【発明の詳細な説明】本発明は、コールタール及びコールタールピッチ（以下
コールタールをもって両者を代表させる）の処理法に関
し、更に詳しくは、コールタールを熱処理した後、高温
遠心分離することによシ得た十ノリン不溶分（以下単に
Ｑ１分という）の含有量が極めて少ないか或いはＱ１分
を実質的に含有しないピッチを原料として、ニードルコ
ークスを製造する方法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for treating coal tar and coal tar pitch (hereinafter referred to as coal tar). The present invention relates to a method for producing needle coke using the obtained pitch which has an extremely low content of tenorine insoluble content (hereinafter simply referred to as Q1 content) or substantially no Q1 content as a raw material.
コールタールを出発原料としてニードルコークスの如き
高品質の炭素材料を製造する場合には、コールタール中
の不純物であるＱ１分を出来るだけ除去しておく必要が
ある。このＱ１分は、０．３μｍ以下の炭素質微粒子（
通常−次Ｑ１分と呼ばれる）でらシ・コールタール中に
要員に含まれている場合には、コールタールの熱処理工
程において、通常二次Ｑ１分と呼ばれるメソフェース（
球晶）の表面に付着して球晶の合体を妨げ、球晶の円滑
な成長を阻害するものと推測されている。When producing a high quality carbon material such as needle coke using coal tar as a starting material, it is necessary to remove as much as possible the impurity Q1 in the coal tar. This Q1 minute is based on carbonaceous fine particles of 0.3 μm or less (
In the heat treatment process of coal tar, mesophase (usually called secondary Q1 min) is included in the coal tar.
It is speculated that it adheres to the surface of spherulites and prevents their coalescence, thereby inhibiting their smooth growth.
このためコールタール中の一次Ｑ１分を除去することの
重要性は、従来から認識されておシ、例えば、次の様な
方法が実施されてｂる。即ち、コールタールと相互に溶
解性の悪い油、例えば、石油系軽質油をコールタールに
添加して一次Ｑ１分を凝集沈殿させ、−次Ｑ１分の粒径
を大とした後、静置によシ肥大した一次Ｑ１分を沈降分
離させる方法がおる（特開昭５２−２８５０１号公報）
。For this reason, the importance of removing the primary Q1 component in coal tar has been recognized for a long time, and for example, the following methods have been implemented. That is, oil that has poor solubility with coal tar, such as petroleum-based light oil, is added to coal tar to coagulate and precipitate the primary Q1 to increase the particle size of the secondary Q1, and then allowed to stand still. There is a method of sedimentation and separation of the enlarged primary Q1 (Japanese Unexamined Patent Publication No. 52-28501).
.
この方法においては、−次Ｑ１分分離後の清澄液を蒸留
することによシ、有用成分マあるタール及び／又はピッ
チを収得するとともに添加した油分を回収する必要があ
り、この際、大量の熱エネル千−を必要とするのみなら
ず、有用成分の収率も低下する。更に、蒸留により回収
された油分は、添加した石油系油分とコールタールに由
来する石炭系油分との混合物であシ、そのままでは利用
価値は低い。一方、静置により分離された沈降相は、多
量の石油系油分を含むので、回収処理を行なわない場合
には添加油の回収率が低くなシ、また回収処理を行なう
場合には蒸留塔、タンク類等の設備が必要となる。更に
また、添加する石油系軽中質油保存用の大型タンクやそ
の他の付随設備類も必要でおり、その為の広大な設置場
所も必要となる。In this method, it is necessary to obtain the useful components tar and/or pitch and to recover the added oil by distilling the clear liquid after the 1-minute separation. Not only does this require thousands of thermal energy, but the yield of useful components is also reduced. Furthermore, the oil recovered by distillation is a mixture of the added petroleum oil and the coal oil derived from coal tar, and has low utility value as it is. On the other hand, since the sedimentation phase separated by standing still contains a large amount of petroleum-based oil, the recovery rate of added oil will be low if no recovery treatment is performed, and if recovery treatment is performed, a distillation column, Equipment such as tanks is required. Furthermore, a large tank for storing the petroleum-based light and medium oil to be added and other accompanying equipment are also required, and a vast installation space is also required for this purpose.
