JPH0741770A - Manufacture of pitch for production of carbonaceous product - Google Patents
Manufacture of pitch for production of carbonaceous productInfo
- Publication number
- JPH0741770A JPH0741770A JP20359093A JP20359093A JPH0741770A JP H0741770 A JPH0741770 A JP H0741770A JP 20359093 A JP20359093 A JP 20359093A JP 20359093 A JP20359093 A JP 20359093A JP H0741770 A JPH0741770 A JP H0741770A
- Authority
- JP
- Japan
- Prior art keywords
- pitch
- porous inorganic
- raw material
- filtration
- substance
- 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.)
- Pending
Links
Landscapes
- Working-Up Tar And Pitch (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、炭素製品製造用ピッチ
の製造方法に関するものであり、詳しくは、コールター
ル、縮合多環芳香族炭化水素などの原料ピッチから不溶
性物質を分離除去して炭素製品の製造に好適なピッチを
製造する方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a pitch for producing carbon products, and more specifically, to a carbon material obtained by separating and removing insoluble substances from raw material pitch such as coal tar and condensed polycyclic aromatic hydrocarbons. The present invention relates to a method for manufacturing a pitch suitable for manufacturing a product.
【０００２】[0002]
【従来の技術】炭素繊維やニードルコークスの前駆体と
なるメソフェーズピッチは、原料ピッチを加熱処理して
得られる。ところで、通常、原料ピッチ中には、不溶性
物質として、炭素質ではあるがキノリン等に不溶で且つ
不融な成分やＡｓｈ成分が含まれている。斯かる不溶性
物質は、メソフェーズピッチを得る際に不均一性の原因
となり乱れた組織の前駆体を与え、例えば、炭素繊維に
おいては、紡糸性、強度、弾性率に悪影響を及ぼし、ニ
ードルコークスにおいてはＣＴＥに対して悪影響を及ぼ
す。従って、原料ピッチから、炭素繊維、ニードルコー
クス等の炭素製品を製造する際、原料ピッチ中の不溶性
物質を分離除去する必要がある。2. Description of the Related Art Mesophase pitch, which is a precursor of carbon fiber and needle coke, is obtained by heating raw material pitch. By the way, normally, the raw material pitch contains a component which is carbonaceous but insoluble in quinoline or the like and an insoluble component or an Ash component as an insoluble substance. Such an insoluble substance causes a heterogeneous structure precursor in obtaining mesophase pitch and gives a disordered tissue precursor. For example, in carbon fiber, spinnability, strength, and elastic modulus are adversely affected, and in needle coke, It has an adverse effect on the CTE. Therefore, when producing carbon products such as carbon fiber and needle coke from the raw material pitch, it is necessary to separate and remove insoluble substances from the raw material pitch.
【０００３】原料ピッチから不溶性物質を分離する主な
方法として、重量沈降法、遠心分離法、濾過法が知られ
ている。しかしながら、濾過法は、特公平４−１７９２
号公報においても指摘されている通り、分離される不溶
性物質の粒子径が極めて小さいために濾過速度が遅く、
しかも、目詰まり等の機械的問題があるため、実用的な
方法ではないとされ、一般的には、重量沈降法および遠
心分離法が採用されている。As a main method for separating an insoluble substance from a raw material pitch, a gravimetric sedimentation method, a centrifugal separation method and a filtration method are known. However, the filtration method is 4-1792.
As pointed out in the publication, since the insoluble substance to be separated has a very small particle size, the filtration rate is slow,
Moreover, it is not a practical method due to mechanical problems such as clogging, and generally, the weight sedimentation method and the centrifugal separation method are adopted.
【０００４】[0004]
【発明が解決しようとする課題】しかしながら、重量沈
降法および遠心分離法の不溶性物質除去能力は、不溶性
物質の粒子径、比重および系の粘度により左右され、非
常に粒径の細かい不溶性物質や系との比重差が小さい不
溶性物質の場合は、重量沈降法および遠心分離法では不
溶性物質の除去が非常に困難である。本発明は、斯かる
実情に鑑みなされたものであり、その目的は、不溶性物
質の改良された除去法を採用した炭素製品製造用ピッチ
の製造方法を提供することにある。However, the ability of the weight sedimentation method and the centrifugal separation method to remove insoluble substances depends on the particle size of the insoluble substance, the specific gravity and the viscosity of the system. In the case of an insoluble substance having a small difference in specific gravity from, it is very difficult to remove the insoluble substance by the weight sedimentation method and the centrifugation method. The present invention has been made in view of the above circumstances, and an object thereof is to provide a method for manufacturing a pitch for carbon product manufacturing that employs an improved method for removing an insoluble substance.
