterized in that a low-softening point firing raw material obtained by mixing a low-softening point pitch and a metal compound is carbonized and activated (hereinafter referred to as the first Method)).
【０００７】本発明はまた、低軟化点ピッチとイッテル
ビウム化合物、サマリウム化合物、ネオジウム化合物及
びイットリウム化合物からなる群の少なくとも１種を混
合してなる焼成原料を紡糸ピッチと混合し、得られた高
軟化点焼成原料を不融化処理又は炭素化処理、及び水蒸
気賦活処理することを特徴とする金属含有活性炭の製造
方法（以下、第２方法という）を提供するものである。According to the present invention, the firing softening material obtained by mixing the low softening point pitch with at least one selected from the group consisting of ytterbium compounds, samarium compounds, neodymium compounds and yttrium compounds is mixed with the spinning pitch to obtain a high softening property. The present invention provides a method for producing metal-containing activated carbon (hereinafter, referred to as a second method), which comprises infusibilizing treatment or carbonizing treatment and steam activation treatment of a point-fired raw material.
【０００８】本発明の第１方法で得られる金属含有活性
炭は、賦活収率が２０％以上で、メソポアの比率が１０
〜９９％、好ましくは賦活収率が４０〜７０％でメソポ
アの比率が３０〜９０％のものである。The metal-containing activated carbon obtained by the first method of the present invention has an activation yield of 20% or more and a mesopore ratio of 10.
˜99%, preferably an activation yield of 40 to 70% and a mesopore ratio of 30 to 90%.
【０００９】本発明の第２方法で得られる金属含有活性
炭は、賦活収率が２５％以上で、メソポアの比率が１５
〜９９％、好ましくは賦活収率が２５〜６０％でメソポ
アの比率が２０〜９０％のものである。The metal-containing activated carbon obtained by the second method of the present invention has an activation yield of 25% or more and a mesopore ratio of 15%.
˜99%, preferably an activation yield of 25 to 60% and a mesopore ratio of 20 to 90%.
【００１０】本発明において低軟化点ピッチとは、軟化
点が６０〜１５０℃程度、好ましくは７０〜１２０℃程
度のピッチであり、その炭素源としては石炭ピッチ、石
油ピッチ及びこれらピッチの有機溶媒可溶分を使用する
ことができる。In the present invention, the low softening point pitch is a pitch having a softening point of about 60 to 150 ° C., preferably about 70 to 120 ° C., and its carbon source is coal pitch, petroleum pitch and an organic solvent for these pitches. Soluble matter can be used.
【００１１】本発明において紡糸ピッチとは、軟化点が
２３０℃以上、好ましくは２７０〜２９０℃程度のピッ
チであり、光学的に等方性及び異方性の両方のピッチを
含み、好ましくは石油系及び石炭系のいずれかのピッチ
をニトロ化合物の存在下に重合化処理したものを用い
る。In the present invention, the spinning pitch is a pitch having a softening point of 230 ° C. or higher, preferably about 270 to 290 ° C., and includes both optically isotropic and anisotropic pitches, preferably petroleum. A pitch obtained by polymerizing any one of pitches of a coal type and a coal type in the presence of a nitro compound is used.
【００１２】低軟化点ピッチに混合される金属化合物中
の金属成分としては、例えばマグネシウム、カルシウム
などのアルカリ土類金属、アルミニウムなどのＩＩＩＡ
族の元素、その他亜鉛、リン、ゲルマニウム、スズ、セ
レンなどの典型金属、スカンジウム、イットリウム及び
ランタン系列元素（イッテルビウム、ランタン、セリウ
ム等）などの希土類金属、アクチニウム、トリウムなど
のアクチニウム系列元素等が挙げられ、該金属化合物は
これら金属の有機金属塩及び無機金属塩のいずれも使用
できる。好ましい金属としてはスカンジウム、イットリ
ウム及びランタン系列元素（イッテルビウム、ランタ
ン、セリウム等）などの希土類元素が挙げられる。ピッ
チに含有される金属成分としての割合は、ピッチに対し
０．１〜１０重量％程度、好ましくは１〜５重量％程度
である。Examples of the metal component in the metal compound mixed in the low softening point pitch include alkaline earth metals such as magnesium and calcium, and IIIA such as aluminum.