本発明者は、従来法の上記の如き問題点を解消若しくれ
軽減すべく種々研究を重ねた結果、コールタールを熱処
理した後、特定条件下に高温遠心分離に供する場合には
、熱処理によシー次Ｑ１分が凝集してその見掛けの粒子
径が大となるので、遠心分離効果が著しく高くなり、−
次ＱＩ分が極めて容易に高効率で分離除去されることを
見出した。そして、遠心分離によシ生成する清澄液とし
てのピッチを常法に従ってコークス化処理する場合には
、高品質のニードルコークスが得られることも見出され
た。本発明は、この様な新知見に基いて完成されたもの
である。As a result of various studies aimed at solving or alleviating the above-mentioned problems of conventional methods, the inventors of the present invention have found that, after heat-treating coal tar, when subjecting it to high-temperature centrifugation under specific conditions, heat treatment is necessary. As the particles aggregate and their apparent particle size increases, the centrifugation effect becomes significantly higher, and -
It has been found that the next QI fraction can be separated and removed very easily and with high efficiency. It has also been found that high-quality needle coke can be obtained when pitch, which is a clarified liquid produced by centrifugation, is coked in accordance with a conventional method. The present invention was completed based on such new knowledge.
即ち、本発明は、コールタールを温度３００〜５００℃
、圧力常圧〜２０ｋｌ／ｄ−Ｇの条件下に０．５〜５０
時間熱処理した後、温度１５０〜４５０°Ｃで遠心分離
処理し、得られる清澄液を常法によシ加熱処理してニー
ドルコークスを製造することを特徴とするコールタール
の処理法に係る。That is, in the present invention, coal tar is heated to a temperature of 300 to 500°C.
, 0.5 to 50 under normal pressure to 20kl/dG
The present invention relates to a method for treating coal tar, which is characterized in that after heat treatment for a period of time, centrifugation treatment is performed at a temperature of 150 to 450°C, and the resulting clear liquid is heat treated in a conventional manner to produce needle coke.
以下添附図面に示すフローシートを参照しつつ、本発明
を更に詳細に説明する。The present invention will be described in more detail below with reference to the flow sheets shown in the accompanying drawings.
第１図において、原料コールタールは）タンク（１）か
らライン（３）を経て脱水塔（５）に送られ、ここで得
られた脱水タールは、ライン（９）を経て熱処理装置（
ロ）に送られ、熱処理される。熱処理は、通常温度３０
０〜５００℃、圧力常圧〜２０に９／ｃｄ−Ｇの条件下
に０．５〜５０時間行なう。この熱処理によシ熱処理物
中に二次ＱＩ分が形成され、この表面に一次Ｑ１分が付
着することによって見掛妙の粒子径が増大するので、後
記の高温遠心分離による一次及び二次ＱＩ分の分離除去
が容易となる。In Fig. 1, the raw material coal tar is sent from the tank (1) through the line (3) to the dehydration tower (5), and the dehydrated tar obtained here is sent through the line (9) to the heat treatment equipment (
b) and heat treated. Heat treatment is usually performed at a temperature of 30
It is carried out under the conditions of 0 to 500°C and a pressure of normal pressure to 20 to 9/cd-G for 0.5 to 50 hours. Due to this heat treatment, a secondary QI component is formed in the heat-treated material, and the apparent particle size increases as the primary Q1 component adheres to the surface of the heat-treated material. This makes it easy to separate and remove the components.
熱処理装置０１で得られた熱処理反応生成物拡、必要な
らば１ライパＪ、Ｑ４１を通って蒸留塔（至）に供給さ
れ、常法に従って低沸点留分をライ：Ｊ（ロ）から除か
れた後、ラインａ呻から遠心分離機（２）に送られる。The heat-treated reaction product obtained in heat treatment equipment 01 is expanded and, if necessary, passed through 1 Lyper J and Q41 and fed to the distillation column (2), and the low boiling point fraction was removed from Lyper J (2) according to a conventional method. After that, it is sent to the centrifuge (2) from line a.
