JPH11349318A - Production of activated carbon - Google Patents

Production of activated carbon

Info

Publication number
JPH11349318A
JPH11349318A JP10155798A JP15579898A JPH11349318A JP H11349318 A JPH11349318 A JP H11349318A JP 10155798 A JP10155798 A JP 10155798A JP 15579898 A JP15579898 A JP 15579898A JP H11349318 A JPH11349318 A JP H11349318A
Authority
JP
Japan
Prior art keywords
raw material
activated carbon
carbonaceous raw
product
kneaded
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
JP10155798A
Other languages
Japanese (ja)
Inventor
Yoshio Yoshino
良雄 吉野
Mitsufumi Matsumoto
充史 松本
Kimihisa Oishi
公寿 大石
Akihide Yoshida
彰秀 吉田
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Mitsubishi Chemical Corp
Original Assignee
Mitsubishi Chemical Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Mitsubishi Chemical Corp filed Critical Mitsubishi Chemical Corp
Priority to JP10155798A priority Critical patent/JPH11349318A/en
Publication of JPH11349318A publication Critical patent/JPH11349318A/en
Pending legal-status Critical Current

Links

Abstract

PROBLEM TO BE SOLVED: To provide a method for producing activated carbon by kneading a carbonaceous raw material with an activating so that the light absorption factor of the kneaded product becomes a specific rate based on the light absorption factor of the carbonaceous raw material, molding the kneaded product and subsequently baking the molded product, capable of efficiently and homogeneously adding the activating agent to the product to impart a sufficient strength and a sufficient adsorption performance to the product. SOLUTION: The carbonaceous raw material used as a raw material for the activated carbon includes cellulosic raw materials such as wood, wood chips and coconut husks as woody raw materials, and starchy materials such as Setaria italica, Panicum crus-galli, corns and Panicum miliaceum. The chemical activating agent is preferably zinc chloride, calcium chloride, sodium hydroxide or phosphoric acid. The chemical activating agent and the carbonaceous raw material are kneaded until the 1710 cm<-1> light absorption factor of the kneaded product is 120-500% based on the 1710 cm<-1> light absorption factor of the carbonaceous raw material. The activated carbon is preferably prepared by kneading the activating agent with the carbonaceous raw material e.g. at the ordinary temperature to 200 deg.C, preferably 100-180 deg.C, to impregnate the activating agent into the carbonaceous raw material, granulating the kneaded product, and subsequently baking the granules.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は薬品賦活法による活
性炭の製造方法に関するものであり、詳しくは、成形活
性炭を製造する際の薬品賦活剤と炭素質原料との混合状
態を調整して、得られる活性炭の強度を改善することを
特徴とする薬品賦活活性炭の製造方法に関するものであ
る。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing activated carbon by a chemical activation method. More specifically, the present invention relates to a method for producing a molded activated carbon by adjusting the mixing state of a chemical activator and a carbonaceous raw material. The present invention relates to a method for producing a chemical activated carbon characterized by improving the strength of the activated carbon obtained.

【0002】活性炭は自動車に搭載されるガソリン蒸散
捕集装置(キャニスター)、防毒マスク、工場、研究施
設等の脱臭設備等に用いられ、気相中の各種汚染物質を
吸着除去したり、廃液中の有機物等を吸着除去する等、
様々な用途に用いられている。活性炭の製造方法とし
て、従来より、燐酸又は塩化亜鉛等を用いた薬品賦活法
による活性炭の製造方法が知られている(特開平3−1
46412号公報、特開平5−163020号公報、特
開平7−138010号広報公報)。すなわち、通常原
料となる椰子柄又は木材等の木質原料を燐酸または塩化
亜鉛水溶液といった炭素賦活機能を有する薬品と混合
し、これを常温〜200℃の温度で充分に含浸混練処理
した後に、必要に応じてバインダーを加えて得られる混
練物を押し出し造粒成形等によって粒径0.35〜5.
0mmの造粒物に成型し、次いで、この造粒物を500〜
700℃の温度で焼成することにより、薬品によって賦
活された活性炭を製造することが出来る。
[0002] Activated carbon is used in gasoline evaporation traps (canisters) mounted on automobiles, gas masks, deodorizing equipment in factories, research facilities, etc., to adsorb and remove various contaminants in the gas phase and in waste liquids. To remove organic substances etc.
It is used for various purposes. As a method for producing activated carbon, a method for producing activated carbon by a chemical activation method using phosphoric acid, zinc chloride, or the like has been conventionally known (Japanese Patent Laid-Open No. 3-1).
No. 46412, JP-A-5-163020 and JP-A-7-138010. That is, a woody raw material such as a palm pattern or wood, which is usually a raw material, is mixed with a chemical having a carbon activating function such as phosphoric acid or an aqueous solution of zinc chloride, and the mixture is sufficiently impregnated and kneaded at a temperature of room temperature to 200 ° C. The kneaded product obtained by adding a binder according to the conditions is extruded and granulated to form a particle size of 0.35 to 5.
Molded into 0 mm granules, and then the granulated
By firing at a temperature of 700 ° C., activated carbon activated by a chemical can be produced.

