JPS60152569A - Novel carbon black - Google Patents

Novel carbon black

Info

Publication number
JPS60152569A
JPS60152569A JP59006928A JP692884A JPS60152569A JP S60152569 A JPS60152569 A JP S60152569A JP 59006928 A JP59006928 A JP 59006928A JP 692884 A JP692884 A JP 692884A JP S60152569 A JPS60152569 A JP S60152569A
Authority
JP
Japan
Prior art keywords
carbon black
carbon
surface area
specific surface
furnace
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
Application number
JP59006928A
Other languages
Japanese (ja)
Inventor
Toshibumi Nishii
俊文 西井
Akira Itsubo
明 伊坪
Hiroshi Yui
浩 由井
Toshihiko Yamashita
俊彦 山下
Kazuo Kikuchi
菊地 一男
Katsuo Shintou
神道 克生
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Mitsubishi Petrochemical Co Ltd
Original Assignee
Mitsubishi Petrochemical Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Mitsubishi Petrochemical Co Ltd filed Critical Mitsubishi Petrochemical Co Ltd
Priority to JP59006928A priority Critical patent/JPS60152569A/en
Publication of JPS60152569A publication Critical patent/JPS60152569A/en
Pending legal-status Critical Current

Links

Abstract

PURPOSE:To provide carbon black which has a high degree of graphitization, is highly porous and excellent in physical and chemical stabilities and has a specified crystalline structure when determined by X-ray diffraction and a specified specific surface area as measuered by BET method. CONSTITUTION:By-product carbon black having a DBP oil absorption of 220ml/ 100g or above and an ash content of 0.3wt% or below obtd. by partially oxidizing a liquid hydrocarbon (e.g. carbon oil) with molecular oxygen in the presence of steam in a quantity of 200-800kg per ton of hydrocarbon at 1,200-1,450 deg.C under a pressure of 10-80kg/cm<2>, is dried at 300-900 deg.C in an N2 gas atmosphere for 0.5-3hr and then heated at 1,000-3,000 deg.C in an inert gas atmosphere to obtain carbon black having a specific surface area of 100m<2>/g or above as measured by BET method and a crystalline structure wherein La is 20-250Angstrom , Lc is 20-250Angstrom and d(002) is 3.55-3.35 when determined by X-ray diffraction.

Description

【発明の詳細な説明】 本発明は、新規なカーボンブラックに関するものである
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a novel carbon black.

本発明の新規なカーボンブラックは、黒鉛化度が高くし
かも多孔性に富んだものである。
The novel carbon black of the present invention has a high degree of graphitization and is highly porous.

カーボンブラックは、炭化水素や炭素を含む化合物を不
完全燃焼まだは、熱分解させることによりできるコロイ
ド領域の粒子径を有する黒色微粉体であり、通常その形
状は球体に近いものである。
Carbon black is a fine black powder having a particle size in the colloidal region, which is produced by incompletely burning or thermally decomposing a compound containing hydrocarbons or carbon, and its shape is usually close to a sphere.

また、カーボンブラックは、タイヤをはじめとする種々
ゴム製品の補強剤並びに印刷インキ、塗料などのカラー
用着色剤等として広く用いられている。
Furthermore, carbon black is widely used as a reinforcing agent for various rubber products such as tires, and as a coloring agent for printing inks, paints, and the like.

従来、カーボンブラックの構造については、X線回折あ
るいは電子顕微鏡等により明らかにされており、炭素原
子からなる六員環網状平面が粒子の中心に対して同心円
状に比較的ルーズに積層しているものでちるとされてい
る。そして、この様なカーボンブラックは、比表面積が
大きく、多孔性粉体として高度の機能を発揮するが、L
a、、Lcは余り大きくなく、一方d(ooz)はかな
り大きく、黒鉛的な性質は高度には発揮できない。
Conventionally, the structure of carbon black has been revealed by X-ray diffraction or electron microscopy, and it is found that six-membered ring network planes made of carbon atoms are relatively loosely stacked concentrically around the center of the particle. It is said to be full of things. Such carbon black has a large specific surface area and exhibits advanced functionality as a porous powder, but L
a, , Lc are not very large, while d(ooz) is quite large, and graphite-like properties cannot be exhibited to a high degree.

また、カーボンブラックの結晶構造の一つの極限である
黒鉛は、カーボンブラックに比べてLa。
Furthermore, graphite, which is one of the extremes of carbon black's crystal structure, has a lower La than carbon black.

