JPS60238387A - Production of pitch for carbonaceous material - Google Patents
Production of pitch for carbonaceous materialInfo
- Publication number
- JPS60238387A JPS60238387A JP9192384A JP9192384A JPS60238387A JP S60238387 A JPS60238387 A JP S60238387A JP 9192384 A JP9192384 A JP 9192384A JP 9192384 A JP9192384 A JP 9192384A JP S60238387 A JPS60238387 A JP S60238387A
- Authority
- JP
- Japan
- Prior art keywords
- pitch
- heat treatment
- thin film
- carbonaceous
- pressure
- 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
Abstract
Description
【発明の詳細な説明】
本発明は炭素材用ピッチの製造方法に関し、詳しくは原
料ピッチから効率よく炭素繊維の製造等に好適な良質の
炭素材用ピッチを製造する方法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for manufacturing pitch for carbon materials, and more particularly, to a method for efficiently manufacturing pitch for carbon materials of high quality suitable for manufacturing carbon fibers etc. from raw material pitch.
プラスチックや金属の複合材料として知られている炭素
繊維は、従来ポリアクリロニトリルの繊維を焼成して製
造されてきたが、原料繊維が高価である上、焼成時の炭
化収率が低いという問題があった。このため近年ではピ
ッチを原料とする炭素繊維の製法が数多く提案されてい
る。例えば、原料ピッチを熱処理してメソ相ピッチ含量
の高い炭素材用ピッチを製造するに際して、攪拌槽、管
形反応器などを用いて行なう方法などが提案されている
。しかし、攪拌槽を用いる方法では、反応において広い
滞在時間分布関数を有し、また、容積効率が低いため、
コーキングを誘発するという欠点がある。Carbon fiber, which is known as a composite material for plastics and metals, has traditionally been produced by firing polyacrylonitrile fibers, but the raw material fibers are expensive and the carbonization yield during firing is low. Ta. For this reason, in recent years, many methods for producing carbon fiber using pitch as a raw material have been proposed. For example, methods have been proposed in which pitch for carbon materials having a high mesophase pitch content is produced by heat-treating raw pitch, using a stirring tank, a tubular reactor, or the like. However, the method using a stirred tank has a wide residence time distribution function in the reaction and has low volumetric efficiency.
It has the disadvantage of inducing caulking.
また、管形反応器では、その半径方向に大きな温度分布
および、濃度分布が発生し、生成物が不均質化するとい
う問題がある。このように、炭素材用ピッチの効率の良
い製造方法は未だ知られていない。Further, in a tubular reactor, a large temperature distribution and concentration distribution occur in the radial direction, resulting in a problem that the product becomes inhomogeneous. As described above, an efficient method for producing pitch for carbon materials is not yet known.
そこで本発明者らは上記問題点を解消した炭素材用ピッ
チの製造方法を開発すべく鋭意研究した結果、原料ピッ
チを薄膜蒸発器を用いて特定の条件下で熱処理すると、
効率良く炭素材用ピンチが得られることを見い出し、こ
の知見に基づいて本発明を完成した。Therefore, the present inventors conducted extensive research to develop a method for producing pitch for carbon materials that solved the above problems. When the raw material pitch was heat-treated under specific conditions using a thin film evaporator,
It was discovered that a pinch for carbon material can be obtained efficiently, and the present invention was completed based on this knowledge.
