JPH02296897A - Production of raw material for high-density, high-strength carbon material - Google Patents
Production of raw material for high-density, high-strength carbon materialInfo
- Publication number
- JPH02296897A JPH02296897A JP11727289A JP11727289A JPH02296897A JP H02296897 A JPH02296897 A JP H02296897A JP 11727289 A JP11727289 A JP 11727289A JP 11727289 A JP11727289 A JP 11727289A JP H02296897 A JPH02296897 A JP H02296897A
- Authority
- JP
- Japan
- Prior art keywords
- density
- raw material
- pitch
- solvent
- strength
- 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
- 239000002994 raw material Substances 0.000 title claims abstract description 15
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 11
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 239000011280 coal tar Substances 0.000 claims abstract description 4
- 239000011295 pitch Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 4
- 238000005194 fractionation Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 6
- 239000011269 tar Substances 0.000 abstract description 5
- 230000007423 decrease Effects 0.000 abstract description 2
- 239000011331 needle coke Substances 0.000 abstract description 2
- 238000005087 graphitization Methods 0.000 abstract 1
- 239000007770 graphite material Substances 0.000 description 9
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- 238000000605 extraction Methods 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 239000011294 coal tar pitch Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000009760 electrical discharge machining Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000011329 calcined coke Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011316 heat-treated pitch Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011301 petroleum pitch Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〈産業上の利用分野〉
本発明は放電加工用電極、治具類、るつぼ、あるいは原
子力用炉壁材などに用いられる高密度高強度炭素材料用
原料の製造方法に関するものである。[Detailed Description of the Invention] <Industrial Application Field> The present invention relates to a method for producing raw materials for high-density, high-strength carbon materials used for electrical discharge machining electrodes, jigs, crucibles, nuclear reactor wall materials, etc. It is something.
〈従来の技術〉
炭素質メソフェーズ小球体とはコールタールピッチや石
油ピッチ類を３５０〜５００℃の温度で加熱する際に光
学的等方性ピッチ中に生成するメソフェーズ小球体をい
う、この小球体は溶剤分別法によりピッチマトリックス
中から分離され等方性・高密度・高強度黒鉛材料用の原
料となることはよく知られている０例えば特公昭６０−
２５３６４号公報によれば、小球体を溶剤分別する際に
ベンゼン、タール中油等のピッチに対して若干抽出力の
弱い溶剤を使用することにより、ピッチ中のβ成分の一
部をメソフェーズ小球体と共に残存させ、しかる後に不
活性雰囲気中において２００〜４５０℃の温度で仮焼処
理することにより、自己焼結性の優れた原料となること
が示されている。<Prior art> Carbonaceous mesophase spherules are mesophase spherules that are generated in optically isotropic pitch when coal tar pitch or petroleum pitch is heated at a temperature of 350 to 500°C. It is well known that it is separated from the pitch matrix by a solvent fractionation method and becomes a raw material for isotropic, high-density, and high-strength graphite materials.
According to Publication No. 25364, a part of the β component in the pitch is extracted together with the mesophase spherules by using a solvent such as benzene or oil in tar that has a slightly weak extraction power for the pitch when separating the spherules with a solvent. It has been shown that by allowing the material to remain and then calcining it at a temperature of 200 to 450° C. in an inert atmosphere, a raw material with excellent self-sintering properties can be obtained.
この方法により得られた原料を使用すればバインダーを
使用することなく成形、焼成、黒鉛化することにより嵩
密度が１．８５ｇ／ｃｊ以上、曲げ強度が８００ｋｇ／
ｃＪ以上の高密度・高強度・等方性黒鉛材が容易に製造
可能である。しかしながら、上記炭素質メソフェーズ小
球体は木質的に黒鉛化性の椰れた材料でないため、得ら
れる黒鉛材料は高市度・高強度であるものの一方で硬度
、熱膨張係数。If the raw material obtained by this method is used, it can be molded, fired, and graphitized without using a binder, resulting in a bulk density of 1.85 g/cj or more and a bending strength of 800 kg/cj.
High-density, high-strength, and isotropic graphite materials with cJ or higher can be easily manufactured. However, since the above-mentioned carbonaceous mesophase spherules are not woody and graphitizable, the resulting graphite material has high marketability and strength, but has low hardness and thermal expansion coefficient.
電気比抵抗等も大きいという特徴をもっている。It is characterized by high electrical specific resistance.
このため、その大きな硬度のために機械加工性が悪く加
工に手間がかかる。またその大きな熱膨張係数のために
ＳＩＣ被覆が難しいといった問題が住している。Therefore, due to its high hardness, it has poor machinability and requires time and effort to process. Further, due to its large coefficient of thermal expansion, it is difficult to coat it with SIC.