Lcは極めて大きいが、d(ooz)が小さく、導電性
、潤滑性、物理的化学的安定性などの性質が極めて優れ
ているが、比表面積が極めて小さく多孔性がほとんどな
いために液体を保持する吸液力はほとんどない。
Although Lc is extremely large, d(ooz) is small, and properties such as conductivity, lubricity, and physical and chemical stability are extremely excellent, but the specific surface area is extremely small and there is almost no porosity, so it retains liquid. There is almost no liquid absorption power.

カーボンブラックの多孔性を有し、黒鉛に近い高結晶性
を持った炭素材料が得られれば実用的価値が極めて大き
い。
If a carbon material with the porosity of carbon black and high crystallinity close to that of graphite could be obtained, it would have extremely great practical value.

そこで従来各種手法でこのような炭素材料を得るための
試みが行なわれてきた。例えば、ファーネスブラック、
チャンネルブラックなどを1000〜3000℃のよう
な高温で加熱処理して黒鉛化度を高めることが行なわれ
ている。このような高温処理カーボンブラックは黒鉛化
度は高まっているが、カーボンブラック本来の多孔性が
損われ比表面積が小さくなるのが通例である。例えば、
2300℃処理7アーネスブラツクでは、La= 39
A、 Lc= 58 A、d(ooz)、= 3.47
 Xと結晶性はかなシ高いが比表面積がs 5.m’ 
/ を程度である。
Therefore, attempts have been made to obtain such carbon materials using various methods. For example, furnace black,
Channel black and the like are heat treated at high temperatures such as 1000 to 3000°C to increase the degree of graphitization. Although the degree of graphitization of such high-temperature-treated carbon black is increased, the inherent porosity of carbon black is generally impaired and the specific surface area is reduced. for example,
For 7 Arnes Black treated at 2300°C, La = 39
A, Lc= 58 A, d(ooz), = 3.47
X and crystallinity are slightly high, but the specific surface area is s5. m'
/ is the degree.

本発明者らは、従来の高温処理カーボンブラックと異な
シ高い黒鉛化度を有し、しかも多孔性を保持したカーボ
ンブラックを得るべく各種の実験を繰シ返した結果、こ
のような新規なカーボンブラックを得ることに成功した
The present inventors have repeatedly conducted various experiments to obtain carbon black that has a high degree of graphitization and retains porosity, which is different from conventional high-temperature-treated carbon black. I succeeded in getting black.

即ち、本発明は、X線回折法にょ請求めた結晶構造が、
Laが20〜25oX1Lcが20〜250Aおよびd
(002)が3・55〜3・asXでありかつBET法
によ請求めた比表面積が1oom’/r以上である新規
なカーボンブラックを提供するものである。
That is, the present invention provides that the crystal structure determined by X-ray diffraction method is
La is 20-25oX1Lc is 20-250A and d
The present invention provides a novel carbon black having (002) of 3.55 to 3.asX and a specific surface area of 1 oom'/r or more as determined by the BET method.

本発明のカーボンブラックは、黒鉛化度が高いため物理
的化学的に極めて安定で、なおかつ多孔性に富んでいる
為比表面積が大きいという特徴を有し、実用的価値が極
めて大である。
The carbon black of the present invention has a high degree of graphitization, so it is physically and chemically extremely stable, and is highly porous, so it has a large specific surface area, and has extremely great practical value.

本発明の新規なカーボンブラックは、X線回折によって
めた結晶構造が、 a軸方向の広が、9Laが20〜250X。
The novel carbon black of the present invention has a crystal structure determined by X-ray diffraction that is spread in the a-axis direction and has a 9La of 20 to 250X.

C軸方向の厚み I、cが20〜250A。Thickness in the C-axis direction I and c are 20 to 250A.

炭素網平面間隔d(Ooz)が3.55〜3.3 s 
X。
Carbon network plane spacing d (Ooz) is 3.55 to 3.3 s
X.

であシ、窒素ガス吸着からBET法によってめた比表面
積が100m”/f以上であるカーボンブラックであ夛
、殊に、 Laが40〜250A1 LCが50〜250 A。
It is carbon black whose specific surface area determined by the BET method from nitrogen gas adsorption is 100 m''/f or more, especially La: 40-250 A1 LC: 50-250 A.

d(0021が3.50〜3.35 A。d (0021 is 3.50-3.35 A.

