JPS6338446B2 - - Google Patents
Info
- Publication number
- JPS6338446B2 JPS6338446B2 JP56093508A JP9350881A JPS6338446B2 JP S6338446 B2 JPS6338446 B2 JP S6338446B2 JP 56093508 A JP56093508 A JP 56093508A JP 9350881 A JP9350881 A JP 9350881A JP S6338446 B2 JPS6338446 B2 JP S6338446B2
- Authority
- JP
- Japan
- Prior art keywords
- fibers
- layer
- activated carbon
- fiber layer
- infusible
- 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
Links
- 239000000835 fiber Substances 0.000 claims description 60
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 36
- 230000004913 activation Effects 0.000 claims description 19
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 18
- 238000011282 treatment Methods 0.000 claims description 14
- 239000003779 heat-resistant material Substances 0.000 claims description 7
- 238000003763 carbonization Methods 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000010410 layer Substances 0.000 description 43
- 239000007789 gas Substances 0.000 description 20
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 18
- 239000002245 particle Substances 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000012298 atmosphere Substances 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 229920003043 Cellulose fiber Polymers 0.000 description 3
- 230000003213 activating effect Effects 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 229920002239 polyacrylonitrile Polymers 0.000 description 3
- 239000004627 regenerated cellulose Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000008602 contraction Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- -1 for example Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000006902 nitrogenation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
Landscapes
- Inorganic Fibers (AREA)
Description
【発明の詳細な説明】
本発明は空気清浄器等に使用される吸着性にす
ぐれた活性炭繊維を高収率で得る方法に関するも
のである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for obtaining activated carbon fibers with excellent adsorption properties for use in air purifiers and the like at a high yield.
従来、活性炭繊維を得るには、再生セルロース
繊維、ポリアクリロニトリル繊維、ピツチ繊維等
の有機繊維を不融化処理して不融化繊維となし、
これを炭化、賦活化していた。 Conventionally, in order to obtain activated carbon fibers, organic fibers such as regenerated cellulose fibers, polyacrylonitrile fibers, and pitch fibers are treated to be infusible to make them infusible fibers.
This was carbonized and activated.
不融化処理は、例えば再生セルロース繊維の場
合は酸素の少ない雰囲気において200〜400℃で
0.5〜３時間程度の加熱処理をする。ポリアクリ
ロニトリル繊維の場合は空気中において200〜300
℃で0.5〜２時間程度の加熱処理をする。またピ
ツチ繊維の場合は空気中において100〜300℃で１
〜10時間程度の加熱処理をする。 For example, in the case of regenerated cellulose fibers, infusibility treatment is performed at 200 to 400°C in an oxygen-poor atmosphere.
Heat treatment for about 0.5 to 3 hours. In the case of polyacrylonitrile fibers, it is 200 to 300 in air.
Heat treatment at ℃ for about 0.5 to 2 hours. In addition, in the case of Pituchi fiber, 1
Heat treatment for ~10 hours.
炭化、賦活化処理は一般に、ガスが自由に通過
できる容器に不融化された繊維を充填し、これを
窒素等の不活性ガスの700〜1100℃程度の雰囲気
中で炭化処理し、更に水蒸気、炭酸ガス、酸素等
の活性ガスの単独またはこれ等を含む活性ガスの
上記と同程度の雰囲気中で賦活化処理を行なつて
いる。 Carbonization and activation treatments are generally performed by filling a container through which gas can freely pass through with infusible fibers, carbonizing the fibers in an atmosphere of an inert gas such as nitrogen at a temperature of about 700 to 1100°C, and then adding water vapor, Activation treatment is performed in an atmosphere similar to that described above using an active gas such as carbon dioxide or oxygen alone or containing an active gas such as these.
炭化、賦活化の温度、時間は不融化繊維の種
類、形状、所望する比表面積、ガスの種類、量な
どにより適宜決定される。 The temperature and time of carbonization and activation are appropriately determined depending on the type and shape of the infusible fiber, the desired specific surface area, the type and amount of gas, and the like.
