JPH03281690A - Preparation of starting powder for carbonaceous material - Google Patents
Preparation of starting powder for carbonaceous materialInfo
- Publication number
- JPH03281690A JPH03281690A JP2084698A JP8469890A JPH03281690A JP H03281690 A JPH03281690 A JP H03281690A JP 2084698 A JP2084698 A JP 2084698A JP 8469890 A JP8469890 A JP 8469890A JP H03281690 A JPH03281690 A JP H03281690A
- Authority
- JP
- Japan
- Prior art keywords
- raw material
- product
- weight
- coal tar
- less
- 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.)
- Granted
Links
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 15
- 239000000843 powder Substances 0.000 title claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 32
- 239000011280 coal tar Substances 0.000 claims abstract description 17
- 238000010298 pulverizing process Methods 0.000 claims abstract 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 16
- 239000001301 oxygen Substances 0.000 claims description 16
- 229910052760 oxygen Inorganic materials 0.000 claims description 16
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 abstract description 8
- 239000000047 product Substances 0.000 description 29
- 238000009760 electrical discharge machining Methods 0.000 description 7
- 239000011347 resin Substances 0.000 description 7
- 229920005989 resin Polymers 0.000 description 7
- 238000000034 method Methods 0.000 description 5
- 238000000465 moulding Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000000571 coke Substances 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000011284 carbonization tar Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000011294 coal tar pitch Substances 0.000 description 1
- 238000009694 cold isostatic pressing Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000002931 mesocarbon microbead Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002006 petroleum coke Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000006253 pitch coke Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は高密度特殊炭素材として有用な原料粉の製造法
に関するものである。さらに詳しくは高密度でかつ放電
加工特性が良い特殊炭素材用原料粉の製造法に関するも
のである。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for producing raw material powder useful as a high-density special carbon material. More specifically, the present invention relates to a method for producing raw material powder for special carbon materials that has high density and good electrical discharge machining properties.
従来特殊炭素材はピッチコークス、及び石油コークスを
所定の割合に粒度配合した粒と粉を加熱、混合しながら
バインダーピンチを適当量添加ねつ合後、成形して製造
される。さらにこの生成形体を焼成、黒鉛化後、加工し
て製品である特殊炭素材を製造している。また、最近ピ
ンチを熱処理後、溶剤で処理して得たメソカーボンマイ
クロビーズを成形して特殊炭素材を製造する方法も報告
されている。Conventionally, special carbon materials are produced by heating and mixing grains and powder of pitch coke and petroleum coke in a predetermined ratio, adding an appropriate amount of binder pinch, kneading, and then molding. Furthermore, this formed body is fired, graphitized, and then processed to produce a special carbon material product. In addition, a method has recently been reported in which a special carbon material is produced by molding mesocarbon microbeads obtained by heat-treating pinches and then treating them with a solvent.
これらの方法は製品の嵩密度が低い、強度が低い等製品
の特性が不十分であり、また工程が複雑で製造コストが
高い等の課題があり、低コストで特性の良い特殊炭素材
の出現が望まれていた。These methods have problems such as insufficient product properties such as low bulk density and low strength, and complicated processes and high manufacturing costs.The emergence of special carbon materials with low cost and good properties. was desired.
又近年炭素材は放電加工用電極としての利用が注目され
、需要が急増の傾向にあるが従来の炭素材では放電加工
特性が不十分であり、もっと放電加工特性の良い炭素材
、特に放電加工時の消耗率が低い炭素材が要求されてい
る。またメソカーボンから製造した炭素材では工程が複
雑なためコストが高く、製造コストが低く高特性のもの
が求められている。In recent years, carbon materials have been attracting attention for their use as electrodes for electrical discharge machining, and demand is rapidly increasing. There is a need for carbon materials that have a low wear rate over time. Furthermore, carbon materials manufactured from mesocarbon are expensive due to complicated processes, and there is a demand for materials with low manufacturing costs and high properties.
そこで、本発明者は、かかる状況に鑑み、高強度でかつ
放電特性の良い特殊炭素材を製造すべく鋭意検討した結
果、コールタール系原料を熱処理しある特性を持つ原料
となし微粉砕して成形後、製品とすると高特性となるこ
とを見出し、本発明に到達した。Therefore, in view of this situation, the inventor of the present invention conducted intensive studies to produce a special carbon material with high strength and good discharge characteristics, and as a result, the inventor heat-treated a coal tar-based raw material to make it a raw material with certain characteristics, and finely pulverized it. It was discovered that the product has high properties after molding, and the present invention was achieved.
