JPH01317110A - Production of fine carbon powder having high purity - Google Patents
Production of fine carbon powder having high purityInfo
- Publication number
- JPH01317110A JPH01317110A JP63149359A JP14935988A JPH01317110A JP H01317110 A JPH01317110 A JP H01317110A JP 63149359 A JP63149359 A JP 63149359A JP 14935988 A JP14935988 A JP 14935988A JP H01317110 A JPH01317110 A JP H01317110A
- Authority
- JP
- Japan
- Prior art keywords
- iron powder
- reaction
- furnace
- carbon
- temperature
- 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
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 239000006227 byproduct Substances 0.000 claims abstract description 17
- 238000002844 melting Methods 0.000 claims abstract description 5
- 230000008018 melting Effects 0.000 claims abstract description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 19
- 239000002245 particle Substances 0.000 claims description 10
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 5
- 238000003723 Smelting Methods 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims 4
- 239000000843 powder Substances 0.000 abstract description 5
- 239000007789 gas Substances 0.000 description 38
- 238000001816 cooling Methods 0.000 description 9
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 8
- 239000010410 layer Substances 0.000 description 8
- 229910000831 Steel Inorganic materials 0.000 description 7
- 239000010419 fine particle Substances 0.000 description 7
- 239000010959 steel Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- 239000002184 metal Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000006229 carbon black Substances 0.000 description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 238000007790 scraping Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000007885 magnetic separation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 239000003831 antifriction material Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 238000005422 blasting Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000007809 chemical reaction catalyst Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000012717 electrostatic precipitator Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
Abstract
Description
【発明の詳細な説明】
（産業上の利用分計）
本発明は９９．９％以上の高純度カーボン微粒子を高い
収率で且つ廉価に製造する方法に関する。DETAILED DESCRIPTION OF THE INVENTION (Industrial Applicability) The present invention relates to a method for producing high-purity carbon particles of 99.9% or more in high yield and at low cost.
（従来の技術）
近年耐熱性、導電性、潤滑性、耐腐食性等にすぐれた特
性を有すカーボンは電極耐火物等の大量使用製品から熱
間加工潤滑剤、カーボンブラック、減摩材、鉛筆用等の
多岐にわたる用途に使用されている。(Prior art) In recent years, carbon, which has excellent properties such as heat resistance, conductivity, lubricity, and corrosion resistance, has been used in products that are used in large quantities such as electrode refractories, hot processing lubricants, carbon black, anti-friction materials, It is used for a wide variety of purposes, including pencils.
これらの用途に応し種々のカーボンの製造プロセスが現
存するが、カーボン微粒子の代表例であるカーボンブラ
ックの製造法を例にとれば、ＬＮＧ或いはオイルで増炭
素した可燃性ガスに適当量の一次空気を混入し、チャン
ネル鋼で構成されたチャンネルハウス内で無数の小さな
火炎を形成しチャンネル鋼に火炎をあてることによりチ
ャンネル鋼表面に生成したカーホンブラックを付着せし
めた後これをかきとり飛散スケールな磁選除去した後粉
砕して粉状製品か得られている（化学プロセス集成３６
０〜３６３頁社口演人化学工学協会発行昭４５．３．３
）。Various carbon manufacturing processes currently exist depending on these uses, but taking the manufacturing method of carbon black, which is a typical example of carbon fine particles, as an example, an appropriate amount of primary carbon is added to combustible gas enriched with LNG or oil. Air is mixed in to form countless small flames in a channel house made of channel steel, and by applying the flame to the channel steel, carbon black generated on the surface of the channel steel is deposited, and then this is scraped off to remove any scattered scale. After magnetic separation and removal, a powder product is obtained by pulverizing (Chemical Process Collection 36)
Pages 0-363 Published by the Society of Chemical Engineers, Shaguchi, March 3, 1972.
).
