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JP4069822B2 - Method for producing activated carbon - Google Patents
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JP4069822B2 - Method for producing activated carbon - Google Patents

Method for producing activated carbon Download PDF

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JP4069822B2
JP4069822B2 JP2003272528A JP2003272528A JP4069822B2 JP 4069822 B2 JP4069822 B2 JP 4069822B2 JP 2003272528 A JP2003272528 A JP 2003272528A JP 2003272528 A JP2003272528 A JP 2003272528A JP 4069822 B2 JP4069822 B2 JP 4069822B2
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activated carbon
carbonaceous material
slurry
alkali metal
double layer
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JP2005029444A (en
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義史 江川
昭典 山端
充則 人見
隆範 北村
健 藤野
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Honda Motor Co Ltd
Kuraray Chemical Co Ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for manufacturing activated carbon that is capable of reducing the amount of a magnetic heavy metal incorporated to the level of electronic materials such as an electrical double layer capacitor and the like. <P>SOLUTION: The method for manufacturing the activated carbon with a small heavy metal content comprises charging the activated carbon obtained by performing the activation treatment of a carbonaceous material using an alkali metal hydroxide into water, filtrating the resulting slurry-like substance, treating the resulting filtered slurry with a magnet having magnetic force of 5,000 gauss or more and then subjecting the same to washing. <P>COPYRIGHT: (C)2005,JPO&amp;NCIPI

Description

本発明は、活性炭の製造方法に関する。さらに詳しくは、炭素質材料をアルカリ金属水酸化物を用いて賦活処理して得た賦活処理物を水中に投入し、得られたスラリー状物を濾過し、得られた濾過スラリーを磁石で処理した後、洗浄する活性炭の製造方法に関する。   The present invention relates to a method for producing activated carbon. More specifically, the activated material obtained by activating the carbonaceous material with an alkali metal hydroxide is put into water, the resulting slurry is filtered, and the resulting filtered slurry is treated with a magnet. Then, the present invention relates to a method for producing activated carbon to be washed.

活性炭は、食品工業、化学工業、医薬品工業、その他各種工業にわたって広く使用されているが、従来、これらに使用される活性炭は、主としてその吸着性能を利用することで開発されてきた。近年、活性炭が電気二重層キャパシタ用の分極性電極として静電容量に優れることに着目し、活性炭を電気二重層キャパシタの電極用とする開発がなされており、エレクトロニクス分野の発展と共に、需要が急成長している。   Activated carbon is widely used in the food industry, chemical industry, pharmaceutical industry, and other various industries. Conventionally, activated carbon used for these has been developed mainly by utilizing its adsorption performance. In recent years, attention has been paid to the fact that activated carbon is excellent in electrostatic capacity as a polarizable electrode for electric double layer capacitors, and activated carbon has been developed for use in electrodes for electric double layer capacitors. Growing.

従来、このような電気二重層キャパシタ向け活性炭としては、ヤシ殻、木粉、石炭などの活性炭原料を水蒸気、ガスなどの酸性条件下で賦活したものが一般的であるが、薬剤を用いたアルカリ条件下での賦活も知られている。例えば、このような活性炭原料をアルカリ金属の水酸化物浴中700℃未満で熱処理する炭素質素材の製造方法が提案されている(特許文献1)。また、活性炭原料としてピッチやコークスを使用することも知られており、例えば、石油コークスまたは石炭ピッチコークスを炭化処理し、アルカリ金属水酸化物で賦活処理する炭素材の製造方法が提案されている(特許文献2)。   Conventionally, as such activated carbon for electric double layer capacitors, activated carbon raw materials such as coconut shell, wood powder, and coal are generally activated under acidic conditions such as water vapor and gas. Activation under conditions is also known. For example, a method for producing a carbonaceous material in which such an activated carbon raw material is heat-treated at less than 700 ° C. in an alkali metal hydroxide bath has been proposed (Patent Document 1). It is also known to use pitch or coke as a raw material for activated carbon. For example, a carbon material production method is proposed in which petroleum coke or coal pitch coke is carbonized and activated with an alkali metal hydroxide. (Patent Document 2).

ところで、上記のような方法で得られた活性炭には、原料、装置などに由来して通常Ni、Fe、Crなどの重金属が含まれているため、そのような重金属を含んだままの活性炭を分極性電極に成型して電気二重層キャパシタに使用すると、重金属の還元析出によるデンドライト化によるショートなどの障害を起こしたり、自己放電保持率が低下するなどの問題が生ずるおそれがある。従って、活性炭を電気二重層キャパシタ用の分極性電極の材料として使用する場合は、特に綿密な洗浄がなされているのが現状である。   By the way, since the activated carbon obtained by the method as described above usually contains heavy metals such as Ni, Fe, Cr, etc. derived from raw materials, equipment, etc., activated carbon containing such heavy metals is used. If the electrode is molded into a polarizable electrode and used in an electric double layer capacitor, problems such as a short circuit due to dendrite formation due to reduction deposition of heavy metals, or a decrease in self-discharge retention rate may occur. Therefore, when activated carbon is used as a material for a polarizable electrode for an electric double layer capacitor, the current situation is that it has been thoroughly cleaned.

一方、活性炭から磁性金属を除くという観点から、活性炭を磁石で処理する技術が知られている(特許文献3、4)。この技術は、木材を乾留し、水蒸気賦活して活性炭を得るに際し、磁力選別機を使用し、比較的大きな磁性金属を磁石で選別する技術である。   On the other hand, from the viewpoint of removing a magnetic metal from activated carbon, techniques for treating activated carbon with a magnet are known (Patent Documents 3 and 4). This technique is a technique in which a relatively large magnetic metal is selected with a magnet using a magnetic separator when carbon is activated to obtain activated carbon by steam activation.