蒸留を必要としない場合には、熱処理反応生成物は、熱
処理装置（ロ）からライニア（至）、鱒及び鵠を経て遠
心分離機ｅ◇に送られる。遠心分離時の温度は、１５０
〜４５０°Ｃである。温度が１５０℃未満の場合には、
ＱＩ分の除去が充分に行なわれ難くなう、一方４５０℃
を上回る場合には、被処理物の熱分解によるガス発生や
変質を生じる傾向が増大する。遠心分離時の温度は、２
５０〜４００℃の範囲内がより好ましい。遠心分離機と
しては、上記温度範囲内で操作可能な各種形式の装置が
使用可能でおる。遠心力は、通常５００〜５０００Ｇ程
度であシ、２０００〜４５００Ｇ程度とすることがよシ
好ましす。ＱＩ分の除去率は、原料コールタールの性状
、最終製品に要求される性状等に応じて、適宜定めれば
良い。例えば、ＱＩ分３．５％のコールタールからニー
ドルコークスを製造する為には、９１分除去率を９０％
以上とすることが好ましい。When distillation is not required, the heat-treated reaction product is sent from the heat treatment device (b) to the centrifuge e◇ via the liner (to), trout and goose. The temperature during centrifugation was 150
~450°C. If the temperature is less than 150℃,
On the other hand, at 450°C, it becomes difficult to remove the QI component sufficiently.
If it exceeds 20%, there is an increased tendency for gas generation and deterioration due to thermal decomposition of the material to be treated. The temperature during centrifugation is 2
The temperature is more preferably within the range of 50 to 400°C. As the centrifuge, various types of devices that can be operated within the above temperature range can be used. The centrifugal force is usually about 500 to 5000G, preferably about 2000 to 4500G. The removal rate of the QI component may be determined as appropriate depending on the properties of the raw material coal tar, the properties required of the final product, etc. For example, to produce needle coke from coal tar with a QI of 3.5%, the removal rate must be 90% in 91 minutes.
It is preferable to set it as above.
遠心分離機（ロ）においてライ：ｌ翰からＱＩ分（−次
Ｑ１分十二次Ｑ１分）を除去された生成物（じとして取
シ出される。ニードルコークス製造装置（財）としては
、公知のディレードクーカー及びカルサイナーからなる
ものを代表例として挙けることが出来る。ニードルコー
クス化の条件としては、公知の条件をそのまま採用する
ことが出来、例えば１じツチをディレートコ−カー中４
００〜５００°Ｃ，４〜１０ｋｌ／ｄの条件下に２４〜
４８時間かけて炭素化し、次いでカルサイチー中１２０
０〜１４００°Ｃで仮焼することにょシ残存する揮発分
を除去してニードルコークスを得る。In the centrifuge (b), the QI component (-Q1 min. 12th Q1 min.) is removed from the rye:l and the product is taken out as the product. A typical example is one consisting of a delayed coker and a calciner.For the conditions of needle coking, known conditions can be used as they are; for example, one
00~500°C, 24~10 kl/d
Carbonized for 48 hours, then 120 hrs.
Needle coke is obtained by calcining at 0 to 1400°C to remove residual volatile matter.
−次Ｑ１分及び二次Ｑ１分を実質的に除去されたコール
タールピッチから得られる本発明のニードルコークスは
、例えば電極用炭素材料として優れた性能を発揮する。The needle coke of the present invention, which is obtained from coal tar pitch from which primary Q1 and secondary Q1 are substantially removed, exhibits excellent performance as, for example, a carbon material for electrodes.
実施例１脱水タール（−次Ｑ１分２重量％）を温度３８５℃、圧
力３ ｋＱ／ｄ −Ｇの条件下に１３．８時間熱処理し
、得られた熱処理反応生成物を高温遠心分離に供してＱ
１分を除去した軟ピツチを得た。Example 1 Dehydrated tar (2 wt. TeQ
A soft pitch with 1 minute removed was obtained.
遠心分離機としては、保有容量４０ｊの横型遠心分離機
を使用し、回転数３０００ ｒｌｔｎ、遠心力２２８０
Ｇ、温度２７０°Ｃ１処理量１ｅａｎ／ｈｒの条件下に
操作した。得られた軟ピツチの性状を第１表に示す。軟
ピツチの収率は、脱水タール基準で７５％であった。A horizontal centrifuge with a holding capacity of 40J was used as the centrifuge, with a rotation speed of 3000 rltn and a centrifugal force of 2280.
G, the operation was carried out under conditions of a temperature of 270° C. and a throughput of 1 ean/hr. The properties of the obtained soft pitch are shown in Table 1. The yield of soft pitch was 75% based on dehydrated tar.