Group elements, other typical metals such as zinc, phosphorus, germanium, tin, and selenium, scandium, yttrium, and rare earth metals such as lanthanum series elements (ytterbium, lanthanum, cerium, etc.), actinium series elements such as actinium, thorium, etc. As the metal compound, both organic metal salts and inorganic metal salts of these metals can be used. Preferred metals include scandium, yttrium, and rare earth elements such as lanthanum series elements (ytterbium, lanthanum, cerium, etc.). The proportion of the metal component contained in the pitch is about 0.1 to 10% by weight, preferably about 1 to 5% by weight, based on the pitch.
【００１３】紡糸ピッチに含有される金属としては、イ
ッテルビウムの有機金属塩及び無機金属塩であるイッテ
ルビウム化合物、イットリウムの有機金属塩及び無機金
属塩であるイットリウム化合物、サマリウムの有機金属
塩及び無機金属塩であるサマリウム化合物、ネオジウム
の有機金属塩及び無機金属塩であるネオジウム化合物、
及びこれらの混合物が挙げられる。高軟化点焼成原料に
含有される金属成分の割合は、高軟化点焼成原料に対し
０．１〜１０重量％程度、好ましくは０．５〜５重量％
程度である。紡糸ピッチと焼成原料の混合比率は、紡糸
ピッチ１００重量部に対し焼成原料を０．１〜１０重量
％程度、好ましくは０．５〜５重量％程度である。高軟
化点焼成原料の軟化点は２３０℃以上、好ましくは２７
０〜２９０℃程度である。The metals contained in the spinning pitch include ytterbium compounds which are ytterbium organometallic salts and inorganic metal salts, yttrium organometallic salts and yttrium compounds which are inorganic metal salts, samarium organometallic salts and inorganic metal salts. A samarium compound, which is a neodymium compound which is an organic metal salt and an inorganic metal salt of neodymium,
And mixtures thereof. The proportion of the metal component contained in the high softening point firing raw material is about 0.1 to 10% by weight, preferably 0.5 to 5% by weight, based on the high softening point firing raw material.
It is a degree. The mixing ratio of the spinning pitch and the firing raw material is about 0.1 to 10% by weight, preferably about 0.5 to 5% by weight, based on 100 parts by weight of the spinning pitch. The softening point of the high softening point firing material is 230 ° C. or higher, preferably 27.
It is about 0 to 290 ° C.
【００１４】本発明の第１方法においては、上記の低軟
化点ピッチと金属化合物を均一に混合する。均一に混合
するためには、例えば低軟化点ピッチと金属化合物をテ
トラヒドロフラン、ジクロロメタン、ベンゼン、キノリ
ンなどの有機溶媒中に溶解し、溶媒を留去すれば良い。
得られた均一混合物は、好ましくは２００〜３６０℃程
度の条件下、１〜２時間程度、不活性ガス雰囲気下で溶
融し、冷却する。この操作を２〜３回繰り返すことによ
り、本第１方法に適した焼成原料が得られる。In the first method of the present invention, the low softening point pitch and the metal compound are uniformly mixed. In order to mix uniformly, for example, the low softening point pitch and the metal compound may be dissolved in an organic solvent such as tetrahydrofuran, dichloromethane, benzene or quinoline, and the solvent may be distilled off.
The obtained homogeneous mixture is preferably melted and cooled in an inert gas atmosphere for about 1 to 2 hours under the condition of about 200 to 360 ° C. By repeating this operation 2 to 3 times, a firing raw material suitable for the first method can be obtained.