すなわち本発明は炭素質ピッチを熱処理して炭素材用ピ
ッチを製造するにあたり、炭素質ピッチを薄膜蒸発器に
導入し、不活性ガスまたは非酸化性ガスの存在下で温度
４００〜５５０℃、圧力０．１〜５９ｍｍ ＨＨにおい
て熱処理することを特徴とする炭素材用ピンチの製造方
法（以下、第１発明とする。）および炭素質ピッチを熱
処理して炭素材用ピンチを製造するにあたり、炭素質ピ
ッチを不活性ガスまたは非酸化性ガスの存在下で二段階
の熱処理を行なうとともに、第一段目の熱処理を温度４
００〜４５０℃、圧力１０〜５Ｑａ＋ｓ＋ Ｈｇの条件
で行ない、かつ第二段目の熱処理を温度４５０〜５５０
℃、圧力０．１〜５ｍｍＨｇの条件で薄膜蒸発器内にて
行なうことを特徴とする炭素材用ピンチの製造方法（以
下、第２発明とする。）を提供するものである。That is, in producing pitch for carbon materials by heat treating carbonaceous pitch, the present invention introduces the carbonaceous pitch into a thin film evaporator and heats the carbonaceous pitch at a temperature of 400 to 550°C and a pressure in the presence of an inert gas or non-oxidizing gas. A method for manufacturing a pinch for carbon material characterized by heat treatment at 0.1 to 59 mm HH (hereinafter referred to as the first invention), and a method for manufacturing a pinch for carbon material by heat treating carbonaceous pitch. The pitch is subjected to a two-step heat treatment in the presence of an inert gas or non-oxidizing gas, and the first heat treatment is carried out at a temperature of 4.
The second stage heat treatment is carried out at a temperature of 00 to 450°C and a pressure of 10 to 5Qa+s+Hg, and a temperature of 450 to 550°C.
The present invention provides a method for manufacturing a pinch for carbon material (hereinafter referred to as the second invention), characterized in that the manufacturing method is carried out in a thin film evaporator under conditions of temperature of 0.1 to 5 mmHg and pressure of 0.1 to 5 mmHg.
本発明における原料の炭素質ピッチとしては、石油系２
石炭系、ナフタリンピンチなど純物質ピンチを用いるこ
とができる。石油系ピッチとしては石油留分の接触分解
残油、ナフサ等の熱分解残油なと芳香族炭化水素含量の
高いものが好適に用いられる。通常は、このような炭素
質ピンチを予め減圧蒸留して、沸点約４００℃以下の軽
質油分を留去した残油を原料ピンチとして用いる。なお
、減圧蒸留するにあたり、予めフィルター等により炭素
質ピンチ中の灰分を除去しておくことが好ましい。The raw material carbonaceous pitch in the present invention is petroleum-based 2
Pure substance pinches such as coal-based and naphthalene pinches can be used. As the petroleum-based pitch, pitches having a high content of aromatic hydrocarbons, such as catalytic cracking residues of petroleum fractions, thermal cracking residues such as naphtha, etc., are suitably used. Usually, such a carbonaceous pinch is previously distilled under reduced pressure to remove light oil components having a boiling point of about 400° C. or less, and the residual oil is used as the raw material pinch. In addition, in performing vacuum distillation, it is preferable to remove the ash content in the carbonaceous pinch using a filter or the like in advance.
第１発明においては、上記の如き原料ピンチを薄膜蒸発
器中にて一段で熱処理することを特徴としている。この
薄膜蒸発器とは、通常の蒸発処理において用いられるも
のであれば特に制限はなく種々のタイプのものを使用す
ることができ、たて型でも横型でもよく、回転羽根が壁
面と接触して掻き取る型のものでもよい。このうち、特
に薄膜遠心蒸発器が好適である。薄膜蒸発器は液膜表面
をたえず回転羽根で膜面が更新されるので揮発分の蒸散
が促進されるものである。回転羽根の羽根が２〜１６枚
程度のものが通常用いられ、回転数は種々の条件により
決定されるがｌＯ〜５００ｒｐｍ程度で良い。The first invention is characterized in that the raw material pinch as described above is heat treated in one stage in a thin film evaporator. There are no particular restrictions on this thin film evaporator, as long as it is used in normal evaporation processing, and various types can be used. A scraping type may also be used. Among these, a thin film centrifugal evaporator is particularly suitable. In a thin film evaporator, the surface of the liquid film is constantly renewed by rotating blades, so that the evaporation of volatile matter is promoted. A rotating blade having about 2 to 16 blades is usually used, and the rotation speed is determined depending on various conditions, but may be about 10 to 500 rpm.
