JPH0551258A - Production of high density and high strength graphite material - Google Patents
Production of high density and high strength graphite materialInfo
- Publication number
- JPH0551258A JPH0551258A JP3235735A JP23573591A JPH0551258A JP H0551258 A JPH0551258 A JP H0551258A JP 3235735 A JP3235735 A JP 3235735A JP 23573591 A JP23573591 A JP 23573591A JP H0551258 A JPH0551258 A JP H0551258A
- Authority
- JP
- Japan
- Prior art keywords
- heavy oil
- graphite material
- graphite
- pitch
- carbonization
- 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.)
- Withdrawn
Links
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、るつぼ等のシリコン単
結晶引き上げ装置用部材、放電加工用電極、半導体製造
用治具、メカニカルシール軸受等の機械用カーボン、原
子炉用カーボン及び医療用カーボン等の用途に適する高
密度かつ高強度の黒鉛材の製造方法に関するものであ
る。FIELD OF THE INVENTION The present invention relates to a member for a silicon single crystal pulling apparatus such as a crucible, an electric discharge machining electrode, a semiconductor manufacturing jig, a mechanical carbon such as a mechanical seal bearing, a nuclear reactor carbon and a medical carbon. The present invention relates to a method for producing a high-density and high-strength graphite material suitable for applications such as
【０００２】[0002]
【従来の技術】従来、黒鉛材の製造に用いられている骨
材は、石油系及び石炭系ピッチか焼コークス及びこれら
にカーボンブラック等を配合したものが使用され、黒鉛
材の嵩密度を増加させるために、ピッチ含浸、再焼成が
繰り返し行われてきた。例えば、特開昭５５−１０９，
２１４号公報においては、焼成体あるいは黒鉛体にピッ
チを含浸し、焼成、黒鉛化する方法が提案されている。
この方法では、ピッチ含浸、再焼成及び再黒鉛化の工程
を行うことにより、黒鉛材の高密度化、高強度化を図っ
ていたために、コストが高く、黒鉛化に長時間がかかる
等の問題があった。2. Description of the Related Art Conventionally, as an aggregate used for producing a graphite material, a petroleum-based or coal-based pitch calcined coke and a mixture thereof with carbon black or the like are used to increase the bulk density of the graphite material. To do so, pitch impregnation and re-firing have been repeatedly performed. For example, JP-A-55-109,
In Japanese Patent Publication No. 214-214, a method of impregnating a fired body or a graphite body with pitch, firing and graphitizing is proposed.
In this method, since the density and strength of the graphite material were increased by performing the steps of pitch impregnation, re-firing and re-graphitization, the cost was high and the graphitization took a long time. was there.
【０００３】[0003]
【発明が解決しようとする課題】そこで、本発明者等
は、各種の高密度、高強度黒鉛材の作り分け技術を確立
するために、黒鉛材の製造方法に関する研究を鋭意行っ
てきた結果、重質油中にこの重質油に対して相溶性を有
する芳香族化合物からなる炭素化助剤を添加し、これを
熱処理してか焼コークスを調製し、このか焼コークスを
骨材として用いることにより、高密度かつ高強度の黒鉛
材を製造できることを突き止めた。従って、本発明の目
的は、ピッチ含浸、再焼成という工程を経ることなく、
品質が安定しており、より広い範囲の用途に適用できる
高密度かつ高強度の黒鉛材を製造する方法を提供するこ
とにある。Therefore, the inventors of the present invention have earnestly conducted research on a method for producing a graphite material in order to establish a technique for producing various high-density and high-strength graphite materials, and as a result, A carbonization aid consisting of an aromatic compound having compatibility with the heavy oil is added to the heavy oil, and heat treated to prepare a calcined coke, which is used as an aggregate. Therefore, it was found that a high-density and high-strength graphite material can be manufactured. Therefore, the object of the present invention is to perform the steps of pitch impregnation and re-baking,
It is an object of the present invention to provide a method for producing a high-density and high-strength graphite material having stable quality and applicable to a wider range of applications.
