JP2006096568A - Method for producing activated carbon - Google Patents
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Abstract
Description
本発明は、吸着能に優れる活性炭の製造方法に関する。 The present invention relates to a method for producing activated carbon having excellent adsorption ability.
活性炭は、原料の合成樹脂や、木材や、ヤシ殻等の植物由来の有機物を低酸素雰囲気で焼成して得るのが一般的である。原料の種類により得られる活性炭の吸着能が異なることがあり、高性能の活性炭を得るためには高価な、あるいは大量入手に問題のある原料を必要とすることが多い。従って、比較的低コストで大量入手可能な原料を用いて高性能の活性炭を得る方法が求められている。 Activated carbon is generally obtained by firing raw material synthetic resin, organic materials derived from plants such as wood and coconut shells in a low oxygen atmosphere. The adsorptive capacity of the obtained activated carbon may vary depending on the type of raw material, and in order to obtain high-performance activated carbon, a raw material that is expensive or problematic in mass acquisition is often required. Therefore, there is a need for a method for obtaining high-performance activated carbon using raw materials that can be obtained in large quantities at a relatively low cost.
比較的低コストで大量入手可能な原料としておからを用い、アルカリ金属化合物とともに窒素雰囲気下で炭化することが開示されている（例えば、特許文献１参照。）。このような薬品賦活法という従来手法に基く方法は、焼成後に活性炭に残留のアルカリ金属成分を除去する必要があり、工程が煩雑であるとともに、アルカリ金属成分の除去工程で活性炭の性能が損なわれることが懸念される。
本発明の目的は、比較的低コストで大量入手可能な原料から高性能な活性炭を単純な工程で得ることができる活性炭製造方法を提供することにある。 An object of the present invention is to provide an activated carbon production method capable of obtaining high-performance activated carbon from raw materials available in large quantities at a relatively low cost by a simple process.
本発明の要旨とするところは、植物由来の有機物から蛋白質を除去し、蛋白質の含有率を５乾燥重量％以下となす蛋白質除去工程、
該蛋白質除去工程により蛋白質が除去された該有機物を炭化する工程
を含む活性炭製造方法であることにある。
The gist of the present invention is to remove a protein from a plant-derived organic material, and to remove the protein to a dry content of 5% by weight or less,
It is an activated carbon production method including a step of carbonizing the organic substance from which protein has been removed by the protein removal step.
前記蛋白質除去工程は、前記有機物をアルカリ金属化合物、酵素から選択される処理物で前記有機物を処理したのち、該有機物を洗浄する洗浄工程を含み得る。 The protein removal step may include a washing step of washing the organic matter after treating the organic matter with a treatment selected from an alkali metal compound and an enzyme.
前記アルカリ金属化合物は、苛性ソーダ、炭酸ナトリウム、次亜塩素酸ナトリウムから選択され得る。 The alkali metal compound may be selected from caustic soda, sodium carbonate, sodium hypochlorite.
前記洗浄工程は、前記処理物で処理された前記有機物を濾別する工程を含み得る。 The washing step may include a step of filtering out the organic matter treated with the treated product.
前記有機物はビール粕であり得る。 The organic material may be beer lees.
本発明によると、比較的低コストで大量入手可能な原料から高性能な活性炭を単純な工程で得ることができる活性炭製造方法が提供される。 According to the present invention, there is provided an activated carbon production method capable of obtaining a high-performance activated carbon from a raw material available in large quantities at a relatively low cost by a simple process.
本発明の活性炭製造方法の実施態様を説明する。本発明においては、原料としてビール粕が用いられることが好ましく、以下の説明はビール粕を原料とする活性炭製造方法を主体になされるが、原料はビール粕に限定されず、蛋白質を含有する、植物由来の有機物であれば使用可能である。蛋白質は有機物の構造組織のなかに組み込まれているものであってもよい。あるいは、セルロース等の炭水化物から成る構造組織を有する有機物と混合されていてもよい。 The embodiment of the activated carbon production method of the present invention will be described. In the present invention, it is preferable to use beer lees as a raw material, and the following description is mainly based on an activated carbon production method using beer lees as a raw material, but the raw materials are not limited to beer lees and contain protein. Any organic material derived from plants can be used. Proteins may be incorporated into the structural structure of organic matter. Alternatively, it may be mixed with an organic substance having a structural structure composed of carbohydrates such as cellulose.
