JPS6135286B2 - - Google Patents

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Publication number
JPS6135286B2
JPS6135286B2 JP53076039A JP7603978A JPS6135286B2 JP S6135286 B2 JPS6135286 B2 JP S6135286B2 JP 53076039 A JP53076039 A JP 53076039A JP 7603978 A JP7603978 A JP 7603978A JP S6135286 B2 JPS6135286 B2 JP S6135286B2
Authority
JP
Japan
Prior art keywords
weight
fibers
activated carbon
fiber
vegetable
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.)
Expired
Application number
JP53076039A
Other languages
Japanese (ja)
Other versions
JPS553354A (en
Inventor
Hiroshi Nishino
Masayuki Suzuki
Hideo Hirota
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.)
Takeda Pharmaceutical Co Ltd
Original Assignee
Takeda Chemical Industries Ltd
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 Takeda Chemical Industries Ltd filed Critical Takeda Chemical Industries Ltd
Priority to JP7603978A priority Critical patent/JPS553354A/en
Priority to US06/266,012 priority patent/US4409125A/en
Priority to PCT/JP1979/000160 priority patent/WO1984001566A1/en
Publication of JPS553354A publication Critical patent/JPS553354A/en
Publication of JPS6135286B2 publication Critical patent/JPS6135286B2/ja
Granted legal-status Critical Current

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  • Inorganic Fibers (AREA)
  • Carbon And Carbon Compounds (AREA)

Description

【発明の詳細な説明】[Detailed description of the invention]

