JP4961756B2 - Carbon material and manufacturing method thereof - Google Patents
Carbon material and manufacturing method thereof Download PDFInfo
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本発明は、炭素材及びその製造方法に関するものである。 The present invention relates to a carbon material and a method for producing the same.
還元雰囲気中での排気ガスを発生しながら処理される炭素前駆体の熱処理による炭素材の製造においては、熱処理炉内の圧力や雰囲気の状態により炭素材の物性に大きな違いが現れる。熱処理炉内の圧力上昇を抑える為、雰囲気ガスの流量調整や、圧力をかけない発生ガスによる雰囲気置換にて圧力上昇を抑えている。又、雰囲気を一定に保つ為、導入雰囲気ガス流量を過剰に流し特性維持又は向上に努める方法（例えば、特許文献１参照）がある。これら従来方法は雰囲気ガスまたは熱処理温度条件を変更する必要があり、大規模設備条件に合わない場合があった。あるいは、小規模設備処理条件と比べて大規模設備処理条件を大きく変えないと熱処理後の炭素材物性が同じ特性を得られなかったり、処理時間が長くなることがあるため、小規模設備から大規模設備への移行は難しいのが現状である。 In the production of a carbon material by heat treatment of a carbon precursor that is processed while generating exhaust gas in a reducing atmosphere, a large difference appears in the physical properties of the carbon material depending on the pressure in the heat treatment furnace and the state of the atmosphere. In order to suppress the pressure increase in the heat treatment furnace, the pressure increase is suppressed by adjusting the flow rate of the atmospheric gas or replacing the atmosphere with the generated gas without applying pressure. Further, in order to keep the atmosphere constant, there is a method (see, for example, Patent Document 1) in which an introduced atmosphere gas flow rate is excessively flowed to maintain or improve characteristics. These conventional methods need to change the atmospheric gas or heat treatment temperature conditions, and may not be suitable for large-scale equipment conditions. Alternatively, if the large-scale equipment treatment conditions are not changed significantly compared to the small-scale equipment treatment conditions, the same physical properties of the carbon material after heat treatment may not be obtained, or the treatment time may become longer. Currently, it is difficult to move to scale equipment.
本発明は、大量生産が可能な大規模設備で生産したものでありながら、従来の小規模設備で生産したものと同等の特性を有する炭素材及びその製造方法を提供するものである。 The present invention provides a carbon material having characteristics equivalent to those produced by a conventional small-scale facility, while being produced by a large-scale facility capable of mass production, and a method for producing the same.
このような目的は、下記の本発明（１）〜（３）により達成される。
（１）排気ガス用配管を有する熱処理炉を用いて、炭素前駆体を熱処理してなる炭素材の製造方法であって、前記熱処理炉容積が前記炭素前駆体１ｇ当たり０．００２Ｌ以上であり、前記排気ガス用配管の内面積は、前記炭素前駆体１ｋｇ当たり０．１ｃｍ 2 以上であり、炉内排気ガス出口圧力は２ｋＰａ以下であることを特徴とする炭素材の製造方法。
（２）前記熱処理は、不活性ガス雰囲気下で行われるものである（１）に記載の炭素材の製造方法。
（３）（１）又は（２）に記載の炭素材の製造方法によって得られることを特徴とする炭素材。
Such an object is achieved by the following present inventions (1) to ( 3 ).
(1) using a heat treatment furnace having an exhaust gas pipe, a method for producing a carbon material obtained by heat-treating the carbon precursor state, and are the heat treatment furnace volume wherein the carbon precursor 1g per 0.002L more The method for producing a carbon material , wherein an inner area of the exhaust gas pipe is 0.1 cm 2 or more per kg of the carbon precursor , and an exhaust gas outlet pressure in the furnace is 2 kPa or less .
(2) The carbon material manufacturing method according to (1), wherein the heat treatment is performed in an inert gas atmosphere.
( 3 ) A carbon material obtained by the method for producing a carbon material according to (1) or (2) .