本発明において使用される、蛋白質を含有する、植物由来の有機物としては、有用成分を抽出した後の植物の果実及び種子の圧搾滓が好適に用いられる。この例としては、ビール粕のほかに、柑橘類即ち、みかん科をはじめ桃、李、林檎などのバラ科、ぶどう科、パイナップル科、つばき科、オリーブなどのもくせい科、ひまわり、サフラワーなどのきく科、綿などのあおい科、大豆、落花生などのまめ科、蓖麻、油桐などのとうだいぐさ科、ごま科、菜種科、亜麻科、うるし科、米などの禾本科等の植物の果実及び種子の搾り滓が挙げられる。 As the plant-derived organic substance containing protein, which is used in the present invention, pressed fruit of plants and seeds after extraction of useful components is preferably used. Examples of this include beer grapes, citrus fruits such as mandarin oranges, peaches, lee, apples, and other roses, vines, pineapples, camellias, olives, sunflowers, safflowers, etc. Plants such as Noiraceae, Aoiaceae such as cotton, Beans such as Soybean, Peanuts, Toudagusa such as Sesame and Oil Tung, Sesameaceae, Rapeseed, Flaxaceae, Urushiaceae, Rice Fruit and seed squeezed rice cake.
本発明においては、先ず、ビール粕を苛性ソーダ、炭酸ナトリウム、次亜塩素酸ナトリウム、酵素から選択される処理物で処理して、ビール粕に含まれる蛋白質を分解及び／又は遊離させる。ビール粕をアルカリ金属化合物、蛋白質分解酵素から選択される処理物の水溶液あるいは混合液に浸漬し液中に遊離あるいは分解した蛋白質を溶出させることが好ましい。あるいはビール粕にこの処理物の水溶液あるいは混合液を含浸させて所定時間放置することによりビール粕に含まれる蛋白質を分解及び／又は遊離させたのち、このビール粕を水等の液に浸漬し液中に遊離あるいは分解した蛋白質を溶出させることが好ましい。 In the present invention, beer lees are first treated with a treatment selected from caustic soda, sodium carbonate, sodium hypochlorite, and enzymes to decompose and / or liberate proteins contained in beer lees. It is preferable to immerse beer lees in an aqueous solution or mixed solution of a treatment product selected from an alkali metal compound and a proteolytic enzyme to elute the released or decomposed protein in the solution. Alternatively, the beer koji is impregnated with an aqueous solution or a mixed solution of the processed product and left for a predetermined time to decompose and / or liberate proteins contained in the beer koji, and then the beer koji is immersed in a liquid such as water. It is preferable to elute the free or degraded protein.
アルカリ金属化合物としては苛性ソーダ、炭酸ナトリウム、次亜塩素酸ナトリウム、苛性カリ、炭酸カリウム、次亜塩素酸カリウム、リチウムブロマイド等が挙げられるが、蛋白質を分解する作用を有するものであればこれらに限定されない。 Examples of the alkali metal compound include caustic soda, sodium carbonate, sodium hypochlorite, caustic potash, potassium carbonate, potassium hypochlorite, and lithium bromide, but are not limited to these as long as they have an action of degrading proteins. .