すなわち、本発明の要旨は、コールタール系原料を熱処
理して得られる生成物であり、コールタール系原料を熱
処理して得られる生成物であり、揮発分（ＶＭ）が２０
％以下で３％以上であり、該コールタール系原料よりの
酸素含有量の増加率が１．５重量％以内のものを微粉砕
することを微粉砕する炭素材用原料粉の製造法にある。That is, the gist of the present invention is a product obtained by heat-treating a coal tar-based raw material, which has a volatile content (VM) of 20
% or less and 3% or more, and the rate of increase in oxygen content from the coal tar-based raw material is within 1.5% by weight. .
以下、本発明の詳細な説明する。The present invention will be explained in detail below.
まず、本発明におけるコールタール系原料は、石炭乾留
時に副生ずるコールタール又はこれより得られるコール
タールピッチであり、ＶＭは３０重量％を超えてもよい
が３０重量％を超えると目標の物性に調整する時間が長
く、処理能力が落ち、コストが高くなるので該原料のＶ
Ｍは３０重量％以下が望ましい。First, the coal tar-based raw material in the present invention is coal tar produced as a by-product during coal carbonization or coal tar pitch obtained from this, and the VM may exceed 30% by weight, but if it exceeds 30% by weight, the target physical properties will not be achieved. The adjustment time is long, the processing capacity is reduced, and the cost is high.
M is desirably 30% by weight or less.
またこれらの原料はトルエン可溶分（ＴＳ）（Ｔ−レジ
ン量）が高過ぎると軽沸点留分が多く融着するために熱
処理効率が悪（該原料のＴレジン量は３０重量％以下が
望ましい。これらのコールタール系原料は通常コールタ
ールをデイレードコーカー、オートクレーブ等により３
５０〜４８０℃、１〜７２時間程度熱処理することでえ
られる。In addition, if the toluene soluble content (TS) (T-resin content) of these raw materials is too high, a large amount of light boiling point fractions will fuse, resulting in poor heat treatment efficiency (the T-resin content of the raw materials should be 30% by weight or less). Desirable.These coal tar-based raw materials are usually prepared by boiling coal tar in a delayed coker, autoclave, etc.
It can be obtained by heat treatment at 50 to 480°C for about 1 to 72 hours.
本発明において、コールタール系原料の熱処理は通常、
２００〜３５０℃、０．５〜４８時間程度で行われるが
、処理を均一に行なうために機械的エネルギーを付与し
た方が効果が大きい。機械エネルギーの種類としては撹
拌、超音波等が挙げられる。また熱処理は不活性ガス中
（アルゴン、窒素等）自生圧下で行なっても良いが、好
ましくは空気の存在下で行なわれる。In the present invention, the heat treatment of coal tar-based raw materials is usually carried out by
The treatment is carried out at 200 to 350° C. for about 0.5 to 48 hours, but it is more effective to apply mechanical energy to ensure uniform treatment. Types of mechanical energy include stirring, ultrasonic waves, and the like. Further, the heat treatment may be performed in an inert gas (argon, nitrogen, etc.) under autogenous pressure, but is preferably performed in the presence of air.
本発明において目的とする熱処理生成物は、ＶＭが３重
量％以上、２０重量％以下であって、コールタール系原
料よりの酸素含有量の増加率が１゜５！量％以内の生成
物である。The target heat-treated product of the present invention has a VM of 3% by weight or more and 20% by weight or less, and has an increase rate of 1.5% in oxygen content from the coal tar-based raw material. % of the product.
該熱処理生成物のＶＭが２０％を超えると焼成時の重量
減少が大き過ぎ特性が低化し、３％未満では焼結性が低
下する。また該熱処理生成物の酸素量が多いと該生成物
内の焼結成分が減少するため成形体の特性が悪化する。If the VM of the heat-treated product exceeds 20%, the weight loss during firing is too large and the properties deteriorate, while if it is less than 3%, the sinterability deteriorates. Moreover, if the amount of oxygen in the heat-treated product is large, the sintered components in the product will decrease, resulting in deterioration of the properties of the molded product.
特に該原料より１．５重量％を超えて酸素量が増加する
と特性が悪くなるので該原料より酸素の増加量が１５重
量％以内のものが用いられる。また該熱処理生成物の酸
素含有量は３重量％以下が望ましい。In particular, if the amount of oxygen increases by more than 1.5% by weight compared to the raw material, the properties deteriorate, so a material in which the amount of oxygen increased by more than 15% by weight compared to the raw material is used. Further, the oxygen content of the heat-treated product is preferably 3% by weight or less.