しかし、この製法は付着したカーホンブラックを容易に
かき落すため、および設備費を安くする目的で市販のチ
ャンネル鋼を使用するため火炎とチャンネル鋼との接触
面積を充分にとれない難点があり、カーボンブラックの
収率は１８〜２５％程度の低いレベルにとどまらざるを
えない難点があった。However, this manufacturing method uses commercially available channel steel in order to easily scrape off the attached carphone black and to reduce equipment costs, so it has the disadvantage that it is not possible to ensure a sufficient contact area between the flame and the channel steel. There was a drawback that the yield of carbon black had to remain at a low level of about 18 to 25%.
また、得られた製品も炭化水素系ガスのクラッキング過
程で得られたものであるためにＨ，Ｏ，Ｓ等の不純物を
含有し、炭素％が９５〜９７％程度のものしか得られず
高純化が困難であった。In addition, since the obtained product is obtained through the cracking process of hydrocarbon gas, it contains impurities such as H, O, and S, and the carbon percentage is only about 95 to 97%. Purification was difficult.
（発明か解決しようとする課題）
本発明は前述した如き従来の炭素粉末製造法の欠点であ
る付着析出カーボンの生産性が極めて高く、しかも回収
されたカーホンを微細粒化できるとともに、不純物か少
なく高純化できる高純度カーホン微粒子の製造法を提供
することにある。(Problems to be Solved by the Invention) The present invention has extremely high productivity of deposited carbon, which is a disadvantage of the conventional carbon powder manufacturing method as described above, and can further reduce the amount of impurities in the recovered carphone. An object of the present invention is to provide a method for producing high-purity carphone fine particles that can be highly purified.
（課題を解決するための手段）
転炉或いはスクラップを多量に溶解させる電炉の如き精
錬炉又は高炉、キュポラ類等の溶解炉においては溶銑中
のＣ１投入炭材、炭化水素の熱分解、黒鉛製電極等の酸
化により多量のＣＯを主成分とする排ガスが発生する。(Means for solving the problem) In smelting furnaces such as converters or electric furnaces that melt large amounts of scrap, blast furnaces, and melting furnaces such as cupolas, C1 input carbonaceous material in hot metal, thermal decomposition of hydrocarbons, graphite Oxidation of electrodes, etc. generates a large amount of exhaust gas containing CO as a main component.
転炉を例にとれは粗ｆｉｌＴｏｎ当り約１００〜１２Ｏ
Ｎｍ３で且つＣＯを７０〜８０％含有した排ガスが発生
するがその排ガスはベンチュリースクラバーで冷却除塵
され極めて清浄なガスとして主として燃料に利用されて
いる。Taking a converter as an example, it is approximately 100 to 12 O per crude filTon.
Exhaust gas containing Nm3 and 70 to 80% CO is generated, but the exhaust gas is cooled and dust-removed by a venturi scrubber and is used as an extremely clean gas mainly for fuel.
本発明者等は第１図に示すように清浄で廉価な副生ガス
をそのまま又は加熱あるいは冷却等の温度制御を行ない
４００℃から６００℃の範囲に保持し粉状或いは繊維状
の鉄粉に接触させれば金属粉体が触媒となって２００→
ＣＯ２＋Ｃなる発熱反応が促進され、鉄粉表面に純度が
９９９％以上のＣ微粒子が多量に付着することを知見し
た。As shown in Fig. 1, the inventors of the present invention converted clean and inexpensive by-product gas into powdered or fibrous iron powder by keeping it in the range of 400°C to 600°C either as it is or by controlling the temperature by heating or cooling. When brought into contact, the metal powder becomes a catalyst and 200 →
It was found that the exothermic reaction of CO2+C was promoted and a large amount of C fine particles with a purity of 999% or more adhered to the surface of the iron powder.
同時に４００℃以下の低温域では、上記反応速度が遅く
かつ６００℃以上の高温域ではＣの収率が極端に悪化す
ることも見いだした。At the same time, it has been found that the reaction rate is slow in a low temperature range of 400°C or lower, and that the yield of C is extremely poor in a high temperature range of 600°C or higher.