酵素としてはセリンプロテアーゼ（トリプシン、キモトリプシン、ズブチリシン等）、システインプロテアーゼ（パパイン、ブロメライン、カスパーゼ群、カテプシン群等）、アスパルチックプロテアーゼ（ペプシン、カテプシンＤ等）、メタプロテアーゼ（コラゲナーゼ、カルボキシペプチダーゼ群、アミノペプチダーゼ群等）等が挙げられる。具体的には、Savinase（製品名：Novo-Nordisk A/S）、Maxacal（製品名：Gist-Brocades/IBIS）、Opticlean（MKC製）、スブチリシン種（AP122（昭和電工製））、Maxatase、Esperase、Alcalase（いずれも製品名）、プロテイナーゼＫ、スブチリシンBPN'が例として挙げられる。又、Ａｓｐｅｒｒｇｉｌｌｕｓ属、Ｐｅｎｉｃｉｌｌｉｕｍ属、Ｂａｃｉｌｌｕｓ属、Ｓｔｒｅｐｔｏｍｙｃｅｓ属、Ｓａｃｃｈａｒｏｍｙｃｅｓ属、Ｆｌａｖｏｂａｃｔｅｒｒｉｕｍ属等の菌類が産出するアルカリプロテアーゼが用いられる。具体的には、ノボノルデイスクバイオインダストリ株式会社製のアルカラーゼ、サビナーゼ、エスペラーゼ、カンナーゼ、デュラザイム、エバラーゼ等が挙げられる。 Enzymes include serine protease (trypsin, chymotrypsin, subtilisin, etc.), cysteine protease (papain, bromelain, caspase group, cathepsin group, etc.), aspartic protease (pepsin, cathepsin D, etc.), metaprotease (collagenase, carboxypeptidase group, amino acid) Peptidase group, etc.). Specifically, Savinase (Product name: Novo-Nordisk A / S), Maxacal (Product name: Gist-Brocades / IBIS), Opticlean (MKC), Subtilisin (AP122 (Showa Denko)), Maxatase, Esperase Alcalase (all are product names), proteinase K, and subtilisin BPN '. Alkaline proteases produced by fungi such as Aspergillus genus, Penicillium genus, Bacillus genus, Streptomyces genus, Saccharomyces genus and Flavobacterium genus are also used. Specific examples include Alcalase, Sabinase, Esperase, Cannase, Durazyme, and Everase manufactured by Novo Nordisk Bio Industry Co., Ltd.
次いで、このような処理により生ずるビール粕と水等の液の混合物に必要ならば水等の液を加えて濾過して、ビール粕と液とを濾別して分離する。これにともなって、液中の上述の処理物（アルカリ金属化合物、蛋白質分解酵素から選択される）と分解及び／又は遊離させた蛋白質がビール粕から分離され除去される。濾過は例えば、吸引濾過や、フィルタプレスによる固液分離で行なうことが出来る。 Next, if necessary, a liquid such as water is added to the mixture of beer lees and water produced by such treatment and filtered, and the beer lees and liquid are separated by filtration. Along with this, the above-mentioned processed product (selected from alkali metal compounds and proteolytic enzymes) in the liquid and the decomposed and / or liberated protein are separated and removed from the beer lees. Filtration can be performed by, for example, suction filtration or solid-liquid separation using a filter press.
蛋白質はビール粕から完全に除去されることが最も好ましいが、この除去処理後のビール粕に、除去処理後のビール粕全量に対して５乾燥重量％以下の蛋白質が残存していても本発明の効果は得られる。残存の蛋白質が２乾燥重量％以下であることが更に好ましい。乾燥重量％は、一般法の乾燥減量法（１０５℃で４時間）による乾燥固形分を基準とした重量％である。 It is most preferable that the protein is completely removed from the beer lees. However, even if the protein remains in the beer lees after the removal treatment in an amount of 5% by dry weight or less with respect to the total amount of beer lees after the removal treatment. The effect is obtained. More preferably, the remaining protein is 2% by weight or less. The dry weight% is a weight% based on the dry solid content by the general method of loss on drying (4 hours at 105 ° C.).
この除去処理後のビール粕は、次いで、炭化焼成により炭化される。炭化焼成は、活性炭を製造するための通常の炭化処理である。一般には、窒素雰囲気中で６００〜８００℃で１乃至数時間焼成することにより行なうが、原料の性状や活性炭の使用目的等によってはこの条件に限定されるものではない。 The beer cake after this removal treatment is then carbonized by carbonization baking. Carbonization firing is a normal carbonization treatment for producing activated carbon. Generally, it is carried out by firing at 600 to 800 ° C. for 1 to several hours in a nitrogen atmosphere, but it is not limited to these conditions depending on the properties of the raw materials and the purpose of use of the activated carbon.
炭化処理は更に吸着能を向上させるためにアルカリ賦活又はガス賦活をともなってもよい。このアルカリ賦活又はガス賦活は炭化焼成の後に行なわれてもよい。炭化焼成とともに行なわれてもよい。 The carbonization treatment may be accompanied by alkali activation or gas activation in order to further improve the adsorption capacity. This alkali activation or gas activation may be performed after the carbonization firing. You may carry out with carbonization baking.