【0003】[0003]

【本発明が解決しようとする課題】このような従来の製
造方法においては、賦活前の造粒成型物の性状が最終製
品の強度に対して大きな影響を及ぼし、製品歩留まりに
対しても影響する。従来より成型物中の被賦活物の充填
状態を密にするために種々の改良が試みられているが、
いまだ充分な方法は見いだされていない。
In such a conventional production method, the properties of the granulated product before activation have a great influence on the strength of the final product and also on the product yield. . Conventionally, various improvements have been attempted in order to densely fill the activator in the molded product.
No satisfactory method has yet been found.

【0004】[0004]

【課題を解決するための手段】本発明は上記実情に鑑
み、塩化亜鉛、燐酸等の賦活活性を持つ薬品を用いた薬
品賦活法による活性炭の製法において、粒状の活性炭を
得るために被賦活材を賦活剤と如何に効率よく均一に充
填し、最終製品に充分な強度を持たせて、製品を工業的
有利に得るための方法を、提供しようとするものであ
る。
SUMMARY OF THE INVENTION In view of the above circumstances, the present invention relates to a method for producing activated carbon by a chemical activation method using a chemical having an activation activity such as zinc chloride or phosphoric acid. It is intended to provide a method for efficiently and uniformly filling an activator with an activator and imparting sufficient strength to a final product to obtain a product in an industrially advantageous manner.

【0005】本発明者等は上記目的を達成するために鋭
意検討を行った結果、賦活剤と被賦活材との混練物にお
いてK−Br錠剤法によるFT−IR法で測定した17
10cm-1光の吸収率をコントロールすることで効率的に
成型炭の粒子密度を上げ、結果的に薬品賦活法による製
品強度の高い活性炭が得られることを見いだした。すな
わち、本発明は、薬品賦活剤と炭素質原料との混練物で
あって、1710cm-1光の吸収率が、炭素質原料の持つ
吸収率の120%以上500%以下であるものを成型、
焼成することを特徴とする活性炭の製造方法に有る。
The present inventors have conducted intensive studies to achieve the above object, and as a result, the kneaded product of the activator and the activator was measured by the FT-IR method using the K-Br tablet method.
It has been found that by controlling the absorptance of 10 cm -1 light, the particle density of the molded carbon can be efficiently increased, and as a result, activated carbon with high product strength can be obtained by the chemical activation method. That is, the present invention provides a kneaded product of a chemical activator and a carbonaceous raw material, in which the absorption of 1710 cm -1 light is 120% or more and 500% or less of the absorption of the carbonaceous raw material,
A method for producing activated carbon characterized by firing.

【0006】[0006]

【発明の実施の形態】以下、本発明を詳細に説明する。
本発明は、薬品賦活剤による活性炭の製造に関するもの
である。まず、本発明で活性炭の原料として用いる物質
としては、薬品賦活しうる炭素質原料であれば、いずれ
も使用することができる。このような物質としては種々
の炭素質原料が知られており、例えば、木質系原料とし
て木材、木屑、椰子殻等のセルロース質や、栗、稗、ト
ウモロコシ、キビ等の澱粉質が挙げられる。その他、泥
炭、褐炭のような鉱物系原料も知られている。これらの
うち、木質系原料、就中、セルロース質原料が、得られ
る活性炭の物性が極めて優れているため好ましい。これ
らの原料の大きさは特に限定されないが、好ましくは粒
度が5mm程度以下のものが、賦活剤と混合しやすいため
賦活をうけやすく、成型もしやすいので好ましい。
DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described below in detail.
The present invention relates to the production of activated carbon using a chemical activator. First, as a substance used as a raw material of the activated carbon in the present invention, any carbonaceous raw material that can be activated with a chemical can be used. Various carbonaceous raw materials are known as such substances. Examples of the woody raw material include cellulosic materials such as wood, wood chips, and coconut shells, and starchy materials such as chestnut, leeches, corn, and millet. In addition, mineral raw materials such as peat and lignite are also known. Among these, wood-based raw materials, especially cellulosic raw materials, are preferable because the obtained activated carbon has extremely excellent physical properties. The size of these raw materials is not particularly limited, but those having a particle size of about 5 mm or less are preferable because they are easily mixed with an activator and thus are easily activated and are easily molded.