更に、前述したようにこの反応は生成Ｃ１ｋｇ当り３２
３０ ｋｃａｌの発熱を伴う反応であることから、例え
ば副生ガスの温度の低い反応の開始時においては反応温
度に達するまでバーナー等による熱エネルギーの供給に
よる温度制御が必要である。しかし、−旦反応が開始す
れば多量の熱エネルギー放出があり反応域の温度が上昇
し６００℃以上の高温になりＣ収率が極端に悪化するた
め、反応域の温度を連続的に検出しつつ冷却による抜熱
操作を行ない４００〜６００℃の範囲に反応域温度を制
御することが必要であることも見出した。Furthermore, as mentioned above, this reaction produces 32
Since the reaction is accompanied by heat generation of 30 kcal, for example, at the start of the reaction when the temperature of the by-product gas is low, it is necessary to control the temperature by supplying thermal energy with a burner or the like until the reaction temperature is reached. However, once the reaction starts, a large amount of thermal energy is released and the temperature in the reaction zone rises to over 600°C, resulting in an extremely poor C yield. Therefore, the temperature in the reaction zone must be continuously detected. It has also been found that it is necessary to control the reaction zone temperature within the range of 400 to 600°C by carrying out a heat extraction operation by cooling.
以上の実験より得られた知見をもとに一例として第２図
に示す如く円筒容器１４内に金属鉄分が９５〜９７％で
平均粒子径が７０〜１００μｍの鉄粉層１を触媒として
充填し予め無酸化τ囲気下で鉄粉層１を４９０〜５２０
℃程度に予熱した。次いで００７０〜７５％、Ｇｏ２１
２〜１５％、ｌ−１２１〜２％、Ｎ２１０〜１３％、
０２０．３％以下の組成をもった転炉排ガスを排ガス供
給管１１から鉄粉層下部の多数の小孔を有する目皿２よ
り鉄粉層１内に導入し円筒容器１４内の転炉排ガスの通
過空塔速度を０１５〜０．２ ｍ／ｓに保持し鉄粉層１
の流動層を形成した。その結果排ガスを導入して数分後
多量のＣ微粒子の生成が始まり、鉄粒子表面に付着した
Ｃ微粒子が流動層内の金属粒子の激しい運動とこれに伴
ない逐次剥ｔｉｌ！離脱し反応した後のガスに随伴しキ
ャリーオーバーすることが判った。Based on the knowledge obtained from the above experiments, as an example, as shown in Fig. 2, a cylindrical container 14 is filled with an iron powder layer 1 having a metallic iron content of 95 to 97% and an average particle diameter of 70 to 100 μm as a catalyst. Iron powder layer 1 was heated to 490 to 520 in advance under a non-oxidizing τ atmosphere.
Preheated to about ℃. Then 0070-75%, Go21
2-15%, l-121-2%, N210-13%,
Converter exhaust gas having a composition of 0.020.3% or less is introduced into the iron powder layer 1 from the exhaust gas supply pipe 11 through the perforated plate 2 having many small holes at the bottom of the iron powder layer, and the converter exhaust gas in the cylindrical container 14 is introduced. The passing superficial velocity of the iron powder layer 1 was maintained at 0.15 to 0.2 m/s.
A fluidized bed was formed. As a result, a few minutes after introducing the exhaust gas, a large amount of C fine particles started to be produced, and the C fine particles adhering to the surface of the iron particles were gradually peeled off due to the intense movement of the metal particles in the fluidized bed! It was found that there was carryover accompanying the gas after the desorption and reaction.
このキャリーオーバーしたＣ微粒子をステンレスファイ
バー製のバグフィルタ−６で捕集し排出系７の適宜部位
で捕集物内に微量に存在する触媒として充填した鉄粉の
微粉を磁力選鉱法により除去した後Ｃの純度を分析した
結果９９９％を上回る高純度Ｃが７３〜７５％の高い収
率で得られた。The carried over C fine particles were collected by a bag filter 6 made of stainless fiber, and a small amount of iron powder filled as a catalyst present in the collected material was removed at an appropriate part of the discharge system 7 by magnetic beneficiation. As a result of analyzing the purity of C, high purity C exceeding 999% was obtained at a high yield of 73 to 75%.