BET比表面積が100〜300m”/f、であるカー
ボンブラックが黒鉛類似の性質が優れておシ好ましいも
のである。
Carbon black having a BET specific surface area of 100 to 300 m''/f is preferred because it has excellent graphite-like properties.

ここでX線回折は、炭素材料学会編炭素材料入門、18
4〜192頁(炭素材料学会、1979年刊)に記載の
学術振興会第117委員会によって確立された手法によ
シ、シリコンを標準物質として測定を行なう。
Here, X-ray diffraction refers to Introduction to Carbon Materials, edited by Carbon Materials Society, 18.
The measurement is performed using silicon as a standard substance according to the method established by the 117th Committee of the Japan Society for the Promotion of Science described in pages 4 to 192 (Japanese Society for Carbon Materials, published in 1979).

比表面積の測定は、Brunauer、 Emmett
 andTeLler、J−’Am、 Chem、 S
oc、、59.1553(1938)に記載の方法によ
って行なう。
Measurement of specific surface area is carried out by Brunauer, Emmett.
and TeLler, J-'Am, Chem, S.
oc, 59.1553 (1938).

このような新規なカーボンブラックは例えば次のような
方法によって製造することができる。即ち、液状炭化水
素を炉内で分子状酸素及び水蒸気の存在下部分酸化反応
せしめて合成ガス化と同時に得られる副生高導電性カー
ボンを窒素雰囲気下300〜900℃で乾燥し、次いで
不活性ガス雰囲気下1000〜3000℃で加熱処理し
て本発明の新規カーボンブラックを製造することができ
る。
Such novel carbon black can be produced, for example, by the following method. That is, liquid hydrocarbons are subjected to a partial oxidation reaction in the presence of molecular oxygen and water vapor in a furnace, and the by-product highly conductive carbon obtained at the same time as synthesis gasification is dried at 300 to 900°C in a nitrogen atmosphere, and then inert. The novel carbon black of the present invention can be produced by heat treatment at 1000 to 3000°C in a gas atmosphere.

上記本発明の新規カーボンブラックの製造法及び得られ
るカーボンブラックの特徴を更に詳しく説明する。
The method for producing the novel carbon black of the present invention and the characteristics of the obtained carbon black will be explained in more detail.

本発明のカーボンブラックを製造するのに適用される液
状炭化水素を原料とする部分酸化法は、該炭化水素を炉
内で分子状酸素及び水蒸気と反応せしめて合成ガスを製
造すると同時にカーボンを副生ずるシェルガス化プロセ
ス、テキサコガス化プロセス等がある。上記プロセスは
、例えばシェルガス化プロセスは、着体幹雄、「重質油
のガス化」(燃料協会編、1972年丸善■刊)などに
テキサコガス化プロセスは、真田宏、石油化学誌、15
.42〜46(1972)などに記載されているもので
ある。
In the partial oxidation method using liquid hydrocarbons as a raw material, which is applied to produce the carbon black of the present invention, the hydrocarbons are reacted with molecular oxygen and water vapor in a furnace to produce synthesis gas, and at the same time, carbon is added as a sub-oxidant. These include the resulting shell gasification process, the Texaco gasification process, etc. The above processes include, for example, the shell gasification process by Mikio Kitai, "Gasification of Heavy Oil" (edited by Japan Fuel Association, published by Maruzen, 1972), and the Texaco gasification process by Hiroshi Sanada, Petrochemical Magazine, 15.
.. 42-46 (1972).

上記部分酸化法によシ製造される副生高導電性カーボン
とは、DBP吸油量が220ゴ/100゛f以上、好ま
しくは300〜s、ooa//1oot殊に好ましくは
350〜500m17100 tであり、灰分が0.3
wt%以下と低いものを言い、このカーボンはそれ自身
でも良好な導電性を示すが例えば、ポリ塩化ビニル、ポ
リエチレン、ポリプロピレン、エチレンとプロピレンと
の共重合体等のポリオレフィン樹脂、ナイロン、ポリス
チレン、ゴム等に混線・混合して使用する場合、その用
いた樹脂等の表面抵抗率、体積抵抗率を著しく低下させ
、灰分が少ない為得られる導電性材料の品質ムラの少な
い優れた導電性材料を提供できるもののことを言う。
The by-product highly conductive carbon produced by the above partial oxidation method has a DBP oil absorption of 220 g/100°f or more, preferably 300 to s, ooa//1oot, particularly preferably 350 to 500 m, and 17,100 t. Yes, ash content is 0.3
Although this carbon exhibits good conductivity by itself, it can also be used in polyolefin resins such as polyvinyl chloride, polyethylene, polypropylene, copolymers of ethylene and propylene, nylon, polystyrene, and rubber. When used in combination with other materials, the surface resistivity and volume resistivity of the resin used are significantly reduced, and the low ash content provides an excellent conductive material with less uneven quality. Talk about what you can do.

