JP2002003211A - Method for producing carbon material and activated carbon - Google Patents
Method for producing carbon material and activated carbonInfo
- Publication number
- JP2002003211A JP2002003211A JP2000184739A JP2000184739A JP2002003211A JP 2002003211 A JP2002003211 A JP 2002003211A JP 2000184739 A JP2000184739 A JP 2000184739A JP 2000184739 A JP2000184739 A JP 2000184739A JP 2002003211 A JP2002003211 A JP 2002003211A
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- Japan
- Prior art keywords
- organic
- carbon material
- hydrogel
- organic hydrogel
- aged
- 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.)
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Carbon And Carbon Compounds (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、炭素材料及び活性
炭の製造方法に関する。本発明で得られる炭素材料及び
活性炭は、電気二重層コンデンサ用電極、ガスセンサー
用電極、上水処理、下水処理、廃液処理等に用いられる
吸着材料又は触媒担体として使用できる。[0001] The present invention relates to a method for producing a carbon material and activated carbon. The carbon material and activated carbon obtained in the present invention can be used as an electrode for an electric double layer capacitor, an electrode for a gas sensor, an adsorbing material or a catalyst carrier used for water treatment, sewage treatment, waste liquid treatment and the like.
【０００２】[0002]
【従来の技術】従来より、炭素材料を賦活することによ
り活性炭を製造する方法が知られている。このための炭
素材料を得る方法としては、R.W.Pekalaらの方法（J.No
n-Cryst.Solids,145,90,1992）が知られており、前駆体
となる有機エアロゲルを炭素化することにより炭素材料
を得ている。この有機エアロゲルは、例えば、フェノー
ル性ＯＨ基を複数有する芳香族化合物（以下、多価フェ
ノール類という）の一種であるレゾルシノール（１，３
−ジヒドロキシベンゼン）、ホルムアルデヒド及び水を
混合させ、炭酸ナトリウム等の塩基を加えて、７５〜９
０℃程度の温度で加熱重合しゲル化させて有機ヒドロゲ
ルを合成した後、乾燥することにより生成される。この
有機エアロゲルを希ガス又は窒素ガス雰囲気下で３００
〜２０００℃程度の温度で熱処理して、炭素化すること
により炭素材料が得られる。さらにこの炭素材料を水蒸
気で賦活したり、アルカリ金属水酸化物等により賦活す
ることにより活性炭が得られる。2. Description of the Related Art A method for producing activated carbon by activating a carbon material has been known. As a method for obtaining a carbon material for this purpose, the method of RWPekala et al. (J. No.
n-Cryst. Solids, 145, 90, 1992) is known, and a carbon material is obtained by carbonizing an organic airgel serving as a precursor. This organic aerogel is, for example, a resorcinol (1,3) which is a kind of aromatic compound having a plurality of phenolic OH groups (hereinafter, referred to as polyhydric phenols).
-Dihydroxybenzene), formaldehyde and water, and a base such as sodium carbonate is added thereto.
It is produced by heating and polymerizing at a temperature of about 0 ° C. to form a gel by synthesizing an organic hydrogel, followed by drying. This organic aerogel is treated under a rare gas or nitrogen gas atmosphere for 300 minutes.
A carbon material is obtained by heat-treating at a temperature of about 2000 ° C. to carbonize. Activated carbon can be obtained by activating this carbon material with steam or activating it with an alkali metal hydroxide or the like.
【０００３】従来、有機ヒドロゲルは、室温で重合反応
を始め、７５〜９０℃程度の温度で、３〜１０日程度保
つことで熟成され、ゲル強度が高くされていた。この熟
成された有機ヒドロゲルを得る工程（以下、有機ヒドロ
ゲルの熟成工程）が不完全であると、ゲル強度が不足
し、有機エアロゲルを生成させるとき、形状を保持でき
ない。また、この従来の方法では、熟成工程に長い時間
がかかるため製造上問題であった。Heretofore, organic hydrogels have been polymerized at room temperature, and aged at a temperature of about 75 to 90 ° C. for about 3 to 10 days to increase the gel strength. If the step of obtaining the aged organic hydrogel (hereinafter, the step of aging the organic hydrogel) is incomplete, the gel strength is insufficient, and the shape cannot be maintained when the organic aerogel is generated. Further, in this conventional method, a long time is required for the aging step, which is a problem in production.