【００１５】得られた低軟化点焼成原料は、次いで炭素
化処理及び賦活処理を行う。炭素化処理は、アルゴン、
窒素などの不活性ガス雰囲気下に、１分あたり５〜１０
℃程度の割合で８００℃程度の温度から１２００℃程度
まで温度を上昇させ、最高温度を最大限１０分間程度保
持して行う。また、賦活処理は、水蒸気、二酸化炭素、
酸素及びこれらの混合物ならびにこれらのガスを窒素な
どの不活性ガスで希釈したガスなどの雰囲気中８００〜
１２００℃程度で５〜１２０分間程度保持することによ
り行う。The low-softening-point firing raw material thus obtained is then subjected to carbonization treatment and activation treatment. Carbonization treatment is argon,
5 to 10 per minute under an atmosphere of an inert gas such as nitrogen
The temperature is raised from about 800 ° C to about 1200 ° C at a rate of about 0 ° C, and the maximum temperature is held for a maximum of about 10 minutes. In addition, activation treatment, steam, carbon dioxide,
800 to 800 in an atmosphere such as oxygen and a mixture thereof and a gas obtained by diluting these gases with an inert gas such as nitrogen.
It is performed by holding at about 1200 ° C. for about 5 to 120 minutes.
【００１６】本発明の第２方法において、イッテルビウ
ム化合物及び／又はイットリウム化合物を混合してなる
低軟化点焼成原料と紡糸ピッチとの混合は、例えば３０
０℃程度の温度で２０〜３０分間加熱処理することによ
り行う。In the second method of the present invention, the low softening point firing raw material obtained by mixing the ytterbium compound and / or the yttrium compound and the spinning pitch are mixed, for example, at 30%.
The heat treatment is performed at a temperature of about 0 ° C. for 20 to 30 minutes.
【００１７】得られた高軟化点焼成原料は、次いで不融
化処理、炭素化処理及び水蒸気賦活処理される。不融化
処理は、常法に従い不活性ガス雰囲気下または酸素含有
雰囲気下に、１分あたり０．１〜５℃程度の割合で３３
０℃程度の温度から４００℃程度まで昇温して行う。ま
た炭素化処理は、アルゴン、窒素などの不活性ガス雰囲
気下に、１分あたり５〜１０℃程度の割合で８００℃程
度の温度から１２００℃程度まで温度を上昇させて行
う。さらに、上記水蒸気賦活処理は、不活性ガス雰囲気
下に８００〜１２００℃程度の温度で５〜１２０分間程
度処理することにより行う。The resulting high softening point firing material is then subjected to infusibilization treatment, carbonization treatment and steam activation treatment. The infusibilizing treatment is carried out according to a conventional method in an inert gas atmosphere or an oxygen-containing atmosphere at a rate of about 0.1 to 5 ° C. per minute for 33 times.
The temperature is raised from about 0 ° C to about 400 ° C. The carbonization treatment is performed in an atmosphere of an inert gas such as argon or nitrogen at a rate of about 5 to 10 ° C. per minute while raising the temperature from about 800 ° C. to about 1200 ° C. Further, the steam activation treatment is performed by performing the treatment at a temperature of about 800 to 1200 ° C. for about 5 to 120 minutes in an inert gas atmosphere.
【００１８】[0018]
【発明の効果】本発明の第１方法によれば、低軟化点ピ
ッチを使用し、従来の方法に比較してメソポア率が１０
％以上という高い活性炭を得ることができる。特に、ピ
ッチに混合する金属の種類を選択することにより、メソ
ポアをほぼ選択的に有する活性炭を得ることができる。According to the first method of the present invention, a low softening point pitch is used, and the mesopore ratio is 10 as compared with the conventional method.
%, High activated carbon can be obtained. In particular, by selecting the kind of metal to be mixed with the pitch, it is possible to obtain activated carbon having mesopores almost selectively.