上記方法に用いられる液状炭化水素には、例えばC重油
、A重油、ナフサの熱分解油(エチレンヘビーエンド)
、芳香族系液状炭化水素にカーボンを混合した液状炭化
水素(カーボンオイル)、芳香族系液状炭化水素にC重
油などを混合した混合オイルなどがある。これらの中で
も元素分析によ請求めた炭素原子及び水素原子の重量組
成の比(炭素原子/水素原子)が9以上のエチレンヘビ
ーエンド、カーボンオイル、芳香族系液状炭化水素にC
重油などを混合した混合オイルが好ましく、これらの中
でも特に炭素原子/水素原子の重量組成の比が12以上
の例えばエチレンヘビーエンド、カーボンオイル等が、
得られるカーボン中の灰分量を低くできるので好ましい
。炭素原子/水素原子の重量比が9未満では、該炉内の
処理条件を変更してもカーボンのDBP吸油量が低下し
たり、又収量が小さくなるなど好ましいカーボンの製造
を維持することが廁(シい。上記原料の炭素原子/水素
原子の重量比が9以上であっても、固体状となったり、
高粘度の液状炭化水素又はカーボンオイル等となって該
炉への供給が困難となるものなどは好ましくない。即ち
、該炉内に供給する原料炭化水素は液状であつ−ご供給
時に、粘度30 cst以下であることが好ましい。
Liquid hydrocarbons used in the above method include, for example, C heavy oil, A heavy oil, and naphtha pyrolysis oil (ethylene heavy end).
, liquid hydrocarbon (carbon oil) which is a mixture of aromatic liquid hydrocarbon and carbon, and mixed oil which is a mixture of aromatic liquid hydrocarbon and C heavy oil. Among these, ethylene heavy ends, carbon oil, and aromatic liquid hydrocarbons with a weight composition ratio of carbon atoms and hydrogen atoms (carbon atoms/hydrogen atoms) as determined by elemental analysis are 9 or more.
Mixed oils such as heavy oils are preferred, and among these, especially ethylene heavy end oils, carbon oils, etc. having a weight composition ratio of carbon atoms/hydrogen atoms of 12 or more are preferred.
This is preferable because the amount of ash in the obtained carbon can be reduced. If the weight ratio of carbon atoms/hydrogen atoms is less than 9, it may be difficult to maintain the desired carbon production, as the DBP oil absorption of carbon may decrease even if the processing conditions in the furnace are changed, or the yield may become small. (Yes. Even if the weight ratio of carbon atoms/hydrogen atoms in the above raw materials is 9 or more, it may become solid or
It is not preferable to use highly viscous liquid hydrocarbons or carbon oil, which would be difficult to supply to the furnace. That is, it is preferable that the raw material hydrocarbon fed into the furnace is in liquid form and has a viscosity of 30 cst or less when fed.

上記部分酸化反応は、部分酸化反応を行う炉が炉内温度
範囲が1200〜1450℃、好ましくは1300〜1
450℃、特に好ましく ij 1360〜1420℃
である。炉内圧力は、10〜80にり/d、好ましくは
25〜80 K9/etl、特に好ましくは25〜35
 Kg / e:rl−、炉内へ供給される水蒸気の量
が原料炭化水素1トン当9200〜800 Kg、好ま
しくは400〜5ooxy、特に好ましくは450〜8
00 Kgの条件で運転される。これらの運転条件と前
記原料炭化水素の特徴とを同時に満たすことによって、
従来公知の条件では達成し得なかった優れた高導電性で
しかも灰分の少ないカーボンを収量良く製造し、しかも
合成ガス製造には何ら悪影響を与えないで製造工程の熱
収支上も好ましく経済的に行うことができる。
In the above partial oxidation reaction, the temperature range in the furnace for performing the partial oxidation reaction is 1200 to 1450 °C, preferably 1300 to 1
450°C, particularly preferably ij 1360-1420°C
It is. The furnace pressure is 10 to 80 K9/d, preferably 25 to 80 K9/etl, particularly preferably 25 to 35 K9/etl.
Kg/e:rl-, the amount of steam supplied into the furnace is 9200 to 800 Kg per ton of raw material hydrocarbon, preferably 400 to 5ooxy, particularly preferably 450 to 8
It is operated under the condition of 00 Kg. By simultaneously satisfying these operating conditions and the characteristics of the feedstock hydrocarbon,
It is possible to produce high-yield carbon with excellent conductivity and low ash content, which could not be achieved under conventionally known conditions, and it is also economical in terms of the heat balance of the production process without any negative impact on synthesis gas production. It can be carried out.