【０００４】[0004]
【発明が解決しようとする課題】本発明は、活性炭及び
炭素材料の原料となる上述の熟成された有機ヒドロゲル
を短時間で生成するためのものである。SUMMARY OF THE INVENTION The present invention is to produce the above-mentioned aged organic hydrogel, which is used as a raw material of activated carbon and carbon material, in a short time.
【０００５】[0005]
【課題を解決するための手段】本発明は、多価フェノー
ル類及びホルムアルデヒドを水中で反応させて有機ヒド
ロゲルを得る工程、前記有機ヒドロゲルに水を添加して
加圧密閉下で加熱処理することにより熟成された有機ヒ
ドロゲルを得る工程、前記熟成された有機ヒドロゲルを
乾燥し有機エアロゲルを生成させる工程、及び前記有機
エアロゲルを炭素化処理する工程、を経る炭素材料の製
造方法を提供する。According to the present invention, a polyhydric phenol and formaldehyde are reacted in water to obtain an organic hydrogel, and water is added to the organic hydrogel, followed by heat treatment under pressure and airtightness. Provided is a method for producing a carbon material, which comprises a step of obtaining an aged organic hydrogel, a step of drying the aged organic hydrogel to form an organic aerogel, and a step of carbonizing the organic aerogel.
【０００６】[0006]
【発明の実施の形態】本発明における有機ヒドロゲル
は、多価フェノール類及びホルムアルデヒドを水中で反
応させることにより得られる。多価フェノール類として
は、レゾルシノールが好ましい。BEST MODE FOR CARRYING OUT THE INVENTION The organic hydrogel of the present invention is obtained by reacting a polyhydric phenol and formaldehyde in water. As the polyhydric phenol, resorcinol is preferable.
【０００７】多価フェノール類とホルムアルデヒドは、
好ましくは、炭酸ナトリウム等の存在下に水中で反応さ
せる。この結果、多価フェノール類とホルムアルデヒド
との共重合体中に水が分散した構造の有機ヒドロゲルが
得られる。[0007] Polyhydric phenols and formaldehyde are
Preferably, the reaction is performed in water in the presence of sodium carbonate or the like. As a result, an organic hydrogel having a structure in which water is dispersed in a copolymer of a polyhydric phenol and formaldehyde is obtained.
【０００８】有機ヒドロゲルの熟成工程において添加す
る水の量は、加圧密閉下において加熱処理される際、容
器内が飽和蒸気圧になるのに充分な水の量であることが
好ましい。特に、加熱処理時に、有機ヒドロゲルが水溶
液中に完全に浸るだけの水の量を添加する場合は、有機
ヒドロゲルが均一に熟成するので好ましい。[0008] The amount of water added in the aging step of the organic hydrogel is preferably an amount of water sufficient to bring the inside of the container to a saturated vapor pressure when subjected to heat treatment under pressure sealing. In particular, it is preferable to add an amount of water sufficient to completely immerse the organic hydrogel in the aqueous solution during the heat treatment, because the organic hydrogel is uniformly aged.
【０００９】有機ヒドロゲルの熟成工程における加圧密
閉容器の加熱温度としては、１００〜１９０℃、特に、
１４０〜１９０℃であることが好ましい。加熱温度が１
００℃未満である場合は、本発明の効果が充分に発現せ
ず、熟成時間がかかるため好ましくない。また、加熱温
度が１９０℃以下の場合は、圧力容器の使用圧力を１Ｍ
Ｐａ以下にでき、圧力容器にかかる法規上有利な点が多
いため好ましい。加圧密閉容器製造上問題なければ、よ
り高温で加熱してもよい。The heating temperature of the pressurized closed container in the aging step of the organic hydrogel is 100 to 190 ° C.,
The temperature is preferably from 140 to 190 ° C. Heating temperature is 1
When the temperature is lower than 00 ° C., the effect of the present invention is not sufficiently exhibited, and it takes an aging time, which is not preferable. When the heating temperature is 190 ° C. or lower, the operating pressure of the pressure vessel is 1 M
Pa or less, which is preferable because there are many legally advantageous points concerning the pressure vessel. If there is no problem in the production of the pressurized closed container, heating may be performed at higher temperature.