【０００５】[0005]
【課題を解決するための手段】本発明者らは、上記の目
的を達成すべく鋭意検討した結果、原料ピッチに特定の
物質を添加して粘度を２００ポイズ以下に調整するなら
ば、濾過などの手段により、不溶性物質が実質上含まれ
ていない精製された原料ピッチを容易に得ることが出来
るとの知見を得た。Means for Solving the Problems As a result of intensive studies to achieve the above object, the present inventors have found that if a specific substance is added to a raw material pitch to adjust the viscosity to 200 poises or less, filtration, etc. It was found that the purified raw material pitch substantially containing no insoluble substance can be easily obtained by the above method.
【０００６】本発明は、上記の知見を基に完成されたも
のであり、その要旨は、原料ピッチに多孔質無機物を添
加し、粘度を２００ポイズ以下に調整した後、該多孔質
無機物を分離除去することを特徴とする炭素製品製造用
ピッチの製造方法に存する。The present invention has been completed based on the above findings, and its gist is to add a porous inorganic material to a raw material pitch and adjust the viscosity to 200 poise or less, and then separate the porous inorganic material. It exists in the manufacturing method of the pitch for carbon product manufacturing characterized by removing.
【０００７】以下、本発明を詳説明する。本発明に用い
られる原料ピッチとしては、例えば、石炭系のコールタ
ールやコールタールピッチ、石炭液化物、石油系の重質
油やピッチ、石油樹脂やその熱重縮合反応生成物、ナフ
タレンやアントラセンの触媒反応による重合反応生成物
などの炭素質原料が挙げられる。また、予備処理を行な
った炭素質原料も用いることが出来、予備処理として
は、例えば、加熱処理した後、特定溶剤で可溶分を抽出
する方法、または、水素供与性溶剤または水素ガスの存
在下に水添処理する方法が挙げられる。The present invention will be described in detail below. Examples of the raw material pitch used in the present invention include coal-based coal tar and coal tar pitch, coal liquefaction, petroleum-based heavy oil and pitch, petroleum resin and its thermal polycondensation reaction product, naphthalene and anthracene. Carbonaceous raw materials such as a polymerization reaction product by a catalytic reaction can be mentioned. A pretreated carbonaceous raw material can also be used. As the pretreatment, for example, a method of extracting a soluble component with a specific solvent after heat treatment, or the presence of a hydrogen donating solvent or hydrogen gas The method of hydrogenation treatment is mentioned below.
【０００８】本発明に用いられる多孔質無機物として
は、原料ピッチに対して化学的に不活性で且つ不溶性で
あり、原料ピッチ中の不溶性物質を吸着し得るようなも
のであれば特に限定されず、種々の多孔質無機物を用い
ることが出来る。具体的には、パーライト、セルロー
ズ、アスベスト、マグネシア、石こう、活性炭素、珪藻
土などが挙げられる。特に、濾過助材として市販されて
いる珪藻土は、透過率が高く、しかも、強固であって圧
縮変形の無いケーキを形成出来るので好ましい。The porous inorganic material used in the present invention is not particularly limited as long as it is chemically inactive and insoluble in the raw material pitch and can adsorb the insoluble substance in the raw material pitch. Various porous inorganic substances can be used. Specific examples include perlite, cellulose, asbestos, magnesia, gypsum, activated carbon and diatomaceous earth. In particular, diatomaceous earth commercially available as a filter aid is preferable because it has a high transmittance and can form a cake that is strong and does not undergo compression deformation.