〈発明が解決しようとする課題〉
本発明の目的は、メソフェーズ小球体単独を成型−焼成
−黒鉛化して得られる黒鉛材に比べ高密度・高強度は維
持して、かつ黒鉛化性を改善し、硬度、熱膨張係数及び
電気比抵抗を小さくすることを可能にした高密度高強度
炭素材料用原料の製造方法を提供することである。<Problems to be Solved by the Invention> The purpose of the present invention is to maintain high density and high strength and improve graphitizability compared to a graphite material obtained by molding, firing, and graphitizing mesophase small spheres alone. Another object of the present invention is to provide a method for producing a raw material for a high-density, high-strength carbon material that makes it possible to reduce hardness, coefficient of thermal expansion, and specific electrical resistance.
＜！！Ｉ！題を解決するための手段〉
本発明は、コールタール等のピッチ類を熱処理してメソ
フェーズ小球体を生成させたのち、これにカーボン粉末
をメソフェーズ小球体（キノリン不溶分） １００ｆ
ｆｉ量部に対して５〜１００重量部添加・混合し、つい
でこれら混合物を溶剤分別し、仮焼処理することを特徴
とする高密度高強度炭素材料用原料の製造方法である。<! ! I! Means for Solving the Problem> The present invention heat-treats pitch such as coal tar to generate mesophase small spheres, and then adds carbon powder to the mesophase small spheres (quinoline insoluble content).
This is a method for producing a raw material for a high-density, high-strength carbon material, which is characterized by adding and mixing 5 to 100 parts by weight with respect to the amount of fi, and then separating the mixture with a solvent and calcining it.
く作 川〉
コールタール等のピッチ類を熱処理してメソフェーズ小
球体を生成するためには、前述した特公昭６Ｏ−２５３
Ｇ４号公報に開示されているように、ピッチ類を３５０
〜５００℃の温度にて加熱処理すればよい。Kusaku Kawa> In order to generate mesophase spherules by heat-treating pitches such as coal tar, the above-mentioned Japanese Patent Publication No. 6 O-253
As disclosed in G4 publication, the pitches are 350
What is necessary is just to heat-process at the temperature of -500 degreeC.
次にメソフェーズ小球体を生成させた熱処理ピッチに対
し°ζ、人造黒鉛粉末、天然黒鉛粉末、針状コークス粉
末等の黒鉛化性の優れたカーボン粉末をメソフェーズ小
球体（キノリン不溶分量）１００重量部に対し５〜１０
０重景部の滑部で添加・混合する。Next, 100 parts by weight of carbon powder with excellent graphitizability such as artificial graphite powder, natural graphite powder, needle coke powder, etc. 5-10 against
Add and mix in the smooth part of the 0-layered part.
添加・混合量が５重量部未満であると混合の効果が小さ
く、混合粉を成型−焼成−黒鉛化して製造される黒鉛材
の硬度、熱膨張係数、電気比抵抗等を小さくする割合が
小さい、一方ｔｏｏｆｆｔＩｔ部超であると黒鉛材の密
度・強度等が低下するという問題が生じる。従って、カ
ーボン粉末の添加量はメソフェーズ小球体（キノリン不
溶分） １００重量部に対し５〜１００重量部に限定
される。If the amount added/mixed is less than 5 parts by weight, the mixing effect will be small, and the ratio of reducing the hardness, thermal expansion coefficient, electrical resistivity, etc. of the graphite material produced by molding, firing, and graphitizing the mixed powder will be small. On the other hand, if it exceeds toofftIt, a problem arises in that the density, strength, etc. of the graphite material decreases. Therefore, the amount of carbon powder added is limited to 5 to 100 parts by weight per 100 parts by weight of mesophase microspheres (quinoline insoluble matter).
続いて、タール中油等の溶剤を用いて粘結成分となるβ
成分と共にピッチマトリックス中からこれらメソフェー
ズ小球体、カーボン粉末を分別する。溶剤としてはピッ
チ中のβ成分を残留させるためにベンゼン、タール中油
等のピッチに対して若干抽出力の弱い溶剤を使用するこ
とが好ましい。Next, β is made into a viscous component using a solvent such as oil in tar.
These mesophase spherules and carbon powder are separated from the pitch matrix together with the components. As the solvent, in order to leave the β component in the pitch, it is preferable to use a solvent that has a slightly weak extraction power against the pitch, such as benzene or oil in tar.
さらに仮焼処理を行い、焼結性の調整を行う。Further, calcination treatment is performed to adjust sinterability.