アルカリ賦活は、不活性ガス気流中で炭化物あるいは炭化すべき原料にアルカリ化合物を添加して行う。反応温度は、５００〜１，０００℃の範囲、好ましくは７００〜９００℃の範囲で実行され、且つ、反応時間は１０分〜２０時間の範囲で、好ましくは１〜１０時間の範囲で実行する。アルカリ化合物としては、リチウム、ナトリウム、カリウム等のアルカリ金属あるいはマグネシウム、カルシウム等のアルカリ土類金属を含むものであれば、その水酸化物、炭酸塩などのいずれも採択することができる。 The alkali activation is performed by adding an alkali compound to a carbide or a raw material to be carbonized in an inert gas stream. The reaction temperature is 500 to 1,000 ° C., preferably 700 to 900 ° C., and the reaction time is 10 minutes to 20 hours, preferably 1 to 10 hours. . As the alkali compound, any of hydroxides and carbonates thereof may be adopted as long as it contains an alkali metal such as lithium, sodium and potassium or an alkaline earth metal such as magnesium and calcium.
ガス賦活は、水蒸気ガス又は二酸化炭素ガスを用いて、反応温度が７００〜１０００℃の範囲で実行され、且つ、反応時間は１０分〜２０時間の範囲で賦活する。 The gas activation is performed using water vapor gas or carbon dioxide gas in a reaction temperature range of 700 to 1000 ° C., and a reaction time is activated in a range of 10 minutes to 20 hours.
この炭化により得られた活性炭は優れた吸着能を有し、高価な、あるいは大量入手が困難な原料から得られる高性能の活性炭と遜色のない性能の活性炭が、比較的低コストで大量入手可能な原料を用いて得られた。 Activated carbon obtained by this carbonization has excellent adsorption capacity, and high-performance activated carbon obtained from expensive or difficult to obtain in large quantities and activated carbon with comparable performance can be obtained in large quantities at a relatively low cost. Obtained using various raw materials.
除去される蛋白質が有機物の構造組織のなかに組み込まれている場合は、その蛋白質が除去されることによってその跡が微細な空隙となって、炭化焼成による微細孔の生成が促進され得られる活性炭の吸着能が向上する。本発明は、蛋白質を１乾燥重量％以上含有する有機物に適用すると特に有効である。 When the protein to be removed is incorporated in the structure of organic matter, activated carbon that can be traced into fine voids by removing the protein and promotes the formation of micropores by carbonization firing. The adsorption ability of is improved. The present invention is particularly effective when applied to an organic substance containing 1% by weight or more of protein.
除去される蛋白質が炭水化物を主成分とする有機物と単に混合されている場合には、その蛋白質とともにその有機物を焼成すると、蛋白質が塊状に炭化されて炭水化物を主成分とする有機物の炭化焼成による微細孔の円滑な生成が妨げられる。この蛋白質を有機物の炭化前に除去することにより、炭化焼成による微細孔の生成が妨げられず、得られる活性炭の吸着能が向上する。 When the protein to be removed is simply mixed with an organic substance mainly composed of carbohydrates, when the organic substance is baked together with the protein, the protein is carbonized in a lump and finely formed by carbonization firing of the organic substance mainly composed of the carbohydrate. Smooth generation of holes is prevented. By removing this protein before carbonization of the organic substance, generation of micropores by carbonization firing is not hindered, and the adsorption ability of the obtained activated carbon is improved.
除去される蛋白質が水溶性である場合は、蛋白質を水中に溶出させて除去してもよい。 When the protein to be removed is water-soluble, the protein may be removed by elution in water.
本発明の活性炭製造方法は、薬品賦活法におけるような焼成後の活性炭に残留のアルカリ金属成分を除去する工程をともなわずに行なうこともできるので、この場合は、工程が簡略であるとともに、このアルカリ金属成分の除去工程で活性炭の性能が損なわれることがない。 Since the activated carbon production method of the present invention can be carried out without the step of removing the remaining alkali metal component in the activated carbon after firing as in the chemical activation method, in this case, the process is simplified, The performance of the activated carbon is not impaired in the step of removing the alkali metal component.