【００１０】有機ヒドロゲルの熟成工程における加熱時
間としては、有機ヒドロゲルの大きさにもよるため一概
には決められないが、一般には、１〜２４時間、特に、
３〜１２時間であることが好ましい。加熱時間が短すぎ
ると、有機ヒドロゲルの内部まで充分に温度が上がら
ず、熟成が進まないためゲル強度が不充分となる可能性
がある。また、加熱時間が長すぎると、製品としての品
質上は問題ないが、本発明の効果が実質的に増大しない
にもかかわらず、不必要に時間を要することになるため
工業的に好ましくない。[0010] The heating time in the aging step of the organic hydrogel cannot be unconditionally determined because it depends on the size of the organic hydrogel.
Preferably, it is 3 to 12 hours. If the heating time is too short, the temperature does not sufficiently rise to the inside of the organic hydrogel, and aging does not proceed, so that the gel strength may be insufficient. On the other hand, if the heating time is too long, there is no problem in terms of the quality of the product, but unnecessarily time is required although the effect of the present invention is not substantially increased, which is not industrially preferable.
【００１１】有機エアロゲルは、熟成された有機ヒドロ
ゲルを乾燥することにより微細な構造を有する多孔性の
有機高分子体として得られる。例えば、超臨界二酸化炭
素中若しくは超臨界水中で乾燥する方法、又は、低表面
張力物質に水を置換後乾燥する方法が好ましい。The organic aerogel is obtained as a porous organic polymer having a fine structure by drying the aged organic hydrogel. For example, a method of drying in supercritical carbon dioxide or supercritical water, or a method of drying after replacing water with a low surface tension substance is preferable.
【００１２】本発明において、炭素化処理は、有機エア
ロゲルから炭素材料へ変換する工程であり、この炭素化
処理により有機エアロゲルは細孔構造を有する多孔性の
炭素材料になる。炭素化は、例えば、窒素、アルゴン、
ヘリウム、キセノン、ネオン、二酸化炭素、燃焼排ガス
等の不活性ガス及びこれらの混合ガスのような非酸化性
雰囲気下に３００〜２０００℃、特に、５００〜１００
０℃程度の温度範囲で加熱することが好ましい。この場
合の加熱時間は、１０分〜８０時間、特に、１０分〜３
０時間であることが好ましい。In the present invention, the carbonization treatment is a step of converting an organic airgel into a carbon material. By this carbonization treatment, the organic airgel becomes a porous carbon material having a pore structure. For carbonization, for example, nitrogen, argon,
In a non-oxidizing atmosphere such as an inert gas such as helium, xenon, neon, carbon dioxide, flue gas or a mixed gas thereof, at 300 to 2000 ° C., particularly 500 to 100 ° C.
It is preferable to heat in a temperature range of about 0 ° C. The heating time in this case is 10 minutes to 80 hours, particularly 10 minutes to 3 hours.
It is preferably 0 hours.
【００１３】炭素化処理を行う装置としては、固定床加
熱炉、流動床加熱炉、移動床加熱炉、内熱式又は外熱式
のロータリーキルン、電気炉等を採用することが好まし
い。As the apparatus for performing the carbonization treatment, it is preferable to employ a fixed-bed heating furnace, a fluidized-bed heating furnace, a moving-bed heating furnace, an internal heating or external heating rotary kiln, an electric furnace, or the like.
【００１４】最後に、この炭素材料を賦活させることに
より活性炭が得られる。Finally, activated carbon is obtained by activating the carbon material.