ガスが自由に通過できる容器としては、金属、
セラミツクなどの耐熱性材料を用い、一般にはパ
ンチングメタルや、多孔質セラミツク等が用いら
れる。また、不融化、炭化、賦括化は別工程で行
なつてもよいし、連続的に実施してもよい。 Containers that allow gas to pass freely include metal,
A heat-resistant material such as ceramic is used, and punching metal, porous ceramic, etc. are generally used. Furthermore, infusibility, carbonization, and embedding may be performed in separate steps or may be performed continuously.
ところで、従来は、不融化繊維を容器に充填す
る場合、不融化繊維の集合体をそのままの状態で
容器に収納していた。従つて、これを賦活すると
繊維層の最外部で先ず反応が起り、次第に活性ガ
スが繊維層内部へ進行して反応が進んでゆくが、
繊維層内部と最外部では反応により発生したガス
の移動状態が異る。即ち、繊維層最外部では発生
ガスの滞溜がなく賦活反応は速かに進行する。そ
れに対して繊維層内部では発生したガスは外部に
移動しにくいために滞溜し、賦活反応はこの滞溜
ガスに抑制されて進行が遅い。従つて繊維層全体
として賦活が均一になされない。また、層内部を
充分に賦活化すると最外部の賦活化が進みすぎ
る。このため活性炭繊維の収率は低かつた。 By the way, conventionally, when filling a container with infusible fibers, an aggregate of infusible fibers was stored in the container as is. Therefore, when activated, the reaction first occurs at the outermost part of the fiber layer, and the activated gas gradually advances inside the fiber layer and the reaction progresses.
The state of movement of the gas generated by the reaction is different between the inside of the fiber layer and the outermost layer. That is, at the outermost part of the fiber layer, the generated gas does not accumulate and the activation reaction proceeds quickly. On the other hand, the gas generated inside the fiber layer is difficult to move to the outside and therefore stagnates, and the activation reaction is suppressed by this stagnation gas and progresses slowly. Therefore, the entire fiber layer is not activated uniformly. Furthermore, if the inside of the layer is sufficiently activated, the outermost layer is activated too much. Therefore, the yield of activated carbon fibers was low.
そこで本発明は繊維層の内層部および最外層部
を均一な条件で賦活化処理することにより活性炭
繊維の収率の向上をはかつたものである。 Therefore, the present invention aims to improve the yield of activated carbon fibers by activating the inner layer and the outermost layer of the fiber layer under uniform conditions.
即ち、有機繊維を賦活用活性ガスが通過し得る
耐熱性容器に収納し、有機繊維層の少くとも上面
を、耐熱性容器とは別体の賦活用活性ガスが通過
し得る耐熱性材料よりなり、有機繊維層の変形に
追従して変位し有機繊維層に常時密着した状態を
維持する被覆材層で被覆して賦活化処理を行な
う。この場合、被覆の具体的手段としては、例え
ば耐熱性材料の粒子を用い、各粒子が流動し得る
状態の粒子層で繊維層のまわりを包んで賦活化処
理を行なう。繊維層は賦活反応の進行に伴なつて
体積が収縮するが、上記のように繊維層の変形に
追従して変位する流動性の流動性の粒子層で被覆
することにより処理中において被覆層とその中の
繊維層との密着は維持される。従つて最外部で発
生したガスが直ちに逸散することなく、また内層
部でも発生ガスの移動が抑制されるので、繊維層
は全体が均一に賦活される。従つて、従来方法に
比して所定の吸着率の活性炭繊維を高い収率で得
ることができる。 That is, the organic fibers are stored in a heat-resistant container through which the activated gas can pass, and at least the upper surface of the organic fiber layer is made of a heat-resistant material that is separate from the heat-resistant container and through which the activated gas can pass. , the activation treatment is performed by covering the organic fiber layer with a coating material layer that displaces following the deformation of the organic fiber layer and always maintains a state in close contact with the organic fiber layer. In this case, as a specific means for coating, for example, particles of a heat-resistant material are used, and the fiber layer is wrapped around the fiber layer with a particle layer in which each particle can flow, and the activation treatment is performed. The fiber layer shrinks in volume as the activation reaction progresses, but by covering it with a fluid particle layer that displaces following the deformation of the fiber layer as described above, it can be used as a coating layer during processing. Close contact with the fiber layer therein is maintained. Therefore, the gas generated at the outermost layer does not immediately dissipate, and the movement of the gas generated at the inner layer is also suppressed, so that the entire fiber layer is activated uniformly. Therefore, activated carbon fibers having a predetermined adsorption rate can be obtained at a higher yield than in conventional methods.