【０００４】[0004]
【課題を解決するための手段】本発明は、重質油１００
重量部中にこの重質油に対して相溶性を有する芳香族化
合物からなる炭素化助剤１〜５０重量部を添加し、熱処
理してか焼コークスを調製し、次いでこのか焼コークス
に結合材を添加して混練し、更に粉砕し、成型後焼成を
行って黒鉛化する高密度、高強度黒鉛材の製造方法であ
る。The present invention provides a heavy oil 100.
1 to 50 parts by weight of a carbonization aid composed of an aromatic compound having compatibility with the heavy oil is added in parts by weight, heat treatment is carried out to prepare a calcined coke, which is then bound to the calcined coke. This is a method for producing a high-density, high-strength graphite material in which a material is added and kneaded, further pulverized, and after molding, firing is performed to graphitize.
【０００５】以下、本発明の内容を更に詳述する。本発
明で原料とする重質油とは、石炭から誘導される石炭分
解抽出物やタールピッチ及び原油熱分解で生成する重質
油、エチレンボトム油、あるいはこれらを分解重合した
重質油等であり、これらは単独で使用できるほか、２種
以上の混合物として使用することもできる。The contents of the present invention will be described in more detail below. The heavy oil used as a raw material in the present invention is a coal decomposition extract derived from coal or a heavy oil produced by tar pitch and crude oil pyrolysis, ethylene bottom oil, or a heavy oil obtained by decomposing and polymerizing these. In addition, these can be used alone or as a mixture of two or more kinds.
【０００６】次に、炭素化助剤とは、原料となる重質油
との相溶性に優れ、しかも、少量添加することによっ
て、加熱重合時の重質油のラジカル反応性を著しく向上
させることができる芳香族化合物のことである。そし
て、ここでいう重質油との相溶性とは、重質油と均一に
混合し、混練可能な状態になる性質を指すものである。
このような炭素化助剤としては、具体的には例えば、芳
香族炭化水素にニトロ基、カルボニル基、スルホン基あ
るいはビニル基等を導入したジニトロナフタリン、ジニ
トロベンゼン、ニトロベンゼン、ニトロアントラキノ
ン、ナフトキノン、ニトロアニリンスルホン酸、ジビニ
ルベンゼン、及びこれらの誘導体、あるいはこれらの化
合物の混合物等を挙げることができる。[0006] Next, the carbonization aid has excellent compatibility with the heavy oil as a raw material, and when it is added in a small amount, the radical reactivity of the heavy oil during heat polymerization is significantly improved. It is an aromatic compound that can And the compatibility with the heavy oil mentioned here refers to the property of being uniformly mixed with the heavy oil and being in a kneadable state.
Examples of such a carbonization aid include, for example, dinitronaphthalene, dinitrobenzene, nitrobenzene, nitroanthraquinone, naphthoquinone, and nitro obtained by introducing a nitro group, a carbonyl group, a sulfone group or a vinyl group into an aromatic hydrocarbon. Examples thereof include anilinesulfonic acid, divinylbenzene, derivatives thereof, and mixtures of these compounds.
【０００７】この炭素化助剤は、その分解温度以下で重
質油と反応する。また、この炭素化助剤は、その分解温
度近傍において官能基を遊離し、それに伴って急激にラ
ジカルを発生するため、重質油中の多環芳香族化合物と
の重縮合反応が促進される。また、重質油の重縮合反応
に伴うメソフェースの合体、成長はラジカルの発生、失
活に大きく左右される。そこで、活性種の半減期が比較
的短いラジカル反応においては、急激にメソフェースが
発生しても、十分な合体成長反応が起こり難いためにプ
レカーサー組織が微細化される。The carbonization aid reacts with the heavy oil below its decomposition temperature. In addition, this carbonization aid releases a functional group in the vicinity of its decomposition temperature and rapidly generates radicals accordingly, so that the polycondensation reaction with the polycyclic aromatic compound in the heavy oil is promoted. .. In addition, the coalescence and growth of mesophase associated with the polycondensation reaction of heavy oil is greatly influenced by the generation and deactivation of radicals. Therefore, in a radical reaction in which the half-life of the active species is relatively short, even if a mesophase is rapidly generated, a sufficient coalescence growth reaction is difficult to occur, so that the precursor structure is miniaturized.