WO91/12203号公報WO91 / 12203 Publication 特開平10−199767号公報Japanese Patent Laid-Open No. 10-199767 特開平10−338513号公報JP 10-338513 A 特開2001−233610号公報JP 2001-233610 A

しかしながら、電気二重層キャパシタ用の分極性電極を形成するための活性炭を製造するためには、煩雑で綿密な洗浄を行う必要があるため、洗浄コストが多大なものとなり、活性炭の生産コストを押し上げてしまうという問題があった。また、活性炭から金属を除くために、活性炭を磁石で処理する技術の場合、活性炭粒や活性炭粉の中に独立的に存在している磁性金属粒や磁性金属粉を取り除くことを意図しており、電気二重層キャパシタ用の分極性電極とする場合のように、金属含有量をデンドライト化が生じない程度にまで精製できる技術ではないという問題がある。このように、電気二重層キャパシタ用の分極性電極に使用する活性炭の重金属含有量を低減させるべきであることは従来からも指摘されてきたが、重金属を簡便かつ低コストで低減させる手法が見出されていないというのが現状である。   However, in order to produce activated carbon for forming polarizable electrodes for electric double layer capacitors, it is necessary to perform complicated and meticulous cleaning, which increases the cleaning cost and increases the production cost of activated carbon. There was a problem that. In addition, in the case of a technology in which activated carbon is treated with a magnet in order to remove the metal from the activated carbon, it is intended to remove the magnetic metal particles and magnetic metal powder that exist independently in the activated carbon particles and activated carbon powder. However, as in the case of a polarizable electrode for an electric double layer capacitor, there is a problem that it is not a technique that can purify the metal content to such an extent that dendrite formation does not occur. As described above, it has been pointed out that the heavy metal content of the activated carbon used for the polarizable electrode for the electric double layer capacitor should be reduced, but there is a method for reducing the heavy metal easily and at low cost. The current situation is that it has not been released.

本発明の目的は、重金属の混入が少ない活性炭を簡単に得ることができる工業的に優れた活性炭の製造方法を提供することにある。   An object of the present invention is to provide an industrially excellent method for producing activated carbon that can easily obtain activated carbon with less heavy metal contamination.

本発明者らは、さらに検討を重ね、活性炭のスラリー状物を濾過し、得られた濾過スラリーを特定の磁力強度を有する磁石で処理し、さらに洗浄することにより、上記目的を達成することができることを見出し、本発明に至った。   The inventors of the present invention can further achieve the above object by further studying, filtering the slurry of activated carbon, treating the obtained filter slurry with a magnet having a specific magnetic strength, and further washing. As a result, the inventors have found out that the present invention can be achieved.

すなわち、本発明は、炭素質材料をアルカリ金属水酸化物を用いて賦活処理して活性炭を製造する活性炭の製造方法において、賦活処理物を水中に投入し、得られたスラリー状物を濾過処理し、得られた濾過スラリーを磁力強度5000ガウス以上の磁石で処理した後、洗浄に付すことを特徴とする活性炭の製造方法を提供する。   That is, the present invention provides an activated carbon production method for producing activated carbon by activating a carbonaceous material using an alkali metal hydroxide, and activating the activated product into water, and filtering the resulting slurry. Then, the obtained filtration slurry is treated with a magnet having a magnetic strength of 5000 gauss or more, and then subjected to washing.

本発明の活性炭の製造方法によれば、磁性重金属の混入量を低減した活性炭を簡便な操作で製造することができる。   According to the method for producing activated carbon of the present invention, activated carbon with a reduced amount of magnetic heavy metal mixed can be produced by a simple operation.

本発明は、炭素質材料をアルカリ金属水酸化物を用いて賦活処理し、得られた賦活処理物を水中に投入し、得られたスラリー状物を濾過処理し、得られた濾過スラリーを磁力強度5000ガウス以上の磁石で処理した後、洗浄に付すことを特徴とする活性炭の製造方法である。   In the present invention, the carbonaceous material is activated using an alkali metal hydroxide, the obtained activated product is put into water, the obtained slurry is filtered, and the obtained filtered slurry is magnetically treated. It is a method for producing activated carbon, characterized by subjecting it to washing after treatment with a magnet having a strength of 5000 gauss or more.

本発明の製造方法においては、まず、炭素質材料をアルカリ金属水酸化物を用いて賦活処理して賦活処理物を得る。より具体的には、塊状、フレーク状等のアルカリ金属水酸化物を微粉砕処理し、得られた微粉砕処理物を所定の配合比で均一に混合し、得られた混合物を固体状態を保ったまま造粒処理し、得られた造粒処理物を脱水処理し、得られた脱水処理物を賦活処理することが好ましい。   In the production method of the present invention, first, the carbonaceous material is activated using an alkali metal hydroxide to obtain an activated product. More specifically, the alkali metal hydroxide such as a lump or flake is finely pulverized, the obtained finely pulverized product is uniformly mixed at a predetermined blending ratio, and the resulting mixture is maintained in a solid state. It is preferable to perform the granulation treatment as it is, dehydrate the obtained granulated product, and activate the obtained dehydrated product.

本発明に使用する炭素質材料としては、賦活することによって活性炭を形成するものであればとくに制限はなく、例えば、ヤシ殻、石油系及び/又は石炭系ピッチ、コークス、フェノール系樹脂、塩化ビニルなどを挙げることができる。なかでも易黒鉛系炭素質材料が好ましい。易黒鉛系炭素質材料としては例えばメソフェーズピッチ系炭素材料を挙げることができる。なかでもメソフェーズピッチ系炭素繊維が好ましい。なお、炭素質材料の形状は限定されるものではなく、粒状、微粉状、繊維状、シート状など種々の形状のものを使用することができる。   The carbonaceous material used in the present invention is not particularly limited as long as activated carbon is formed by activation. For example, coconut shell, petroleum-based and / or coal-based pitch, coke, phenolic resin, vinyl chloride. And so on. Of these, an easily graphite-based carbonaceous material is preferable. Examples of the easily graphite-based carbonaceous material include mesophase pitch-based carbon materials. Of these, mesophase pitch-based carbon fibers are preferred. The shape of the carbonaceous material is not limited, and various shapes such as a granular shape, a fine powder shape, a fiber shape, and a sheet shape can be used.

本発明で用いられるアルカリ金属水酸化物としては、例えば、水酸化ナトリウム、水酸化カリウム、水酸化リチウム、水酸化セシウムなどのアルカリ金属水酸化物の粒状物、又はこれらの混合物が挙げられる。大きな静電容量を得る観点からは、水酸化ナトリウム及び/又は水酸化カリウムを使用するのが好ましい。なかでも、水酸化カリウムが好ましい。これらのアルカリ金属水酸化物は、一般に市販されているものを使用することが可能である。金属水酸化物の含水量としては、1〜20重量%のものを使用することができるが、取扱いの点から1〜10重量%のものが好ましい。アルカリ金属水酸化物が塊状物である場合は、前記のような粉砕機により粉砕して100μm以下程度の粒状とするのが好ましい。   Examples of the alkali metal hydroxide used in the present invention include particulates of alkali metal hydroxides such as sodium hydroxide, potassium hydroxide, lithium hydroxide and cesium hydroxide, or mixtures thereof. From the viewpoint of obtaining a large capacitance, it is preferable to use sodium hydroxide and / or potassium hydroxide. Of these, potassium hydroxide is preferable. As these alkali metal hydroxides, commercially available ones can be used. The water content of the metal hydroxide can be 1 to 20% by weight, but is preferably 1 to 10% by weight from the viewpoint of handling. In the case where the alkali metal hydroxide is a lump, it is preferably pulverized by the pulverizer as described above to have a particle size of about 100 μm or less.