以下、本発明の実施例を示す。 Examples of the present invention will be shown below.
実施例 １
第１図に示すように、グラフアイトのフエルト
よりなる直径100mmの筒状容器１に、粒径２〜３
mmのアルミナ粒子よりなる流動変形可能な厚さ10
mmの層３に包んだ状態で、ピツチ繊維を不融化し
た不融化繊維２を収納した。不融化繊維２の層厚
さは30mmで充填密度は0.025ｇ／cm3とした。Example 1 As shown in Fig. 1, particles with a diameter of 2 to 3
Flow deformable thickness 10 mm made of alumina particles
Infusible fibers 2 made of infusible pitch fibers were housed in a state of being wrapped in a layer 3 of mm. The layer thickness of the infusible fiber 2 was 30 mm, and the packing density was 0.025 g/cm 3 .
そして、容器全体を平炉内に入れ、900℃の窒
素雰囲気中に３時間保持し、不融化繊維３を炭化
した。 Then, the entire container was placed in an open hearth and kept in a nitrogen atmosphere at 900° C. for 3 hours to carbonize the infusible fibers 3.
次に炉内を水蒸気68容量％、窒素32容量％の雰
囲気とし、上記と同温度で賦活化処理を行なつ
た。そして容器１を炉から取出すことにより活性
炭繊維を得た。 Next, the inside of the furnace was made into an atmosphere of 68% by volume of steam and 32% by volume of nitrogen, and activation treatment was performed at the same temperature as above. Activated carbon fibers were obtained by taking out the container 1 from the furnace.
活性炭繊維の収率（不融化繊維に対する活性炭
繊維の重量比）は15.1％であり、活性炭繊維のベ
ンゼン吸着量（JIS−Ｋ−1474の方法により求め
た値）は48重量％であつた。 The yield of activated carbon fibers (weight ratio of activated carbon fibers to infusible fibers) was 15.1%, and the amount of benzene adsorbed by the activated carbon fibers (value determined by the method of JIS-K-1474) was 48% by weight.
ちなみに、不融化ピツチ繊維をそのままの状態
で容器内に収納し、他は上記実施例と同一の方法
で処理してた場合の活性炭繊維の収率は4.8％で、
ベンゼン吸着量は47重量％であつた。 By the way, when the infusible pitch fibers were stored in a container as they were, and other things were treated in the same manner as in the above example, the yield of activated carbon fibers was 4.8%.
The amount of benzene adsorbed was 47% by weight.
実施例 ２
実施例１と同一の容器に不融化ピツチ繊維を充
填密度0.030ｇ／cm3で収納し、この場合、実施例
１と同様のアルミナ粒子層で包んだ状態とし、炉
内で900℃の窒素雰囲気で３時間炭化処理し、次
に同温度で水蒸気64容量％、窒素36容量％からな
る活性ガスで30分間賦活化処理を行なつて後炉外
へ取出し、活性炭繊維を得た。Example 2 Infusible pitch fibers were stored in the same container as in Example 1 at a packing density of 0.030 g/cm 3 , in this case wrapped in the same alumina particle layer as in Example 1, and heated at 900°C in a furnace. The fibers were carbonized for 3 hours in a nitrogen atmosphere, and then activated at the same temperature for 30 minutes with an active gas containing 64% by volume of steam and 36% by volume of nitrogen, and then taken out of the furnace to obtain activated carbon fibers.
活性炭繊維の収率は40.3％でベンゼン吸着量は
30重量％であつた。 The yield of activated carbon fiber is 40.3% and the amount of benzene adsorbed is
It was 30% by weight.
比較例として、不融化繊維をそのままの状態で
容器内に収納し、他は上記実施例２と同一方法で
処理した場合の活性炭繊維の収率は32.0％で、ベ
ンゼン吸着量は28重量％であつた。 As a comparative example, the yield of activated carbon fiber was 32.0%, and the amount of benzene adsorbed was 28% by weight, when the infusible fibers were stored in a container as they were and otherwise treated in the same manner as in Example 2 above. It was hot.