【０００８】このような炭素化助剤の添加量は、重質油
１００重量部に対して、１〜５０重量部、好ましくは５
〜３５重量部である。炭素化助剤の添加量が５０重量部
を越えると、反応に関与しない炭素化助剤が残留し、そ
の未反応の炭素化助剤が分解温度近傍で昇華等を引き起
こすために、反応装置内から半生コークスが突出した
り、それに伴って品質の不均一化を生じるので好ましく
ない。また、炭素化助剤の添加量が１重量部未満では、
未添加時のか焼コークスの光学的組織と差異が見られ
ず、添加効果が認められない。The amount of such a carbonization aid to be added is 1 to 50 parts by weight, preferably 5 parts by weight, relative to 100 parts by weight of heavy oil.
~ 35 parts by weight. If the addition amount of the carbonization aid exceeds 50 parts by weight, the carbonization aid not involved in the reaction remains, and the unreacted carbonization aid causes sublimation or the like in the vicinity of the decomposition temperature. It is not preferable because semi-raw coke will stick out from the product and uneven quality will occur. If the amount of carbonization aid added is less than 1 part by weight,
No difference is seen from the optical structure of the calcined coke before addition, and no effect of addition is observed.
【０００９】本発明で使用するか焼コークスは、重質油
１００重量部中に、炭素化助剤１〜５０重量部を添加
し、攪拌し、混合した後、ディレイドコーカー及びオー
トクレーブ等で熱処理して生ピッチコークスとし、更に
この生ピッチコークスをロータリーキルン又はマッフル
炉等でか焼することによって製造される。The calcined coke used in the present invention is obtained by adding 1 to 50 parts by weight of a carbonization aid to 100 parts by weight of heavy oil, stirring and mixing, and then heat treating with a delayed coker and an autoclave. To produce a raw pitch coke, and the raw pitch coke is calcined in a rotary kiln or a muffle furnace.
【００１０】前述の方法によって得られたか焼コークス
は、次に、微粉砕した後、石油系及び石炭系のバインダ
ーピッチや、フェノール樹脂、フラン樹脂、ポリエチレ
ン樹脂等の結合材と混練され、得られた塊状の混練物は
破砕あるいは磨砕することによって一定の粒度以下に微
粉砕される。微粉砕された混練物は、通常の型込めプレ
スあるいはラバープレス等を使用する成型方法により、
ハンドリングに十分耐え得る強度を有する所定の形状の
成型体に成型され、次の焼成及び黒鉛化の工程に移行さ
れる。そして、この焼成及び黒鉛化の工程では、成型体
は、不活性ガス雰囲気下あるいは粉コークス中で、マッ
フル炉又はリードハンマー炉等を用いて焼成された後、
再び不活性ガス雰囲気下あるいは粉コークス中で、タン
マン炉又はアチソン炉等を用いて黒鉛化処理され、所望
の黒鉛材が製造される。The calcined coke obtained by the above-mentioned method is then finely pulverized and then kneaded with a petroleum-based and coal-based binder pitch and a binder such as phenol resin, furan resin and polyethylene resin to obtain a coke. The lump-shaped kneaded product is crushed or ground to be finely pulverized to have a certain particle size or less. The finely pulverized kneaded product can be molded by a usual molding method such as a molding press or a rubber press.
It is molded into a molded body having a predetermined shape having a strength sufficient to withstand handling, and the process proceeds to the subsequent firing and graphitization steps. Then, in this firing and graphitization step, the molded body is fired using a muffle furnace or a reed hammer furnace in an inert gas atmosphere or in powder coke,
Again, in an inert gas atmosphere or in coke powder, graphitization is performed using a Tammann furnace, an Acheson furnace, etc., and a desired graphite material is manufactured.