塊状、フレーク状等のアルカリ金属水酸化物を微粉砕する粉砕処理の方法は、とくに限定されないが、アルカリ金属水酸化物に炭素質材料を0.5〜10重量%、好ましくは1〜5重量%添加してボールミル、ダイナミックミル等公知の粉砕装置を用いてバッチまたは連続方式で実施すると粉砕処理を効率よく行うことができ、製造工程の面から好ましい。アルカリ金属水酸化物は一般に吸湿、潮解性を有するため−10℃以下程度の低露点空気または湿分を含まない窒素、ヘリウム、アルゴン等の不活性ガス雰囲気下で実施するのが好ましい。   The method for pulverizing the alkali metal hydroxide such as a lump or flake is not particularly limited, but the carbonaceous material is added to the alkali metal hydroxide in an amount of 0.5 to 10% by weight, preferably 1 to 5% by weight. When added in a batch or continuous mode using a known pulverizer such as a ball mill or a dynamic mill, the pulverization can be efficiently performed, which is preferable from the viewpoint of the manufacturing process. Since alkali metal hydroxide generally has moisture absorption and deliquescence properties, it is preferably carried out in a low dew point air of about −10 ° C. or less or in an inert gas atmosphere such as nitrogen, helium, or argon that does not contain moisture.

上述の粉砕処理により微粉砕されたアルカリ金属水酸化物に、炭素質材料を所定の配合比で均一に混合処理する。この処理においては、炭素質材料とアルカリ金属水酸化物をできるだけ均一になるように十分に混合することが、賦活効率の点で好ましい。アルカリ金属水酸化物は賦活のバラツキと過賦活の防止を考慮し、一般的には重量割合で炭素質材料1に対して好ましくは1.2〜4、さらに好ましくは1.3〜3で配合される。アルカリ金属水酸化物として炭素質材料の共存下に微粉砕したアルカリ金属水酸化物の微粒子を用いると混合性が良好となり、組成比の変動の少ない均一な混合物が得られ、好ましい。   The alkali metal hydroxide finely pulverized by the above pulverization process is uniformly mixed with a carbonaceous material at a predetermined mixing ratio. In this treatment, it is preferable in terms of activation efficiency that the carbonaceous material and the alkali metal hydroxide are sufficiently mixed so as to be as uniform as possible. In consideration of variation in activation and prevention of overactivation, the alkali metal hydroxide is generally blended at a weight ratio of preferably 1.2 to 4, more preferably 1.3 to 3 with respect to the carbonaceous material 1. Is done. It is preferable to use fine particles of alkali metal hydroxide finely pulverized in the coexistence of a carbonaceous material as the alkali metal hydroxide, because the mixing property is improved and a uniform mixture with little variation in composition ratio is obtained.

混合する温度はとくに限定されず、通常は室温下で十分である。混合機の種類はとくに限定されるものではなく、公知の回転容器型混合機や固定容器型混合機を用いることができるが、より均一な混合が得られる点で回転容器型混合機を用いるのがよい。混合機の材質は腐食をできるだけ低減させる点からニッケルとするのが好ましい。   The mixing temperature is not particularly limited, and is usually sufficient at room temperature. The type of the mixer is not particularly limited, and a known rotary container type mixer or a fixed container type mixer can be used, but the rotary container type mixer is used in that a more uniform mixing can be obtained. Is good. The material of the mixer is preferably nickel from the viewpoint of reducing corrosion as much as possible.

次に、後述する脱水での取扱いを容易にするため、炭素質材料及びアルカリ金属水酸化物に対して造粒処理を行う。得られる造粒処理物の粒径は特に制限されないが、直径0.2mm〜10mmが取扱い上好ましい。造粒は、好ましくは、0.01〜300Torr(1.33〜40000Pa)の減圧下、120℃〜140℃まで昇温することにより、固体状態を保ったまま実施することができる。昇温速度は限定されないが、0.1〜10℃/分程度が好ましい。造粒はダブルコーン型混合機等で実施できるが、造粒物の粒径、粒径分布、機壁への付着抑止等を考慮し、上記条件に回転速度を加味した条件で実施するのが好ましい。   Next, a granulating process is performed on the carbonaceous material and the alkali metal hydroxide in order to facilitate handling in dehydration described later. The particle size of the resulting granulated product is not particularly limited, but a diameter of 0.2 mm to 10 mm is preferable for handling. The granulation is preferably carried out while maintaining a solid state by raising the temperature to 120 ° C. to 140 ° C. under a reduced pressure of 0.01 to 300 Torr (1.33 to 40000 Pa). Although the rate of temperature increase is not limited, it is preferably about 0.1 to 10 ° C./min. Granulation can be carried out with a double cone type mixer, etc., but considering the particle size of the granulated product, particle size distribution, deterring of adhesion to the machine wall, etc., it should be carried out under the above conditions with the rotational speed taken into account. preferable.

造粒処理により得られた造粒処理物(即ち、炭素質材料/アルカリ金属水酸化物混合物)に対し脱水処理を施す。この場合、造粒処理物の溶融温度とその含水率の間には密接な関係があり、系の圧力を大気圧以下の適切な圧力に保ちながら、適切な昇温速度で昇温することにより、炭素質材料/アルカリ金属水酸化物混合物を、溶融させることなく固体状態のまま脱水し、その含水率を下げることができる。   A dehydration process is performed on the granulated product (ie, the carbonaceous material / alkali metal hydroxide mixture) obtained by the granulation process. In this case, there is a close relationship between the melting temperature of the granulated product and its moisture content, and the temperature is raised at an appropriate rate of temperature while maintaining the system pressure at an appropriate pressure below atmospheric pressure. The carbonaceous material / alkali metal hydroxide mixture can be dehydrated in the solid state without melting and its water content can be lowered.