【００１５】賦活は、炭素化処理で生成した炭素材料の
細孔構造を、より微細構造に成長・発達させる工程であ
る。賦活は、ガス賦活を行う場合には、水蒸気、二酸化
炭素、酸素、塩化水素、塩素等のいずれか一種以上を含
む酸化性のガス雰囲気下、加熱温度が５００〜１１００
℃（特に、７００〜１０００℃が好ましい）で、５分〜
１０時間程度加熱することにより行われる。また、アル
カリ金属水酸化物で賦活する場合は、水酸化カリウム、
水酸化ナトリウム、水酸化リチウム、水酸化ルビジウム
及び水酸化セシウムからなる群から選ばれる１種又は２
種以上を使用できる。例えば、アルカリ金属水酸化物を
質量比で０．２〜５．０倍量の炭素材料と混合し、アル
カリ金属水酸化物の融点以上の３００〜１０００℃（特
に、４００〜９００℃が好ましい）の温度範囲におい
て、３０分〜１０時間（特に、８０分〜５時間が好まし
い）非酸化性ガス雰囲気下で加熱することにより行われ
る。Activation is a process of growing and developing the fine pore structure of the carbon material generated by the carbonization treatment. In the case of performing gas activation, a heating temperature is 500 to 1100 in an oxidizing gas atmosphere containing any one or more of steam, carbon dioxide, oxygen, hydrogen chloride, and chlorine.
° C (particularly, preferably 700 to 1000 ° C) for 5 minutes to
It is performed by heating for about 10 hours. When activated with an alkali metal hydroxide, potassium hydroxide,
One or two selected from the group consisting of sodium hydroxide, lithium hydroxide, rubidium hydroxide and cesium hydroxide
More than species can be used. For example, an alkali metal hydroxide is mixed with a carbon material in a mass ratio of 0.2 to 5.0 times the mass, and the melting point of the alkali metal hydroxide is higher than or equal to 300 to 1000C (particularly, preferably 400 to 900C). Is carried out in a non-oxidizing gas atmosphere for 30 minutes to 10 hours (particularly, preferably 80 minutes to 5 hours).
【００１６】賦活は、上記の酸化性ガスによる賦活とア
ルカリ金属水酸化物による賦活を組合わせて数度にわた
って行うこともできる。この場合は、活性炭の細孔構造
が所期の数値範囲に入るように、適宜処理条件を変更す
ればよい。The activation can be performed several times by combining the activation with the oxidizing gas and the activation with the alkali metal hydroxide. In this case, the treatment conditions may be appropriately changed so that the pore structure of the activated carbon falls within a desired numerical range.
【００１７】賦活を行う装置としては、炭素化に使用し
たものと同様の装置を使用でき、固定床加熱炉、流動床
加熱炉、移動床加熱炉、内熱式又は外熱式のロータリー
キルン、電気炉等を採用することが好ましい。As a device for performing the activation, the same device as that used for the carbonization can be used, and a fixed-bed heating furnace, a fluidized-bed heating furnace, a moving-bed heating furnace, an internal heating or external heating rotary kiln, It is preferable to employ a furnace or the like.
【００１８】本発明により得られる炭素材料の比表面積
は、１００ｍ2／ｇ以上、特に、４００〜１０００ｍ2／
ｇであることが好ましい。また、炭素材料より賦活して
得られる活性炭の比表面積は、７００ｍ2／ｇ以上であ
ることが好ましい。[0018] The specific surface area of the carbon material obtained by the present invention, 100 m 2 / g or more, particularly, 400 to 1000 m 2 /
g is preferable. Further, the specific surface area of activated carbon obtained by activating from a carbon material is preferably 700 m 2 / g or more.
【００１９】本発明では、比表面積は窒素の吸脱着によ
るＢＥＴ法により測定する。比表面積は、あらかじめ真
空中で２００℃で１２時間以上乾燥させた試料に液体窒
素温度で窒素ガスを吸着させて得られた吸着等温線の相
対圧力０．００１〜０．０５の範囲をＢＥＴ多点法で解
析して算出する。測定装置としては、カンタクローム社
の商品名オートソーブ１等が例示できる。In the present invention, the specific surface area is measured by the BET method using adsorption and desorption of nitrogen. The specific surface area is determined by adsorbing nitrogen gas at a liquid nitrogen temperature to a sample previously dried at 200 ° C. for 12 hours or more in a vacuum. Calculate by analyzing with the point method. Examples of the measuring device include Autosorb 1 (trade name, manufactured by Kantachrome Co., Ltd.).