本発明は、植物性繊維を原料とし、これを炭
化、賦活化することによつて活性炭素繊維を製造
する方法に関する。 活性炭素繊維は粉末状の活性炭に比べて取り扱
いが容易で、しかも吸着性能もすぐれているの
で、最近、非常に注目されている吸着剤である。 従来、活性炭素繊維はアクリル繊維を原料とし
て製造されてきた。この従来法では、まずアクリ
ル繊維を酸化性雰囲気中、約200〜300℃の温度で
約2〜20時間張力を与えながら酸化処理をして十
分に耐炎化をおこなう。ついで、この耐炎化され
たものを水蒸気雰囲気中、約900〜1000℃の温度
で約20分〜3時間処理することによつて賦活化さ
れた活性炭素繊維が得られる。 しかしながら、従来法ではアクリル繊維を原料
とするので耐炎化工程に長時間要するうえに、賦
活化工程の時間も長く、しかもその温度もまた高
くしなければならないという欠点があつた。 このような事情に鑑み、本発明者らは鋭意研究
した結果、原料繊維として植物性繊維を用い、こ
れに(1)塩化亜鉛と(2)塩化アンモニウム、ホウ酸お
よび硝酸からなる群から選ばれた少なくとも一種
とを組み合わせた溶液を含浸させた後、炭化、賦
活化することによつて活性炭素繊維の収率が飛躍
的に向上するうえに、吸着性能も向上することが
わかつた。このような知見にもとづき本発明を完
成するに至つた。 すなわち、本発明は(1)塩化亜鉛と(2)塩化アンモ
ニウム、ホウ酸および硝酸からなる群から選ばれ
た少なくとも一種を含有する溶液を植物性繊維に
含浸させた後、炭化、賦活化することを特徴とす
る活性炭素繊維の製造方法である。 本発明において用いられる植物性繊維は、植物
を原料とするすべての繊維を意味し、たとえば植
子毛繊維(例;綿、カポツク、バンボツクス綿、
パンヤ、植物綿など)、靭皮繊維(例;亜麻、大
麻、ジユート、ラミー、ケナフ、三椏など)、葉
脈繊維(例;マニラ麻、ニユージーランド麻、シ
ザル麻、ヒタ繊維など)、果実繊維(例;ヤシな
ど)、その他(例:藺、藁類、海草すがも繊維、
いらくさなど)、たとえばビスコースレーヨン、
銅アンモニアレーヨンなどのセルロース系再生人
造繊維、たとえばアセテート、酢化スフなどのセ
ルロース系半合成繊維などがあげられる。これら
の繊維は、繊維状であつてもよく、また、これら
の繊維をたとえば織物、不織布、フエルト紙状等
の繊維構造体にしたものでもよい。 〓〓〓〓
本発明では、まず上記植物性繊維に(1)塩化亜鉛
と(2)塩化アンモニウム、ホウ酸および硝酸からな
る群から選ばれた少なくとも一種とを含有する溶
液を含浸させる。 上記溶液中、塩化亜鉛の量は約5〜40重量%、
特に約10〜30重量%が好ましい。また、塩化アン
モニウム、ホウ酸または硝酸の量は約0.5〜25重
量%、特に約2〜20重量%が好ましい。植物性繊
維に対する塩化亜鉛の含浸量は約5〜60重量%、
特に約10〜30重量%が好ましい。塩化アンモニウ
ムを用いる場合、その量は約5〜25重量%、特に
約10〜20重量%が好ましい。ホウ酸を用いる場合
は約0.1〜10重量%、特に約0.5〜5重量%が好ま
しい。硝酸を用いる場合は約0.1〜10重量%、特
に約0.5〜5重量%が好ましい。上記の化合物を
含有する溶液は、水溶液であつてもよく、あるい
はアルコールなどを含む溶液であつてもよい。ま
た、塩化亜鉛などの水に対する溶解度をあげるた
めに、上記溶液にたとえば塩酸などを加えてもよ
い。その量は通常、約5重量%以内である。 上記溶液を植物性繊維に含浸させる手段として
は、たとえば植物性繊維を上記溶液に浸漬する手
段や上記溶液を植物性繊維に散布する手段などが
あげられる。 つぎに、本発明では前記化合物を含浸させた植
物性繊維を炭化、賦活化する。炭化、賦活化の温
度は約400〜750℃、特に約450〜650℃が好まし
く、その時間は約0.25〜2時間、特に約0.5〜1
時間が好ましい。炭化、賦活化は通常、たとえば
窒素ガス、重油、軽油、灯油などの燃焼排ガスな
どの不活性ガス雰囲気下でおこなわれる。 このようにして炭化、賦活化された植物性繊維
は必要ならば常法により洗浄、乾燥する操作を施
してもよい。 本発明の方法によれば活性炭素繊維の収率が飛
躍的に向上するので従来法よりもはるかに安価に
活性炭素繊維を供給できるうえに、得られた製品
の吸着性能もすぐれたものであり、産業上極めて
有用な方法である。 以下に実施例ならびに比較例をあげ、本発明を
具体的に説明する。 比較例 1 市販の綿布(晒)を20重量%の塩化亜鉛 0.2
重量%の塩化水素を含む水溶液に約5分間浸漬し
たのちゴムローラーを用いて絞り薬液を均一に担
持させた。塩化亜鉛の担持量は0.35g/g−原料
布であつた。薬液を担持せしめた原料布を16メツ
シユのステンレス製金網のロールに巻きとり窒素
気流中600℃の温度で約1/2時間焼成した。このよ
うにして活性炭素繊維Aが得られた。該活性炭素
繊維Aの収率および吸着力は表−1のとうりであ
つた。 実施例 1 20重量%の塩化亜鉛、15.5重量%の塩化アンモ
ニウム、1重量%の塩化水素を含む水溶液を担持
するほかは比較例1と同じ方法で活性炭素繊維B
を製造した。該活性炭素繊維Bの収率および吸着
力は表−1のとうりであつた。 なお薬品担持量は0.4g/g−原料布であつた。 実施例 2 市販の麻布を25重量%の塩化亜鉛、2.5重量%
のホウ酸、2重量%の塩化水素を含む水溶液に約
5分間浸漬したのち遠心分離器により脱水をおこ
ない薬液を均一に担持させた。薬品担持量は0.43
g/g−原料布であつた。薬液を担持せしめた原
料布を16メツシユのステンレス製金網に巻きとり
窒素気流中550℃の温度で3/4時間焼成し、活性炭
素繊維Cを製造した。該活性炭素繊維Cの収率お
よび吸着力は表−1のとうりであつた。 実施例 3 25重量%の鉛化亜鉛、12.5重量%の塩化アンモ
ニウム、5重量%のホウ酸、1重量%の塩化水素
を含む水溶液を担持するほかは実施例2と同じ方
法で活性炭素繊維Dを製造した。該活性炭素繊維
Dの収率および吸着力は表−1のとうりであつ
た。 なお薬品担持量は0.47g/g−原料布であつ
た。 実施例 4 15重量%の塩化亜鉛、2重量%の硝酸、1重量
%の塩化水素を含む水溶液を担持する水溶液を担
持するほかは比較例1と同じ方法で活性炭素繊維
Eを製造した。該活性炭素繊維Eの収率および吸
着力は表−1のとうりであつた。 なお薬品担持量は0.25g/g−原料布であつ
た。 〓〓〓〓
The present invention relates to a method for producing activated carbon fibers by carbonizing and activating vegetable fibers using vegetable fibers as raw materials. Activated carbon fiber is an adsorbent that has recently attracted much attention because it is easier to handle than powdered activated carbon and has superior adsorption performance. Conventionally, activated carbon fibers have been manufactured using acrylic fibers as raw materials. In this conventional method, acrylic fibers are first oxidized in an oxidizing atmosphere at a temperature of about 200 to 300° C. while applying tension for about 2 to 20 hours to make them sufficiently flame resistant. Then, this flame-resistant fiber is treated in a steam atmosphere at a temperature of about 900 to 1000° C. for about 20 minutes to 3 hours, thereby obtaining an activated carbon fiber. However, in the conventional method, since acrylic fibers are used as raw materials, the flame resistance process takes a long time, and the activation process also takes a long time and has the disadvantage that the temperature also has to be high. In view of these circumstances, as a result of intensive research, the present inventors used vegetable fiber as the raw material fiber, and added a mixture of (1) zinc chloride, (2) ammonium chloride, boric acid, and nitric acid to the vegetable fiber. It has been found that by impregnating the activated carbon fibers with a solution containing at least one type of carbon fibers, followed by carbonization and activation, the yield of activated carbon fibers is dramatically improved, and the adsorption performance is also improved. Based on such knowledge, we have completed the present invention. That is, the present invention involves impregnating vegetable fibers with a solution containing at least one selected from the group consisting of (1) zinc chloride and (2) ammonium chloride, boric acid, and nitric acid, and then carbonizing and activating the solution. This is a method for producing activated carbon fiber characterized by the following. The vegetable fiber used in the present invention refers to all fibers made from plants, such as flocked fibers (e.g. cotton, kapok, bamboo cotton,
Panya, vegetable cotton, etc.), bast fibers (e.g., flax, hemp, jute, ramie, kenaf, mitsumata, etc.), leaf vein fibers (e.g., Manila hemp, New Zealand hemp, sisal hemp, hita fiber, etc.), fruit fibers (e.g. ; coconut, etc.), others (e.g. straw, straw, seaweed sugamo fiber,
(irritability, etc.), such as viscose rayon,