【０００９】多孔質無機物の粒径分布に関しては特に制
限はないが、多孔質無機物自体の粒径が小さ過ぎる場合
は、それ自身がフィルターの目詰まりを起こして濾過性
を低下させたり、濾液側への目洩れを起こして原料ピッ
チを汚染することになる。また、粒径が大き過ぎる場
合、それ自体が系の中で沈降して原料ピッチとの均一な
スラリーを形成することが困難となる。There is no particular limitation on the particle size distribution of the porous inorganic material, but when the particle size of the porous inorganic material itself is too small, the porous inorganic material itself causes clogging of the filter to deteriorate the filterability, or the filtrate side. This will lead to leakage of water to pollute the raw material pitch. If the particle size is too large, it will settle in the system itself and it will be difficult to form a uniform slurry with the raw material pitch.
【００１０】従って、多孔質無機物としては、平均粒径
が２〜５０μｍ、１μｍ以下のものが２％以下、１００
μｍ以上のものが２０％以下である粒径分布の多孔質無
機物が好ましい。特に、平均粒径が５〜２０μｍ、１μ
ｍ以下のものが実質的に０％、５０μｍ以上のものが１
０％以下である粒径分布の多孔質無機物が好ましい。Therefore, as the porous inorganic substance, those having an average particle size of 2 to 50 μm and 1 μm or less are 2% or less, 100% or less.
A porous inorganic material having a particle size distribution in which particles having a particle size of μm or more is 20% or less is preferable. In particular, the average particle size is 5 to 20 μm, 1 μ
Substantially 0% for m or less, 1 for 50 μm or more
A porous inorganic material having a particle size distribution of 0% or less is preferable.
【００１１】多孔質無機物は、通常、原料ピッチ１００
部に対して０．０１〜２０重量部、好ましくは、０．０
５〜５重量部の範囲で添加される。原料ピッチへの添加
方法は特に限定されず、例えば、所定量の多孔質無機物
をピッチ中に投入して機械的な攪拌により分散させる方
法などが採用される。The porous inorganic substance is usually a raw material pitch of 100.
0.01 to 20 parts by weight, preferably 0.0
It is added in the range of 5 to 5 parts by weight. The addition method to the raw material pitch is not particularly limited, and, for example, a method of introducing a predetermined amount of porous inorganic material into the pitch and dispersing it by mechanical stirring is adopted.
【００１２】ところで、濾過時のピッチスラリーの粘度
は濾過速度に影響を与えることが知られている。すなわ
ち、定圧濾過の場合、スラリー粘度が低いほど濾過速度
は速くなる。従って、本発明においては、原料ピッチに
多孔質無機物を添加して得られるピッチスラリーの粘度
は、２００ポイズ以下、好ましくは０．００１〜５０ポ
イズ、更に好ましくは０．００１〜１０ポイズに調整す
る。By the way, it is known that the viscosity of the pitch slurry during filtration affects the filtration rate. That is, in the case of constant pressure filtration, the lower the slurry viscosity, the faster the filtration rate. Therefore, in the present invention, the viscosity of the pitch slurry obtained by adding the porous inorganic material to the raw material pitch is adjusted to 200 poises or less, preferably 0.001 to 50 poises, and more preferably 0.001 to 10 poises. .
【００１３】ピッチスラリーの粘度を低下させる方法と
しては、ピッチスラリーの温度を上げる方法、溶媒によ
って希釈する方法の何れであってもよい。より高い効果
を得るため、これらの方法を組み合わせてもよい。希釈
溶媒としては、例えば、タール蒸留により得られる、洗
浄油、アントラセン油などが挙げられる。The method for decreasing the viscosity of the pitch slurry may be either a method of raising the temperature of the pitch slurry or a method of diluting it with a solvent. These methods may be combined to obtain a higher effect. Examples of the diluting solvent include cleaning oil and anthracene oil obtained by tar distillation.