次に、脱水処理物(即ち炭素質材料/アルカリ金属水酸化物の粒状混合物)に対し賦活処理を施す。具体的には、この粒状混合物を窒素、アルゴンなどの不活性ガス中で、バッチ又は連続で熱処理すればよい。熱処理の温度(賦活温度)としては、水酸化カリウムを使用した場合には、予想外にも700℃を超える領域で静電容量が臨界的に増加するので、700℃〜850℃とすることが好ましい。   Next, an activation treatment is performed on the dehydrated product (that is, the granular mixture of carbonaceous material / alkali metal hydroxide). Specifically, the granular mixture may be heat-treated in batch or continuously in an inert gas such as nitrogen or argon. As the temperature of heat treatment (activation temperature), when potassium hydroxide is used, the capacitance increases unexpectedly in a region exceeding 700 ° C., so that it may be 700 ° C. to 850 ° C. preferable.

前記の粉砕処理、混合処理、脱水処理を経て得られる炭素質材料/アルカリ金属水酸化物の粒状混合物は、賦活処理におけるアルカリ溶融による装置の腐食を回避するため、各処理内(特に賦活処理)内の昇温速度を厳密にコントロ−ルすることが好ましい。本発明者らの詳細な検討の結果によれば、該昇温速度を5℃/分以下に保持することで初期の目的に到達できる。また、昇温速度と共に昇温後の保持時間も活性炭の性能に影響を及ぼすので、700℃以上での保持時間は0.5〜8時間とすることが好ましい。   The granular mixture of carbonaceous material / alkali metal hydroxide obtained through the above pulverization, mixing, and dehydration processes is used in each process (particularly activation process) in order to avoid corrosion of the apparatus due to alkali melting in the activation process. It is preferable to strictly control the temperature rising rate. According to the results of detailed studies by the present inventors, the initial purpose can be reached by maintaining the temperature rising rate at 5 ° C./min or less. Moreover, since the holding time after temperature rising influences the performance of activated carbon together with the temperature rising rate, the holding time at 700 ° C. or higher is preferably 0.5 to 8 hours.

熱処理を行うための装置(賦活装置)としては、従来公知の回転式、流動式、移動式などの賦活装置が採用される。賦活装置の材質は腐食をできるだけ低減させる点からニッケルを主成分とする材質のものを使用するのが好ましい。賦活装置及び処理方式に関して、工業的な優位性を加味して検討を行い、賦活装置としては上記範疇の中でロータリーキルンが好ましく、処理方式としては連続方式が生産性、賦活活性炭の性能の両面から好ましい。   As an apparatus (activation apparatus) for performing heat treatment, conventionally known activation apparatuses such as a rotary type, a fluid type, and a mobile type are adopted. It is preferable to use a material mainly composed of nickel from the viewpoint of reducing corrosion as much as possible. With regard to the activation device and the processing method, the industrial superiority is taken into consideration, and as the activation device, the rotary kiln is preferable in the above category, and as the processing method, the continuous method is from both the productivity and the activated carbon performance. preferable.

なお、賦活処理により得られた賦活処理物は、後述するスラリー状物の調製に先だって、所定の温度(例えば室温)まで冷却しておくことが好ましい。冷却は、賦活処理物の燃焼を抑制するために、窒素、アルゴン、二酸化炭素などの不活性ガス気流下で行うのがよい。   In addition, it is preferable to cool the activation treatment product obtained by the activation treatment to a predetermined temperature (for example, room temperature) prior to preparation of a slurry-like material described later. Cooling is preferably performed under a stream of inert gas such as nitrogen, argon, carbon dioxide, etc., in order to suppress the combustion of the activated product.

次に、得られた賦活処理物を水中に投入し、得られたスラリー状物を濾過処理する。濾過処理は、炭素質材料に含まれる形状不良材料や不純物及び混合、脱水、賦活の各処理の際に生じる塊状の副成物や装置腐食に由来する金属塊と炭素質材料の混合物等の篩除去に有効である。   Next, the obtained activation treatment product is put into water, and the obtained slurry is filtered. Filtration treatment is performed by sieving such as poorly shaped materials contained in carbonaceous materials, impurities, and bulk by-products generated during mixing, dehydration and activation treatments, and mixtures of metal masses and carbonaceous materials derived from equipment corrosion. Effective for removal.

賦活処理物からスラリー状物の調製は、撹拌している水中に賦活処理物を投入すればよい。また、賦活処理物100重量部に対する水の量は、少なすぎると粘度が高くなりすぎ、濾過処理が円滑に進まず、多すぎると濾過処理や排水処理が煩雑となるので、好ましくは200〜2000重量部である。使用する水としては、特に金属イオンが含まれていない精製水やイオン交換水が好ましい。   Preparation of the slurry-like material from the activation treatment product may be performed by putting the activation treatment product into the stirring water. Further, if the amount of water relative to 100 parts by weight of the activated product is too small, the viscosity will be too high, the filtration process will not proceed smoothly, and if it is too large, the filtration process and the wastewater treatment will be complicated. Parts by weight. As water to be used, purified water or ion exchange water containing no metal ions is particularly preferable.

また、濾過処理に使用する濾過装置、濾過素材等は従来公知のものから選択できるが、後続の洗浄処理での酸類(例えば塩酸)を用いて洗浄する場合があることを考慮すると、耐アルカリ性、耐酸性の材質を選択するのが好ましい。耐腐食性金属材料を使用した濾過装置や耐腐食性のフッ素系樹脂等をコーティングした濾過装置を採用するのが好ましい。   In addition, a filtration device, a filtration material, and the like used for the filtration treatment can be selected from conventionally known ones, but considering that there are cases where washing is performed using acids (for example, hydrochloric acid) in the subsequent washing treatment, alkali resistance, It is preferable to select an acid-resistant material. It is preferable to employ a filtration device using a corrosion-resistant metal material or a filtration device coated with a corrosion-resistant fluororesin.

濾過素材の目開きは、炭素質材料の形状にもよるが、大きすぎると金属類を含有する活性炭粒が捕捉されないので、好ましくは75μm以下、より好ましくは60μm以下である。なお、見開きの下限は、それが小さすぎると濾過圧が高く、濾過に長時間を要するので、好ましくは10μm以上である。   The opening of the filtering material is preferably 75 μm or less, more preferably 60 μm or less, because activated carbon particles containing metals are not captured if it is too large, although it depends on the shape of the carbonaceous material. The lower limit of the spread is preferably 10 μm or more because if it is too small, the filtration pressure is high and the filtration takes a long time.