薄膜蒸発器で原料ピンチを熱処理する場合、得られるピ
ッチの酸化による劣化等を防止するため、不活性ガスあ
るいは非酸化性ガスの存在下で行なわなければならない
。ここで不活性ガスとしては、ネオン、ヘリウム、アル
ゴン、窒素等であり、非酸化性ガスとしてはメタン、エ
タンなどが挙げられる。When heat treating a pinch of raw material in a thin film evaporator, it must be carried out in the presence of an inert gas or a non-oxidizing gas in order to prevent the resulting pitch from deteriorating due to oxidation. Here, examples of the inert gas include neon, helium, argon, nitrogen, etc., and examples of the non-oxidizing gas include methane, ethane, etc.
第１発明の方法では、薄膜蒸発器を不活性ガスあるいは
非酸化性ガス雰囲気下におき、ここへ原料ピッチを導入
し、一段にて熱処理を行なう。この際の熱処理条件とじ
ｔは、液膜の厚さ、すなわち器壁と回転羽根のクリアラ
ンスあるいは原料ピッチの組成などにより適宜選択され
るものであるが、温度４００〜５５０℃、好ましくは４
２０〜５００℃、圧力０．１〜５’ＱｍｍＨｇ 、、好
ましくは０．５〜１０ｍｍ ＨＨの範囲から選択すれば
よい。ここで温度が低すぎたり、あるいは圧力が高すぎ
ると、炭素質ピ・ノ千〇熱改良速度が抑制され、また軽
質分の除去が不十分となって、炭素材用ピッチの品質の
低下を招くことになる。逆に温度が高すぎると炭素質ピ
ッチがコーキングを起こすようになり、圧力が低すぎる
と炭素材用ピンチの収率低下を招くほか真空装置を大型
化する必要があり、設備費および動力費の増大を招き好
ましくない。液膜の厚さは、クリアランスの調節により
種々選択できるが、効率などの点より通常は０〜１０ｍ
ｍ、好ましくは０．５〜３ＩｌｌＩＩ＋程度の範囲で行
なわれる。ここで、クリアランスが零の場合は掻き取り
型となり、このタイプでは遠心力あるいはバネにより回
転羽根を壁面に回転羽根の回転速度によって調節するこ
とができ、原料の性状や反応条件により、０．１〜６０
分間の範囲で制御することができる。In the method of the first invention, a thin film evaporator is placed in an inert gas or non-oxidizing gas atmosphere, raw material pitch is introduced therein, and heat treatment is performed in one step. The heat treatment conditions at this time are appropriately selected depending on the thickness of the liquid film, that is, the clearance between the vessel wall and the rotary blade, or the composition of the raw material pitch.
It may be selected from the range of 20 to 500°C, pressure 0.1 to 5'QmmHg, preferably 0.5 to 10mm HH. If the temperature is too low or the pressure is too high, the rate of thermal improvement of carbonaceous pitch will be suppressed, and the removal of light components will be insufficient, resulting in a decrease in the quality of pitch for carbonaceous materials. I will invite you. On the other hand, if the temperature is too high, the carbonaceous pitch will cause coking, and if the pressure is too low, the yield of carbon material pinch will decrease and the vacuum equipment will need to be larger, which will reduce equipment and power costs. This is undesirable because it leads to increase. The thickness of the liquid film can be variously selected by adjusting the clearance, but from the viewpoint of efficiency etc. it is usually 0 to 10 m.
m, preferably in the range of about 0.5 to 3IllII+. Here, if the clearance is zero, it will be a scraping type, and in this type, the rotation speed of the rotary blade can be adjusted by centrifugal force or a spring against the wall surface, and depending on the properties of the raw material and reaction conditions, 0.1 ~60
Can be controlled in a range of minutes.