【００１４】本発明においては、粘度を２００ポイズ以
下に調整したピッチスラリーから多孔質無機物を分離除
去することにより不溶性物質を分離する。多孔質無機物
の分離除去方のためには、例えば、既知の目開きを有す
るフィルターを通してピッチスラリーを濾過をすればよ
い。濾過操作により、原料ピッチ中の不溶性物質は、多
孔質無機物に吸着され、また、多孔質無機物粒子中に分
散されることにより、濾過抵抗を減じ、更には、フィル
ターへの目詰まりを防止し、工業的な連続濾過が可能と
なる。In the present invention, the insoluble substance is separated by separating and removing the porous inorganic substance from the pitch slurry whose viscosity is adjusted to 200 poise or less. In order to separate and remove the porous inorganic substance, for example, the pitch slurry may be filtered through a filter having a known mesh. By the filtration operation, the insoluble substance in the raw material pitch is adsorbed to the porous inorganic substance, and by being dispersed in the porous inorganic substance particles, the filtration resistance is reduced, and further, clogging of the filter is prevented, Industrial continuous filtration becomes possible.
【００１５】濾過により、多孔質無機物は不溶性物質を
捕捉して濾過残渣としてフィルター上に残り、それらが
除去された精製されたピッチが濾液として得られる。濾
過の形式は特に限定されず、加圧濾過、減圧濾過、遠心
濾過などが適宜採用される。粘度調整のために溶媒を添
加した場合には、蒸留などの後工程にて溶媒を除去すれ
ばよい。By filtration, the porous inorganic substance captures the insoluble substance and remains on the filter as a filtration residue, and purified pitch obtained by removing them is obtained as a filtrate. The form of filtration is not particularly limited, and pressure filtration, vacuum filtration, centrifugal filtration, etc. are appropriately adopted. When a solvent is added to adjust the viscosity, the solvent may be removed in a subsequent step such as distillation.
【００１６】また、本発明においては、ピッチスラリー
から多孔質無機物を分離除去する方法として、遠心分離
を採用することも出来る。遠心分離操作においても、原
料ピッチ中の不溶性物質は多孔質無機物に吸着され、そ
の結果、不溶性物質の見かけの粒径が大きくなり分離が
容易になる。Further, in the present invention, centrifugation can be adopted as a method for separating and removing the porous inorganic material from the pitch slurry. Even in the centrifugal separation operation, the insoluble substance in the raw material pitch is adsorbed by the porous inorganic substance, and as a result, the apparent particle size of the insoluble substance becomes large and the separation becomes easy.
【００１７】本発明の製造方法で得られたピッチは、キ
ノリン不溶分量が実質的に０％、また、Ａｓｈ成分が５
ｐｐｍ以下であり、物理的欠陥となり得る不溶性物質を
実質的に含有していない。従って、原料として、本発明
の製造方法で得られたピッチを用いることにより、不溶
性物質の存在による不均一性に起因する組織の乱れが改
善されて配向性が向上したメソフェーズピッチが得られ
る。その結果、紡糸性が良好で高強度かつ高弾性率の炭
素繊維や低ＣＴＥのニードルコークスの製造が可能とな
る。The pitch obtained by the production method of the present invention has a quinoline insoluble content of substantially 0% and an Ash component of 5%.
It is less than or equal to ppm, and substantially does not contain an insoluble substance that may become a physical defect. Therefore, by using the pitch obtained by the production method of the present invention as the raw material, the disorder of the structure due to the non-uniformity due to the presence of the insoluble substance is improved, and the mesophase pitch having the improved orientation is obtained. As a result, it becomes possible to manufacture carbon fiber having good spinnability, high strength and high elastic modulus, and needle coke having low CTE.
【００１８】[0018]
【実施例】以下、本発明を実施例により更に詳細に説明
するが、本発明は、その要旨を超えない限り、以下の実
施例に限定されるものではない。EXAMPLES The present invention will be described in more detail with reference to examples below, but the present invention is not limited to the following examples as long as the gist thereof is not exceeded.
【００１９】実施例１ ナフタレンをＡｌＣｌ3 触媒の存在下２５０℃で重合さ
せた後、触媒を回収し、キノリン不溶分量が１重量％の
原料ピッチを得た。また、この原料ピッチのＡｓｈ量を
測定した結果、２０ｐｐｍのＡｓｈ成分が含まれてい
た。上記の原料ピッチ１重量部に沸点範囲が２４０〜２
９０℃の洗浄油を３重量部加えて混合した後、多孔質無
機物として、市販の珪藻土濾過助剤「セライト５０５」
（商品名、セライト社製）を０．０１重量部加え、さら
に、タンク内で循環させて「セライト５０５」を分散さ
せた。Example 1 After naphthalene was polymerized at 250 ° C. in the presence of AlCl 3 catalyst, the catalyst was recovered to obtain a raw material pitch having a quinoline insoluble content of 1% by weight. Moreover, as a result of measuring the Ash amount of this raw material pitch, 20 ppm of Ash component was contained. The boiling point range is 240 to 2 per 1 part by weight of the above raw material pitch.