【0007】次に、本発明で用いられる薬品賦活剤とし
ては、賦活活性を有する薬品であれば特に限定されず、
いわゆる薬品賦活法において使用されるものはいずれも
用いることができる。例えば、塩化亜鉛、塩化カルシウ
ム、苛性ソーダまたは燐酸が好適であり、これらのうち
塩化亜鉛又は燐酸が、得られる活性炭の物性が極めて優
れるために望ましい。その他、硫化カリウム、硫酸、各
種アルカリ等脱水、酸化、浸食性を有する薬品として知
られたものを用いることができる。
Next, the chemical activator used in the present invention is not particularly limited as long as it has a activating activity.
Any of those used in the so-called chemical activation method can be used. For example, zinc chloride, calcium chloride, caustic soda or phosphoric acid is preferred, and among these, zinc chloride or phosphoric acid is desirable because the properties of the obtained activated carbon are extremely excellent. In addition, potassium sulfide, sulfuric acid, various alkalis, and other known chemicals having dehydration, oxidation, and erosion properties can be used.

【0008】これら薬品賦活剤の濃度、使用量は、用い
る薬品の種類、原料の量等に応じて適宜選択することが
できる。例えば燐酸の場合はオルト燐酸基準で40〜8
5重量%、好ましくは50〜75重量%、炭素質原料と
の混合割合は乾燥固形物重量比で〔燐酸〕/〔炭素質原
料〕=2/1〜1/1程度が好適である。上記の炭素質
原料と薬品賦活剤とを混練する。この混練工程は、通
常、これらを機械的な混合・混練能力を持つ装置、例え
ばニーダーに仕込み、混練し、薬品賦活剤を被賦活材で
ある炭素質原料に含浸させる。
[0008] The concentration and amount of these chemical activators can be appropriately selected according to the type of chemicals used, the amount of raw materials and the like. For example, in the case of phosphoric acid, 40 to 8 on the basis of orthophosphoric acid.
5% by weight, preferably 50 to 75% by weight, and the mixing ratio with the carbonaceous raw material is preferably about [phosphoric acid] / [carbonaceous raw material] = 2/1 to 1/1 in terms of dry solid weight ratio. The above carbonaceous raw material and the chemical activator are kneaded. In the kneading step, these are usually charged into a device having a mechanical mixing / kneading ability, for example, a kneader, kneaded, and the chemical activator is impregnated into the carbonaceous raw material as the activator.

【0009】ここで本発明においては、これら薬品賦活
剤と炭素質原料との混練物が、1710cm−1光の吸収
率が、炭素質原料の持つ吸収率の120%以上500%
以下となるまで混練することを特徴とする。混練物がこ
のような状態となる方法であれば、混練方法は特に限定
されないが、混練の態様として、例えば常温〜200
℃、好ましくは、100〜180℃で、薬品賦活剤と炭
素質原料とを混練する(初期混練)。尚、その後にグリ
セリン等の多価アルコールを添加して混練する場合は、
添加後の混練(終期混練)として常温〜200℃、好ま
しくは、100〜180℃で、30分間以内、好ましく
は15分以内混練を行う。かかる混練により、薬品賦活
剤が炭素質原料に含浸される。
In the present invention, the kneaded product of the chemical activator and the carbonaceous raw material has an absorptivity of 1710 cm-1 light of 120% to 500% of the absorptivity of the carbonaceous raw material.
It is characterized by kneading until the following is achieved. The kneading method is not particularly limited as long as the kneaded material is in such a state.
The chemical activator and the carbonaceous material are kneaded at a temperature of preferably from 100 to 180 ° C (initial kneading). In addition, when adding and kneading a polyhydric alcohol such as glycerin,
As kneading after the addition (final kneading), kneading is performed at room temperature to 200 ° C., preferably 100 to 180 ° C., within 30 minutes, preferably within 15 minutes. By this kneading, the chemical activator is impregnated into the carbonaceous raw material.

【0010】混練工程は、常圧で行うこともできるが、
減圧して揮発分を速やかに除去することもできる。こう
して得られた混練物は、通常パサパサの粉体であるが、
この混練物として本発明では、1710cm-1光の吸収率
が、炭素質原料の持つ1710cm-1光の吸収率の120
%以上500%以下、望ましくは200%以上400%
以下であるものとする。ここで1710cm-1光の吸収率
は、K−Br錠剤法によるFT−IR法により測定した
ものである。
The kneading step can be carried out at normal pressure,
The pressure can be reduced to quickly remove volatile components. The kneaded material thus obtained is usually a powder of pasa pasa,
In the present invention as the kneaded product, 1710 cm -1 light absorption rate of, the absorptivity of 1710 cm -1 light with a carbonaceous feedstock 120
% To 500%, preferably 200% to 400%
It is assumed that: Here, the absorptance of 1710 cm -1 light was measured by the FT-IR method using the K-Br tablet method.

