JPS6131051B2 - - Google Patents
Info
- Publication number
- JPS6131051B2 JPS6131051B2 JP52093791A JP9379177A JPS6131051B2 JP S6131051 B2 JPS6131051 B2 JP S6131051B2 JP 52093791 A JP52093791 A JP 52093791A JP 9379177 A JP9379177 A JP 9379177A JP S6131051 B2 JPS6131051 B2 JP S6131051B2
- Authority
- JP
- Japan
- Prior art keywords
- pulp
- fibers
- activated carbon
- paper
- bulk density
- 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 30
- 230000004913 activation Effects 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 28
- 229920001131 Pulp (paper) Polymers 0.000 description 16
- 239000007789 gas Substances 0.000 description 8
- 238000001179 sorption measurement Methods 0.000 description 8
- 239000004698 Polyethylene Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- -1 polyethylene Polymers 0.000 description 5
- 229920000573 polyethylene Polymers 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 229910052740 iodine Inorganic materials 0.000 description 4
- 239000011630 iodine Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- KEQGZUUPPQEDPF-UHFFFAOYSA-N 1,3-dichloro-5,5-dimethylimidazolidine-2,4-dione Chemical compound CC1(C)N(Cl)C(=O)N(Cl)C1=O KEQGZUUPPQEDPF-UHFFFAOYSA-N 0.000 description 1
- 239000004254 Ammonium phosphate Substances 0.000 description 1
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 1
- 235000019289 ammonium phosphates Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- XTHPWXDJESJLNJ-UHFFFAOYSA-N chlorosulfonic acid Substances OS(Cl)(=O)=O XTHPWXDJESJLNJ-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- LBDROUOCQSGOFI-UHFFFAOYSA-N methanol;phosphoric acid Chemical compound OC.OP(O)(O)=O LBDROUOCQSGOFI-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 235000011007 phosphoric acid Nutrition 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- HIFJUMGIHIZEPX-UHFFFAOYSA-N sulfuric acid;sulfur trioxide Chemical compound O=S(=O)=O.OS(O)(=O)=O HIFJUMGIHIZEPX-UHFFFAOYSA-N 0.000 description 1
- 229920001059 synthetic polymer Polymers 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Landscapes
- Carbon And Carbon Compounds (AREA)
- Inorganic Fibers (AREA)
Description
【発明の詳細な説明】
本発明は高度の吸着性を有する繊維状活性炭の
製造法に関するものであり、紙状に成形可能な短
繊維状の活性炭を提供するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing fibrous activated carbon having high adsorption properties, and provides short fibrous activated carbon that can be formed into paper.
本発明は平均繊維長が0.1〜10m／ｍの範囲
に、あり、かつ嵩密度が0.6ｇ／cm2以下となるよ
うに開繊されたパルプを不融化処理の後350〜900
℃に加熱して炭化し引きつづいて活性化ガス雰囲
気中で700〜1200℃に加熱賦活化することを特徴
とする繊維状活性炭素繊維の製造法である。 The present invention uses pulp that has been opened so that the average fiber length is in the range of 0.1 to 10 m/m and the bulk density is 0.6 g/cm 2 or less.
This is a method for producing fibrous activated carbon fibers, which is characterized by heating to a temperature of 0.degree. C. to carbonize, followed by activation by heating to 700 to 1200.degree. C. in an activated gas atmosphere.
本発明によつて得られる短繊維状活性炭はガス
吸着に適した細孔分布を有し、しかも単独或は他
のパルプ材料と共に抄紙して紙に抄くことが可能
であり、紙状の吸着材料を提供出来るものであ
る。 The short fibrous activated carbon obtained by the present invention has a pore distribution suitable for gas adsorption, and can be made into paper alone or together with other pulp materials, and can be used for paper-like adsorption. Materials can be provided.
本発明に用いることのできるパルプは木材パル
プのほかポリエチレン等の合成パルプである。 Pulps that can be used in the present invention include wood pulp and synthetic pulps such as polyethylene.