After adding 3 parts by weight of 90 ° C. washing oil and mixing, a commercially available diatomaceous earth filter aid “Celite 505” as a porous inorganic substance.
0.01 part by weight (trade name, manufactured by Celite) was added and further circulated in the tank to disperse "Celite 505".
【００２０】「セライト５０５」の粒径分布を測定した
結果、平均粒径（メジアン径）６．１μｍであり、１μ
ｍ以下および３０μｍ以上の粒径を有する粒子は夫々実
質的に０％であった。As a result of measuring the particle size distribution of "Celite 505", the average particle size (median size) was 6.1 μm, and 1 μm.
Particles having a particle size of m or less and 30 μm or more were substantially 0%, respectively.
【００２１】上記のピッチスラリーを１５０℃に加温し
て粘度を０．０２ポイズに調整し、１５０℃の温度を維
持しながら、目開き１０μｍのキャンドルフィルターに
より、濾過圧力２ｋｇ／ｃｍ2 で連続的に濾過を行な
い、ピッチと洗浄油の混合液を得た。この濾過操作にお
いては、濾過面積１ｍ2 当り、０．２トン／時の濾過速
度が可能であった。The above pitch slurry was heated to 150 ° C. to adjust the viscosity to 0.02 poise, and while maintaining the temperature of 150 ° C., a candle filter having an opening of 10 μm continuously applied at a filtration pressure of 2 kg / cm 2 . Filtration was performed to obtain a mixed solution of pitch and cleaning oil. In this filtration operation, a filtration rate of 0.2 ton / hour was possible per 1 m 2 of filtration area.
【００２２】上記の混合液から洗浄油を蒸留分離してピ
ッチを得た。得られたピッチのキノリン不溶分量および
Ａｓｈ量を測定した結果、キノリン不溶分量は実質的に
０％、Ａｓｈ量は１．５ｐｐｍ以下であった。このピッ
チを４００℃で１５０分加熱処理し、光学異方性１００
％のピッチに変換し、紡糸、不融化処理を行った後、２
１００℃で黒鉛化して炭素繊維を調製した。得られた炭
素繊維の引張強度は３００ｋｇ／ｍｍ2 、引張弾性率は
６５ｔｏｎ／ｍｍ2 であった。The cleaning oil was distilled off from the above mixture to obtain pitch. As a result of measuring the quinoline insoluble content and the Ash content of the obtained pitch, the quinoline insoluble content was substantially 0% and the Ash content was 1.5 ppm or less. This pitch is heat-treated at 400 ° C. for 150 minutes to obtain an optical anisotropy of 100.
% After converting to pitch, spinning and infusibilizing treatment, 2
Graphitized at 100 ° C. to prepare carbon fibers. The obtained carbon fiber had a tensile strength of 300 kg / mm 2 and a tensile modulus of 65 ton / mm 2 .
【００２３】比較例１ 多孔質無機物を添加しない点を除いては、実施例１と全
く同様にして１５０℃で０．０２ポイズのピッチスラリ
ーを調製した。この加温したスラリーを実施例１と同じ
キャンドルフィルターにより、濾過圧力２ｋｇ／ｃｍ2
で連続濾過を試みたが、フィルターの目詰まりのため、
濾過圧力が上昇し、５時間後に連続濾過が不能となっ
た。Comparative Example 1 A pitch slurry of 0.02 poise at 150 ° C. was prepared in exactly the same manner as in Example 1 except that the porous inorganic substance was not added. This heated slurry was filtered with the same candle filter as in Example 1 at a filtration pressure of 2 kg / cm 2.
I tried continuous filtration with, but because the filter was clogged,
The filtration pressure increased and continuous filtration became impossible after 5 hours.