【0011】なお、炭素質原料と薬品賦活剤の他、必要
に応じてバインダー等を加えることもできる。バインダ
ーとしてはリグニンスルホン酸ナトリウム、樹脂等の有
機系バインダー、ベントナイト、ピッチ等の無機系バイ
ンダーが知られている。次に上記の混練物を、造粒成型
する。成型に用いる装置は特に限定されず、通常押し出
し成型機、或いはプレス成型機が一般的である。例えば
特開平7−138010号公報に記述されるように、9
0℃〜180℃に加温しながら成型する方法、或いは混
練物を常温まで冷却した後常温で成型する方法等が用い
られる。本発明では特に加熱する必要もないので、常温
で行えば充分である。得られる造粒物の形状は、押し出
し成型では0.5〜10mmφ程度のペレット状粒、プレ
ス成型では成型後、破砕して0.5〜10mmφ程度の破
砕状粒となる。
[0011] In addition to the carbonaceous raw material and the chemical activator, a binder or the like can be added as required. As the binder, organic binders such as sodium ligninsulfonate and resin, and inorganic binders such as bentonite and pitch are known. Next, the above kneaded material is granulated and formed. The apparatus used for molding is not particularly limited, and an extrusion molding machine or a press molding machine is generally used. For example, as described in Japanese Patent Application Laid-Open No.
A method of molding while heating to 0 ° C. to 180 ° C. or a method of cooling the kneaded material to room temperature and then molding at room temperature is used. In the present invention, since it is not necessary to particularly heat, it is sufficient to carry out at normal temperature. The shape of the obtained granulated product is pellet-like particles of about 0.5 to 10 mmφ in extrusion molding, and crushed into granules of about 0.5 to 10 mmφ after molding in press molding.

【0012】造粒成型して得られた造粒物を、焼成に先
立ち予め転動操作に処することも好適である。転動操作
により、最終的に得られる活性炭の耐磨耗性が更に優れ
たものとなる。転動操作は例えばトロンメル、或いは同
種の転動を行える装置で、常温〜100℃、2時間以内
行えば充分である。上記の造粒物を焼成して、活性炭と
する。焼成方法は特に限定されず、公知の方法を採用す
ることができる。一般には最高温度500〜700℃ま
で昇温加熱することにより行われる。トンネル炉、ロー
タリーキルン等、ガス雰囲気をコントロールでき、加熱
処理を行える設備を用いることができる。また例えば特
開平6−127912号公報に記載の二段加熱により活
性炭の吸着能を向上する方法を採ることもできる。
It is also preferable that the granulated material obtained by granulation molding is subjected to a rolling operation before firing. The rolling operation further enhances the wear resistance of the finally obtained activated carbon. The rolling operation is, for example, trommel or a device capable of performing the same type of rolling, and it is sufficient to perform the rolling operation at room temperature to 100 ° C. within 2 hours. The above granulated material is fired to obtain activated carbon. The firing method is not particularly limited, and a known method can be employed. Generally, the heating is performed by heating to a maximum temperature of 500 to 700 ° C. Equipment capable of controlling the gas atmosphere and performing heat treatment, such as a tunnel furnace and a rotary kiln, can be used. Further, for example, a method described in JP-A-6-127912, in which the adsorption capacity of activated carbon is improved by two-stage heating, can be adopted.

【0013】焼成後、常法により焼成物を温水で懸濁洗
浄することにより賦活剤薬品を除去してから乾燥する。
懸濁洗浄は、常温〜100℃で、焼成物を水と懸濁さ
せ、5分〜12時間、好ましくは20〜40分間放置し
たのち濾過分離する。この操作を、濾過液から賦活剤が
検知できなくなるまで繰り返す。また乾燥は、500℃
以下、好ましくは100〜150℃で行うのが一般的で
ある。
After firing, the fired product is suspended and washed with warm water by a conventional method to remove the activator chemical and then dried.
In the suspension washing, the calcined product is suspended in water at normal temperature to 100 ° C., left for 5 minutes to 12 hours, preferably 20 to 40 minutes, and then separated by filtration. This operation is repeated until no activator can be detected from the filtrate. Drying at 500 ° C
Hereinafter, it is general that the heat treatment is preferably performed at 100 to 150 ° C.