このような熱処理を行なって得られる炭素材用ピッチは
、原料性状や操作条件を選択することによって、等方性
相、メソ相のいずれかを主とする炭素材用ピッチを得る
ことができるが、炭素繊維用とする場合には実質的にメ
ソ相の含有量が１００％のものが好適である。The pitch for carbon materials obtained through such heat treatment can be made to have either an isotropic phase or a meso phase as its main component by selecting the raw material properties and operating conditions. When used for carbon fibers, it is preferable that the mesophase content is substantially 100%.
次に第２発明について説明する。Next, the second invention will be explained.
この第２発明は前述の原料ピッチを用いて行なわれるが
、より組成的にトルエン不溶分が多いものを用いた場合
にも、好適な炭素材用ピッチが得られるものである。Although the second invention is carried out using the above-mentioned raw material pitch, a suitable pitch for carbon materials can also be obtained when using a material having a composition with a higher content of toluene insolubles.
この発明は二段の熱処理を行ない、第二段目の熱処理を
薄膜蒸発器で行なうことを特徴としている。This invention is characterized in that a two-stage heat treatment is performed, and the second stage heat treatment is performed in a thin film evaporator.
まず、第一段目の熱処理は、キノリンネ溶分ならびにピ
リジン不溶分を低下させ、メソ相ピッチ含量を増加させ
ることを目的としている。第一段目の熱処理は攪拌槽反
応器、管形反応器、薄膜蒸発器などで行なうことができ
るが、特に第１発明で述べた如き薄膜蒸発器で行なうこ
とが好ましい。First, the purpose of the first heat treatment is to reduce the quinoline-soluble content and the pyridine-insoluble content, and increase the mesophase pitch content. The first stage heat treatment can be carried out in a stirred tank reactor, a tubular reactor, a thin film evaporator, etc., but it is particularly preferable to carry out the heat treatment in a thin film evaporator as described in the first invention.
薄膜蒸発器のなかでも、薄膜遠心蒸発器により好適に行
なわれる。熱処理は、温度４００〜４５０℃。Among thin film evaporators, a thin film centrifugal evaporator is preferably used. The heat treatment is performed at a temperature of 400 to 450°C.
好ましくは４１０〜４５０℃、圧力１０〜５０ＩＩＩＩ
ｎＨｇ、好ましくは１０〜４Ｑ＋ｎｍ Ｈｇで行なう。Preferably 410-450°C, pressure 10-50III
It is carried out at nHg, preferably 10-4Q+nm Hg.
圧力が上記範囲よりも高すぎると軽質分の揮発が抑制さ
れ、重質化速度の低下を招き、圧力が低すぎると炭素材
用ピンチの収率低下を招（。一方、温度が上記範囲より
も低すぎると、反応速度が低下し、温度が高すぎると、
キノリンネ溶分が第一段反応器で生成するため好ましく
ない。熱処理は通常、前述の如き不活性ガスあるいは非
酸化性ガスの存在下で行なわれる。If the pressure is too high than the above range, the volatilization of light components will be suppressed, leading to a decrease in the rate of weighting, and if the pressure is too low, the yield of carbon material pinch will decrease (on the other hand, if the temperature is higher than the above range) If the temperature is too low, the reaction rate will decrease, and if the temperature is too high,
This is not preferable because a quinoline solution is generated in the first stage reactor. The heat treatment is usually carried out in the presence of an inert gas or non-oxidizing gas as described above.
第一段目の熱処理は、メソ相ピッチ含量がθ〜３０重量
％程度であり、かつ生成ピンチ中のトルエン不溶分が０
〜７０重量％、好ましくはＩＯ〜６０重景％となるよう
時間などの条件を選択して行なうことが好ましい。In the first heat treatment, the mesophase pitch content is approximately θ ~ 30% by weight, and the toluene insoluble content in the produced pinch is 0.
It is preferable to select conditions such as time so that the weight ratio is ~70% by weight, preferably IO ~60% by weight.