Examples include cellulose-based regenerated artificial fibers such as cuprammonium rayon, and cellulose-based semi-synthetic fibers such as acetate and acetate sulphur. These fibers may be in the form of fibers, or may be formed into a fiber structure such as a woven fabric, a nonwoven fabric, or a felt paper. 〓〓〓〓
In the present invention, the vegetable fiber is first impregnated with a solution containing (1) zinc chloride and (2) at least one selected from the group consisting of ammonium chloride, boric acid, and nitric acid. In the above solution, the amount of zinc chloride is about 5 to 40% by weight,
Particularly preferred is about 10 to 30% by weight. The amount of ammonium chloride, boric acid or nitric acid is preferably about 0.5 to 25% by weight, particularly about 2 to 20% by weight. The amount of zinc chloride impregnated into vegetable fiber is approximately 5 to 60% by weight,
Particularly preferred is about 10 to 30% by weight. If ammonium chloride is used, the amount is preferably about 5 to 25% by weight, especially about 10 to 20% by weight. If boric acid is used, it is preferably about 0.1 to 10% by weight, particularly about 0.5 to 5% by weight. If nitric acid is used, it is preferably about 0.1 to 10% by weight, especially about 0.5 to 5% by weight. The solution containing the above compound may be an aqueous solution or a solution containing alcohol or the like. Furthermore, in order to increase the solubility of zinc chloride and the like in water, for example, hydrochloric acid or the like may be added to the above solution. The amount is usually within about 5% by weight. Examples of means for impregnating the vegetable fibers with the solution include immersing the vegetable fibers in the solution and spraying the solution onto the vegetable fibers. Next, in the present invention, the vegetable fiber impregnated with the compound is carbonized and activated. The carbonization and activation temperature is preferably about 400 to 750°C, particularly about 450 to 650°C, and the time is about 0.25 to 2 hours, especially about 0.5 to 1
time is preferable. Carbonization and activation are usually performed under an inert gas atmosphere such as nitrogen gas, combustion exhaust gas such as heavy oil, light oil, and kerosene. The thus carbonized and activated vegetable fibers may be washed and dried by conventional methods, if necessary. According to the method of the present invention, the yield of activated carbon fibers is dramatically improved, so activated carbon fibers can be supplied at a much lower cost than conventional methods, and the resulting product has excellent adsorption performance. This is an extremely useful method industrially. EXAMPLES The present invention will be specifically explained below with reference to Examples and Comparative Examples. Comparative Example 1 Commercially available cotton cloth (bleached) was mixed with 20% by weight of zinc chloride 0.2
After being immersed in an aqueous solution containing % by weight of hydrogen chloride for about 5 minutes, a rubber roller was used to uniformly support the squeeze chemical solution. The amount of zinc chloride supported was 0.35 g/g of the raw cloth. The raw material cloth carrying the chemical solution was wound around a 16-mesh stainless steel wire mesh roll and fired at a temperature of 600°C in a nitrogen stream for about 1/2 hour. In this way, activated carbon fiber A was obtained. The yield and adsorption power of the activated carbon fiber A were as shown in Table-1. Example 1 Activated carbon fiber B was prepared in the same manner as in Comparative Example 1 except that an aqueous solution containing 20% by weight of zinc chloride, 15.5% by weight of ammonium chloride, and 1% by weight of hydrogen chloride was supported.
was manufactured. The yield and adsorption power of the activated carbon fiber B were as shown in Table 1. The amount of chemicals supported was 0.4 g/g of the raw material cloth. Example 2 Commercial linen cloth was treated with 25% by weight zinc chloride and 2.5% by weight.
After being immersed in an aqueous solution containing 2% by weight of boric acid and 2% by weight of hydrogen chloride, the sample was dehydrated using a centrifuge to uniformly support the chemical solution. The amount of drug supported is 0.43
g/g - raw material cloth. The raw material cloth carrying the chemical solution was wound around a 16-mesh stainless steel wire mesh and fired at a temperature of 550° C. for 3/4 hours in a nitrogen stream to produce activated carbon fiber C. The yield and adsorption power of the activated carbon fiber C were as shown in Table-1. Example 3 Activated carbon fiber D was prepared in the same manner as in Example 2 except that an aqueous solution containing 25% by weight of zinc leadide, 12.5% by weight of ammonium chloride, 5% by weight of boric acid, and 1% by weight of hydrogen chloride was supported. was manufactured. The yield and adsorption power of the activated carbon fiber D were as shown in Table 1. The amount of chemicals supported was 0.47 g/g of the raw material cloth. Example 4 Activated carbon fiber E was produced in the same manner as in Comparative Example 1, except that an aqueous solution containing 15% by weight of zinc chloride, 2% by weight of nitric acid, and 1% by weight of hydrogen chloride was supported. The yield and adsorption power of the activated carbon fiber E were as shown in Table 1. The amount of chemicals supported was 0.25 g/g of the raw material cloth. 〓〓〓〓