ここでDBP吸油量はJIS−に6221に準拠して測
定され、試料97のカーボンにジブチルフタレート(D
BP)が吸収される量(tnl :)を1002のカー
ボン量に換算した値であり、この値が大きい程導電性に
優れる。
Here, DBP oil absorption was measured in accordance with JIS-6221, and dibutyl phthalate (DBP) was measured in accordance with JIS-6221.
It is a value obtained by converting the amount of absorbed BP) (tnl:) into the amount of carbon of 1002, and the larger this value is, the better the conductivity is.

上記の様にして得られた副生高導電性、カーボンブラッ
クは、このままでは電池用として適さないが、これを乾
燥し、次いで加熱処理することにより初めて本発明の新
規カーボンブラックを得ることができる。
The highly conductive by-product carbon black obtained as described above is not suitable for use in batteries as it is, but by drying it and then heat-treating it, the novel carbon black of the present invention can be obtained for the first time. .

上記乾燥は、窒素ガス雰囲気下300〜900℃の温度
範囲で0.5〜3時間行われる。この乾燥によって上記
高導電性カーボンブラックは1重量%以下、好ましくは
0.5重量%以下の水分を含有するものとなる。
The above drying is performed at a temperature range of 300 to 900° C. for 0.5 to 3 hours under a nitrogen gas atmosphere. By this drying, the highly conductive carbon black has a moisture content of 1% by weight or less, preferably 0.5% by weight or less.

次いでこの乾燥カーボンブラックを窒素、アルゴン等の
不活性ガス雰囲気下、1000〜3000℃、好ましく
は1500〜2500℃の温度範囲で1分以上、好まし
くは0.5〜5時間加熱処理する。
Next, this dried carbon black is heat-treated in an inert gas atmosphere such as nitrogen or argon at a temperature range of 1000 to 3000°C, preferably 1500 to 2500°C for 1 minute or more, preferably 0.5 to 5 hours.

上記の通り詳述した方法により製造された本発明の新規
なカーボンブラックは、黒鉛化度を示す炭素網平面間隔
d(002)が3.55〜3.35 Aと黒鉛化度が高
く、DBP吸油量が220m//100f以上と優れた
吸油性を示し、かつ灰分(JIS−に6221に準じて
測定される)が帆3重量%以下及び揮発分(J IS−
に6’221に準じて測定される)が0.5重量%以下
の特徴を有するものである。
The novel carbon black of the present invention produced by the method detailed above has a high degree of graphitization with a carbon network plane spacing d (002) indicating the degree of graphitization of 3.55 to 3.35 A, and has a high degree of graphitization. It exhibits excellent oil absorption with an oil absorption of 220 m//100 f or more, and has an ash content (measured according to JIS-6221) of 3% by weight or less and a volatile content (JIS-6221).
6'221) is 0.5% by weight or less.

本発明の新規なカーボンブラックは、高い黒鉛化臀及び
多孔性に富み大きな比表面積を有するので黒鉛に類似し
た物理的・化学的安定性を有し、黒鉛よりもはるかに優
れた高い吸液性を有する。
The novel carbon black of the present invention has high graphitization, high porosity, and a large specific surface area, so it has physical and chemical stability similar to graphite, and has high liquid absorption properties that are far superior to graphite. has.

この様な特徴を有する本発明の新規なカーボンブラック
は、ルクランシエ区池、アルカリ土類金属電池、リチウ
ム電池などの電池の正極合剤、触媒担体等の用途に使用
できる他、通常のカーボンブラック、黒鉛の用途に使用
することもできる。
The novel carbon black of the present invention having such characteristics can be used for applications such as positive electrode mixtures and catalyst supports for batteries such as Lecrancier batteries, alkaline earth metal batteries, and lithium batteries, as well as ordinary carbon black, It can also be used in graphite applications.