本発明によれば、大量生産が可能な大規模設備で生産したものでありながら、従来の小規模設備で生産したものと同等の特性を有する炭素材を得ることができる。 According to the present invention, it is possible to obtain a carbon material having characteristics equivalent to those produced by a conventional small-scale facility while being produced by a large-scale facility capable of mass production.
本発明は、排気ガス配管を有する熱処理炉を用いて、炭素前駆体を熱処理してなる炭素材の製造方法であって、前記熱処理炉容積が前記炭素前駆体１ｇ当たり０．００２Ｌ以上であることを特徴とする炭素材の製造方法である。
また、本発明は上記炭素材の製造方法で得られることを特徴とする炭素材である。
まず、本発明の炭素材の製造方法（以下、単に「製造方法」ということがある）について詳細に説明する。
The present invention is a method for producing a carbon material obtained by heat treating a carbon precursor using a heat treatment furnace having an exhaust gas pipe, wherein the heat treatment furnace volume is 0.002 L or more per 1 g of the carbon precursor. Is a method for producing a carbon material.
Moreover, this invention is a carbon material characterized by the above-mentioned.
First, a method for producing a carbon material of the present invention (hereinafter sometimes simply referred to as “manufacturing method”) will be described in detail.
本発明の製造方法においては、上記熱処理炉容積が炭素前駆体１ｇ当たり０．００２Ｌ以上であることを特徴とする。さらに好ましくは０．００５Ｌ以上である。特に好ましくは０．０１Ｌ以上である。
炭素前駆体１ｇに対して熱処理炉容積を上記とすることで、熱処理の際に炭素前駆体より発生する揮発分が炉内に拡散しやすく、揮発分の発生を促すことになり、大規模設備に移行しても小規模設備で熱処理して得られるものと同等の細孔を有する炭素材を得ることができる。
In the production method of the present invention, the volume of the heat treatment furnace is 0.002 L or more per 1 g of the carbon precursor. More preferably, it is 0.005L or more. Especially preferably, it is 0.01L or more.
By setting the heat treatment furnace volume to 1 g of the carbon precursor, the volatile matter generated from the carbon precursor during the heat treatment is easily diffused into the furnace, and the generation of the volatile matter is promoted. Even if it moves to, the carbon material which has the pore equivalent to what is obtained by heat-processing with a small-scale installation can be obtained.
本発明の製造方法における上記熱処理は、不活性ガス雰囲気下で行われることが好ましい。不活性ガス雰囲気下で熱処理することで、特に処理時の過剰な酸化劣化による品質低下を防ぐことができる。
上記不活性ガスとしては、例えば、窒素、アルゴン、二酸化炭素等を用いることができる。この中でも汎用性、コスト及び品質制御の観点から窒素を用いることが好ましい。
又、通常、還元ガスを流すことにより炉内排ガス出口付近の圧力は５ｋＰａ以下が好ましい。この炉内排ガス出口圧力で熱処理することで炭素材の構造を壊すことなく処理することができる。
The heat treatment in the production method of the present invention is preferably performed in an inert gas atmosphere. By performing the heat treatment in an inert gas atmosphere, it is possible to prevent deterioration in quality due to excessive oxidative deterioration during the treatment.
As said inert gas, nitrogen, argon, a carbon dioxide etc. can be used, for example. Among these, it is preferable to use nitrogen from the viewpoint of versatility, cost, and quality control.
In general, the pressure near the exhaust gas outlet in the furnace is preferably 5 kPa or less by flowing a reducing gas. It can process without destroying the structure of a carbon material by heat-processing by this exhaust gas exit pressure in a furnace.
熱処理温度は、８００℃以上で行われることが好ましい。８００℃以上で熱処理が行われることで活性な官能基反応が減少し、環縮合反応がメインとなり品質を安定させることができる。
熱処理温度までの昇温速度は４００℃／時間以下が好ましい。昇温速度４００℃／時間以下で処理を行うことで、熱源への付加も抑えられるとともに、処理内温度が昇温スピードへ追いつき、品質の安定化を図ることができる。
また、熱処理温度に到達後の処理時間は３０分以上が好ましい。処理時間を３０分以上とすることで、到達温度での反応が落ち着き、処理品の品質を安定させることができる。
The heat treatment temperature is preferably 800 ° C. or higher. By heat treatment at 800 ° C. or higher is performed active government functional group reaction is reduced, the quality cyclocondensation reaction becomes the main can be stabilized.