第 １ 表次いで、得られた軟ピツチを温度４７０℃、圧力６．３
ｋｇ／ｄ、ｃ；の条件下に炭素化して生コークスを得た
後、これを１４００℃で仮焼して、かさ密度２．１３の
ニードルコークスを製造した。次いで、該ニードルコー
クスをパインターじツチとともに直径１６ｆｆＸ長さ１
３０１ｆＮに成型し、２７００°Ｃで黒鉛化処理を行な
った。得られた電極じ−スの性能を従来品の性能ととも
に第２表に示す。Table 1 Next, the obtained soft pitch was heated at a temperature of 470°C and a pressure of 6.3°C.
After carbonizing to obtain raw coke under the conditions of kg/d, c;, this was calcined at 1400° C. to produce needle coke with a bulk density of 2.13. Next, the needle coke and pinter joint were placed in a container with a diameter of 16ff and a length of 1
It was molded to 301 fN and graphitized at 2700°C. The performance of the obtained electrode base is shown in Table 2 along with the performance of the conventional product.
第 ２ 表Table 2
第１図は、本発明方法の概要を示すフローシートである
。（１）・・・コールタールタンク、（５）・・・脱水搭
、（ロ）・・・熱処理装置、ｏす・・・蒸留塔、（ハ）
・・・遠心分離機、■・・・ニードルコークス製造装置
。Ｃ以 上）FIG. 1 is a flow sheet showing an overview of the method of the present invention. (1) Coal tar tank, (5) Dehydration tower, (b) Heat treatment equipment, osu... distillation column, (c)
...Centrifugal separator, ■...Needle coke production equipment. C or above)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15865783AJPS6049084A (en) | 1983-08-29 | 1983-08-29 | Method for treating coal tar or coal tar pitch |
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15865783AJPS6049084A (en) | 1983-08-29 | 1983-08-29 | Method for treating coal tar or coal tar pitch |
| Publication Number | Publication Date |
|---|---|
| JPS6049084Atrue JPS6049084A (en) | 1985-03-18 |
| JPH0149315B2 JPH0149315B2 (en) | 1989-10-24 |
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP15865783AGrantedJPS6049084A (en) | 1983-08-29 | 1983-08-29 | Method for treating coal tar or coal tar pitch |
| Country | Link |
|---|---|
| JP (1) | JPS6049084A (en) |
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62124188A (en)* | 1985-11-26 | 1987-06-05 | Nippon Steel Chem Co Ltd | Method for producing coal-based needle coke |
| JPS63210187A (en)* | 1987-02-27 | 1988-08-31 | Nippon Steel Chem Co Ltd | Method for producing coal-based needle pitch coke |
| JP2002274444A (en)* | 2001-03-19 | 2002-09-25 | Tokyu Car Corp | Pole trailer safety equipment |
| US10080473B2 (en) | 2009-03-13 | 2018-09-25 | Omachron Intellectual Property Inc. | Hand vacuum cleaner |
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4916528A (en)* | 1972-06-05 | 1974-02-14 | ||
| JPS4943103A (en)* | 1972-09-04 | 1974-04-23 | ||
| JPS5941387A (en)* | 1982-08-30 | 1984-03-07 | Osaka Gas Co Ltd | Manufacture of quinoline-insoluble free-pitch |
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4916528A (en)* | 1972-06-05 | 1974-02-14 | ||
| JPS4943103A (en)* | 1972-09-04 | 1974-04-23 | ||
| JPS5941387A (en)* | 1982-08-30 | 1984-03-07 | Osaka Gas Co Ltd | Manufacture of quinoline-insoluble free-pitch |
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62124188A (en)* | 1985-11-26 | 1987-06-05 | Nippon Steel Chem Co Ltd | Method for producing coal-based needle coke |
| JPS63210187A (en)* | 1987-02-27 | 1988-08-31 | Nippon Steel Chem Co Ltd | Method for producing coal-based needle pitch coke |
| JP2002274444A (en)* | 2001-03-19 | 2002-09-25 | Tokyu Car Corp | Pole trailer safety equipment |
| US10080473B2 (en) | 2009-03-13 | 2018-09-25 | Omachron Intellectual Property Inc. | Hand vacuum cleaner |
| Publication number | Publication date |
|---|---|
| JPH0149315B2 (en) | 1989-10-24 |
| Publication | Publication Date | Title |
|---|---|---|
| JPH0340076B2 (en) | ||
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