実施例1 (部分酸化反応による副生カーボンブラックの製造) 原料液状炭化水素の性状が 初留温度 iso〜190℃ 10チ留出温度 205〜215℃ 50%留出温度 250〜260℃ 97チ留出温度 320〜340℃ 粘度(80℃) 約10cst 炭素原子/水素原子(重量比) 12.5’ナルエチレ
ンヘビーエンドをシェルガス化フロセスの炉に使用した
。該炉の炉内温度1400℃、炉内圧力30Kf/61
で炉内へ供給する水蒸気の量を原料炭化水素1トン当り
390 Kg、メタン濃度0.8容量%で運転した。
Example 1 (Manufacture of by-product carbon black by partial oxidation reaction) The properties of the raw material liquid hydrocarbon are initial distillation temperature iso ~ 190°C 10th distillation temperature 205 ~ 215°C 50% distillation temperature 250 ~ 260°C 97th distillation temperature Output temperature 320-340°C Viscosity (80°C) Approximately 10 cst Carbon atom/Hydrogen atom (weight ratio) 12.5'Nal ethylene heavy end was used in a shell gasification process furnace. The temperature inside the furnace is 1400℃, the pressure inside the furnace is 30Kf/61
The furnace was operated with an amount of steam supplied into the furnace at 390 kg per ton of hydrocarbon feedstock and a methane concentration of 0.8% by volume.

この時得られた合成ガスの組成は、−酸化炭素51.7
容量%、水素43.6容量%、炭酸ガス3.8容量%、
その他0.9容量%であシ、合成ガ哀と同時にDBP吸
油量290w、l/fの副生じたカーボンブラックを得
た。
The composition of the synthesis gas obtained at this time was -carbon oxide 51.7
Volume%, hydrogen 43.6% by volume, carbon dioxide 3.8% by volume,
In addition, carbon black with a DBP oil absorption of 290 w and 1/f was obtained as a by-product at the same time as the synthetic resin.

(副生カーボンブラックの乾燥及び加熱処理)上記の様
にして得た副生カーボンブラックを500℃、1時間、
窒素ガス雰囲気中で乾燥した。
(Drying and heat treatment of by-product carbon black) The by-product carbon black obtained as above was heated at 500°C for 1 hour.
It was dried in a nitrogen gas atmosphere.

この乾燥カーボンブラックは、水分含有率1重量%以下
であった。
This dry carbon black had a moisture content of 1% by weight or less.

この乾燥カーボンブラックをアルゴンガス雰囲気下23
00℃の温度で2時間で加熱処理した。
This dry carbon black was heated for 23 minutes under an argon gas atmosphere.
Heat treatment was performed at a temperature of 00°C for 2 hours.

得られた本発明の新規なカーボンブラックは、Laが4
7 A、 Lcが55.5 XXd(002)が3.4
7 A、比表面積が107 n?/ fと黒鉛化度が高
く、多孔性を有するものであった。
The obtained novel carbon black of the present invention has La of 4
7 A, Lc is 55.5 XXd (002) is 3.4
7 A, specific surface area is 107 n? /f, the degree of graphitization was high, and it had porosity.

実施例2 実施例10部分酸化反応による副生カーボンブラックの
製造条件の、炉の運転条件を変えて該炉の炉内温度13
80℃、炉内圧力30Kg/cr4で炉内へ供給する水
蒸気の量を原料炭化水素1トン当り730 Kf、メタ
ン濃度0.28容量%で運転し、DBP吸油量が490
R1/1002の副生カーボンブラックを得た。
Example 2 Example 10 The furnace operating conditions of the production conditions of by-product carbon black by partial oxidation reaction were changed to increase the furnace internal temperature of the furnace to 13.
It was operated at 80℃, the furnace pressure was 30Kg/cr4, the amount of steam supplied to the furnace was 730Kf per ton of feedstock hydrocarbon, the methane concentration was 0.28% by volume, and the DBP oil absorption was 490%.
A by-product carbon black of R1/1002 was obtained.

この副生カーボンブラックを実施例1と同様に加熱処理
して本発明の新規なカーボンブラックを得た。このカー
ボンブラックは、Laが60X、LcW?/2であった
This by-product carbon black was heat treated in the same manner as in Example 1 to obtain a novel carbon black of the present invention. This carbon black has La of 60X and LcW? /2.