The heating rate up to the heat treatment temperature is preferably 400 ° C./hour or less. By performing the treatment at a temperature increase rate of 400 ° C./hour or less, addition to the heat source can be suppressed, and the temperature in the process can catch up with the temperature increase rate, thereby stabilizing the quality.
The treatment time after reaching the heat treatment temperature is preferably 30 minutes or more. By setting the treatment time to 30 minutes or more, the reaction at the ultimate temperature is settled, and the quality of the treated product can be stabilized.
また、本発明の製造方法に用いられる排気ガス用配管を有する熱処理炉においては、排出ガス用配管の内面積が炭素前駆体１ｋｇ当り０．１ｃｍ2以上であることが好ましい。更に好ましくは、０．３５ｃｍ2以上である。排出ガス用配管の内面積を上記範囲とすることで、大規模設備に移行しても炉内で発生した揮発性ガスを炉外に容易に排出することができ、熱処理雰囲気の変化が少なく、安定した品質の炭素材を生産することができる。
Further, in the heat treatment furnace having the exhaust gas pipe used in the production method of the present invention, the inner area of the exhaust gas pipe is preferably 0.1 cm 2 or more per 1 kg of the carbon precursor. More preferably, it is 0.35 cm 2 or more. By setting the inner area of the exhaust gas pipe within the above range, the volatile gas generated in the furnace can be easily discharged out of the furnace even when shifting to a large-scale facility, and there is little change in the heat treatment atmosphere, Stable quality carbon material can be produced.
次に、本発明の炭素材について説明する。
本発明の炭素材は、上記本発明の製造方法によって得られることを特徴とする。上記製造方法によって得られる本発明の炭素材は、大規模設備で生産されたものでありながら、小規模設備で製造されたものと同等の性能を有し、大量生産による大幅なコストダウンが可能となるものである。
Next, the carbon material of the present invention will be described.
The carbon material of the present invention is obtained by the production method of the present invention. The carbon material of the present invention obtained by the above production method has the same performance as that produced by a small-scale facility, while being produced by a large-scale facility, and can greatly reduce the cost by mass production. It will be.
以下、本発明の製造方法を実施例により説明する。しかし、本発明は実施例に限定されるものではない。 Hereinafter, the production method of the present invention will be described with reference to examples. However, the present invention is not limited to the examples.
（基準例）炉内容積３２Ｌ、炉外に発生ガスを排出する排ガス用配管内面積０．５ｃｍ2、雰囲気窒素ガスの熱処理炉にて６００℃処理フェノール樹脂系炭素前駆体（住友ベークライト社製ＰＲ−２１７の６００℃処理品、炭素組成比８９％）０．５ｋｇを高さ５０ｍｍ、２００ｍｍ角の匣鉢に仕込み、窒素雰囲気下、昇温１００℃／ｈ、１０００℃３ｈ処理し、炭素材Ａ０．４５ｋｇを得た。（炉容積：０．０６４Ｌ／ｇ、排ガス用配管内面積：１ｃｍ2／ｋｇ、炉内排ガス出口圧力：２ｋＰａ）
得られた炭素材Ａの炭素組成比、及び比表面積を評価した。
(Reference Example) Furnace volume 32 L, exhaust gas piping area 0.5 cm 2 for discharging generated gas outside the furnace, 600 ° C. phenolic resin carbon precursor (PR manufactured by Sumitomo Bakelite Co., Ltd.) in a heat treatment furnace of atmospheric nitrogen gas -217, 600 ° C treated product, carbon composition ratio 89%) 0.5 kg in a 50 mm high, 200 mm square mortar, heated at 100 ° C / h, 1000 ° C for 3 h in a nitrogen atmosphere, and carbon material A0 .45 kg was obtained. (Furnace volume: 0.064 L / g, exhaust gas piping area: 1 cm 2 / kg, furnace exhaust gas outlet pressure: 2 kPa)
The carbon composition ratio and specific surface area of the obtained carbon material A were evaluated.