【0014】以上説明した本発明の薬品賦活法による活
性炭の製造では、例えば燐酸、塩化亜鉛等と被賦活材で
ある炭素質原料との混練物において、1710cm-1光の
吸収率を炭素質原料における1710cm-1光の吸収率に
対して適切な量となっており、このことが得られる製品
である活性炭の強度と容積当たりの吸着性能に対して良
い効果を示すことが本発明者らにより見出されたのであ
る。この1710cm-1光の吸収率は、炭素質の炭化が進
むことによって増加することから、被賦活材の炭化度合
いをコントロールし、成型時の賦活材の充填密度を高く
するのに有効であることを見出したのである。
In the above-described production of activated carbon by the chemical activation method of the present invention, in a kneaded product of, for example, phosphoric acid, zinc chloride, etc. and a carbonaceous raw material as an activator, the absorptivity of 1710 cm -1 light is adjusted to the carbonaceous raw material. It is an appropriate amount for the absorptance of light at 1710 cm -1 in the above, and the present inventors have shown that this has a good effect on the strength and adsorption performance per volume of the obtained activated carbon. It was found. Since the absorptance of this 1710 cm -1 light increases as carbonization proceeds, it is effective to control the degree of carbonization of the activator and increase the packing density of the activator during molding. Was found.

【0015】混練物の1710cm-1光の吸収率が、炭素
質原料の有する1710cm-1光の吸収率の120%より
も少ない場合には、より高温で焼成される賦活工程で炭
素質由来の水酸基が飛び、気孔を生じ、賦活反応に対し
て寄与せず、粒子内での被賦活材の結合を阻害する為、
製品の強度が低下し、嵩密度も低下するため容積当たり
の吸着性能が低下すると考えられる。このために、この
1710cm-1光の吸収率を、炭素質原料の有する吸収率
の120%よりも大きくすることが、製品の強度を上
げ、容積当たりの吸着性能を向上させる事に効果を及ぼ
すと考えられる。しかし、この1710cm-1光の吸収率
を、木質系原料の持つ吸収率の500%よりも大きくし
すぎると、成型性が悪くなり、製品を作ることが困難に
なる。特開平6−56416号公報や、特開平7−13
8010号公報に記述されるような従来の製造方法で
は、混練したものの1710cm-1光の吸収率で、成形前
の状態をコントロールしていないために、製品生産に対
して最適な成型物を得ることができず、安定的に高品質
の製品を得ることができない。しかしながら、本発明の
ように混練したものの1710cm-1光の吸収率でコント
ーロールすれば、より高性能な製品を得ることができる
ため生産面でよりすぐれている。
[0015] 1710 cm -1 light absorption rate of the kneaded product, if less than 120% of the absorptivity of 1710 cm -1 light with the carbonaceous feedstock is derived from carbonaceous in activation process are more fired at a high temperature Hydroxyl groups fly, generate pores, do not contribute to the activation reaction, and inhibit the binding of the activator in the particles,
It is considered that the strength of the product is reduced and the bulk density is also reduced, so that the adsorption performance per volume is reduced. For this reason, increasing the absorptance of this 1710 cm -1 light to more than 120% of the absorptivity of the carbonaceous material has the effect of increasing the strength of the product and improving the adsorption performance per volume. it is conceivable that. However, if the absorptance of this 1710 cm -1 light is too much larger than 500% of the absorptivity of the woody raw material, the moldability deteriorates and it becomes difficult to produce a product. JP-A-6-56416 and JP-A-7-13
In the conventional manufacturing method as described in JP-A-8010, the state before molding is controlled by the absorptivity of 1710 cm -1 light of the kneaded product, so that an optimal molded product for product production is obtained. And it is not possible to stably obtain high quality products. However, if the kneaded material as in the present invention is controlled at an absorptance of 1710 cm -1 light, a higher performance product can be obtained, so that the production is more excellent.

【0016】本発明者らは、賦活剤と被賦活材とを混合
する課程で加熱処理又は減圧処理等の処理で混合物を処
理し、混練したものの1710cm-1光の吸収率が、炭素
質原料の有する吸収率の120%以上500%以下、望
ましくは200%以上400%以下に調整して成形する
ことで、強度が高く、容積当たりの吸着性能の高い製品
を得ることが出来ることを見いだしたのである。
The present inventors have found that the mixture of the activator and the activator is treated by heat treatment or decompression treatment in a process of mixing the activator and the activator, and the kneaded mixture has an absorptivity of 1710 cm -1 light and a carbonaceous material. By adjusting the absorption rate to 120% or more and 500% or less, desirably 200% or more and 400% or less, and molding, it has been found that a product having high strength and high adsorption performance per volume can be obtained. It is.