参考例1 実施例2で得られた本発明の新規なカーボンブラックの
物理的・化学的安定性及び吸液性を評価すべくルクラン
シエ電池の正極合剤としての性能評価試験を行った。
Reference Example 1 In order to evaluate the physical and chemical stability and liquid absorption properties of the novel carbon black of the present invention obtained in Example 2, a performance evaluation test was conducted as a positive electrode mixture for Leclancier batteries.

正極合剤として電解二酸化マンガン50重量部、30重
量%塩化亜鉛水溶液50重量部、本発明のカーボンブラ
ック6重量部からなシ、電解液として30重量%塩化亜
鉛水溶液を正極合剤に対し重量比で2:3の割合で加え
、正極に白金、負極に亜鉛を使用したルクランシエ電池
を形成し、開回路を組み初期起電力及び、45℃30日
間保持した後の起電力を測定した。
The positive electrode mixture consists of 50 parts by weight of electrolytic manganese dioxide, 50 parts by weight of a 30% by weight zinc chloride aqueous solution, and 6 parts by weight of the carbon black of the present invention, and the weight ratio of a 30% by weight zinc chloride aqueous solution to the positive electrode mixture as an electrolyte. were added at a ratio of 2:3 to form a Lecrancier battery using platinum as the positive electrode and zinc as the negative electrode, and an open circuit was constructed to measure the initial electromotive force and the electromotive force after being maintained at 45°C for 30 days.

比較のために、本発明のカーボンブラックの代シに、ケ
ッチェンブラックEC(オランダアクゾ社製特殊ファー
ネスブラック)、アセチレンブラック、アルゴン雰囲気
下2300℃で加熱処理したファーネスブラック及び黒
鉛を用いたものについても同様の測定を行なった(本拠
明のカーボンブラック及びケッチェンブラックEC以外
のものは6重量部配合での吸液力が著しく不足していた
ので、10重量部配合についても実験を行なった。)各
種炭素材料の物性を第1表に、電池性能を第2表に示す
For comparison, in place of the carbon black of the present invention, Ketjenblack EC (special furnace black manufactured by Akzo in the Netherlands), acetylene black, furnace black heat-treated at 2300°C in an argon atmosphere, and graphite were used. (Since carbon black and Ketjen black EC other than Honmei's carbon black and Ketjen black EC were found to have significantly insufficient liquid absorption power when mixed with 6 parts by weight, experiments were also conducted with 10 parts by weight mixed. ) The physical properties of various carbon materials are shown in Table 1, and the battery performance is shown in Table 2.

(以下余白) 第1表 第2表 *吸液力不足:正極合剤として使用不可で6D、起電力
測定も不可であった。
(Margin below) Table 1 Table 2 * Insufficient liquid absorption power: Unusable as a positive electrode mixture, 6D, and electromotive force measurement was also impossible.

第2表から明らかな通シ、本発明の新規なカーボンブラ
ックは吸液力、起電力が他の炭素材料と比べて極めて優
れていることが明らかである。
It is clear from Table 2 that the novel carbon black of the present invention has extremely superior liquid absorption power and electromotive force compared to other carbon materials.

特許出願人 三菱油化株式会社 代理人 弁理士 古 川 秀 利 代理人 弁理士 長 谷 正 久Patent applicant Mitsubishi Yuka Co., Ltd. Agent: Patent Attorney Hidetoshi Furukawa Agent: Patent Attorney Masahisa Nagatani

Claims (1)

【特許請求の範囲】[Claims] (1)X線回折法によ請求めた結晶構造が、臘がd(o
oz)が3・55〜3・35AでありかつBET法によ
りめた比表、面積が100m”79以上である新規なカ
ーボンブラック。
(1) The crystal structure determined by X-ray diffraction is d(o
oz) is 3.55 to 3.35 A, and the specific surface area determined by the BET method is 100 m''79 or more.
JP59006928A 1984-01-18 1984-01-18 Novel carbon black Pending JPS60152569A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP59006928A JPS60152569A (en) 1984-01-18 1984-01-18 Novel carbon black

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP59006928A JPS60152569A (en) 1984-01-18 1984-01-18 Novel carbon black

Publications (1)

Publication Number Publication Date
JPS60152569A true JPS60152569A (en) 1985-08-10