【００１９】本発明の第２方法によれば、イッテルビウ
ム化合物及び／又はイットリウム化合物を含有している
ため、特に高いメソポア比率を有する活性炭を得ること
ができる。According to the second method of the present invention, since it contains the ytterbium compound and / or the yttrium compound, activated carbon having a particularly high mesopore ratio can be obtained.
【００２０】[0020]
【実施例】以下、本発明を実施例を用いてより詳しく説
明するが、本発明はこれら実施例に限定されるものでは
ない。EXAMPLES The present invention will now be described in more detail with reference to examples, but the present invention is not limited to these examples.
【００２１】なお、以下の実施例において、比表面積は
ＢＥＴ一点法、メソポア比表面積は窒素の吸着等温線か
らＢＪＨ法により求めた。In the following examples, the specific surface area was determined by the BET one-point method, and the mesopore specific surface area was determined by the BJH method from the adsorption isotherm of nitrogen.
【００２２】[0022]
【実施例１】 ＊第１方法による金属含有活性炭の調製 常法に従って精製及び熱処理を行った軟化点８５℃のピ
ッチに、金属成分としてｔ−ブチルマグネシウムクロリ
ドをマグネシウム含量が２重量％になるように加えた。
テトラヒドロフランを加えて均一に溶解し、溶媒を留去
して低軟化点焼成原料を得た。Example 1 * Preparation of metal-containing activated carbon by the first method Pitch refined and heat-treated according to a conventional method and having a softening point of 85 ° C., t-butylmagnesium chloride as a metal component so that the magnesium content was 2% by weight. Added to.
Tetrahydrofuran was added and dissolved uniformly, and the solvent was distilled off to obtain a low-softening-point firing material.
【００２３】得られた低軟化点焼成原料を窒素雰囲気
下、２００℃から１分間に１０℃の割合で９００℃まで
昇温させて炭素化処理を行った。次いで、水蒸気飽和窒
素を３リットル／分の割合で流しながら９００℃で３０
分間賦活処理を行い、金属含有活性炭を得た。The low-softening-point firing raw material thus obtained was carbonized in a nitrogen atmosphere by raising the temperature from 200 ° C. to 900 ° C. at a rate of 10 ° C. for 1 minute. Then, steam saturated nitrogen is flown at a rate of 3 liter / min for 30 minutes at 900 ° C.
The activation treatment was performed for minutes to obtain metal-containing activated carbon.
【００２４】[0024]
【実施例２〜５】金属成分及びその含有量並びに賦活条
件を以下の表１に示すように変更した他は実施例１と同
様にして金属含有活性炭を得た。Examples 2 to 5 Metal-containing activated carbon was obtained in the same manner as in Example 1 except that the metal components, their contents, and activation conditions were changed as shown in Table 1 below.
【００２５】[0025]
【比較例１】金属成分を加えなかった他は実施例１と同
様にして、活性炭を得た。Comparative Example 1 Activated carbon was obtained in the same manner as in Example 1 except that no metal component was added.
【００２６】[0026]
【比較例２】金属成分としてのｔ−ブチルマグネシウム
クロリドの代わりに９−ＢＢＮをホウ素含量が２重量％
になるように加えた他は実施例１と同様にして、金属含
有活性炭を得た。[Comparative Example 2] 9-BBN was used in place of t-butylmagnesium chloride as a metal component, and the boron content was 2% by weight.
A metal-containing activated carbon was obtained in the same manner as in Example 1 except that the above was added.
【００２７】実施例１〜５、比較例１及び２で得られた
金属含有活性炭の各種物性値を合わせて以下の表１−１
及び表１−２に示す。Various physical property values of the metal-containing activated carbons obtained in Examples 1 to 5 and Comparative Examples 1 and 2 are shown in Table 1-1 below.
And Table 1-2.