【0017】[0017]

【実施例】次に、本発明を実施例により更に詳細に説明
する。尚、強度及びn-Butane吸着性能は下記の測定方法
により求めた。 (強度)13mm直径の鋼球20個が入ったステンレス製
ポット(内容積150ml)に試料1.00gを入れ、1
20rpmで15分間回転させる。次いで試料を60メッ
シュの篩で篩い分けして篩上の重量を測定し、供試試料
に対するに対する篩上試料の重量百分率を強度とする。 (n-Butane吸着性能) (1)試料を150℃、3時間乾燥し、デシケータ中で
放冷する。 (2)内径15.4mmφのガラスカラムの空重量を測定
する。(Dg) (3)このカラムに、層高5.4cmで試料を充填する。 (4)カラムを密栓して重量を測定する。(Eg) (5)25℃の恒温水槽にセットし、n-Butane(純度9
9.9%以上)を105.4ml/分の流速で15分間上
向流で通気させる。 (6)カラムを取り外し秤量する。(Fg) (7)吸着後のカラムを再度装置にセットし、下降流で
25℃の乾燥空気を100ml/分の流速で20分間通気
する。 (8)カラムを取り外し秤量する。(Gg) (9)以上の測定データより、飽和有効吸着量を計算す
る。
Next, the present invention will be described in more detail with reference to examples. The strength and the n-Butane adsorption performance were determined by the following measurement methods. (Strength) 1.00 g of a sample was placed in a stainless steel pot (internal volume: 150 ml) containing 20 13 mm-diameter steel balls.
Spin at 20 rpm for 15 minutes. Next, the sample is sieved with a 60-mesh sieve, the weight on the sieve is measured, and the weight percentage of the sample on the sieve relative to the test sample is defined as the strength. (N-Butane adsorption performance) (1) The sample is dried at 150 ° C. for 3 hours and allowed to cool in a desiccator. (2) The empty weight of a glass column having an inner diameter of 15.4 mmφ is measured. (Dg) (3) This column is filled with a sample at a layer height of 5.4 cm. (4) Seal the column and measure the weight. (Eg) (5) Set in a constant temperature water bath at 25 ° C., and add n-Butane (purity 9).
9.9%) at a flow rate of 105.4 ml / min for 15 minutes in an upward flow. (6) Remove the column and weigh. (Fg) (7) The column after the adsorption is set in the apparatus again, and dry air at 25 ° C. is flown in a downward flow at a flow rate of 100 ml / min for 20 minutes. (8) Remove the column and weigh. (Gg) (9) The saturated effective adsorption amount is calculated from the above measurement data.

【0018】n-Butane飽和有効吸着量[g/dl活性炭]=
100×(F−G)÷(E−D)÷(活性炭の嵩密度) (実施例1)粒径2.0mm以下の木屑乾燥品1.0kgと
85重量%濃度の燐酸水溶液2.0kgとを、バッチ式ニ
ーダーを使用し、140℃で120分間、混練した。次
に、バインダーとしてリグニンスルホン酸ナトリウム水
溶液150gを加えて、15分間ニーダーで混練した。
この混練物の有する1710cm-1光の吸収率の、炭素質
原料の有する吸収率に対する百分率(%)を、表−1に
示す。
N-Butane saturated effective adsorption amount [g / dl activated carbon] =
100 × (FG) {(ED)} (bulk density of activated carbon) (Example 1) 1.0 kg of dried wood chips having a particle size of 2.0 mm or less and 2.0 kg of a 85% by weight phosphoric acid aqueous solution Was kneaded at 140 ° C. for 120 minutes using a batch kneader. Next, 150 g of an aqueous solution of sodium ligninsulfonate was added as a binder, and kneaded with a kneader for 15 minutes.
Table 1 shows the percentage (%) of the absorptivity of the kneaded material at 1710 cm -1 with respect to the absorptivity of the carbonaceous raw material.

【0019】この混練物を直径2.5mmφのダイスを有
するディスクペレッターで、押し出し造粒し、長さ3〜
5mm程度のペレットを得た。このペレットをトロンメル
にて、1時間転動を行った。転動後、ペレットを外熱式
のロータリーキルンで、窒素と空気との混合ガスを通気
して焼成するにあたり、先ず、酸素濃度0%で、100
℃から250℃まで12℃/分で昇温した。さらにその
後、酸素濃度を21%とし、250℃から350℃を2
時間かけて昇温し、この後、酸素濃度を4%にして、3
50℃から550℃まで、12℃/分で昇温した。55
0℃に達した後、直ちに冷却した。この焼成品を定法に
従って、湯洗浄し、燐酸を除去したのち、乾燥した。
The kneaded material is extruded and granulated with a disk pelleter having a die having a diameter of 2.5 mmφ and has a length of 3 to
A pellet of about 5 mm was obtained. The pellets were rolled with a trommel for one hour. After rolling, the pellets were fired in an externally heated rotary kiln by passing a mixed gas of nitrogen and air.
The temperature was increased from 12 ° C to 250 ° C at 12 ° C / min. After that, the oxygen concentration was set to 21%, and 250 ° C to 350 ° C was changed to 2%.
The temperature was raised over time, after which the oxygen concentration was increased to 4% and 3
The temperature was raised from 50 ° C. to 550 ° C. at 12 ° C./min. 55
After reaching 0 ° C., it was cooled immediately. The calcined product was washed with hot water to remove phosphoric acid and dried according to a standard method.