【００２４】比較例２ 実施例１で得られたキノリン不溶分量１％、Ａｓｈ成分
２０ｐｐｍのピッチを原料とし、濾過をすることなしに
実施例１と同様な方法で光学異方性１００％のピッチを
調製し、紡糸、不融化、黒鉛化処理して炭素繊維を調製
した。得られた炭素繊維の引張強度は２２０ｋｇ／ｍｍ
2 、引張弾性率は５７ｔｏｎ／ｍｍ2 であった。また、
この繊維の断面および表面を観察した結果、Ａｓｈ成分
に起因したと考えられるボイドが観察され、これが原因
で炭素繊維の強度低下が起きたと考えられる。Comparative Example 2 A pitch having an optical anisotropy of 100% was prepared in the same manner as in Example 1 without filtering, using a pitch having a quinoline insoluble content of 1% and an Ash component of 20 ppm obtained in Example 1 as a raw material. Was prepared and spun, infusibilized and graphitized to prepare carbon fibers. The tensile strength of the obtained carbon fiber is 220 kg / mm.
2 , the tensile elastic modulus was 57 ton / mm 2 . Also,
As a result of observing the cross section and the surface of this fiber, a void that is considered to be caused by the Ash component was observed, and it is considered that the strength of the carbon fiber decreased due to this.
【００２５】[0025]
【発明の効果】以上説明した本発明によれば、原料ピッ
チに多孔質無機物を添加し、粘度を２００ポイズ以下に
調整すると言った簡便な処理により、工業的な連続濾過
によるピッチ中の不溶性物質除去が可能である。また、
本発明の製造方法にるピッチは、不溶性物質を実質的に
含んでいないため、炭素繊維、ニードルコークス等の原
料として有用である。According to the present invention described above, an insoluble substance in pitch by industrial continuous filtration can be obtained by a simple treatment of adding a porous inorganic substance to the raw material pitch and adjusting the viscosity to 200 poise or less. It can be removed. Also,
Since the pitch according to the production method of the present invention does not substantially contain an insoluble substance, it is useful as a raw material for carbon fiber, needle coke and the like.
Claims (7)
度を２００ポイズ以下に調整した後、該多孔質無機物を
分離除去することを特徴とする炭素製品製造用ピッチの
製造方法。1. A method for producing a pitch for producing carbon products, which comprises adding a porous inorganic substance to a raw material pitch to adjust the viscosity to 200 poise or less, and then separating and removing the porous inorganic substance.
行なう請求項１に記載の製造方法。2. The production method according to claim 1, wherein the porous inorganic substance is separated and removed by filtration.
って行なう請求項１記載の製造方法。3. The method according to claim 1, wherein the porous inorganic substance is separated and removed by centrifugation.
である請求項１乃至３の何れかに記載の製造方法。4. The average particle size of the porous inorganic material is 2 to 50 μm.
The manufacturing method according to claim 1, wherein
至４の何れかに記載の製造方法。5. The production method according to claim 1, wherein the porous inorganic substance is diatomaceous earth.
５の何れかに記載の製造方法。6. The method according to claim 1, wherein the carbon product is carbon fiber.
項１乃至６の何れかに記載の製造方法。7. The production method according to claim 1, wherein the carbon product is needle coke.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20359093A JPH0741770A (en) | 1993-07-26 | 1993-07-26 | Manufacture of pitch for production of carbonaceous product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20359093A JPH0741770A (en) | 1993-07-26 | 1993-07-26 | Manufacture of pitch for production of carbonaceous product |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0741770A true JPH0741770A (en) | 1995-02-10 |
Family
ID=16476595
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP20359093A Pending JPH0741770A (en) | 1993-07-26 | 1993-07-26 | Manufacture of pitch for production of carbonaceous product |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0741770A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1076011C (en) * | 1998-01-13 | 2001-12-12 | 南通碳素厂 | Porous carbon material producing process |
-
1993
- 1993-07-26 JP JP20359093A patent/JPH0741770A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1076011C (en) * | 1998-01-13 | 2001-12-12 | 南通碳素厂 | Porous carbon material producing process |
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