【００２８】 表１−１ 実施例又は比較例 添加した金属成分 金属含有率（％） 実施例１ ｔ−ＢｕＭｇＣｌ Ｍｇ＝５ 実施例２ ｔ−ＢｕＭｇＣｌ Ｍｇ＝２ 実施例３ （Ｃ3 Ｈ7 Ｏ）3 Ａｌ Ａｌ＝２ 実施例４ （Ｃ5 Ｈ4 ＳｉＭｅ2 ）2 Ｙｂ Ｙｂ＝２ 実施例５ ＹｂＩ2 （ＴＨＦ） Ｙｂ＝２ 比較例１ 添加せず 比較例２ ９−ＢＢＮ Ｂ＝２ 表１−２ 実施例 賦活収率 ＢＥＴ メソポア メソポア率 細孔半径 又は （％） 比表面積 比表面積 （％） （ｎｍ）比較例 (m 2 /g) (m 2 /g) 実施例１ ３６．９５ ２５３ ９５．０ ３７．５ ４．６２ 実施例２ ６１．７０ ２３３ ４３．４ １８．６ ２．３９ 実施例３ ６４．６４ ２２０ １１１．８ ５０．８ １．９２ 実施例４ ２２．４３ ３２．７ ３２．２ ９８．５ ５．７８ 実施例５ ４４．３８ ６５．６ ４８．２ ７３．６ ７．３６ 比較例１ ７８．６７ ８０．９ １４．０ １７．３ １．５１比較例２ ５２．０２ ６０．３ １２．７ ２１．１ １．７３ Table 1-1 Examples or Comparative Examples Metal Component Added Metal Content (%) Example 1 t-BuMgCl Mg = 5 Example 2 t-BuMgCl Mg = 2 Example 3 (C 3 H 7 O) 3 Al Al = 2 Example 4 (C 5 H 4 SiMe 2 ) 2 Yb Yb = 2 Example 5 YbI 2 (THF) Yb = 2 Comparative Example 1 No addition Comparative Example 2 9-BBN B = 2 Table 1- 2 Examples Activation yield BET Mesopore Mesopore ratio Pore radius or (%) Specific surface area Specific surface area (%) (nm) Comparative example (m 2 / g) (m 2 / g) Example 1 36.95 253 95. 0 37.5 4.62 Example 2 61.70 233 43.4 18.6 2.39 Example 3 64.64 220 111.8 50.8 1.92 Example 4 22.43 32.7 32. 2 98.5 5.78 Example 5 44.38 65.6 48. 73.6 7.36 Comparative Example 1 78.67 80.9 14.0 17.3 1.51 Comparative Example 2 52.02 60.3 12.7 21.1 1.73
【００２９】[0029]
【実施例６】 ＊第２方法による金属含有活性炭の調製 常法に従って精製及び熱処理を行った軟化点８５℃のピ
ッチに、金属成分としてＣｐ3 ＹｂをＹｂ含量が５重量
％になるように加えた。テトラヒドロフランを加え均一
に溶解し、溶媒を留去して低軟化点焼成原料を得た。な
お、Ｃｐはシクロペンタジエンを表す。Example 6 * Preparation of metal-containing activated carbon by the second method Cp 3 Yb as a metal component was added to a pitch having a softening point of 85 ° C. which had been refined and heat-treated in a conventional manner so that the Yb content was 5% by weight. It was Tetrahydrofuran was added and dissolved uniformly, and the solvent was distilled off to obtain a low-softening-point calcination raw material. Cp represents cyclopentadiene.
【００３０】得られた低軟化点焼成原料に軟化点２７０
℃の紡糸ピッチを１：１の割合になるように加えて粉砕
・混合し、窒素ガス雰囲気下、３００℃で１０分間加熱
し、次いで冷却した。この操作を３回繰り返し、均一な
高軟化点焼成原料を得た。この混合物をアルゴンガス雰
囲気下に１００℃から１分間に３℃の割合で３６０℃ま
で昇温する不融化処理を行い、そのままアルゴンガス雰
囲気下に９００℃で１時間炭素化処理した。次いで水蒸
気飽和窒素を３リットル／分の割合で流しながら９００
℃で３０分間賦活処理を行い、金属含有活性炭を得た。The softening point 270 was added to the obtained low-softening point firing raw material.