【００２０】有機ヒドロゲルを生成させる工程におい
て、原料中には重合反応に関与しないその他の成分を加
えることもできる。例えば、二酸化チタンを添加するこ
とにより、二酸化チタンの分散された炭素材料が得られ
る。In the step of forming the organic hydrogel, other components not involved in the polymerization reaction may be added to the raw materials. For example, by adding titanium dioxide, a carbon material in which titanium dioxide is dispersed can be obtained.
【００２１】[0021]
【実施例】以下、本発明を実施例（例１〜３）及び比較
例（例４、５）によって具体的に説明するが、本発明は
これらに限定されない。EXAMPLES Hereinafter, the present invention will be described specifically with reference to Examples (Examples 1 to 3) and Comparative Examples (Examples 4 and 5), but the present invention is not limited thereto.
【００２２】実施例、比較例において得られた有機ヒド
ロゲルを超臨界水中で乾燥し、有機エアロゲルを生成
し、この有機エアロゲルを、温度９５０℃で、２時間加
熱し炭素化して、炭素材料を得た。さらに、この炭素材
料を賦活することにより、活性炭が得られる。The organic hydrogels obtained in Examples and Comparative Examples were dried in supercritical water to produce an organic aerogel, and the organic aerogel was heated at a temperature of 950 ° C. for 2 hours to be carbonized to obtain a carbon material. Was. Further, activated carbon can be obtained by activating the carbon material.
【００２３】実施例、比較例で得られた炭素材料及び活
性炭の比表面積は、カンタクローム社のオートソーブ１
を使用し以下のように測定した。The specific surface area of the carbon material and the activated carbon obtained in Examples and Comparative Examples was determined by Autosorb 1 manufactured by Kantachrome.
Was measured as follows.
【００２４】比表面積は、あらかじめ真空中で２００℃
で１２時間以上乾燥させた試料に液体窒素温度で窒素ガ
スを吸着させて得られた吸着等温線において相対圧力
０．００１〜０．０５の範囲でＢＥＴ多点法で解析して
算出した。The specific surface area should be 200 ° C. in a vacuum beforehand.
The sample was dried for 12 hours or more by a nitrogen gas adsorption at a liquid nitrogen temperature to obtain an isotherm obtained by analyzing by a BET multipoint method in a relative pressure range of 0.001 to 0.05.
【００２５】〔例１〕容量５０ｃｍ3の容器中に、レゾ
ルシノール３．１２５ｇ、３６質量％ホルムアルデヒド
水溶液４．７３ｇ、炭酸ナトリウム０．１２ｇ及び水２
５ｇを入れ、撹拌溶解後、室温にて１６時間放置し、形
状の定まった有機ヒドロゲルを得た。この有機ヒドロゲ
ルを容量５０ｃｍ3の容器から出し、容量３００ｃｍ3の
密閉容器に移し、水を１５０ｃｍ3加え、１４０℃で３
時間加熱し、熟成された有機ヒドロゲルを得た。Example 1 In a container having a capacity of 50 cm 3 , 3.125 g of resorcinol, 4.73 g of a 36% by mass aqueous formaldehyde solution, 0.12 g of sodium carbonate and water 2
5 g was added, and after stirring and dissolving, the mixture was allowed to stand at room temperature for 16 hours to obtain an organic hydrogel having a fixed shape. The organic hydrogel was taken out of a container having a capacity of 50 cm 3 , transferred to a closed container having a capacity of 300 cm 3 , and 150 cm 3 of water was added.
After heating for an hour, an aged organic hydrogel was obtained.
【００２６】この熟成された有機ヒドロゲルは、表面か
ら内部にかけて透明褐色を呈し、また、取り扱い強度も
充分であり、形状を保持していた。さらに、イソプロピ
ルアルコール中に浸漬しても形状を保持していた。この
熟成された有機ヒドロゲルを上述の条件で炭素化処理
し、炭素材料を得た。得られた炭素材料の比表面積は８
７０ｍ2／ｇであった。The aged organic hydrogel exhibited a transparent brown color from the surface to the inside, had sufficient handling strength, and maintained its shape. Furthermore, the shape was maintained even when immersed in isopropyl alcohol. The aged organic hydrogel was carbonized under the above conditions to obtain a carbon material. The specific surface area of the obtained carbon material is 8
70 m 2 / g.