【００１１】[0011]
実施例１〜９ コールタールピッチに表１に示す種々の炭素化助剤を添
加した後、オートクレーブ中で４５０℃、４時間の熱処
理を行い、得られた生ピッチコークスをマッフル炉中で
１，０００℃、１時間か焼してか焼コークスを得た。こ
のようにして得られたか焼コークスについて、炭素化助
剤によって微細化されたその光学的異方性組織の単位寸
法を測定した。結果を表１に示す。なお、表１中に示さ
れるコークス組織の単位寸法は、光学的異方性組織を有
するプレカーサーの反射率をデジタル化し、疑似粒子に
置き換えることによって求めた。Examples 1 to 9 After adding various carbonization aids shown in Table 1 to coal tar pitch, heat treatment was carried out at 450 ° C. for 4 hours in an autoclave, and the obtained raw pitch coke was treated in a muffle furnace in a muffle furnace. It was calcined at 000 ° C for 1 hour to obtain a calcined coke. With respect to the calcined coke thus obtained, the unit size of its optically anisotropic structure refined by a carbonization aid was measured. The results are shown in Table 1. The unit size of the coke structure shown in Table 1 was determined by digitizing the reflectance of the precursor having an optically anisotropic structure and replacing it with pseudo particles.
【００１２】このか焼コークスを平均粒径４μｍに微粉
砕した後、か焼コークス６０重量部に対してバインダー
ピッチを４０重量部の割合で添加し、２８５℃に予熱し
ておいたニーダー中で１時間混練して混練物を得た。そ
の後、得られた塊状の混練物を平均粒径９μｍに粉砕
し、金型で直径５０ｍｍ、高さ４５ｍｍの円柱状に一次
成型した後、１．５ｔ／ｃｍ2 の圧力で水圧等方加圧成
型を行った。次いで、この成型体を粉コークスを詰めた
容器内でアルゴン雰囲気中で１，１００℃まで加熱して
焼成し、更に黒鉛化炉でアルゴン気流中で２，８００℃
にて黒鉛化を行った。得られた黒鉛材の物性を表２に示
す。This calcined coke was finely pulverized to an average particle size of 4 μm, and then 40 parts by weight of binder pitch was added to 60 parts by weight of calcined coke and the mixture was preheated to 285 ° C. in a kneader. The mixture was kneaded for 1 hour to obtain a kneaded product. Then, the obtained lump-shaped kneaded product was crushed to an average particle size of 9 μm, primary-molded into a cylindrical shape having a diameter of 50 mm and a height of 45 mm with a mold, and then hydrostatically isostatically pressed at a pressure of 1.5 t / cm 2. Molded. Next, this molded body is heated to 1,100 ° C. in an argon atmosphere in a container filled with powdered coke and fired, and further in a graphitizing furnace in an argon stream at 2,800 ° C.
Was graphitized. Table 2 shows the physical properties of the obtained graphite material.
【００１３】比較例１〜２ コールタールピッチ及び石油系ピッチに炭素化助剤を添
加することなくか焼コークスを調製し、このか焼コーク
スを平均粒径４μｍに微粉砕した後、実施例１〜９と同
じ条件で、混練、粉砕、成型、焼成、黒鉛化して黒鉛材
を得た。得られたか焼コークスの組織の単位寸法及び黒
鉛材の物性を表１及び表２に示す。Comparative Examples 1-2 Calcined coke was prepared without adding a carbonization aid to coal tar pitch and petroleum pitch, and the calcined coke was finely pulverized to have an average particle size of 4 μm. Kneading, pulverizing, molding, firing, and graphitization under the same conditions as described above to obtain a graphite material. Tables 1 and 2 show the unit size of the structure of the obtained calcined coke and the physical properties of the graphite material.