The spinning pitch at 0 ° C was added at a ratio of 1: 1 and the mixture was pulverized and mixed, heated under a nitrogen gas atmosphere at 300 ° C for 10 minutes, and then cooled. This operation was repeated 3 times to obtain a uniform high softening point firing material. This mixture was subjected to an infusibilizing treatment in which the temperature was raised from 100 ° C. to 360 ° C. at a rate of 3 ° C. for 1 minute in an argon gas atmosphere, and then carbonized at 900 ° C. for 1 hour in an argon gas atmosphere. Then, while flowing steam saturated nitrogen at a rate of 3 l / min, 900
Activation treatment was performed at 30 ° C. for 30 minutes to obtain metal-containing activated carbon.
【００３１】[0031]
【実施例７】金属成分として、Ｃｐ3 ＹをＹ含量が５重
量％になるように加えた他は実施例６と同様にして金属
含有活性炭を得た。Example 7 A metal-containing activated carbon was obtained in the same manner as in Example 6 except that Cp 3 Y was added as a metal component so that the Y content was 5% by weight.
【００３２】[0032]
【比較例３】金属成分を加えなかった他は実施例６と同
様にして金属含有活性炭を得た。Comparative Example 3 A metal-containing activated carbon was obtained in the same manner as in Example 6 except that no metal component was added.
【００３３】実施例６、実施例７及び比較例３で得られ
た活性炭の各種物性値を合わせて以下の表２に示す。Table 2 below shows various physical property values of the activated carbons obtained in Examples 6 and 7 and Comparative Example 3.
【００３４】 表 ２ 実施例 賦活収率 ＢＥＴ メソポア メソポア率 細孔半径 又は （％） 比表面積 比表面積 （％） （ｎｍ）比較例 (m 2 /g) (m 2 /g) 実施例６ ３０．６６ ２１５ ２０９．３ ９７．３ ２．８１ 実施例７ ６１．７０ ２３３ ２０１．０ ９０．１ ２．５７比較例３ ５０．００ ４０．０ ５．０ １２．５ − 表２の結果から、イッテルビウム及び／又はイットリウ
ム含有活性炭は、金属を含まない比較例３の活性炭に比
べ非常に大きな比表面積を有し、メソポア率も十分大き
く中分子以上の大きさの分子を吸着するのに好ましいこ
とが明らかとなった。Table 2 Examples Activation yield BET Mesopore Mesopore ratio Pore radius or (%) Specific surface area Specific surface area (%) (nm) Comparative example (m 2 / g) (m 2 / g) Example 6 30. 66 215 209.3 97.3 2.81 Example 7 61.70 233 201.0 90.1 2.57 Comparative Example 3 50.00 40.0 5.0 12.5-From the results of Table 2, ytterbium. And / or yttrium-containing activated carbon has a very large specific surface area as compared with the activated carbon of Comparative Example 3 containing no metal, and has a sufficiently large mesopore ratio, which is preferable for adsorbing molecules having a size of medium or larger. Became.
【００３５】なお、実施例では示さないが、本発明者
は、イッテルビウム、イットリウムの代わりにサマリウ
ム化合物、ネオジウム化合物を用いた場合にも同様に高
いＢＥＴ比表面積、メソポア比表面積、メソポア率を有
し且つ賦活収率も十分実用化可能な範囲である金属含有
活性炭が得られることを確認した。Although not shown in the examples, the present inventor also has a high BET specific surface area, mesopore specific surface area, and mesopore ratio when a samarium compound or a neodymium compound is used instead of ytterbium or yttrium. In addition, it was confirmed that a metal-containing activated carbon having an activation yield in a sufficiently practical range can be obtained.
【図１】活性炭のポアのサイズ（マクロポア、メソポ
ア、マイクロポア、サブ−マイクロポア）を模式的に示
す図である。FIG. 1 is a diagram schematically showing the pore size of activated carbon (macropore, mesopore, micropore, sub-micropore).