【００２７】〔例２〕容量５０ｃｍ3の耐熱性容器中
に、レゾルシノール３．１２５ｇ、３６質量％ホルムア
ルデヒド水溶液４．７３ｇ、炭酸ナトリウム０．１２ｇ
及び水２５ｇを入れ、撹拌溶解後、室温にて１６時間放
置し、形状の定まった有機ヒドロゲルを得た。この有機
ヒドロゲルの入った容量５０ｃｍ3耐熱性容器を該容器
ごと容量３００ｃｍ3の密閉容器内に移し、水３ｃｍ3を
容量５０ｃｍ3耐熱性容器の外に加え、１４０℃で３時
間加熱し、熟成された有機ヒドロゲルを得た。Example 2 In a heat-resistant container having a capacity of 50 cm 3 , 3.125 g of resorcinol, 4.73 g of a 36% by mass aqueous solution of formaldehyde, and 0.12 g of sodium carbonate
Then, 25 g of water and 25 g of water were added, and the mixture was dissolved by stirring. Transfer the entered capacity 50 cm 3 heat resistant container of this organic hydrogel in a closed vessel the vessel per volume 300 cm 3, adding water 3 cm 3 to the outside of the capacitor 50 cm 3 heat resistant vessel and heated for 3 hours at 140 ° C., aged The obtained organic hydrogel was obtained.
【００２８】この熟成された有機ヒドロゲルは、表面か
ら内部にかけて透明褐色を呈し、また、取り扱い強度も
充分であり、形状を保持していた。さらに、イソプロピ
ルアルコール中に浸漬しても形状を保持していた。この
熟成された有機ヒドロゲルを上述の条件で炭素化処理
し、炭素材料を得た。得られた炭素材料の比表面積は６
９０ｍ2／ｇであった。This aged organic hydrogel exhibited a transparent brown color from the surface to the inside, had sufficient handling strength, and maintained its shape. Furthermore, the shape was maintained even when immersed in isopropyl alcohol. The aged organic hydrogel was carbonized under the above conditions to obtain a carbon material. The specific surface area of the obtained carbon material is 6
It was 90 m 2 / g.
【００２９】〔例３〕容量５０ｃｍ3の耐熱性容器中
に、レゾルシノール３．１２５ｇ、３６質量％ホルムア
ルデヒド水溶液４．７３ｇ、炭酸ナトリウム０．１２
ｇ、水２５ｇ及び二酸化チタン粉末３ｇを入れ、二酸化
チタン粉末が沈降しない程度に撹拌し、室温にて１６時
間放置し、形状の定まった有機ヒドロゲルを得た。この
有機ヒドロゲルの入った容量５０ｃｍ3耐熱性容器を該
容器ごと容量３００ｃｍ3の密閉容器内に移し、水１０
０ｃｍ3を容量５０ｃｍ3耐熱性容器の外に加え、１７０
℃で１時間加熱し、熟成された有機ヒドロゲルを得た。Example 3 In a heat-resistant container having a capacity of 50 cm 3 , 3.125 g of resorcinol, 4.73 g of a 36% by weight aqueous solution of formaldehyde, and 0.12 of sodium carbonate
g, 25 g of water and 3 g of titanium dioxide powder were added, stirred to such an extent that the titanium dioxide powder did not settle, and allowed to stand at room temperature for 16 hours to obtain an organic hydrogel having a fixed shape. The 50 cm 3 heat-resistant container containing the organic hydrogel was transferred into a closed container having a capacity of 300 cm 3 together with the container.
Added 0 cm 3 outside the volume 50 cm 3 heat resistant container, 170
Heating at 1 ° C. for 1 hour gave an aged organic hydrogel.