第２発明ではこのようにして得られたピンチを、さらに
第二段目の熱処理を行なって高品質のメソ相ピッチを得
る。In the second invention, the pinch thus obtained is further subjected to a second heat treatment to obtain a high quality mesophase pitch.
第二段目の熱処理は第１発明で述べた薄膜蒸発器で行な
われ、特に薄膜遠心蒸発器で行なうことが好ましい。熱
処理は温度４５０〜５５０℃、好ましくは４６０〜５０
０℃、圧力０．１〜５Ｉｌ１ｗｌＨｇ、好ましくは０．
５〜５＋＋＋ｍＨｇの範囲内で、原料の性状により、器
壁と回転羽根のクリアランスや回転羽根の回転数、原料
供給量を調整することにより行なえばよい。The second stage heat treatment is carried out in the thin film evaporator mentioned in the first invention, and is particularly preferably carried out in the thin film centrifugal evaporator. Heat treatment at a temperature of 450 to 550°C, preferably 460 to 50°C
0°C, pressure 0.1-5Il1wlHg, preferably 0.
This may be carried out within the range of 5 to 5+++ mHg by adjusting the clearance between the vessel wall and the rotary blade, the rotation speed of the rotary blade, and the amount of raw material supplied depending on the properties of the raw material.
圧力が高すぎると、炭素質ピンチの熱改質速度が抑制さ
れ、また軽質分の除去が不十分となって、炭素材用ピッ
チの品質の低下を招くことになる。If the pressure is too high, the rate of thermal modification of the carbonaceous pinch will be suppressed, and the removal of light components will be insufficient, resulting in a deterioration in the quality of the pitch for carbon materials.
逆に、温度が高すぎると炭素質ピッチがコーキングを起
こすようになり、圧力が低すぎると炭素材用ピンチの収
率低下を招くばか真空装置を大型化する必要があり、設
備費および動力費の増大を招き、好ましくない。熱処理
は前述の如き、不活性ガスあるいは非酸化性ガスの存在
下で行なわれる。また、滞留時間分布はできるだけ狭い
方がよい。On the other hand, if the temperature is too high, the carbonaceous pitch will cause coking, and if the pressure is too low, the yield of carbonaceous pitch will decrease, and the vacuum equipment will need to be larger, increasing equipment and power costs. This is undesirable as it leads to an increase in The heat treatment is performed in the presence of an inert gas or non-oxidizing gas as described above. Further, it is better that the residence time distribution be as narrow as possible.
このようにして得られるピンチは実質的にメソ相ピッチ
を１００％含有するもので、分子量分布も狭く、軟化点
の高いピッチであり、炭素材用ピンチとして極めて好適
である。The pinch thus obtained contains substantially 100% mesophase pitch, has a narrow molecular weight distribution, and has a high softening point, making it extremely suitable as a pinch for carbon materials.
このように第１発明および第２発明において得られるピ
ンチは、炭素繊維の製造の他、炭素フィルム、フィラメ
ント、ヤーンなど各種炭素製品の製造に有効に利用する
ことができる。As described above, the pinch obtained in the first invention and the second invention can be effectively used for manufacturing carbon fibers as well as various carbon products such as carbon films, filaments, and yarns.
本発明によって得られた実質的にメソ相１００％のピン
チからピンチ系炭素繊維を製造するには常法によりまず
このピンチを紡糸し、次いで不融化処理し、さらに焼成
すればよい。In order to produce pinch-based carbon fibers from the essentially 100% mesophase pinch obtained by the present invention, the pinch may be first spun by a conventional method, then subjected to infusibility treatment, and then fired.