次に、得られた濾過スラリーを磁石を用いて処理することにより、磁性重金属(例えば、鉄、ニッケル、コバルト等)の除去を行う。前述したように、電気二重層キャパシタ用の活性炭は磁性重金属の含有量を極度に低減する必要があり、本発明において使用する磁石としては、磁性重金属除去向上効果の点で、その磁力強度が好ましくは5000ガウス以上、より好ましくは8000ガウス以上である。また、磁石は濾過スラリーとの接触効率を考慮し、数本の磁石を直列に配置するのが望ましい。また、磁石は永久磁石及び電磁石を適宜用いることができる。なお、磁性金属類の磁石への付着効率は、濾過スラリーと磁石の接触時間にも影響される。本発明者らの詳細な検討によれば濾過スラリーの移動速度は、好ましくは10cm/秒以下、より好ましくは5cm/秒以下である。   Next, the obtained filtered slurry is treated with a magnet to remove magnetic heavy metals (eg, iron, nickel, cobalt, etc.). As described above, the activated carbon for the electric double layer capacitor needs to extremely reduce the content of magnetic heavy metal, and the magnet used in the present invention preferably has a magnetic strength in terms of the effect of improving the removal of magnetic heavy metal. Is 5000 Gauss or more, more preferably 8000 Gauss or more. Moreover, it is desirable to arrange several magnets in series in consideration of the contact efficiency with the filtration slurry. Moreover, a permanent magnet and an electromagnet can be used suitably for a magnet. The adhesion efficiency of magnetic metals to the magnet is also affected by the contact time between the filtration slurry and the magnet. According to the detailed study by the present inventors, the moving speed of the filtration slurry is preferably 10 cm / second or less, more preferably 5 cm / second or less.

次に、以上説明したように、磁石で処理した濾過スラリーは、洗浄処理に付す。洗浄処理は常法により行うことができ、例えば、濾過スラリーを比較的目の細かい濾材で濾過して活性炭を濾取し、それを水洗し、必要に応じて酸洗し、更に水洗してアルカリ金属や不純物を除去し、大気圧下又は減圧下で常温又は加熱下で乾燥することにより目的の活性炭を得る。   Next, as explained above, the filtration slurry treated with a magnet is subjected to a washing treatment. The washing treatment can be performed by a conventional method. For example, the filter slurry is filtered with a relatively fine filter medium, and the activated carbon is collected, washed with water, pickled as necessary, washed with water, and washed with alkali. The target activated carbon is obtained by removing metals and impurities and drying at room temperature or under reduced pressure at atmospheric pressure or under heating.

以上説明した本発明の製造方法により得られる活性炭は、特に電気二重層キャパシタ用に適した分極性電極の材料として有用なものとなる。   The activated carbon obtained by the production method of the present invention described above is useful as a material for a polarizable electrode particularly suitable for an electric double layer capacitor.

このような分極性電極は、本発明の製造方法により得られた活性炭に、少なくともポリビニリデンフロライド、ポリテトラフロロエチレン等のバインダー及びカーボンブラックなどの導電性材料を混合し、成型してなるものである。導電性材料を混合することにより、電極の抵抗を低下させることができ、これにより、分極性電極の内部抵抗を下げ、電極体積を小さくするのに有効である。   Such a polarizable electrode is obtained by mixing and molding at least a binder such as polyvinylidene fluoride and polytetrafluoroethylene and a conductive material such as carbon black into the activated carbon obtained by the production method of the present invention. It is. By mixing the conductive material, the resistance of the electrode can be reduced, which is effective in reducing the internal resistance of the polarizable electrode and reducing the electrode volume.

このような電気二重層キャパシタ用に適した分極性電極を製造するには、通常知られた方法を適用することが可能である。例えば、市販されている、ポリビニリデンフロライド、ポリテトラフロロエチレンなどバインダーとして知られた物質やカーボンブラックなどの導電性材料を必要に応じて、数%程度まで加えてよく混練した後、金型に入れて加圧成形したり、圧延してシート化し、必要な形状に打ちぬくことで電極に成形することができる。また、混練物を集電体に塗布して塗布電極としてもよい。電極化の際、必要に応じて、アルコールやN−メチルピロリドンなどの有機化合物や水などの溶剤、分散剤、各種添加物を使用してもよい。また、発明の効果を損なわない範囲で熱を加えることも可能である。   In order to manufacture a polarizable electrode suitable for such an electric double layer capacitor, a generally known method can be applied. For example, commercially available materials known as binders such as polyvinylidene fluoride and polytetrafluoroethylene, and conductive materials such as carbon black are added to a few percent as necessary, and kneaded well, then the mold It can be molded into an electrode by pressing it into a mold or rolling it into a sheet and punching it into the required shape. Alternatively, the kneaded product may be applied to a current collector to form a coated electrode. When forming an electrode, if necessary, an organic compound such as alcohol or N-methylpyrrolidone, a solvent such as water, a dispersant, or various additives may be used. It is also possible to apply heat within a range that does not impair the effects of the invention.

以上説明した分極性電極は、図1(概略断面図)に示すような電気二重層キャパシタの電極として有用である。図1のキャパシタを構成する各構成要素は、本発明による分極性電極を使用する以外は、公知の電気二重層キャパシタと同様の構成とすることができ、例えば、図中、1及び2はアルミニウムなどからなる集電部材、3及び4は本発明の活性炭からなる分極性電極、5はポリプロピレン不織布などから構成されるセパレータ、6はステンレスなどの素材で構成される電池蓋、7はステンレスなどの素材で構成されるケース、8はポリプロピレン、ポリエチレン、ポリアミド、ポリアミドイミド、ポリブチレンなどから構成されるガスケット、9は電解液を示す。   The polarizable electrode described above is useful as an electrode of an electric double layer capacitor as shown in FIG. 1 (schematic cross-sectional view). Each component constituting the capacitor of FIG. 1 can have the same configuration as a known electric double layer capacitor except that the polarizable electrode according to the present invention is used. For example, in the figure, 1 and 2 are aluminum. Current collecting members made of, etc., 3 and 4 are polarizable electrodes made of activated carbon of the present invention, 5 is a separator made of polypropylene nonwoven fabric, 6 is a battery lid made of a material such as stainless steel, 7 is made of stainless steel, etc. A case made of a material, 8 is a gasket made of polypropylene, polyethylene, polyamide, polyamideimide, polybutylene or the like, and 9 is an electrolyte.