ここで１２は副生ガス供給管１１から供給されるガスの
温度が熱電対９の計測により低い場合に該副生ガスを加
熱する熱交換器であり、燃焼用ガスの供給管８及び燃焼
用空気管１０とを燃焼するバーナー３１及びその集合排
ガス管１３が設けである。また鉄粉中に当該副生ガスを
吹込む方式の場合あまりにも反応が急激て鉄粉層中でＣ
が多量に生成し鉄粉粒子表面を逐次被覆し触媒効果が減
した場合は第３図に示すごとく円筒容器１４の側壁に鉄
粉のオーバーフロー管１５を設置し摩鉱機１６内に導入
しＣ粒子を剥離除去した後にリサイクルルート１７を経
て円筒容器１４の上から再投入する連続循環再生ライン
を設けることで容易に解決でとる。Here, 12 is a heat exchanger that heats the by-product gas when the temperature of the gas supplied from the by-product gas supply pipe 11 is low as measured by the thermocouple 9; A burner 31 for burning the air pipe 10 and its collective exhaust gas pipe 13 are provided. In addition, in the case of the method in which the by-product gas is blown into the iron powder, the reaction is too rapid, resulting in carbon dioxide in the iron powder layer.
If a large amount of C is generated and successively covers the surface of the iron powder particles, reducing the catalytic effect, an overflow pipe 15 for iron powder is installed on the side wall of the cylindrical container 14 as shown in FIG. 3, and the iron powder is introduced into the grinder 16. This problem can easily be solved by providing a continuous circulation regeneration line that re-injects the particles from above into the cylindrical container 14 via the recycling route 17 after peeling them off.
あるいはオーバーフロー管１５より流下する鉄粉は表層
が浸炭された硬いものであるためこれをショツトブラス
ト用等に利用することも可能である。Alternatively, since the iron powder flowing down from the overflow pipe 15 is hard and has a carburized surface layer, it can also be used for shot blasting.
この場合は円筒容器１４上からオーバーフロー分に見合
う処女鉄粉を補給してやれば良い。In this case, it is sufficient to replenish virgin iron powder from above the cylindrical container 14 in an amount corresponding to the overflow.
また円筒客器１４内で発生する多量の反応熱を抜熱する
ため円筒客器１４の側壁には冷却水と空気が冷媒として
導入できる供給口４及び排出口５を持った冷却管３を取
付けておくことが望ましい。つまり、円筒容器１４内鉄
粉温度を熱電対９で検出しその温度レベルにより多量の
抜熱が必要な場合は冷却水を僅かな抜熱で良い場合は空
気をその中間の抜熱量の場合は気水混相流を冷却管に流
すことにより自由に鉄粉温度を制御することができるか
らである。In addition, in order to remove a large amount of reaction heat generated within the cylindrical passenger container 14, a cooling pipe 3 having a supply port 4 and a discharge port 5 through which cooling water and air can be introduced as a refrigerant is attached to the side wall of the cylindrical passenger container 14. It is desirable to keep it. In other words, the temperature of the iron powder inside the cylindrical container 14 is detected by the thermocouple 9, and depending on the temperature level, if a large amount of heat is required to be removed, if a small amount of heat is required to be removed from the cooling water, or if the amount of heat removed is between the two, This is because the temperature of the iron powder can be freely controlled by flowing the air-water multiphase flow through the cooling pipe.
また、キャリーオーバーされたＣ微粒子の捕集にあたっ
てはハゲフィルタ一方式以外に電気集塵機による方式を
用いても良い。Furthermore, in order to collect the carried over C fine particles, an electrostatic precipitator may be used instead of the bald filter method.