（実施例１）炉内容積５００Ｌ、炉外に発生ガスを排出する排ガス用配管内面積７８．５ｃｍ2、雰囲気窒素ガスの熱処理炉にて６００℃処理フェノール樹脂系炭素前駆体（住友ベークライト社製ＰＲ−２１７の６００℃処理品、炭素組成比８９％）３０ｋｇを高さ５０ｍｍ、２５０ｍｍ角の匣鉢に１ｋｇづつ仕込み、計３０個を２列３段で炉内に配置させた以外は基準例と同法で行い、炭素材Ｂ２４ｋｇを得た。（炉容積：０．０１７Ｌ／ｇ、排ガス用配管内面積：２．６ｃｍ2／ｋｇ、炉内圧力：１ｋＰａ）
（実施例２）６００℃処理フェノール樹脂系炭素前駆体６０ｋｇを実施例１と同形状の匣鉢を用い１．２ｋｇづつ仕込み、計５０個を２列５段で炉内に配置させた以外は実施例１と同法で行い炭素材Ｃ４８ｋｇを得た。（炉容積：０．００８Ｌ／ｇ、排ガス用配管内面積：１．３ｃｍ2／ｋｇ、炉内排ガス出口圧力：２ｋＰａ）
（実施例３）炉内容積を２０００Ｌにし、炉外に発生ガスを排出する排ガス用配管内面積を２８．３ｃｍ2にした以外は実施例２と同法で行い、炭素材Ｄ４８ｋｇを得た。（炉容積：０．０３３Ｌ／ｇ、排ガス用配管内面積：０．４７ｃｍ2／ｋｇ、炉内排ガス出口圧力：２ｋＰａ）
(Example 1) Furnace volume 500 L, exhaust gas piping internal area 78.5 cm 2 for exhausting generated gas outside the furnace, 600 ° C. phenol resin carbon precursor (manufactured by Sumitomo Bakelite Co., Ltd.) in a heat treatment furnace of atmospheric nitrogen gas PR-217 treated product at 600 ° C, carbon composition ratio 89%) 30 kg of 50kg high and 250mm square mortars were charged 1kg at a time, and a total of 30 pieces were placed in the furnace in two rows and three stages. In the same manner, 24 kg of carbon material B was obtained. (Furnace volume: 0.017 L / g, exhaust gas piping area: 2.6 cm 2 / kg, furnace pressure: 1 kPa)
(Example 2) 60 kg of a phenol resin-based carbon precursor treated at 600 ° C. was charged in 1.2 kg using a mortar having the same shape as in Example 1, and a total of 50 pieces were arranged in a furnace in two rows and five stages. It carried out by the same method as Example 1, and obtained carbon material C48kg. (Furnace volume: 0.008 L / g, exhaust gas pipe area: 1.3 cm 2 / kg, furnace exhaust gas outlet pressure: 2 kPa)
(Example 3) A carbon material D of 48 kg was obtained in the same manner as in Example 2 except that the furnace volume was 2000 L and the area inside the exhaust gas pipe for discharging the generated gas to the outside of the furnace was 28.3 cm 2 . (Furnace volume: 0.033 L / g, exhaust gas piping area: 0.47 cm 2 / kg, furnace exhaust gas outlet pressure: 2 kPa)
（比較例１）熱処理炉内容積３２Ｌ、炉外に発生ガスを排出する排ガス用配管内面積７８．５ｃｍ2、雰囲気窒素ガスの熱処理炉にて６００℃処理フェノール樹脂系炭素前駆体（住友ベークライト社製ＰＲ−２１７の６００℃処理品、炭素組成比８９％）２５ｋｇを高さ１００ｍｍ、１００×３１５ｍｍ角の匣鉢に仕込み、計１個を炉内に配置させた以外は基準例１と同法で行い、炭素材Ｅ２０ｋｇを得た。（炉容積：０．００１２８Ｌ／ｇ、排ガス用配管内面積：３．１４ｃｍ2／ｋｇ、炉内排ガス出口圧力：４ｋＰａ）
（比較例２）炉外に発生ガスを排出する排ガス用配管内面積１２．５６ｃｍ2、６００℃処理フェノール樹脂系炭素前駆体３００ｋｇを実施例１と同様な容器に２．４ｋｇづつ仕込み、計１２５個にした以外は実施例１と同法で行い、炭素材Ｆ２４ｋｇを得た。（炉容積：０．００１７Ｌ／ｇ、排ガス用配管内面積：０．０４ｃｍ2／ｋｇ、炉内排ガス出口圧力：２３ｋＰａ）
(Comparative Example 1) Heat treatment furnace internal volume 32L, exhaust gas piping internal area 78.5cm 2 for discharging generated gas outside the furnace, 600 ° C treated phenol resin carbon precursor (Sumitomo Bakelite Co., Ltd.) in a heat treatment furnace of atmospheric nitrogen gas PR-217 manufactured at 600 ° C., carbon composition ratio 89%) 25 kg in a 100 mm high, 100 × 315 mm square mortar, and placed in the furnace in the same way as in Reference Example 1 The carbon material E20kg was obtained. (Furnace volume: 0.00128 L / g, exhaust gas piping area: 3.14 cm 2 / kg, furnace exhaust gas outlet pressure: 4 kPa)