なお、電気二重層キャパシタとして機能させるためには、ケース7内に、テトラエチルアンモニウムテトラフロロボレート、テトラメチルアンモニウムテトラフロロボレートなど公知の電解質を、エチレンカーボネート、ジメチルカーボネート、ジエチルカーボネート、プロピレンカーボネートなどのカーボネート類、アセトニトリルなどのニトリル類、α−メチル−γ−ブチロラクトンなどのラクトン類、ジメチルスルホキシドなどのスルホキシド類、ジメチルフォルムアミドなどのアミド類などの溶媒に溶解した電解液を封入する必要がある。   In order to function as an electric double layer capacitor, a known electrolyte such as tetraethylammonium tetrafluoroborate or tetramethylammonium tetrafluoroborate is placed in case 7 with a carbonate such as ethylene carbonate, dimethyl carbonate, diethyl carbonate or propylene carbonate. It is necessary to enclose an electrolytic solution dissolved in a solvent such as nitriles such as acetonitrile, lactones such as α-methyl-γ-butyrolactone, sulfoxides such as dimethyl sulfoxide, amides such as dimethylformamide.

図1に示した構成の電気二重層キャパシタは、本発明の活性炭を使用しているので、小型でありながら静電容量の高いものとなる。   Since the electric double layer capacitor having the configuration shown in FIG. 1 uses the activated carbon of the present invention, it has a small capacitance and a high capacitance.

以下、実施例により本発明を具体的に説明するが、本発明はこれらにより限定されるものではない。   EXAMPLES Hereinafter, the present invention will be specifically described with reference to examples, but the present invention is not limited thereto.

参考例1Reference example 1

石油の分解残渣を熱処理して得たメトラー軟化点285℃の光学的異方性ピッチを幅2mmのスリット中に直径0.2mmの紡糸孔を1000個有するノズルを用いてメルトブロー紡糸し、不融化処理及び炭化処理してメソフェーズピッチ系炭素繊維を製造した。   Melt blow spinning using an optically anisotropic pitch with a Mettler softening point of 285 ° C obtained by heat treatment of petroleum cracking residue using a nozzle having 1,000 spinning holes with a diameter of 0.2 mm in a slit with a width of 2 mm, and infusible The mesophase pitch carbon fiber was produced by treatment and carbonization.

温度計を装着した直径400mm、長さ300mmのニッケル製回分式外熱タイプのロータリーキルンに、参考例1で作製したメソフェーズピッチ系炭素繊維を長軸方向の最大長さが200μm以下になるように粉砕したピッチ0.7kg及び平均粒径1mm以下に粉砕した95%水酸化カリウム1.3kgを投入し、0.3Torr(40.0Pa)の減圧下、30rpmでロータリーキルンを回転させた。メソフェーズピッチ系炭素繊維と水酸化カリウムとの混合物を、室温から0.5℃/分の速度で100℃まで昇温した後、ロータリーキルンの回転数と減圧条件をこのまま維持しながら電源を切り、冷却し、造粒物を得た。造粒物は10mm以下の大きさであった。   A mesophase pitch-based carbon fiber produced in Reference Example 1 is pulverized into a nickel batch external heat type rotary kiln with a diameter of 400 mm and a length of 300 mm equipped with a thermometer so that the maximum length in the major axis direction is 200 μm or less. A pitch of 0.7 kg and 1.3 kg of 95% potassium hydroxide pulverized to an average particle size of 1 mm or less were added, and a rotary kiln was rotated at 30 rpm under a reduced pressure of 0.3 Torr (40.0 Pa). After heating the mixture of mesophase pitch-based carbon fiber and potassium hydroxide from room temperature to 100 ° C at a rate of 0.5 ° C / min, the power is turned off while maintaining the rotational speed of the rotary kiln and the decompression condition as it is, cooling To obtain a granulated product. The granulated product had a size of 10 mm or less.

同一のロータリーキルンを使用し、30rpmで回転させながら前記造粒物を0.3Torr(40.0Pa)の減圧下、室温から0.5℃/分の速度で320℃まで昇温し、その温度で1時間保持して、脱水を行った。   Using the same rotary kiln, the granulated product was heated from room temperature to 320 ° C. at a rate of 0.5 ° C./min under reduced pressure of 0.3 Torr (40.0 Pa) while rotating at 30 rpm. After holding for 1 hour, dehydration was performed.

賦活炉として、温度計、窒素導入口、水トラップを有するガス排出口を備え、温度可変の賦活ゾーン(賦活ゾーン内径100mm、内容積400ミリリットル(mL))を有する外熱式ロータリーキルン型電気炉を使用した。窒素通流下、賦活ゾーンに上記脱水品50gを仕込んだ。   As an activation furnace, an externally heated rotary kiln type electric furnace having a thermometer, a nitrogen introduction port, a gas discharge port having a water trap, and a temperature variable activation zone (activation zone inner diameter 100 mm, inner volume 400 ml (mL)) used. Under nitrogen flow, 50 g of the dehydrated product was charged into the activation zone.

窒素を300mL/分で通流させながら賦活ゾーンを室温〜730℃まで、200℃/時間の速度で昇温し、所定の温度に到達後3時間保持した。その後、窒素通流下に50℃以下まで冷却し、その後、賦活して得た活性炭素材を炭酸ガスと水蒸気の混合ガスの通流下に処理して残存金属カリウムを失活させた。以上の賦活操作を16回繰返した。   The activation zone was heated from room temperature to 730 ° C. at a rate of 200 ° C./hour while flowing nitrogen at 300 mL / min, and held for 3 hours after reaching the predetermined temperature. Then, it cooled to 50 degrees C or less under nitrogen flow, and after that, the activated carbon raw material obtained by activating was processed under the flow of the mixed gas of a carbon dioxide gas and water vapor | steam, and the residual metal potassium was deactivated. The above activation operation was repeated 16 times.

賦活して得た活性炭と炭酸カリウム主体の混合物を蒸留水中に添加撹拌して10%の活性炭を含有するスラリーを調製し、このスラリーを目開き45μmのナイロン樹脂製フィルターにより濾過した。続いて、得られた濾過スラリーを8000ガウスの棒状磁石を3本直列に配置した槽内を流速2cm/秒で通流させ、含有されている金属類の除去を行った。本濾過操作と磁石による除金属操作により活性炭中の約0.4重量%の不良物を除去した。この不良物は鉄(Fe)及びニッケル(Ni)を約30重量%含有していた。   The activated carbon and potassium carbonate-based mixture obtained by activation was added to and stirred in distilled water to prepare a slurry containing 10% activated carbon, and this slurry was filtered through a nylon resin filter having an opening of 45 μm. Subsequently, the obtained filtration slurry was passed through a tank in which three 8000 Gauss rod-shaped magnets were arranged in series at a flow rate of 2 cm / second to remove contained metals. About 0.4% by weight of defectives in the activated carbon was removed by this filtration operation and metal removal operation with a magnet. This defect contained about 30% by weight of iron (Fe) and nickel (Ni).