比表面積の測定：定容系の吸着量測定装置（日本ベル（株）製、ＢＥＬＳＯＲＰ ８８）を用い液体窒素温度での窒素の吸着等温線を測定し、ＢＥＴ法で解析して求めた。 Measurement of specific surface area: The adsorption isotherm of nitrogen at liquid nitrogen temperature was measured using a constant volume adsorption amount measuring device (BELSORP 88, manufactured by Nippon Bell Co., Ltd.), and analyzed by the BET method.
実施例１
原料としてのビール粕（蛋白質含有量２５乾燥重量％）１００ｇを４％苛性ソーダ水溶液３００ｃｃに浸漬し、１０分間煮沸した。次いで、濾紙による吸引濾過により、このビール粕をこの苛性ソーダ水溶液から分離し、所定量の希塩酸にて中和後、水洗した。得られたビール粕の蛋白質含有量は１乾燥重量％であった。
Example 1
100 g of beer cake (protein content 25 dry weight%) as a raw material was immersed in 300 cc of 4% aqueous sodium hydroxide solution and boiled for 10 minutes. Subsequently, the beer cake was separated from the aqueous caustic soda solution by suction filtration with a filter paper, neutralized with a predetermined amount of dilute hydrochloric acid, and washed with water. The protein content of the obtained beer koji was 1% by dry weight.
この得られたビール粕を乾燥後窒素雰囲気中で８００℃１５分の炭化処理を行ない、次いで、９００〜１０００℃で炭酸ガスによる賦活処理を行ない活性炭を得た。得られた活性炭の比表面積は２２００ｍ２／ｇであった。 The obtained beer cake was dried and then subjected to carbonization treatment at 800 ° C. for 15 minutes in a nitrogen atmosphere, and then activated treatment with carbon dioxide gas at 900 to 1000 ° C. to obtain activated carbon. The specific surface area of the obtained activated carbon was 2200 m 2 / g.
実施例２
原料としてのビール粕（蛋白質含有量２５乾燥重量％）１００ｇを２％苛性ソーダ水溶液３００ｃｃに浸漬し、１０分間煮沸した。次いで、水洗により、このビール粕をこの苛性ソーダ水溶液から分離し、所定量の希塩酸にて中和後、水洗した。得られたビール粕の蛋白質含有量は４乾燥重量％であった。
Example 2
100 g of beer koji as a raw material (protein content 25 dry weight%) was immersed in 300 cc of a 2% aqueous sodium hydroxide solution and boiled for 10 minutes. Next, the beer cake was separated from the aqueous caustic soda solution by washing with water, neutralized with a predetermined amount of dilute hydrochloric acid, and washed with water. The protein content of the obtained beer koji was 4% by dry weight.
この得られたビール粕を乾燥後窒素雰囲気中で８００℃１５分の炭化処理を行ない、次いで、９００〜１０００℃で炭酸ガスによる賦活処理を行ない活性炭を得た。得られた活性炭の比表面積は１９００ｍ２／ｇであった。 The obtained beer cake was dried and then subjected to carbonization treatment at 800 ° C. for 15 minutes in a nitrogen atmosphere, and then activated treatment with carbon dioxide gas at 900 to 1000 ° C. to obtain activated carbon. The specific surface area of the obtained activated carbon was 1900 m 2 / g.
比較例１
実施例１用いたと同様のビール粕を乾燥後窒素雰囲気中で８００℃１５分の炭化処理を行ない、次いで、９００〜１０００℃で炭酸ガスによる賦活処理を行ない活性炭を得た。
得られた活性炭の比表面積は９８０ｍ２／ｇであった。
Comparative Example 1
The same beer koji used in Example 1 was dried and then carbonized at 800 ° C. for 15 minutes in a nitrogen atmosphere, and then activated at 900 to 1000 ° C. with carbon dioxide to obtain activated carbon.
The specific surface area of the obtained activated carbon was 980 m 2 / g.