次に第４図に示す如く反応触媒たる金属鉄製細線で製作
したメツシュベルト１８を反応炉２７内を通過させメッ
シュベルト１８自体は炉内と炉外な駆動ロール２６及び
支持ロール２６ａ〜２６ｃにより循環させる機構とし、
メツシュベルト１８の炉出側にはメツシュベルト１８へ
の付着Ｃをすみやかに冷却し酸化を防止するための水冷
ジャケット２２を内蔵した冷却帯及びメツシュベルト下
面の付着Ｃをそぎ落す当接板２３、メツシュベルト上面
の付着Ｃをそぎ落す当接板３２、メツシュ内に付着した
Ｃを払い落す加振装置２４、同じくベンディングロール
２９等で構成した設備を設は更に反応炉２７内には転炉
或いは溶解炉副生ガスの吹込み口１９、炉内反応ガスの
メツシュベルト１８との接触効率を良くし且つ炉内温度
を４００〜６００℃の範囲に制御するための抜熱間（図
示せず）を有する炉内仕切板２０、また反応開始温度ま
で炉内温度を昇熱させるいわゆるウオーミングアツプ用
熱源供給装置としてのバーナー３１を具備した設備にて
も前記組成の転炉副生ガスを吹込むことにより同様の結
果か得られる。ここで、２１は反応炉２７の炉内を示し
、２５は捕集炭素ホッパーを示し、３０は反応炉内のガ
スの流れを示すとともに、他は第２図、第３図と同様の
要素を表わすが、特に熱交換器１２は反応炉２７の排ガ
スを直接用いた場合を示す。Next, as shown in FIG. 4, a mesh belt 18 made of thin metal wire serving as a reaction catalyst is passed through the reactor 27, and the mesh belt 18 itself is circulated by a drive roll 26 and support rolls 26a to 26c inside and outside the furnace. As a mechanism,
On the exit side of the mesh belt 18 from the furnace, there is a cooling zone with a built-in water cooling jacket 22 for quickly cooling the C adhering to the mesh belt 18 and preventing oxidation, an abutment plate 23 for scraping off the C adhering to the lower surface of the mesh belt, and a contact plate 23 for scraping off the C adhering to the lower surface of the mesh belt. Equipment consisting of a contact plate 32 for scraping off the adhered C, a vibrating device 24 for scraping off the C adhered to the inside of the mesh, and a bending roll 29 are also installed in the reactor 27. A gas inlet 19, a furnace partition having a heat removal space (not shown) for improving the contact efficiency of the reaction gas in the furnace with the mesh belt 18 and controlling the furnace temperature in the range of 400 to 600°C. Similar results can be obtained by injecting the converter byproduct gas having the above composition into equipment equipped with the plate 20 and a burner 31 as a so-called warming-up heat source supply device for raising the temperature inside the furnace to the reaction starting temperature. can get. Here, 21 indicates the inside of the reactor 27, 25 indicates the captured carbon hopper, 30 indicates the flow of gas in the reactor, and other elements are the same as in FIGS. 2 and 3. In particular, the heat exchanger 12 shows the case where the exhaust gas from the reactor 27 is directly used.
この場合もステンレスファイバー製バグフィルタ−６や
当接板２３．３２等で得られたＣ粒子バルク中に微量に
含まれるメツシュベルトから剥離した微量の酸化鉄を磁
力遷鉱機３３で除去した後のＣの純度は９９９％を上回
るものが７１〜７５％の高い収率て得られた。In this case as well, after removing a trace amount of iron oxide exfoliated from the mesh belt contained in the C particle bulk obtained by the stainless fiber bag filter 6 and the contact plate 23. The purity of C was over 999% and the yield was as high as 71-75%.
この時の原料ガスとしての転炉副生ガス１ｍ３当りのＣ
生成量は、前述した鉄粉層内への吹込み法、後述したメ
ツシュベルトへの吹付は法いずれの場合も０．１ｋｇ程
度の高い生産１生が実現できる。C per 1 m3 of converter byproduct gas as raw material gas at this time
A high production amount of approximately 0.1 kg can be achieved in both the above-mentioned method of blowing into the iron powder layer and the method of blowing onto the mesh belt described below.
（実 施 例） 以下、本発明の実施例について述へる。(Example) Examples of the present invention will be described below.
Ｃ析出に用いた原料ガスは転炉の副生ガス（ＬＤＧ ）
でソノ組成はＣｏ；７．１％、ＣＯ２，１４，５％、
Ｎ２ ： １２ｊ％ ソ（７）他）１２．０２等の微量
ガスが１．７％である。The raw material gas used for C precipitation is converter byproduct gas (LDG)
Sono composition is Co; 7.1%, CO2, 14.5%,
N2: 12j% Trace gases such as (7) and others) 12.02 are 1.7%.