【図２】水蒸気による賦活処理の方法を示す概略図であ
る。FIG. 2 is a schematic diagram showing a method of activation treatment with steam.
Claims (2)
る低軟化点焼成原料を炭素化処理及び賦活処理すること
を特徴とする金属含有活性炭の製造方法。1. A process for producing a metal-containing activated carbon, which comprises carbonizing and activating a low-softening point firing raw material obtained by mixing a low-softening point pitch and a metal compound.
サマリウム化合物、ネオジウム化合物及びイットリウム
化合物からなる群の少なくとも１種を混合してなる焼成
原料を紡糸ピッチと混合し、得られた高軟化点焼成原料
を不融化処理又は炭素化処理、及び水蒸気賦活処理する
ことを特徴とする金属含有活性炭の製造方法。2. A low softening point pitch and a ytterbium compound,
A firing raw material obtained by mixing at least one selected from the group consisting of samarium compounds, neodymium compounds and yttrium compounds is mixed with a spinning pitch, and the obtained high softening point firing raw material is infusibilized or carbonized, and steam activated. A method for producing a metal-containing activated carbon, comprising:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP09411892A JP3195963B2 (en) | 1992-04-14 | 1992-04-14 | Method for producing metal-containing activated carbon |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP09411892A JP3195963B2 (en) | 1992-04-14 | 1992-04-14 | Method for producing metal-containing activated carbon |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05294607A true JPH05294607A (en) | 1993-11-09 |
| JP3195963B2 JP3195963B2 (en) | 2001-08-06 |
Family
ID=14101517
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP09411892A Expired - Lifetime JP3195963B2 (en) | 1992-04-14 | 1992-04-14 | Method for producing metal-containing activated carbon |
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| JP (1) | JP3195963B2 (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10335189A (en) * | 1997-06-05 | 1998-12-18 | Furukawa Co Ltd | Electric double-layer capacitor |
| WO2003033135A1 (en) * | 2001-09-21 | 2003-04-24 | Ad'all Co., Ltd. | Activated carbon fiber for the removal of organochlorine compounds |
| KR100417688B1 (en) * | 2001-07-20 | 2004-02-11 | 재단법인 포항산업과학연구원 | Mesoporous activated carbon fiber and preparation method of the same |
| KR100426125B1 (en) * | 2001-11-12 | 2004-04-08 | 재단법인 포항산업과학연구원 | Mesoporous activated carbon fiber and preparation method of the same |
| CN1302987C (en) * | 2004-12-28 | 2007-03-07 | 华南理工大学 | Surface-activated carbon fiber and its preparation method |
| JP2007091557A (en) * | 2005-09-30 | 2007-04-12 | Jfe Steel Kk | Carbon material and its production method |
-
1992
- 1992-04-14 JP JP09411892A patent/JP3195963B2/en not_active Expired - Lifetime
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10335189A (en) * | 1997-06-05 | 1998-12-18 | Furukawa Co Ltd | Electric double-layer capacitor |
| KR100417688B1 (en) * | 2001-07-20 | 2004-02-11 | 재단법인 포항산업과학연구원 | Mesoporous activated carbon fiber and preparation method of the same |
| WO2003033135A1 (en) * | 2001-09-21 | 2003-04-24 | Ad'all Co., Ltd. | Activated carbon fiber for the removal of organochlorine compounds |
| KR100426125B1 (en) * | 2001-11-12 | 2004-04-08 | 재단법인 포항산업과학연구원 | Mesoporous activated carbon fiber and preparation method of the same |
| CN1302987C (en) * | 2004-12-28 | 2007-03-07 | 华南理工大学 | Surface-activated carbon fiber and its preparation method |
| JP2007091557A (en) * | 2005-09-30 | 2007-04-12 | Jfe Steel Kk | Carbon material and its production method |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3195963B2 (en) | 2001-08-06 |
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