Family

ID=11651904

Family Applications (1)

Application Number Title Priority Date Filing Date
JP59006928A Pending JPS60152569A (en) 1984-01-18 1984-01-18 Novel carbon black

Country Status (1)

Country Link
JP (1) JPS60152569A (en)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH035313A (en) * 1989-06-01 1991-01-11 Mitsubishi Petrochem Co Ltd Granular porous graphitic carbon material and supporting material for chromatography using the same
WO1994014900A1 (en) * 1992-12-18 1994-07-07 Cabot Corporation Low ash carbon blacks
WO2000011739A1 (en) * 1998-05-01 2000-03-02 Eveready Battery Company, Inc. Heat treated fine carbon for alkaline manganese cathodes
WO2001092151A1 (en) * 2000-05-31 2001-12-06 Showa Denko K.K. Electrically conductive fine carbon composite, catalyst for solid polymer fuel cell and fuel battery
US6780388B2 (en) 2000-05-31 2004-08-24 Showa Denko K.K. Electrically conducting fine carbon composite powder, catalyst for polymer electrolyte fuel battery and fuel battery
JP2014241279A (en) * 2013-05-14 2014-12-25 ライオン株式会社 Electrode mixture
KR20160010399A (en) 2013-05-14 2016-01-27 라이온 스페셜티 케미칼즈 가부시키가이샤 Carbon black, electrically conductive resin composition, and electrode mixture
WO2016039268A1 (en) * 2014-09-09 2016-03-17 株式会社東北テクノアーチ Method for producing porous graphite, and porous graphite
JPWO2019065018A1 (en) * 2017-09-28 2019-11-14 新日本テクノカーボン株式会社 Graphite material

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS54126691A (en) * 1978-03-27 1979-10-02 Raion Akuzo Kk Method of manufacturing high electric conductive carbon black
JPS5558259A (en) * 1978-10-25 1980-04-30 Hoechst Ag Method and apparatus for increasing graphitization degree of carbon black

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS54126691A (en) * 1978-03-27 1979-10-02 Raion Akuzo Kk Method of manufacturing high electric conductive carbon black
JPS5558259A (en) * 1978-10-25 1980-04-30 Hoechst Ag Method and apparatus for increasing graphitization degree of carbon black

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH035313A (en) * 1989-06-01 1991-01-11 Mitsubishi Petrochem Co Ltd Granular porous graphitic carbon material and supporting material for chromatography using the same
WO1994014900A1 (en) * 1992-12-18 1994-07-07 Cabot Corporation Low ash carbon blacks
US5352289A (en) * 1992-12-18 1994-10-04 Cabot Corporation Low ash carbon blacks
EP0867478A1 (en) * 1992-12-18 1998-09-30 Cabot Corporation Low Ash carbon blacks
WO2000011739A1 (en) * 1998-05-01 2000-03-02 Eveready Battery Company, Inc. Heat treated fine carbon for alkaline manganese cathodes
US6780388B2 (en) 2000-05-31 2004-08-24 Showa Denko K.K. Electrically conducting fine carbon composite powder, catalyst for polymer electrolyte fuel battery and fuel battery
WO2001092151A1 (en) * 2000-05-31 2001-12-06 Showa Denko K.K. Electrically conductive fine carbon composite, catalyst for solid polymer fuel cell and fuel battery
JP2014241279A (en) * 2013-05-14 2014-12-25 ライオン株式会社 Electrode mixture
KR20160010399A (en) 2013-05-14 2016-01-27 라이온 스페셜티 케미칼즈 가부시키가이샤 Carbon black, electrically conductive resin composition, and electrode mixture
WO2016039268A1 (en) * 2014-09-09 2016-03-17 株式会社東北テクノアーチ Method for producing porous graphite, and porous graphite
JPWO2016039268A1 (en) * 2014-09-09 2017-06-22 株式会社 東北テクノアーチ Method for producing porous graphite and porous graphite
US10403900B2 (en) 2014-09-09 2019-09-03 Tohoku Techno Arch Co., Ltd. Method for producing porous graphite, and porous graphite
US10763511B2 (en) 2014-09-09 2020-09-01 Tohoku Techno Arch Co., Ltd. Method for producing porous graphite, and porous graphite
JPWO2019065018A1 (en) * 2017-09-28 2019-11-14 新日本テクノカーボン株式会社 Graphite material

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