実施例 ３
パンチングメタル製の一辺100mmの箱状容器に
不融化ピツチ繊維を充填密度0.050ｇ／cm3で収納
し、その囲りを上記各実施例と同様にアルミナ粒
子層で包んだ状態とし、炉内で900℃の窒素雰囲
気で１時間炭化し、続いて同温度の水蒸気67容量
％、窒素33容量％の活性ガス雰囲気で賦活化処理
をした後、炉外へ取出し活性炭繊維を得た。Example 3 Infusible pitch fibers were stored in a box-shaped container made of punched metal with a side of 100 mm at a packing density of 0.050 g/cm 3 , and the surroundings were wrapped with an alumina particle layer in the same manner as in each of the above examples. Carbonization was carried out in a nitrogen atmosphere at 900°C for 1 hour in a furnace, followed by activation treatment in an active gas atmosphere containing 67% by volume of steam and 33% by volume of nitrogen at the same temperature, and then taken out of the furnace to obtain activated carbon fibers.
活性炭繊維の収率は32.8％で、ベンゼン吸着量
は32重量％であつた。 The yield of activated carbon fibers was 32.8%, and the amount of benzene adsorbed was 32% by weight.
比較例として不融化繊維をそのままの状態で上
記のパンチングメタルの容器に収納し、他は実施
例３と同一の方法で処理した場合の活性炭繊維の
収率は21.5％でベンゼン吸着量は30重量％であつ
た。 As a comparative example, when the infusible fibers were stored as they were in the above punched metal container and otherwise treated in the same manner as in Example 3, the yield of activated carbon fibers was 21.5% and the amount of benzene adsorbed was 30% by weight. It was %.
上記実施例ではいずれも被覆材としてアルミナ
の粒子を用いたが、その他にセラミツク等の耐熱
性材料の粒子を用いてもよい。粒子の大きさは特
に限定はなく、要は層を形成したときに通気性を
有し、かつ各粒子が互に流動して層の形が自由に
変形できればよい。 In all of the above embodiments, alumina particles were used as the coating material, but particles of a heat-resistant material such as ceramic may also be used. There is no particular limitation on the size of the particles, as long as they have air permeability when the layer is formed, and the particles can mutually flow and freely deform the shape of the layer.
また第２図に示すように容器１内の不融化繊維
層２の側面および上面を粒子層３ａで覆つて賦活
化処理をした場合でも、従来法に比して賦活均一
化ならびに収率向上に効果がある。更に第３図に
示すように容器１内の不融化繊維層２の上面にの
み通気性の耐熱材プレート３ｂ、例えば多孔質セ
ラミツク等を繊維の収縮による上面の変位に追従
し得るように載置する場合にも従来法に比べて賦
活の均一化、収率向上の効果がある。 Furthermore, even when the side and top surfaces of the infusible fiber layer 2 in the container 1 are covered with the particle layer 3a as shown in FIG. effective. Furthermore, as shown in FIG. 3, a breathable heat-resistant material plate 3b, such as porous ceramic, is placed only on the upper surface of the infusible fiber layer 2 in the container 1 so that it can follow the displacement of the upper surface due to contraction of the fibers. In this case, the activation is more uniform and the yield is improved compared to the conventional method.
また本発明は上記実施例の如きバツチ式の賦活
に限らず、ベルト炉やトンネル炉内で行なう連続
的賦活化処理にも適用できる。 Further, the present invention is not limited to batch-type activation as in the above embodiments, but can also be applied to continuous activation treatment carried out in a belt furnace or tunnel furnace.
また、有機繊維としてはピツチ繊維に限らず再
生セルロース繊維、ポリアクリロニトリル繊維等
を用いても、いずれも同様の効果が得られ、賦活
用活性ガスとしては水蒸気以外の賦活用活性ガス
を用いたときも同様の効果が得られる。 In addition, the same effect can be obtained by using not only pitch fiber but also regenerated cellulose fiber, polyacrylonitrile fiber, etc. as the organic fiber, and when using a reactivating active gas other than water vapor as the reactivating active gas. A similar effect can be obtained.