【表】 量増加から求めた。
〓〓〓〓
[Table] Calculated from increase in amount.
〓〓〓〓

Claims (1)

【特許請求の範囲】[Claims] 1 (1)塩化亜鉛と(2)塩化アンモニウム、ホウ酸お
よび硝酸からなる群から選ばれた少なくとも一種
を含有する溶液を植物性繊維に含浸させた後、炭
化、賦活化することを特徴とする活性炭素繊維の
製造方法。
1. It is characterized by impregnating vegetable fiber with a solution containing at least one selected from the group consisting of (1) zinc chloride and (2) ammonium chloride, boric acid, and nitric acid, and then carbonizing and activating it. Method for producing activated carbon fiber.
JP7603978A 1978-06-22 1978-06-22 Production of activated carbon fiber Granted JPS553354A (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
JP7603978A JPS553354A (en) 1978-06-22 1978-06-22 Production of activated carbon fiber
US06/266,012 US4409125A (en) 1978-06-22 1979-06-22 Process for producing activated fibrous carbon
PCT/JP1979/000160 WO1984001566A1 (en) 1978-06-22 1979-06-22 Process for producing fibrous active carbon

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP7603978A JPS553354A (en) 1978-06-22 1978-06-22 Production of activated carbon fiber

Publications (2)

Publication Number Publication Date
JPS553354A JPS553354A (en) 1980-01-11
JPS6135286B2 true JPS6135286B2 (en) 1986-08-12

Family

ID=13593656

Family Applications (1)

Application Number Title Priority Date Filing Date
JP7603978A Granted JPS553354A (en) 1978-06-22 1978-06-22 Production of activated carbon fiber

Country Status (1)

Country Link
JP (1) JPS553354A (en)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS57191328A (en) * 1981-05-13 1982-11-25 Toho Rayon Co Ltd Preparation of fibrous active carbon
CN102381703B (en) * 2011-07-27 2012-12-05 福建农林大学 Method for preparing activated carbon by using flax straws
CN107385559A (en) * 2017-08-11 2017-11-24 南通金康弘纺织品有限公司 A kind of preparation method of NACF
CN107827107B (en) * 2017-12-18 2020-05-22 中国科学院山西煤炭化学研究所 Preparation method of kapok-based hollow porous carbon micro-tube or porous carbon micro-strip
CN109796013A (en) * 2018-12-25 2019-05-24 南京工程学院 A kind of multistage mesoporous activated carbon and preparation method thereof of the compound bombax cotton preparation of paper mill sludge
CN110203929A (en) * 2019-05-13 2019-09-06 中国地质大学(武汉) A kind of Chinese hemp stalk pilum shaped activated carbon with wide spectrum characterization of adsorption

Also Published As

Publication number Publication date
JPS553354A (en) 1980-01-11

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