以上、第１発明および第２発明によれば、原料ピッチの
熱改質に要する時間を短縮でき、コーキングの抑制が図
れ、実質的にメソ相ピッチを１００％含有する炭素材用
ピンチを効率良く製造することができる。また、第２発
明においては、第二段目の熱処理を厳しい条件で行なう
ため、比較的分子量分布が狭く、紡糸性が良好で、軟化
点も高く、不融化時間も短いピンチが得られる。As described above, according to the first and second inventions, the time required for thermal modification of raw material pitch can be shortened, coking can be suppressed, and pinches for carbon materials containing substantially 100% mesophase pitch can be efficiently produced. can be manufactured. Further, in the second invention, since the second stage heat treatment is performed under severe conditions, a pinch having a relatively narrow molecular weight distribution, good spinnability, a high softening point, and a short infusibility time can be obtained.
このように本発明は炭素材用ピッチの製造において極め
て有用である。As described above, the present invention is extremely useful in producing pitch for carbon materials.
次に本発明を実施例により、さらに詳しく説明する。Next, the present invention will be explained in more detail with reference to Examples.
実施例１
石油系残油より得た炭素質ピッチをフィルターで固形分
を除去し、横型の薄膜蒸発器に導入し、窒素気流下に平
均滞留時間３０分間として熱処理を行なった。原料ピッ
チのトルエン不溶分は１２ｗｔ％であり、熱処理温度は
４５０℃、圧力は１０ｍｍＨｇとした。この蒸発器は器
壁と回転羽根のクリアランスが零の掻き取り型であり、
回転羽根の回転数は２０Ｏｒｐｍとした。この結果得ら
れた炭素材用ピンチは、メソ相含量が９３％であり、ピ
リジン不溶分は３５ｗｔ％、数平均分子量１０８０．軟
化点３００℃であった。次にこの炭素材用ピンチを３４
５℃において溶融紡糸し、直径１１μのピッチ繊維を得
た。このピッチ繊維は、空気中において３００℃で３０
分間不融化処理した後、アルゴン雰囲気下１５００℃で
１０分間焼成処理することにより炭素繊維を得た。得ら
れた炭素繊維の引張強度は２３５ｋｇ／ｍｍ”であり、
また弾性率は２５ｔ／ｍｍ”であった。Example 1 Carbonaceous pitch obtained from petroleum residual oil was filtered to remove solid content, introduced into a horizontal thin film evaporator, and heat-treated under a nitrogen stream for an average residence time of 30 minutes. The toluene insoluble content of the raw pitch was 12 wt%, the heat treatment temperature was 450°C, and the pressure was 10 mmHg. This evaporator is a scraped type with zero clearance between the vessel wall and the rotating blades.
The rotation speed of the rotating blade was 20 rpm. The resulting pinch for carbon material has a mesophase content of 93%, a pyridine insoluble content of 35 wt%, and a number average molecular weight of 1080. The softening point was 300°C. Next, use this carbon material pinch
Melt spinning was performed at 5° C. to obtain pitch fibers with a diameter of 11 μm. This pitch fiber is heated at 300°C in air.
After infusibility treatment for 1 minute, carbon fibers were obtained by firing treatment at 1500° C. for 10 minutes in an argon atmosphere. The tensile strength of the obtained carbon fiber was 235 kg/mm'',
Further, the elastic modulus was 25 t/mm''.
実施例２
重質軽油の接触分解装置から得られた接触分解残油をフ
ィルターにより灰分除去し、ついで減圧蒸留により軽質
留分を留去した残油を攪拌槽に導入し、４２０℃、 １
０ｍｍ Ｈｇにおいて１時間熱処理し、生成物中のトル
エン不溶分（Ｊ Ｉ Ｓ−に−２４２５）の含量が３５
重量％のピッチを得た。次いで得られたピッチをギヤー
ポンプにより薄膜遠心蒸発器に導入して、窒素ガス流通
下に４６０℃、ｌｍｍＨｇにおいて熱処理を行なった。Example 2 A catalytic cracking residual oil obtained from a heavy gas oil catalytic cracking apparatus was filtered to remove ash, and then the residual oil from which light fractions were removed by vacuum distillation was introduced into a stirring tank and heated at 420°C.