【0020】得られた最終製品である活性炭の強度とn-
Butane吸着性能を測定し、表−1に示す結果を得た。 (実施例2〜4)混練処理時の温度と処理時間が異な
り、成型造粒前の混練物の1710cm-1光吸収率と木質
系原料の持つ吸収率の比が異なる以外は、実施例1と同
一条件で製造したものについて、強度とn-Butane吸着性
能の測定を実施し、表−1に示す結果を得た。 (比較例1〜4)混練処理時の温度と処理時間が異な
り、成型造粒前の混練物の1710cm-1光吸収率と木質
系原料の持つ吸収率の比が異なる以外は、実施例1と同
一条件で製造したものについて、強度とn-Butane吸着性
能の測定を実施し、表−1に示す結果を得た。
[0020] The strength and n-
The Butane adsorption performance was measured and the results shown in Table 1 were obtained. (Examples 2 to 4) Example 1 was the same as Example 1 except that the temperature and the processing time during the kneading process were different, and the ratio of the absorptivity of the wood-based raw material to the light absorption of 1710 cm -1 of the kneaded product before molding and granulation was different. For those manufactured under the same conditions as those described above, the strength and the n-Butane adsorption performance were measured, and the results shown in Table 1 were obtained. (Comparative Examples 1 to 4) Example 1 except that the temperature and the processing time during the kneading process were different, and the ratio of the light absorption of 1710 cm -1 of the kneaded product before molding and granulation was different from that of the wood-based raw material. For those manufactured under the same conditions as those described above, the strength and the n-Butane adsorption performance were measured, and the results shown in Table 1 were obtained.

【0021】[0021]

【表1】 [Table 1]

【0022】[0022]

【発明の効果】本発明によれば、燐酸等を用いた薬品賦
活法による粒状活性炭の製法において、高い強度と吸着
性能を保持した活性炭を工業的に有利に得ることができ
る。
According to the present invention, in a method for producing granular activated carbon by a chemical activation method using phosphoric acid or the like, activated carbon having high strength and adsorption performance can be industrially advantageously obtained.

───────────────────────────────────────────────────── フロントページの続き (72)発明者 吉田 彰秀 北九州市八幡西区黒崎城石1番1号 三菱 化学株式会社黒崎事業所内 ──────────────────────────────────────────────────の Continued on the front page (72) Inventor Akihide Yoshida 1-1 Kurosaki Castle Stone, Yawatanishi-ku, Kitakyushu City Inside Mitsubishi Chemical Corporation Kurosaki Office

Claims (3)

【特許請求の範囲】[Claims] 【請求項1】薬品賦活剤と炭素質原料との混練物であっ
て、1710cm-1光の吸収率が、炭素質原料の持つ吸収
率の120%以上500%以下であるものを成型、焼成
することを特徴とする活性炭の製造方法。
1. A kneaded product of a chemical activator and a carbonaceous raw material having an absorptivity of 1710 cm -1 light of 120% or more and 500% or less of an absorptivity of a carbonaceous raw material is molded and fired. A method for producing activated carbon.
【請求項2】薬品賦活剤と炭素質原料との混練物が、1
00℃で加熱しながら混練することにより得られたもの
である請求項1記載の活性炭の製造方法。
2. A kneaded product of a chemical activator and a carbonaceous raw material,
The method for producing activated carbon according to claim 1, wherein the method is obtained by kneading while heating at 00 ° C.
【請求項3】薬品賦活剤が燐酸であることを特徴とする
請求項1又は2記載の活性炭の製造方法。
3. The method for producing activated carbon according to claim 1, wherein the chemical activator is phosphoric acid.
JP10155798A 1998-06-04 1998-06-04 Production of activated carbon Pending JPH11349318A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP10155798A JPH11349318A (en) 1998-06-04 1998-06-04 Production of activated carbon

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP10155798A JPH11349318A (en) 1998-06-04 1998-06-04 Production of activated carbon

Publications (1)

Publication Number Publication Date
JPH11349318A true JPH11349318A (en) 1999-12-21

Family

ID=15613682

Family Applications (1)

Application Number Title Priority Date Filing Date
JP10155798A Pending JPH11349318A (en) 1998-06-04 1998-06-04 Production of activated carbon

Country Status (1)