一方触媒には、平均粒径８５μｍのＨ２還元処理を行な
った鉄粉を槽径２００ｍｍの円筒型反応槽に充填し、反
応槽下部より前記ＬＤＧを１８８℃／分吹込んだ。On the other hand, as a catalyst, iron powder subjected to H2 reduction treatment and having an average particle size of 85 μm was filled in a cylindrical reaction tank with a tank diameter of 200 mm, and the LDG was blown at 188° C./min from the bottom of the reaction tank.
この場合反応槽内の鉄粉温度は４９０〜５２０℃に操業
し、その結果出側排ガス組成は、ｃｏ；ａ、ａ９６、ｃ
ｏ２；７ｏ、ｏ絋その他（Ｎ２．８２．８２０．０２
） ；２１．２商であった。この排ガスにキャリーオー
バーされたダストを出側バグフィルタ−により除塵し磁
選分離した結果、１．１ ｋｇ／Ｈｒのカーボンが回収
され約７０％のカーボン収率がえられることを確認した
。In this case, the iron powder temperature in the reaction tank is operated at 490 to 520°C, and as a result, the exhaust gas composition on the outlet side is co; a, a96, c
o2;7o, o 狋 and others (N2.82.820.02
) ; The quotient was 21.2. As a result of removing the dust carried over into the exhaust gas by a bag filter on the outlet side and performing magnetic separation, it was confirmed that 1.1 kg/Hr of carbon was recovered and a carbon yield of about 70% was obtained.
一方メッシュベルト方式を採用し、前記反応槽内に線径
１００μｍの鋼線を充填し同様な温度条件原料ガス条件
で実施した。このときの出側排ガス組成はＣＯ； ８．
５％、ＣＯ２； ７０．４％、その他（Ｎ２． ）１２
． Ｎ２０ 、０２） ； ２１．１％と流動層方式
とほとんど同様な結果が得られた。但しカーボンの回収
量は１．０ｋｇ／Ｈｒと若干少ない結果が得られた。こ
れは鋼線表面にトラップされたものが通気カスにキャリ
ーオーバーされることなく槽内に留ったためであり、従
って実機プラント設計に際しては第４図に示すごとくメ
ツシュベルトからカーホンを払落とす機構を設けること
が有効である。On the other hand, a mesh belt system was adopted, and the reaction vessel was filled with steel wire having a wire diameter of 100 μm, and the experiments were carried out under the same temperature and raw gas conditions. The outlet exhaust gas composition at this time is CO; 8.
5%, CO2; 70.4%, other (N2.) 12
．． N20, 02); 21.1%, which is almost the same result as the fluidized bed method, was obtained. However, the amount of carbon recovered was slightly lower at 1.0 kg/Hr. This is because the material trapped on the surface of the steel wire remained in the tank without being carried over to the ventilation scum.Therefore, when designing the actual plant, a mechanism to remove the carphone from the mesh belt is provided as shown in Figure 4. This is effective.
（発明の効果）
以上述へた如く本発明により転炉あるいは溶解炉より副
生ガスとして得られるＧＯを主成分とした廉価な原料ガ
スを用いて、気体からＣを生成するため極めて純度の高
いＣが高い収率で得ることができ、その効果は甚大であ
る。(Effects of the Invention) As described above, the present invention generates C from gas using an inexpensive raw material gas mainly composed of GO obtained as a by-product gas from a converter or melting furnace, resulting in extremely high purity. C can be obtained in high yield, and the effect is enormous.