【００３０】この熟成された有機ヒドロゲルは、表面か
ら内部にかけて均一な色を呈し、また、取り扱い強度も
充分であり、形状を保持していた。さらに、イソプロピ
ルアルコール中に浸漬しても形状を保持していた。この
熟成された有機ヒドロゲルを上述の条件で炭素化処理
し、炭素材料を得た。得られた炭素材料の比表面積は８
３０ｍ2／ｇであった。The aged organic hydrogel exhibited a uniform color from the surface to the inside, had sufficient handling strength, and maintained its shape. Furthermore, the shape was maintained even when immersed in isopropyl alcohol. The aged organic hydrogel was carbonized under the above conditions to obtain a carbon material. The specific surface area of the obtained carbon material is 8
It was 30 m 2 / g.
【００３１】〔例４〕容量５０ｃｍ3の耐熱性容器中
に、レゾルシノール３．１２５ｇ、３６質量％ホルムア
ルデヒド水溶液４．７３ｇ、炭酸ナトリウム０．１２ｇ
及び水２５ｇを入れ、撹拌溶解後、室温にて１６時間放
置し、形状の定まった有機ヒドロゲルを得た。この有機
ヒドロゲルを容量５０ｃｍ3の耐熱性容器に入れたま
ま、密閉して１４０℃で３時間加熱処理した。Example 4 In a heat-resistant container having a capacity of 50 cm 3 , 3.125 g of resorcinol, 4.73 g of a 36% by mass aqueous formaldehyde solution, and 0.12 g of sodium carbonate
Then, 25 g of water and 25 g of water were added, and the mixture was dissolved by stirring. While keeping this organic hydrogel in a heat-resistant container having a capacity of 50 cm 3 , it was sealed and heat-treated at 140 ° C. for 3 hours.
【００３２】この加熱処理された有機ヒドロゲルは、乾
燥し、表面は黒く不透明に変色し、亀裂が入っていた。
また、取り扱い強度も不充分であり、耐熱容器から取り
出すとき形状を保持できなかった。そのため、その後の
炭素化処理は行わなかった。The heat-treated organic hydrogel was dried, the surface turned black and opaque, and had cracks.
In addition, the handling strength was insufficient, and the shape could not be maintained when taken out of the heat-resistant container. Therefore, subsequent carbonization treatment was not performed.
【００３３】〔例５〕容量５０ｃｍ3の耐熱性容器中
に、レゾルシノール３．１２５ｇ、３６質量％ホルムア
ルデヒド水溶液４．７３ｇ、炭酸ナトリウム０．１２ｇ
及び水２５ｇを入れ、撹拌溶解後、室温にて１６時間放
置し、形状の定まった有機ヒドロゲルを得た。この有機
ヒドロゲルを容量５０ｃｍ3の耐熱性容器に入れたま
ま、密閉して８０℃で３時間加熱処理した。Example 5 In a heat-resistant container having a capacity of 50 cm 3 , 3.125 g of resorcinol, 4.73 g of a 36% by mass aqueous formaldehyde solution, and 0.12 g of sodium carbonate
Then, 25 g of water and 25 g of water were added, and the mixture was dissolved by stirring. While keeping this organic hydrogel in a heat-resistant container having a capacity of 50 cm 3, the organic hydrogel was sealed and heated at 80 ° C. for 3 hours.
【００３４】この加熱処理された有機ヒドロゲルは、表
面から内部にかけて均一な色を呈していたが、取り扱い
強度が不充分であり、耐熱容器から取り出すとき形状を
保持できなかった。アルコール中に浸漬すると、端から
崩れていった。この加熱処理された有機ヒドロゲルを上
述の条件で炭素化処理し、炭素材料を得た。得られた炭
素材料の比表面積は８５ｍ2／ｇであった。Although the heat-treated organic hydrogel exhibited a uniform color from the surface to the inside, the handling strength was insufficient, and the shape could not be maintained when the organic hydrogel was taken out of the heat-resistant container. When immersed in alcohol, it collapsed from the edge. The heat-treated organic hydrogel was carbonized under the above conditions to obtain a carbon material. The specific surface area of the obtained carbon material was 85 m 2 / g.
【００３５】[0035]
【発明の効果】本発明により、従来の方法よりも短時間
で有機ヒドロゲルから炭素材料及び活性炭を製造でき
る。According to the present invention, a carbon material and activated carbon can be produced from an organic hydrogel in a shorter time than conventional methods.