After heat treatment at 0 mm Hg for 1 hour, the content of toluene insoluble matter (JIS-2425) in the product was 35
Weight percent pitch was obtained. Next, the obtained pitch was introduced into a thin film centrifugal evaporator using a gear pump, and heat-treated at 460° C. and lmmHg under nitrogen gas flow.
薄膜遠心蒸発器は回転羽４１４枚を有するもので、回転
数１００ｒｐＨとして、羽根と器壁のクリアランスは０
．５ｍｍ 、滞留時間は１２分の条件で行なった。The thin film centrifugal evaporator has 414 rotating blades, and the rotation speed is 100 rpm, and the clearance between the blades and the vessel wall is 0.
．． The test was carried out under conditions of 5 mm and a residence time of 12 minutes.
このようにして、メソ相ピンチ１００％であり、キノリ
ンネ溶分２１％、数平均分子量１２００、軟化点３１０
℃の炭素材用ピッチを得た。In this way, the mesophase pinch is 100%, the quinoline soluble content is 21%, the number average molecular weight is 1200, and the softening point is 310.
℃ pitch for carbon material was obtained.
次に、得られたピッチを３４０℃において直径７μの繊
維に紡糸し、空気中３００℃において２０分間不融化処
理した後、アルゴン雰囲気下に１５００℃で１０分間焼
成することにより、炭素繊維を得た。Next, the obtained pitch was spun into fibers with a diameter of 7μ at 340°C, infusible in air at 300°C for 20 minutes, and then fired at 1500°C for 10 minutes in an argon atmosphere to obtain carbon fibers. Ta.
得られた炭素繊維の引張強度２９０ｋｇ／ｍｍ２、弾性
率２７ｔ／＋ｎｍ”であった。The obtained carbon fiber had a tensile strength of 290 kg/mm 2 and an elastic modulus of 27 t/+nm.
Claims (3)
するにあたり、炭素質ピッチを薄膜蒸発器に導入し、不
活性ガスまたは非酸化性ガスの存在下で温度４００〜５
５０℃、圧力０．１〜５０ｍｍ Ｈｇにおいて熱処理す
ることを特徴とする炭素材用ピンチの製造方法。(1) When producing pitch for carbon materials by heat-treating carbonaceous pinch, carbonaceous pitch is introduced into a thin film evaporator and heated to 400 to 500℃ in the presence of an inert gas or non-oxidizing gas.
A method for manufacturing a pinch for carbon material, characterized by heat treating at 50°C and a pressure of 0.1 to 50 mm Hg.
するにあたり、炭素質ピッチを不活性ガスまたは非酸化
性ガスの存在下で二段階の熱処理を行なうとともに、第
一段目の熱処理を温度４００〜４５０℃、圧力１０〜５
０ｍｍ Ｈｇの条件で行ない、かつ第二段目の熱処理を
温度４５０〜５５０℃、圧力０．１〜５ｍｍＨｇの条件
で薄膜蒸発器内にて行なうことを特徴とする炭素材用ピ
ッチの製造方法。(2) When manufacturing pinches for carbon materials by heat treating carbonaceous pitch, the carbonaceous pitch is subjected to two stages of heat treatment in the presence of an inert gas or non-oxidizing gas, and the first stage heat treatment is Temperature 400-450℃, pressure 10-5
A method for producing pitch for a carbon material, characterized in that the second stage heat treatment is carried out in a thin film evaporator at a temperature of 450 to 550°C and a pressure of 0.1 to 5 mmHg.