また上記のコールタール系原料の熱処理物は、これを粉
砕して平均粒度１５〜２０μとした時のＴＳ量が１０重
量％以下でありかつ１重量％以上であるのが好ましい。Further, it is preferable that the heat-treated product of the above-mentioned coal tar-based raw material has a TS amount of 10% by weight or less and 1% by weight or more when pulverized to an average particle size of 15 to 20μ.
ＴＳ量を１０重量％以下とすることにより成形体焼成時
の発泡割れの傾向が低下し、また１重量％以上とするこ
とにより焼結特性が向上する。By setting the TS amount to 10% by weight or less, the tendency for foam cracking during firing of the compact is reduced, and by setting the TS amount to 1% by weight or more, the sintering properties are improved.
ついで、上記熱処理物を微粉砕して原料粉を得る。良好
な成形品を得るためには原料粉の平均粒度は５０μ以下
が望ましいが製品組織の均一性をさらムこ向上させるた
めには好ましくは３０μ以下、さらに好ましくは２０μ
以下、最も好ましくは１０μ以下に微粉砕したが望まし
い。成形は通常のモールド成形、冷間等方圧成形等が用
いられる。Next, the heat-treated product is pulverized to obtain raw material powder. In order to obtain a good molded product, the average particle size of the raw material powder is preferably 50μ or less, but in order to improve the uniformity of the product structure, it is preferably 30μ or less, more preferably 20μ.
Hereinafter, it is most preferably finely pulverized to 10 μm or less. For forming, ordinary molding, cold isostatic pressing, etc. are used.
また焼成は不活性ガス中、コークスプリーズ中いずれも
可能であり、８００〜１０００℃の温度でなされる。さ
らに黒鉛化はタンマン炉、アチソン炉、誘導加熱等によ
る常法が使用でき、通常２０００〜３０００℃でなされ
る。Further, the calcination can be carried out either in an inert gas or in a coke pleat, and is carried out at a temperature of 800 to 1000°C. Further, graphitization can be carried out by conventional methods such as a Tammann furnace, an Acheson furnace, or induction heating, and is usually carried out at a temperature of 2000 to 3000°C.
Ｃ実施例〕
以下、本発明を実施例によりさらに詳細に説明する。な
お実施例中、「％」は「重量％」を意味する。C Example] Hereinafter, the present invention will be explained in more detail with reference to Examples. In the Examples, "%" means "% by weight".
実施例Ｉ
ＶＭが２０．６％でかつＴレジン量が２１．１％のコー
ルタール系原料を空気の存在下で機械エネルギーを付与
しながら約２５０℃、７０分で熱処理を行なった。生成
物のＶＭは１３．６％であり、γレジン量は５．０％で
あった。また生成物中の酸素含有量は１．７％であり、
原料（１，２％）よりの酸素含有量は０．５％であった
。この生成物を微粉砕し、平均粒度２６μとし、モール
ドブレスにて成形し、成形体を得た。この成形体を酸化
防止のためコークスプリーズ中１０００℃まで焼成後、
アチソン炉で２８００℃まで黒鉛化して製品を得た。Example I A coal tar-based raw material having a VM of 20.6% and a T resin amount of 21.1% was heat-treated at about 250° C. for 70 minutes while applying mechanical energy in the presence of air. The VM of the product was 13.6% and the amount of gamma resin was 5.0%. In addition, the oxygen content in the product is 1.7%,
The oxygen content from the raw material (1.2%) was 0.5%. This product was finely pulverized to an average particle size of 26 μm, and molded using a mold press to obtain a molded product. After baking this molded body to 1000℃ in coke pleat to prevent oxidation,
The product was graphitized to 2800°C in an Acheson furnace.
黒鉛成形体の嵩密度は１．９２であり、放電加工時の消
耗率は０．３％であった。The bulk density of the graphite molded body was 1.92, and the consumption rate during electrical discharge machining was 0.3%.
実施例２
ＶＭ２１．４％、ｒ ２２．９％のコールタール系原料
を約２３０℃、１８０分で熱処理してＶＭ１４゜０％、
γレジン量５．１％のものを得た。生成物の酸素含有量
は１．８％であり、原料（１，２％）より酸素増加量は
０．６％であった。この生成物を微粉砕し平均粒度３２
μとし、実施例１と同様の方法で成形体を製造した。そ
の嵩密度は１．９２、放電加工時の消耗率は０．５％で
あった。Example 2 A coal tar-based raw material with a VM of 21.4% and an r of 22.9% was heat-treated at about 230°C for 180 minutes to obtain a VM of 14°0% and
A product containing 5.1% of γ resin was obtained. The oxygen content of the product was 1.8%, and the oxygen increase was 0.6% compared to the raw material (1.2%). This product was pulverized with an average particle size of 32
μ, and a molded body was produced in the same manner as in Example 1. Its bulk density was 1.92, and its wear rate during electrical discharge machining was 0.5%.