Claims (4)
合物及びホルムアルデヒドを水中で反応させて有機ヒド
ロゲルを得る工程、前記有機ヒドロゲルに水を添加して
加圧密閉下で加熱処理することにより熟成された有機ヒ
ドロゲルを得る工程、前記熟成された有機ヒドロゲルを
乾燥し有機エアロゲルを生成させる工程、及び前記有機
エアロゲルを炭素化処理する工程、を経る炭素材料の製
造方法。1. An organic hydrogel obtained by reacting an aromatic compound having a plurality of phenolic OH groups and formaldehyde in water to obtain an organic hydrogel. A method for producing a carbon material, comprising: a step of obtaining an organic hydrogel, a step of drying the aged organic hydrogel to form an organic airgel, and a step of carbonizing the organic airgel.
ける添加する水の量が、加熱処理時に加圧密閉容器内が
飽和蒸気圧になるのに充分な量である請求項１に記載の
炭素材料の製造方法。2. The carbon material according to claim 1, wherein the amount of water to be added in the step of obtaining an aged organic hydrogel is an amount sufficient for the inside of the pressurized closed vessel to reach a saturated vapor pressure during the heat treatment. Manufacturing method.
ける加熱温度が、１００〜１９０℃である請求項１又は
２に記載の炭素材料の製造方法。3. The method for producing a carbon material according to claim 1, wherein the heating temperature in the step of obtaining an aged organic hydrogel is 100 to 190 ° C.
られた炭素材料を、さらに賦活処理する活性炭の製造方
法。4. A method for producing activated carbon, wherein the carbon material obtained by the production method according to claim 1, 2 or 3 is further activated.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000184739A JP2002003211A (en) | 2000-06-20 | 2000-06-20 | Method for producing carbon material and activated carbon |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000184739A JP2002003211A (en) | 2000-06-20 | 2000-06-20 | Method for producing carbon material and activated carbon |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2002003211A true JP2002003211A (en) | 2002-01-09 |
Family
ID=18685147
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2000184739A Pending JP2002003211A (en) | 2000-06-20 | 2000-06-20 | Method for producing carbon material and activated carbon |
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| Country | Link |
|---|---|
| JP (1) | JP2002003211A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005187320A (en) * | 2003-12-01 | 2005-07-14 | Hajime Tamon | Method for producing carbon material and tablet-like dried gel |
| JP2006319321A (en) * | 2005-04-12 | 2006-11-24 | Sumitomo Chemical Co Ltd | Active carbon and manufacturing method therefor |
| JP2006319322A (en) * | 2005-04-12 | 2006-11-24 | Sumitomo Chemical Co Ltd | Electric double-layer capacitor |
| JP2008184359A (en) * | 2007-01-30 | 2008-08-14 | Sumitomo Chemical Co Ltd | Activated carbon |
| CN108298536A (en) * | 2018-03-29 | 2018-07-20 | 北方民族大学 | The preparation method of wheat stalk matrix activated carbon |
| CN113277864A (en) * | 2020-02-20 | 2021-08-20 | 中国科学院化学研究所 | Preparation method of carbonaceous aerogel and aerogel |
-
2000
- 2000-06-20 JP JP2000184739A patent/JP2002003211A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005187320A (en) * | 2003-12-01 | 2005-07-14 | Hajime Tamon | Method for producing carbon material and tablet-like dried gel |
| JP2006319321A (en) * | 2005-04-12 | 2006-11-24 | Sumitomo Chemical Co Ltd | Active carbon and manufacturing method therefor |
| JP2006319322A (en) * | 2005-04-12 | 2006-11-24 | Sumitomo Chemical Co Ltd | Electric double-layer capacitor |
| JP2008184359A (en) * | 2007-01-30 | 2008-08-14 | Sumitomo Chemical Co Ltd | Activated carbon |
| CN108298536A (en) * | 2018-03-29 | 2018-07-20 | 北方民族大学 | The preparation method of wheat stalk matrix activated carbon |
| CN113277864A (en) * | 2020-02-20 | 2021-08-20 | 中国科学院化学研究所 | Preparation method of carbonaceous aerogel and aerogel |
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