第１図は副生ガス温度と炭素収率（％）の関係を示す図
、第２図は本発明により高純度カーボン微粒子を製造す
る態様例の略断面図及びガスフロー図、第３図は第２図
に金属粉体の循環再生系を付設した場合を示す図、第４
図は金属粉体にかえてメツシュベルトを用いた場合の実
施態様例を示す図である。
１・・・鉄粉層 ３・・・冷却管６・・・バッ
グフィルター
９・・・熱電対
１１・・・副生ガスの供給管
１２・・・熱交換器 １４・・・円筒客器１７・・
・リサイクルルート
１８・・・メツシュベルト
２２・・・水冷ジャケット ２３．３２・・・当接板第
１図
温度（°ｄ）Fig. 1 is a diagram showing the relationship between by-product gas temperature and carbon yield (%), Fig. 2 is a schematic cross-sectional view and gas flow diagram of an embodiment of producing high-purity carbon particles according to the present invention, and Fig. 3 is a diagram showing the relationship between by-product gas temperature and carbon yield (%). Figure 2 shows a case where a metal powder circulation regeneration system is attached, Figure 4
The figure shows an example of an embodiment in which a mesh belt is used instead of metal powder. 1... Iron powder layer 3... Cooling pipe 6... Bag filter 9... Thermocouple 11... By-product gas supply pipe 12... Heat exchanger 14... Cylindrical passenger device 17・・・
・Recycling route 18...Mesh belt 22...Water cooling jacket 23.32...Temperature (°d) of contact plate Figure 1
Claims (1)
主成分とする副生ガスを４００〜６００℃に温度制御し
て鉄粉層内に導入し該鉄粉層内を流動せしめつつ、前記
の副生ガス中の一酸化炭素を ２ＣＯ→ＣＯ＿２＋Ｃ なる反応を行なわしめ該鉄粉の表面に付着した微粉炭素
を分解回収することを特徴とした高純度カーボン微粒子
の製造法。 ２ 精錬炉、あるいは溶解炉から発生する一酸化炭素を
主成分とする副生ガスを４００〜６００℃に温度制御し
て炉内を移動する鉄製メッシュベルトに接触せしめ、前
記の副正ガス中の一酸化炭素を ２ＣＯ→ＣＯ＿２＋Ｃ なる反応を行なわしめて、該鉄粉の表面に付着した微粉
炭素を分離回収することを特徴とした高純度カーボン微
粒子の製造法。[Claims] 1. A by-product gas containing carbon monoxide as a main component generated from a smelting furnace or a melting furnace is controlled at a temperature of 400 to 600°C and introduced into the iron powder layer. A method for producing high-purity carbon particles, characterized in that carbon monoxide in the by-product gas undergoes a reaction of 2CO→CO_2+C while flowing, and fine carbon adhering to the surface of the iron powder is decomposed and recovered. 2. By-product gas mainly composed of carbon monoxide generated from a smelting furnace or melting furnace is temperature-controlled at 400 to 600°C and brought into contact with an iron mesh belt moving inside the furnace. A method for producing high-purity carbon particles, which comprises subjecting carbon monoxide to a reaction of 2CO→CO_2+C and separating and recovering fine carbon adhering to the surface of the iron powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63149359A JPH01317110A (en) | 1988-06-17 | 1988-06-17 | Production of fine carbon powder having high purity |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63149359A JPH01317110A (en) | 1988-06-17 | 1988-06-17 | Production of fine carbon powder having high purity |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01317110A true JPH01317110A (en) | 1989-12-21 |
Family
ID=15473408
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63149359A Pending JPH01317110A (en) | 1988-06-17 | 1988-06-17 | Production of fine carbon powder having high purity |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01317110A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0945402A1 (en) * | 1998-03-25 | 1999-09-29 | Research Institute of Innovative Technology for the Earth | Method for producing carbon |
| JP2018104282A (en) * | 2012-04-16 | 2018-07-05 | シーアストーン リミテッド ライアビリティ カンパニー | Method for producing solid carbon by reducing carbon dioxide |
-
1988
- 1988-06-17 JP JP63149359A patent/JPH01317110A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0945402A1 (en) * | 1998-03-25 | 1999-09-29 | Research Institute of Innovative Technology for the Earth | Method for producing carbon |
| JP2018104282A (en) * | 2012-04-16 | 2018-07-05 | シーアストーン リミテッド ライアビリティ カンパニー | Method for producing solid carbon by reducing carbon dioxide |
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