不良物が除かれた活性炭は、その後、水洗、0.5規定(N)塩酸溶液(95℃)での酸洗浄、熱水洗浄(95℃)の後、110℃で乾燥し製品化した。製品中のNi及びFeの含有率はそれぞれ5ppm、3ppmであった。   The activated carbon from which the defectives were removed was then washed with water, acid washed with 0.5 N (N) hydrochloric acid solution (95 ° C.), hot water washed (95 ° C.), dried at 110 ° C. and commercialized. The contents of Ni and Fe in the product were 5 ppm and 3 ppm, respectively.

得られた活性炭を、振動ミルにより平均粒径5〜30μmに粉砕して粉末活性炭とし、この粉末活性炭80重量部に、導電性カーボン10重量部とポリテトラフロオロエチレン(PTFE)10重量部とを添加し、メノウ乳鉢で混練した。次いで、得られた混練物をロール圧延により、厚さ200μm程度のシートに成形し、直径2cmの円形に打ち抜き、150℃で4時間減圧下で乾燥することにより分極性電極を作製した。   The obtained activated carbon was pulverized to an average particle size of 5 to 30 μm by a vibration mill to obtain powdered activated carbon. 80 parts by weight of the powdered activated carbon, 10 parts by weight of conductive carbon and 10 parts by weight of polytetrafluoroethylene (PTFE) And kneaded in an agate mortar. Subsequently, the obtained kneaded material was formed into a sheet having a thickness of about 200 μm by roll rolling, punched into a circle having a diameter of 2 cm, and dried under reduced pressure at 150 ° C. for 4 hours to produce a polarizable electrode.

作製した分極性電極を、露点−50℃以下のクローブボックス内で、図1に示すように、ステンレスケースにアルミ集電極とガラスセパレータを用いてセルに組み立て、テトラエチルアンモニウムテトラフルオロボレートを含有するプロピレンカーボネート溶液を含侵させ、グローブボックス内でかしめ封印し、電気二重層キャパシタを10個得た。得られた電気二重層キャパシタについて、パワーシステム製電気二重層キャパシタ評価装置を用い、室温中2.7V定電流、充放電サイクル試験を行い、ショートが発生するか否かを試験した。その結果、1000回の充放電サイクル試験では、ショートの現象が認められた電気二重層キャパシタは一つもなかった。   Propylene containing tetraethylammonium tetrafluoroborate was assembled in a cell using a stainless steel case and an aluminum collector electrode and a glass separator in a clove box having a dew point of −50 ° C. or less, as shown in FIG. The carbonate solution was impregnated and caulked and sealed in a glove box to obtain 10 electric double layer capacitors. The obtained electric double layer capacitor was subjected to a 2.7 V constant current and charge / discharge cycle test at room temperature using a power system electric double layer capacitor evaluation apparatus to test whether or not a short circuit occurred. As a result, in the charge / discharge cycle test of 1000 times, there was no electric double layer capacitor in which a short-circuit phenomenon was recognized.

実施例1に準じて調製した活性炭と炭酸カリウム主体の混合物からなる活性炭濃度20重量%のスラリーを目開き70μmのナイロン樹脂製フィルターにより濾過した。次いで、濾過物を6000ガウスの棒状磁石を3本直列に配置した槽内を流速4cm/秒で通流させ、含有される金属類の除去を磁石により行った以外は実施例1と同様な操作を繰返した。本濾過操作と磁石による除金属操作により活性炭中の約0.25重量%の不良物を除去した。該不良物はFe及びNiを約20重量%含有していた。該操作を行った活性炭は、水洗、0.5N塩酸溶液(95℃)での酸洗浄、熱水洗浄(95℃)をした後、110℃で乾燥し製品化した。製品中のNi及びFeの含有率はそれぞれ7ppm、5ppmであった。   A slurry having an activated carbon concentration of 20% by weight made of a mixture of activated carbon and potassium carbonate mainly prepared according to Example 1 was filtered through a filter made of nylon resin having an opening of 70 μm. Next, the same operation as in Example 1 was carried out except that the filtrate was passed through a tank in which three 6000 Gauss rod-shaped magnets were arranged in series at a flow rate of 4 cm / sec and the contained metals were removed by the magnet. Was repeated. About 0.25% by weight of defectives in the activated carbon was removed by this filtration operation and metal removal operation with a magnet. The defective product contained about 20% by weight of Fe and Ni. The activated carbon thus treated was washed with water, acid washed with 0.5N hydrochloric acid solution (95 ° C.) and hot water washed (95 ° C.), and then dried at 110 ° C. to obtain a product. The contents of Ni and Fe in the product were 7 ppm and 5 ppm, respectively.

得られた活性炭から、実施例1と同様に電気二重層キャパシタを作成し、充放電サイクル試験を行った。その結果、500回の充放電サイクル試験では、ショートの現象が認められた電気二重層キャパシタは一つもなかった。   An electric double layer capacitor was prepared from the obtained activated carbon in the same manner as in Example 1, and a charge / discharge cycle test was conducted. As a result, in the 500 charge / discharge cycle tests, there was no electric double layer capacitor in which a short-circuit phenomenon was observed.

比較例1Comparative Example 1

実施例1により賦活して得た活性炭と炭酸カリウム主体の混合物を蒸留水に添加し10重量%の活性炭を含有するスラリーを調製した。このスラリーを、濾過および磁石による金属類の除去を行なわずに、水洗、0.5N塩酸溶液(95℃)での酸洗浄、熱水洗浄(95℃)した後、110℃で乾燥し製品化した。製品中のNi及びFeの含有率はそれぞれ20ppm、15ppmであった。   A mixture mainly containing activated carbon and potassium carbonate obtained by activation in Example 1 was added to distilled water to prepare a slurry containing 10 wt% activated carbon. The slurry was washed with water, acid washed with 0.5N hydrochloric acid solution (95 ° C.) and hot water washed (95 ° C.) without filtration and removal of metals with a magnet, and then dried at 110 ° C. to produce a product. did. The contents of Ni and Fe in the product were 20 ppm and 15 ppm, respectively.