【００１４】[0014]
【表１】 [Table 1]
【００１５】[0015]
【表２】 [Table 2]
【００１６】実施例１〜９と比較例１との比較から、コ
ールタールピッチに炭素化助剤として様々な官能基を有
する芳香族化合物を添加することにより、光学的異方性
組織サイズの小さなか焼コークスが得られることが判明
した。更に、これらのか焼コークスを使用して混練、粉
砕、成型、焼成、黒鉛化することにより、比較例の場合
よりも嵩密度が高く、かつ、機械的強度の高い黒鉛材が
得られることが判明した。実施例１〜９と比較例２との
比較から、石油系ピッチから得られたか焼コークスにお
いても組織のサイズを小さくすることは可能であるが、
本発明の炭素化助剤を添加した方が、組織サイズのより
小さなか焼コークスが得られることが判明した。また、
これらのか焼コークスを混練、粉砕、成型、焼成、黒鉛
化することによって、比較例より嵩密度が高く、機械的
強度の強いかつ高硬度黒鉛材の得られることも判明し
た。なお、表１に示す比較例２の結果から明らかなよう
に、組織のサイズを小さくするというだけの観点からは
コールタールピッチに代えて石油系ピッチを使用すれば
よいが、この場合には表２の結果から明らかなように本
願発明が目的とする高密度及び高強度の黒鉛材を得るこ
とができない。ところで、コールタールピッチを使用し
た場合に比べて石油系ピッチを使用した場合に組織のサ
イズが比較的小さくなるのは、コールタールピッチが芳
香族系であるのに対して石油系ピッチが脂肪族系であ
り、このためにこれらの間に重合反応性の差異が生じた
ためであると思われる。以上のような比較より、本発明
のか焼コークスを用いることによって、嵩密度が高く、
機械的強度に優れ、硬度の高い黒鉛材の得られることが
判明した。これは、表１からも分かる様に、本発明のか
焼コークスの光学的組織サイズが微細に制御されている
ことに起因しているものと思われる。つまり、か焼コー
クスの光学的組織サイズが微細化されることによって、
コークス自体の強度及び収縮性が向上し、黒鉛材の高密
度化及び高強度化等に大きく寄与したのであろうと考え
られる。From comparison between Examples 1 to 9 and Comparative Example 1, addition of aromatic compounds having various functional groups as a carbonization aid to coal tar pitch results in a small optically anisotropic texture size. It was found that calcined coke was obtained. Further, by kneading, pulverizing, molding, firing and graphitizing using these calcined cokes, it was found that a graphite material having a higher bulk density and higher mechanical strength than that of the comparative example can be obtained. did. From the comparison between Examples 1 to 9 and Comparative Example 2, it is possible to reduce the size of the structure even in the calcined coke obtained from petroleum pitch.
It has been found that the addition of the carbonization aid of the present invention produces a calcined coke having a smaller texture size. Also,
It was also found that by kneading, crushing, molding, firing and graphitizing these calcined cokes, a graphite material having a higher bulk density, higher mechanical strength and higher hardness than the comparative example can be obtained. As is clear from the results of Comparative Example 2 shown in Table 1, petroleum-based pitch may be used in place of coal tar pitch from the viewpoint of only reducing the size of the structure. As is clear from the result of No. 2, it is not possible to obtain the high-density and high-strength graphite material targeted by the present invention. By the way, compared to the case of using coal tar pitch, the size of the structure is relatively smaller when petroleum pitch is used, because coal tar pitch is aromatic while petroleum pitch is aliphatic. It is believed that this is due to the difference in the polymerization reactivity between these systems. From the above comparison, by using the calcined coke of the present invention, the bulk density is high,
It was found that a graphite material having excellent mechanical strength and high hardness can be obtained. It is considered that this is due to the fact that the optical texture size of the calcined coke of the present invention is finely controlled, as can be seen from Table 1. In other words, by refining the optical texture size of calcined coke,
It is considered that the strength and shrinkage of the coke itself were improved, and it may have contributed to the high density and high strength of the graphite material.