以上説明したように、本発明は不融化繊維を活
性ガス中で賦活化処理して活性炭繊維を得るに際
し、有機繊維を賦活用活性ガスが通過し得る耐熱
性容器に収納し、有機繊維層の少なくとも上面を
容器とは別体の通気性耐熱材料にて有機繊維層の
収縮による変形に追従して変位する有機繊維層に
常時密着した状態を保持し得るように覆つて賦活
化処理を行なうことを特徴とするもので、これに
より繊維層の外表面および内層部の賦活化条件を
均一にすることができる。従つて、所定の吸着率
の活性炭繊維を得ようとする場合、本発明によれ
ば従来法に比して高い収率で活性炭繊維を得るこ
とが可能である。 As explained above, in the present invention, when obtaining activated carbon fibers by activating infusible fibers in an active gas, the organic fibers are stored in a heat-resistant container through which the activating active gas can pass, and the organic fiber layer is Activation treatment is performed by covering at least the upper surface of the container with a breathable heat-resistant material separate from the container so as to maintain a state in close contact with the organic fiber layer that is displaced following the deformation due to contraction of the organic fiber layer. This makes it possible to make the activation conditions of the outer surface and inner layer of the fiber layer uniform. Therefore, when it is desired to obtain activated carbon fibers with a predetermined adsorption rate, according to the present invention, it is possible to obtain activated carbon fibers with a higher yield than in the conventional method.
第１図、第２図、第３図はそれぞれ本発明にお
ける賦活化処理時の繊維の収納状態を示す図であ
る。
１……容器、２……繊維層、３，３ａ，３ｂ…
…被覆材層。
FIG. 1, FIG. 2, and FIG. 3 are views showing the storage state of fibers during the activation treatment in the present invention, respectively. 1... Container, 2... Fiber layer, 3, 3a, 3b...
...covering material layer.
Claims (1)
化処理を順次施して活性炭繊維を製造する方法に
おいて、有機繊維を賦活用活性ガスが通過し得る
耐熱性容器に収納し、有機繊維層の少くとも上面
を、耐熱性容器とは別体の賦活用活性ガスが通過
し得る耐熱性材料よりなり、有機繊維層の変形に
追従して変位し有機繊維層に常時密着した状態を
維持する被覆材層で被覆して賦活化処理を行なう
ことを特徴とする活性炭繊維の製造方法。1. In a method for producing activated carbon fibers by sequentially subjecting organic fibers to infusible treatment, carbonization treatment, and activation treatment, the organic fibers are stored in a heat-resistant container through which the activation gas can pass, and at least the organic fiber layer is A covering material layer whose upper surface is made of a heat-resistant material through which the activated gas separate from the heat-resistant container can pass, and which displaces following the deformation of the organic fiber layer and maintains a state in close contact with the organic fiber layer at all times. 1. A method for producing activated carbon fiber, which comprises coating the fiber with activated carbon fiber and subjecting it to activation treatment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9350881A JPS57210017A (en) | 1981-06-17 | 1981-06-17 | Preparation of active carbon fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9350881A JPS57210017A (en) | 1981-06-17 | 1981-06-17 | Preparation of active carbon fiber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS57210017A JPS57210017A (en) | 1982-12-23 |
| JPS6338446B2 true JPS6338446B2 (en) | 1988-07-29 |
Family
ID=14084283
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9350881A Granted JPS57210017A (en) | 1981-06-17 | 1981-06-17 | Preparation of active carbon fiber |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS57210017A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60173118A (en) * | 1984-02-17 | 1985-09-06 | Nippon Soken Inc | Activation treatment and device of carbon yarn therefor |
| CN106829915B (en) * | 2017-03-03 | 2018-10-30 | 中国科学院合肥物质科学研究院 | A kind of method of growth in situ carbon fiber in graphite felt |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS54160588A (en) * | 1978-06-08 | 1979-12-19 | Toyobo Co Ltd | Production of short fibrous active carbon |
-
1981
- 1981-06-17 JP JP9350881A patent/JPS57210017A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS54160588A (en) * | 1978-06-08 | 1979-12-19 | Toyobo Co Ltd | Production of short fibrous active carbon |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS57210017A (en) | 1982-12-23 |
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