得られた活性炭から、実施例1と同様に電気二重層キャパシタを10個作成し、充放電サイクル試験を行った。その結果、100回の充放電サイクルで、ショートの現象が認められた電気二重層キャパシタは3個であった。   Ten electric double layer capacitors were produced from the obtained activated carbon in the same manner as in Example 1, and a charge / discharge cycle test was conducted. As a result, there were three electric double layer capacitors in which a short-circuit phenomenon was observed in 100 charge / discharge cycles.

比較例2Comparative Example 2

実施例1において、該スラリーの濾過を行わず、磁石処理のみを実施した。磁石による除金属操作により活性炭中の約0.1重量%の不良物を除去した。この操作を行った活性炭は、水洗、0.5N塩酸溶液(95℃)での酸洗浄、熱水洗浄(95℃)した後、110℃で乾燥し製品化した。この不良物はFe及びNiを約50重量%含有していた。製品中のNi及びFeの含有率はそれぞれ15ppm、10ppmであった。   In Example 1, the slurry was not filtered and only the magnet treatment was performed. About 0.1% by weight of defectives in the activated carbon was removed by a metal removal operation with a magnet. The activated carbon subjected to this operation was washed with water, acid washed with a 0.5N hydrochloric acid solution (95 ° C.), and washed with hot water (95 ° C.), and then dried at 110 ° C. to obtain a product. This defective contained about 50% by weight of Fe and Ni. The contents of Ni and Fe in the product were 15 ppm and 10 ppm, respectively.

得られた活性炭から、実施例1と同様に電気二重層キャパシタを10個作成し、充放電サイクル試験を行った。その結果、100回の充放電サイクルで、ショートの現象が認められた電気二重層キャパシタは2個であった。   Ten electric double layer capacitors were produced from the obtained activated carbon in the same manner as in Example 1, and a charge / discharge cycle test was conducted. As a result, there were two electric double layer capacitors in which a short-circuit phenomenon was observed in 100 charge / discharge cycles.

比較例3Comparative Example 3

実施例1において、スラリーの濾過操作のみを行い、磁石処理を実施しなかった。濾過操作により活性炭中の約0.03重量%の不良物を除去した。この不良物はFe及びNiを約20重量%含有していた。この操作を行った活性炭は、水洗、0.5N塩酸溶液(95℃)での酸洗浄、熱水洗浄(95℃)した後、110℃で乾燥し製品化した。製品中のNi及びFeの含有率はそれぞれ18ppm、13ppmであった。   In Example 1, only the slurry filtration operation was performed, and the magnet treatment was not performed. About 0.03% by weight of defectives in the activated carbon was removed by filtration. This defective contained about 20% by weight of Fe and Ni. The activated carbon subjected to this operation was washed with water, acid washed with a 0.5N hydrochloric acid solution (95 ° C.), and washed with hot water (95 ° C.), and then dried at 110 ° C. to obtain a product. The contents of Ni and Fe in the product were 18 ppm and 13 ppm, respectively.

得られた活性炭から、実施例1と同様に電気二重層キャパシタを100個作成し、充放電サイクル試験を行った。その結果、100回の充放電サイクルで、ショートの現象が認められた電気二重層キャパシタは1個であった。   From the obtained activated carbon, 100 electric double layer capacitors were prepared in the same manner as in Example 1, and a charge / discharge cycle test was performed. As a result, there was one electric double layer capacitor in which a short-circuit phenomenon was observed in 100 charge / discharge cycles.

本発明の製造方法によれば、磁性重金属の混入量を低減した活性炭を簡便に得ることができる。また、本発明の製造方法により得られる活性炭を使用して分極性電極に成形し、電気二重層キャパシタに用いると、磁性重金属の含有量が少ないので、磁性重金属の還元析出によるデンドライト化によるショートなどの障害を起こしたり、自己放電保持率が低下することがない。従って、この電気二重層キャパシタは、小容量のメモリーバックアップ用途から、大容量のモータの補助電源用途まで、広い範囲で利用することができる。   According to the production method of the present invention, it is possible to easily obtain activated carbon with a reduced amount of magnetic heavy metal mixed therein. In addition, when activated carbon obtained by the production method of the present invention is used to form a polarizable electrode and used for an electric double layer capacitor, the content of magnetic heavy metal is low, so short due to dendrite formation due to reduction precipitation of magnetic heavy metal, etc. The self-discharge retention rate does not decrease. Therefore, the electric double layer capacitor can be used in a wide range from a small-capacity memory backup application to a large-capacity motor auxiliary power supply application.

電気二重層キャパシタの一例を示す概略断面図である。It is a schematic sectional drawing which shows an example of an electrical double layer capacitor.

符号の説明Explanation of symbols

1,2 集電部材
3,4 分極性電極
5 セパレータ
6 電池蓋
7 ケース
8 ガスケット
9 電解液
1, 2 Current collecting member 3, 4 Polarized electrode 5 Separator 6 Battery cover 7 Case 8 Gasket 9 Electrolyte

Claims (5)

炭素質材料をアルカリ金属水酸化物を用いて賦活処理して活性炭を製造する活性炭の製造方法において、炭素質材料をアルカリ金属水酸化物を用いて賦活処理して得られた賦活処理物を水中に投入し、得られたスラリー状物を濾過処理し、得られた濾過スラリーを磁力強度5000ガウス以上の磁石で処理した後、洗浄に付すことを特徴とする活性炭の製造方法。   In the method for producing activated carbon in which activated carbon is produced by activating a carbonaceous material using an alkali metal hydroxide, the activated material obtained by activating the carbonaceous material using an alkali metal hydroxide is submerged in water. A method for producing activated carbon, wherein the obtained slurry is subjected to filtration treatment, the obtained filtration slurry is treated with a magnet having a magnetic strength of 5000 gauss or more, and then subjected to washing. 該濾材の目開きが75μm以下である請求項1記載の活性炭の製造方法。   The method for producing activated carbon according to claim 1, wherein the opening of the filter medium is 75 μm or less. 該アルカリ金属水酸化物が水酸化カリウムである請求項1又は2記載の活性炭の製造方法。   The method for producing activated carbon according to claim 1 or 2, wherein the alkali metal hydroxide is potassium hydroxide. 該炭素質材料が易黒鉛系炭素質材料である請求項1〜3いずれかに記載の活性炭の製造方法。   The method for producing activated carbon according to any one of claims 1 to 3, wherein the carbonaceous material is an easily graphite-based carbonaceous material. 易黒鉛系炭素質材料がメソフェーズピッチ系炭素繊維である請求項4記載の活性炭の製造方法。   The method for producing activated carbon according to claim 4, wherein the easily graphite-based carbonaceous material is mesophase pitch-based carbon fiber.
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