【００１７】[0017]
【発明の効果】本発明によれば、ピッチ含浸、再焼成と
いう工程を行うことなく、容易に高品質で広い範囲の用
途に適応し得る高密度で高強度かつ高硬度の黒鉛材を製
造することができる。According to the present invention, a high-density, high-strength and high-hardness graphite material which can be easily applied to a wide range of applications with high quality is manufactured without performing the steps of pitch impregnation and re-firing. be able to.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 山田 正弘 神奈川県川崎市中原区井田1618番地 新日 本製鐵株式会社先端技術研究所内 (72)発明者 向井 幸一郎 神奈川県川崎市中原区井田1618番地 新日 本製鐵株式会社先端技術研究所内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Masahiro Yamada 1618 Ida, Nakahara-ku, Kawasaki-shi, Kanagawa Inside Nippon Steel Corporation Advanced Technology Research Laboratories (72) Koichiro Mukai 1618 Ida, Nakahara-ku, Kawasaki-shi, Kanagawa Nippon Steel Corporation Advanced Technology Research Center
Claims (1)
して相溶性を有する芳香族化合物からなる炭素化助剤１
〜５０重量部を添加し、熱処理してか焼コークスを調製
し、次いでこのか焼コークスに結合材を添加して混練
し、更に粉砕し、成型後焼成を行って黒鉛化することを
特徴とする高密度、高強度黒鉛材の製造方法。1. A carbonization aid 1 comprising an aromatic compound compatible with a heavy oil in 100 parts by weight of the heavy oil.
˜50 parts by weight is added and heat treated to prepare a calcined coke, then a binder is added to the calcined coke, and the mixture is kneaded, further pulverized, and calcined after molding to graphitize. High-density, high-strength graphite material manufacturing method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3235735A JPH0551258A (en) | 1991-08-23 | 1991-08-23 | Production of high density and high strength graphite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3235735A JPH0551258A (en) | 1991-08-23 | 1991-08-23 | Production of high density and high strength graphite material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0551258A true JPH0551258A (en) | 1993-03-02 |
Family
ID=16990449
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3235735A Withdrawn JPH0551258A (en) | 1991-08-23 | 1991-08-23 | Production of high density and high strength graphite material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0551258A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005019097A (en) * | 2003-06-24 | 2005-01-20 | Nec Corp | Resin composition for cathode active material of secondary battery, carbon material for cathode active material, its manufacturing method, and secondary battery |
| CN115974065A (en) * | 2022-12-06 | 2023-04-18 | 昆明理工大学 | Method for preparing hard carbon material based on aromatized petroleum asphalt and application thereof |
| CN116496087A (en) * | 2023-05-22 | 2023-07-28 | 湖南大学 | Superfine structure special carbon material and preparation method thereof |
-
1991
- 1991-08-23 JP JP3235735A patent/JPH0551258A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005019097A (en) * | 2003-06-24 | 2005-01-20 | Nec Corp | Resin composition for cathode active material of secondary battery, carbon material for cathode active material, its manufacturing method, and secondary battery |
| JP4511811B2 (en) * | 2003-06-24 | 2010-07-28 | 日本電気株式会社 | Lithium ion secondary battery negative electrode active material resin composition, negative electrode active material carbon material, method for producing the same, and lithium ion secondary battery |
| CN115974065A (en) * | 2022-12-06 | 2023-04-18 | 昆明理工大学 | Method for preparing hard carbon material based on aromatized petroleum asphalt and application thereof |
| CN115974065B (en) * | 2022-12-06 | 2023-09-22 | 昆明理工大学 | Method for preparing hard carbon material based on aromatized petroleum asphalt and application thereof |
| CN116496087A (en) * | 2023-05-22 | 2023-07-28 | 湖南大学 | Superfine structure special carbon material and preparation method thereof |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A300 | Withdrawal of application because of no request for examination |
Free format text: JAPANESE INTERMEDIATE CODE: A300 Effective date: 19981112 |