比較例１
実施例１と同じ原料を熱処理してＶＭ１４．６％、γレ
ジン量６．０％のものを得た。生成物の酸素含有量は３
．５％であり、原料（１，２％）よりの酸素増加量は２
．３％であった。この生成物を微粉砕し平均粒度２５μ
とし、実施例１と同様の方法で成形体を製造した。その
嵩密度は１．７７、放電加工時の消耗率は４．５％であ
った。Comparative Example 1 The same raw material as in Example 1 was heat-treated to obtain one with a VM of 14.6% and a γ resin content of 6.0%. The oxygen content of the product is 3
．． 5%, and the increase in oxygen from the raw material (1,2%) is 2
．． It was 3%. This product was finely pulverized with an average particle size of 25 μm.
A molded article was produced in the same manner as in Example 1. Its bulk density was 1.77, and its wear rate during electrical discharge machining was 4.5%.
比較例２
実施例２と同じ原料を熱処理してＶＭが１４．４％、Ｔ
レジン量が７．４％のものを得た。生成物の酸素含有量
は３．８％であり、原料（１，２％）よりの酸素増加量
は２．６％であった。この生成物を微粉砕し平均粒度３
０μとし、実施例１と同様の方法で成形体を製造した。Comparative Example 2 The same raw material as in Example 2 was heat-treated to have a VM of 14.4% and a T
A product with a resin content of 7.4% was obtained. The oxygen content of the product was 3.8%, and the oxygen increase from the raw material (1.2%) was 2.6%. This product was pulverized with an average particle size of 3
A molded body was manufactured in the same manner as in Example 1, with the molded body having a diameter of 0μ.
その嵩密度は１．７８、放電加工時の消耗率は９．８％
であった。Its bulk density is 1.78, and the wear rate during electrical discharge machining is 9.8%.
Met.
比較例３
市販品の嵩密度、放電加工時の消耗率を同時に測定した
らそれぞれ１．８４．４．４％であった。Comparative Example 3 The bulk density and wear rate during electrical discharge machining of a commercially available product were simultaneously measured and found to be 1.84% and 4.4%, respectively.
本発明の方法による原料粉を用いた炭素材は嵩密度が高
く、放電加工特性（消耗率が低い）が非常に良い。The carbon material using the raw material powder produced by the method of the present invention has a high bulk density and very good electric discharge machining characteristics (low wear rate).
Claims (3)
であり、揮発分が２０重量％以下で３重量％以上であり
、かつ該コールタール系原料よりの酸素含有量の増加率
が１．５重量％以内のものを微粉砕することを特徴とす
る炭素材用原料粉の製造法。(1) A product obtained by heat-treating a coal tar-based raw material, with a volatile content of 20% by weight or less and 3% by weight or more, and an increase rate of oxygen content from the coal tar-based raw material of 1. A method for producing raw material powder for carbon materials, which comprises finely pulverizing a powder containing less than 5% by weight.
を微粉砕する請求項１記載の製造法。(2) The manufacturing method according to claim 1, wherein a heat-treated product having an oxygen content of 3% by weight or less is pulverized.
ン可溶分が１０重量％以下で１重量％以上であるものを
微粉砕する請求項１記載の製造法。(3) The production method according to claim 1, wherein the heat-treated product has an average particle size of 15 to 20 microns and has a toluene soluble content of 10% by weight or less and 1% by weight or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2084698A JP2924061B2 (en) | 1990-03-30 | 1990-03-30 | Production method of raw material powder for carbon material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2084698A JP2924061B2 (en) | 1990-03-30 | 1990-03-30 | Production method of raw material powder for carbon material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03281690A true JPH03281690A (en) | 1991-12-12 |
| JP2924061B2 JP2924061B2 (en) | 1999-07-26 |
Family
ID=13837887
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2084698A Expired - Lifetime JP2924061B2 (en) | 1990-03-30 | 1990-03-30 | Production method of raw material powder for carbon material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2924061B2 (en) |
-
1990
- 1990-03-30 JP JP2084698A patent/JP2924061B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JP2924061B2 (en) | 1999-07-26 |
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