(Comparative example 2) The inside area of the exhaust gas pipe for discharging the generated gas to the outside of the furnace was 12.56 cm 2 , and 300 kg of a 600 ° C.-treated phenol resin-based carbon precursor was charged into a container similar to that of Example 1 in an amount of 2.4 kg. A carbon material F24 kg was obtained in the same manner as in Example 1 except that the carbon material F was used. (Furnace volume: 0.0017 L / g, exhaust gas piping area: 0.04 cm 2 / kg, furnace exhaust gas outlet pressure: 23 kPa)
（炭素材の評価）
１．炭素材の元素組成比
パーキンエルナー社製元素分析装置ＣＨＮＳ２４００を用いて測定した。
(Evaluation of carbon materials)
1. Elemental composition ratio of carbon material The carbon material was measured using an element analyzer CHNS2400 manufactured by Perkin Elner.
２．比表面積
ユアサアイオニクス社製ＮＯＶＡ１２００を用い、窒素ガスＢＥＴ３点法にて測定した。
以上の評価結果を表１に示す。
2. Specific surface area Using a NOVA 1200 manufactured by Yuasa Ionics Co., Ltd., a nitrogen gas BET three-point method was used for measurement.
The above evaluation results are shown in Table 1.
表１の結果より、実施例１は、基準例の約６０倍量の処理を行い、実施例２、３は、基準例の約１２０倍量の処理を行ったものであるが、熱処理炉容積が炭素前駆体１ｇ当たり０．００２Ｌ以上である本発明の製造方法を用いたことにより、基準例で得られた炭素材の元素組成比、比表面積と同等の炭素材を得ることできた。すなわち、本発明の製造方法によって、大規模生産設備ながら小規模設備で生産しものと同等の特性を有する炭素材を得ることができることを証明できた。
一方、熱処理炉容積が炭素前駆体１ｇ当たり０．００２Ｌ以下であった比較例１、２は炭素材の元素組成比は良好であったが、比表面積は基準例に比較し、大幅に小さなものであった。
From the results in Table 1, Example 1 was processed about 60 times the amount of the reference example, and Examples 2 and 3 were processed about 120 times the amount of the reference example. By using the production method of the present invention in which the amount is 0.002 L or more per 1 g of carbon precursor, a carbon material equivalent to the elemental composition ratio and specific surface area of the carbon material obtained in the reference example could be obtained. That is, it has been proved that the carbon material having the same characteristics as those produced by the small-scale equipment can be obtained by the production method of the present invention.
On the other hand, Comparative Examples 1 and 2 in which the volume of the heat treatment furnace was 0.002 L or less per 1 g of the carbon precursor had a good elemental composition ratio of the carbon material, but the specific surface area was significantly smaller than that of the reference example. Met.
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