比較例２
実施例１用いたと同様のビール粕１００ｇを乾燥した乾燥ビール粕を炭酸ナトリウム３０ｇを含む水溶液と練り合わせ、１１０℃１２時間乾燥して固形物を得た。この固形物に実施例１と同様の炭化処理と賦活処理を行ない活性炭状物を得た。この活性炭状物を熱水で洗浄して活性炭を得た。得られた活性炭の比表面積は１７００ｍ２／ｇであった。
Comparative Example 2
A dry beer lees obtained by drying 100 g of beer lees similar to those used in Example 1 was kneaded with an aqueous solution containing 30 g of sodium carbonate, and dried at 110 ° C. for 12 hours to obtain solids. The solid material was subjected to the same carbonization treatment and activation treatment as in Example 1 to obtain an activated carbon. This activated carbon was washed with hot water to obtain activated carbon. The specific surface area of the obtained activated carbon was 1700 m 2 / g.
実施例３
原料としてのおから（蛋白質含有量２５乾燥重量％）１００ｇを５％炭酸カリウム水溶液３００ｃｃに浸漬し、１０分間煮沸した。次いで、濾紙による吸引濾過により、このおからをこの炭酸カリウム水溶液から分離し、所定量の希塩酸にて中和後、水洗した。得られたおからの蛋白質含有量は２乾燥重量％であった。
Example 3
100 g of okara (protein content 25% by dry weight) as a raw material was immersed in 300 cc of 5% aqueous potassium carbonate solution and boiled for 10 minutes. Next, the okara was separated from the potassium carbonate aqueous solution by suction filtration with a filter paper, neutralized with a predetermined amount of dilute hydrochloric acid, and washed with water. The protein content from the obtained okara was 2% by dry weight.
この得られたおからを乾燥後実施例１と同様の炭化処理と賦活処理を行ない活性炭を得た。得られた活性炭の比表面積は２７００ｍ２／ｇであった。 The obtained okara was dried and then subjected to the same carbonization treatment and activation treatment as in Example 1 to obtain activated carbon. The specific surface area of the obtained activated carbon was 2700 m 2 / g.
本発明の活性炭製造方法で得られる活性炭は、水浄化、脱臭、薬品の精製等に広く活用される。 The activated carbon obtained by the activated carbon production method of the present invention is widely used for water purification, deodorization, chemical purification and the like.
本発明はビール粕のみならず有機の産業廃棄物全般の活用手段として有用である。 The present invention is useful not only for beer lees but also for utilizing organic industrial waste in general.
Claims (5)
該蛋白質除去工程により蛋白質が除去された該有機物を炭化する工程
を含む活性炭製造方法。 A protein removal step of removing the protein from the plant-derived organic matter and reducing the protein content to 5% by dry weight or less;
An activated carbon production method comprising a step of carbonizing the organic substance from which the protein has been removed by the protein removal step.
The method for producing activated carbon according to claim 1, wherein the organic substance is beer lees.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2006315875A (en) * | 2005-05-10 | 2006-11-24 | Kikkoman Corp | Activated carbon obtained by using soy sauce lee and method for producing the same |
| KR20140087399A (en) * | 2012-12-28 | 2014-07-09 | 재단법인 포항산업과학연구원 | Method for manufacturing activated carbon |
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| JPS5761610A (en) * | 1980-09-30 | 1982-04-14 | Honda Motor Co Ltd | Preparation of active carbon |
| JP2001040361A (en) * | 1999-07-27 | 2001-02-13 | Ishii Shoji Kk | Production of bamboo charcoal and liquid for boiling bamboo |
| JP2001292705A (en) * | 2000-04-10 | 2001-10-23 | Maywa Co Ltd | Method for treating waste vegetable |
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| JP2001040361A (en) * | 1999-07-27 | 2001-02-13 | Ishii Shoji Kk | Production of bamboo charcoal and liquid for boiling bamboo |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2006315875A (en) * | 2005-05-10 | 2006-11-24 | Kikkoman Corp | Activated carbon obtained by using soy sauce lee and method for producing the same |
| KR20140087399A (en) * | 2012-12-28 | 2014-07-09 | 재단법인 포항산업과학연구원 | Method for manufacturing activated carbon |
| KR101874086B1 (en) * | 2012-12-28 | 2018-08-02 | 재단법인 포항산업과학연구원 | Method for manufacturing activated carbon |
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