仮焼処理は不活性雰囲気中で２００〜４５０°Ｃの温度
で加熱することが望ましい。Preferably, the calcination treatment is performed at a temperature of 200 to 450°C in an inert atmosphere.
このようにして自己焼結性にも優れる均一な高密度・高
強度・炭素材用原料が製造される。In this way, a uniform high-density, high-strength raw material for carbon material with excellent self-sintering properties is produced.
次に只体的実施例で本発明をさらに詳細に説明する。The present invention will now be explained in more detail by way of exemplary embodiments.
〈実施例〉
コールタールピッチを４５０℃で熱処理してメソフェー
ズ小球体を発生させた０次に該熱処理ピッチ中のメソフ
ェーズ小球体（キノリン不溶分！！ｔ）１００重量部に
対して平均粒子径５ｐ−の仮焼コークスを表１に示す割
合で添加・混合後、タール中油を用いて抽出・濾過を行
い、得られた濾過残留物を引き続き３６０℃で３時間不
活性ガス雰囲気下で仮焼処理を行い、炭素材用原料を製
造した。<Example> Coal tar pitch was heat-treated at 450°C to generate mesophase spherules, and the average particle size was 5p per 100 parts by weight of mesophase spherules (quinoline insoluble!!t) in the heat-treated pitch. - After adding and mixing the calcined coke in the ratio shown in Table 1, extraction and filtration are performed using oil in tar, and the resulting filtration residue is subsequently calcined at 360°C for 3 hours under an inert gas atmosphere. A raw material for carbon material was produced.
次にこの原料を９００ｋｇ／ｃｊの圧力で１００φＸ６
０ｈｓｓサイズに冷間静水圧（ＣＩＰ）成型し、ついで
コークスプリーズ中ｌＯ°Ｃ／ｈｒの昇温速度で１００
０°Ｃまで焼成した。さらにこの焼成体を２５００”Ｃ
の温度で黒鉛化処理した。各々の黒鉛材の物理特性を表
１に示す。Next, this raw material was heated to 100φX6 at a pressure of 900kg/cj.
Cold isostatic pressure (CIP) molding to 0 hss size, then 100 °C at a heating rate of 10°C/hr in coke pleat.
It was baked to 0°C. Furthermore, this fired body was heated to 2500"C.
It was graphitized at a temperature of . Table 1 shows the physical properties of each graphite material.
本発明法の原料で製造した黒鉛材は高密度・高強度でし
かも、硬度、電気比抵抗、熱膨張係数が低く、ＳｉＣ被
覆に適した黒鉛材が得られた。The graphite material produced using the raw material of the method of the present invention has high density and high strength, and has low hardness, electrical resistivity, and coefficient of thermal expansion, and is suitable for SiC coating.
〈発明の効果〉
本発明の炭素材料用原料から製造される黒鉛材は高密度
・高強度でかつ、硬度、熱膨張係数、電気比抵抗等が低
く、放電加工用電極、治具類、るつぼあるいは原子力用
炭素材の原料として好適である。<Effects of the Invention> The graphite material produced from the raw material for carbon materials of the present invention has high density, high strength, and low hardness, thermal expansion coefficient, electrical resistivity, etc., and is suitable for electrical discharge machining electrodes, jigs, crucibles, etc. Alternatively, it is suitable as a raw material for carbon materials for nuclear power use.
Claims (1)
球体を生成させたのち、これにカーボン粉末をメソフェ
ーズ小球体（キノリン不溶分）１００重量部に対して５
〜１００重量部添加・混合し、ついでこれら混合物を溶
剤分別し、仮焼処理することを特徴とする高密度高強度
炭素材料用原料の製造方法。After heat-treating pitches such as coal tar to generate mesophase spherules, carbon powder was added to the mesophase spherules at a rate of 5 parts by weight per 100 parts by weight of the mesophase spherules (quinoline insoluble content).
A method for producing a raw material for a high-density, high-strength carbon material, which comprises adding and mixing ~100 parts by weight, followed by solvent fractionation of the mixture and calcining treatment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11727289A JPH02296897A (en) | 1989-05-12 | 1989-05-12 | Production of raw material for high-density, high-strength carbon material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11727289A JPH02296897A (en) | 1989-05-12 | 1989-05-12 | Production of raw material for high-density, high-strength carbon material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02296897A true JPH02296897A (en) | 1990-12-07 |
Family
ID=14707653
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11727289A Pending JPH02296897A (en) | 1989-05-12 | 1989-05-12 | Production of raw material for high-density, high-strength carbon material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02296897A (en) |
-
1989
- 1989-05-12 JP JP11727289A patent/JPH02296897A/en active Pending
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