Country Link
JP (1) JPH11349318A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002104816A (en) * 1999-11-16 2002-04-10 Kuraray Co Ltd Activated carbon and its manufacturing method
CN101913603A (en) * 2010-08-16 2010-12-15 西北农林科技大学 Method for preparing activated carbon from peeled branch wood of initiated branches in eucommia bark leaf forest
JP2012512130A (en) * 2008-12-15 2012-05-31 コーニング インコーポレイテッド Method of forming activated carbon material for ultracapacitor with high energy density
CN108439403A (en) * 2018-06-12 2018-08-24 中国林业科学研究院林产化学工业研究所 A kind of method that low-temperature prewarming solution, raw material fine prepare biomass moulding activated carbon
CN113474287A (en) * 2019-03-06 2021-10-01 株式会社可乐丽 Activated carbon and method for producing same

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002104816A (en) * 1999-11-16 2002-04-10 Kuraray Co Ltd Activated carbon and its manufacturing method
JP2012512130A (en) * 2008-12-15 2012-05-31 コーニング インコーポレイテッド Method of forming activated carbon material for ultracapacitor with high energy density
US8784764B2 (en) 2008-12-15 2014-07-22 Corning Incorporated Methods for forming activated carbon material for high energy density ultracapacitors
CN101913603A (en) * 2010-08-16 2010-12-15 西北农林科技大学 Method for preparing activated carbon from peeled branch wood of initiated branches in eucommia bark leaf forest
CN108439403A (en) * 2018-06-12 2018-08-24 中国林业科学研究院林产化学工业研究所 A kind of method that low-temperature prewarming solution, raw material fine prepare biomass moulding activated carbon
CN108439403B (en) * 2018-06-12 2021-08-17 中国林业科学研究院林产化学工业研究所 Method for preparing biomass-formed activated carbon by low-temperature pre-pyrolysis and superfine raw materials
CN113474287A (en) * 2019-03-06 2021-10-01 株式会社可乐丽 Activated carbon and method for producing same

Similar Documents

Publication Publication Date Title
JP4277065B2 (en) Molded activated carbon
JP2790328B2 (en) Chemically activated molded activated carbon and its production method and use
US5324703A (en) Method of preparation of gasoline vapor adsorptive activated carbon
US5538932A (en) Preparation of high activity, high density activated carbon with activatable binder
US4857243A (en) Process of making microspherules of activated carbon
JP3669373B2 (en) Process for producing activated coke for simultaneous desulfurization and denitrification
JP3746509B1 (en) Spherical activated carbon and its manufacturing method
JP2000026114A (en) Aggregate based on activated carbon, its preparation and its use as adsorbent
US5736481A (en) Shaped lignocellulosic-based activated carbon
JP2000313611A (en) Active carbon and its production
US5736485A (en) Shaped lignocellulosic-based activated carbon
US20220096981A1 (en) Pelletized activated carbon and methods of production
JPH11349320A (en) Production of activated carbon
JP2007331986A (en) Activated carbon
JPH11349318A (en) Production of activated carbon
JPS6323125B2 (en)
JPH11349319A (en) Production of activated carbon
RU2597400C1 (en) Method of producing composite sorbent based on mineral and vegetable carbon-containing material
JP3092477B2 (en) Granular activated carbon and method for producing the same
PL111361B1 (en) Process for manufacturing granulated activated carbon
JP4708409B2 (en) Molded activated carbon for waste gas treatment and method for producing the same
CN105983389B (en) The preparation method of activated carbon containing lanthanum
KR101176587B1 (en) Method of preparing spherical active carbon for adsorptive removal of Iodide and Hydrogen sulfide and superior active carbon prepared therefrom
JP2009057239A (en) Activated carbon preparation method
JP3125808B2 (en) Activated carbon honeycomb structure and manufacturing method thereof

Legal Events

Date Code Title Description
A621 Written request for application examination

Effective date: 20040311

Free format text: JAPANESE INTERMEDIATE CODE: A621

A977 Report on retrieval

Free format text: JAPANESE INTERMEDIATE CODE: A971007

Effective date: 20060414

A131 Notification of reasons for refusal

Free format text: JAPANESE INTERMEDIATE CODE: A131

Effective date: 20060523

A521 Written amendment

Effective date: 20060722

Free format text: JAPANESE INTERMEDIATE CODE: A523

TRDD Decision of grant or rejection written
A01 Written decision to grant a patent or to grant a registration (utility model)

Free format text: JAPANESE INTERMEDIATE CODE: A01

Effective date: 20061024

A61 First payment of annual fees (during grant procedure)

Free format text: JAPANESE INTERMEDIATE CODE: A61

Effective date: 20061025

R150 Certificate of patent (=grant) or registration of utility model

Free format text: JAPANESE INTERMEDIATE CODE: R150

LAPS Cancellation because of no payment of annual fees