求の範囲第２項記載の製造方法。(3) The manufacturing method according to claim 2, wherein the first stage heat treatment is performed in a thin film evaporator.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9192384A JPS60238387A (en) | 1984-05-10 | 1984-05-10 | Production of pitch for carbonaceous material |
| DE3509861A DE3509861C2 (en) | 1984-03-26 | 1985-03-19 | Pitch material for a carbon-containing molded body and process for its manufacture |
| GB08507267A GB2156378B (en) | 1984-03-26 | 1985-03-20 | Pitch materials |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9192384A JPS60238387A (en) | 1984-05-10 | 1984-05-10 | Production of pitch for carbonaceous material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60238387A true JPS60238387A (en) | 1985-11-27 |
| JPH0315954B2 JPH0315954B2 (en) | 1991-03-04 |
Family
ID=14040100
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9192384A Granted JPS60238387A (en) | 1984-03-26 | 1984-05-10 | Production of pitch for carbonaceous material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60238387A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62116688A (en) * | 1985-11-18 | 1987-05-28 | Mitsubishi Chem Ind Ltd | Manufacture of carbon fiber spinning pitch |
| WO1989000618A2 (en) * | 1987-07-21 | 1989-01-26 | Didier Engineering Gmbh | Process and device for manufacturing anisotropic carbon fibres |
| US5091072A (en) * | 1987-06-18 | 1992-02-25 | Maruzen Petrochemical Co., Ltd. | Process for preparing pitches |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4933571A (en) * | 1972-07-26 | 1974-03-28 | ||
| JPS51521A (en) * | 1974-06-24 | 1976-01-06 | Kureha Chemical Ind Co Ltd | Pitsuchino shoshitsukahoho |
| JPS5238855A (en) * | 1975-09-22 | 1977-03-25 | Nec Corp | Error correcting unit |
| JPS5887187A (en) * | 1981-11-18 | 1983-05-24 | Nippon Oil Co Ltd | Raw pitch for carbon fiber |
| JPS5887188A (en) * | 1981-11-18 | 1983-05-24 | Nippon Oil Co Ltd | Raw pitch for carbon fiber |
| JPS58142974A (en) * | 1982-02-18 | 1983-08-25 | Mitsubishi Petrochem Co Ltd | Mesophase pitch and preparation of carbon fiber using it |
| JPS58214531A (en) * | 1982-06-08 | 1983-12-13 | Agency Of Ind Science & Technol | Preparation of pitch for producing pitch type carbon fiber |
-
1984
- 1984-05-10 JP JP9192384A patent/JPS60238387A/en active Granted
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4933571A (en) * | 1972-07-26 | 1974-03-28 | ||
| JPS51521A (en) * | 1974-06-24 | 1976-01-06 | Kureha Chemical Ind Co Ltd | Pitsuchino shoshitsukahoho |
| JPS5238855A (en) * | 1975-09-22 | 1977-03-25 | Nec Corp | Error correcting unit |
| JPS5887187A (en) * | 1981-11-18 | 1983-05-24 | Nippon Oil Co Ltd | Raw pitch for carbon fiber |
| JPS5887188A (en) * | 1981-11-18 | 1983-05-24 | Nippon Oil Co Ltd | Raw pitch for carbon fiber |
| JPS58142974A (en) * | 1982-02-18 | 1983-08-25 | Mitsubishi Petrochem Co Ltd | Mesophase pitch and preparation of carbon fiber using it |
| JPS58214531A (en) * | 1982-06-08 | 1983-12-13 | Agency Of Ind Science & Technol | Preparation of pitch for producing pitch type carbon fiber |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62116688A (en) * | 1985-11-18 | 1987-05-28 | Mitsubishi Chem Ind Ltd | Manufacture of carbon fiber spinning pitch |
| JPH0635580B2 (en) * | 1985-11-18 | 1994-05-11 | 三菱化成株式会社 | Method for producing spinning pitch for carbon fiber |
| US5091072A (en) * | 1987-06-18 | 1992-02-25 | Maruzen Petrochemical Co., Ltd. | Process for preparing pitches |
| WO1989000618A2 (en) * | 1987-07-21 | 1989-01-26 | Didier Engineering Gmbh | Process and device for manufacturing anisotropic carbon fibres |
| GR880100059A (en) * | 1987-07-21 | 1989-04-12 | Didier Eng | A process and apparatus for producing anisotropic carbon fibres |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0315954B2 (en) | 1991-03-04 |
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