木材パルプは、木材からリグニン等の非繊維素
物質を除去されたセルロース系繊維の集団であ
り、リグニン等を化学的手段によつて溶出して繊
維を分離した化学パルプ、機械的に繊維を解舒し
た機械パルプのいずれでも用いることが出来る。 Wood pulp is a group of cellulosic fibers obtained by removing non-cellulose substances such as lignin from wood. Any seeded mechanical pulp can be used.
本発明には以上の木材パルプの他、ポリエチレ
ン、ポリアクリロニトリル等の合成重合体を剪断
力でパルプ化した合成パルプも使用出来る。 In addition to the above-mentioned wood pulps, synthetic pulps obtained by pulping synthetic polymers such as polyethylene and polyacrylonitrile using shearing force can also be used in the present invention.
かかるパルプを熱処理して炭化する前に開繊し
て平均繊維長を0.1〜10m／ｍ、嵩密度を0.6ｇ／
cm2以下となるように開繊処理することが本発明に
おいて重要である。 Before heat-treating and carbonizing the pulp, it is opened to give an average fiber length of 0.1 to 10 m/m and a bulk density of 0.6 g/m.
In the present invention, it is important to perform the opening treatment so that the fiber size becomes less than cm 2 .
パルプの開繊は、湿式ミキサーで開繊後水溶性
の有機溶剤に浸漬し、開繊する方法やハンマー・
ミル等の粉砕機により開繊する方法等により行う
ことが出来るが、嵩密度0.6ｇ／c.c.以下になるよ
うに開繊する必要がある。 Pulp can be opened using a wet mixer, then immersed in a water-soluble organic solvent, and then opened using a hammer.
This can be done by opening the fibers using a pulverizer such as a mill, but it is necessary to open the fibers so that the bulk density is 0.6 g/cc or less.
嵩密度が0.6ｇ／c.c.以上の場合はパルプを不融
化、炭化する際に発生するガス、タールが、繊維
表面に付着したまま炭化し、粉状の炭化物を与え
やすくなり、又、賦活の均一な反応の進行が妨げ
られ、繊維状の形態が失われやすくなる。またパ
ルプの繊維長が10m／ｍ以上の場合は、得られる
活性炭素せんいの性能が不均一となり、またこれ
を抄紙して紙状物とする時に嵩密度の大きいもの
を得ることが出来ない。 If the bulk density is 0.6 g/cc or more, the gas and tar generated during infusibility and carbonization of the pulp will carbonize while adhering to the fiber surface, making it easier to form powdery carbide, and the activation will be more uniform. The progress of the reaction is hindered, and the fibrous morphology is easily lost. If the fiber length of the pulp is 10 m/m or more, the performance of the obtained activated carbon fiber will be uneven, and it will not be possible to obtain a paper with a high bulk density when it is made into paper.
不融化処理は、木材パルプ、リンター・パルプ
等のセルロース系繊維の場合は、燐酸、燐酸アン
モン、塩化アンモニウム等の化合物を含浸後、
150℃〜300℃で加熱することにより行われる。又
ポリエチレン系合成パルプの場合は、濃硫酸、発
煙硫酸、クロルスルフオン酸中、50℃〜300℃で
加熱することにより実施される。 In the case of cellulose fibers such as wood pulp and linter pulp, infusibility treatment is performed by impregnating them with compounds such as phosphoric acid, ammonium phosphate, and ammonium chloride.
This is done by heating at 150°C to 300°C. In the case of polyethylene synthetic pulp, it is carried out by heating at 50°C to 300°C in concentrated sulfuric acid, fuming sulfuric acid, or chlorosulfonic acid.
上記不融化された黒色パルプ繊維を350℃〜900
℃に加熱し、炭化せしめる。加熱は、通常のロー
タリー・キルンスクリユー炉、静置炉、流動炉等
を使用して行うことが出来る。 The above infusible black pulp fiber is heated to 350℃~900℃.
Heat to ℃ and carbonize. Heating can be performed using a conventional rotary kiln screw furnace, static furnace, fluidized furnace, etc.
炭化処理を施された繊維は、水蒸気、炭酸ガ
ス、空気、アンモニア等の活性化ガスにより、
700〜1200℃で賦活処理される。 Carbonized fibers are treated with activated gases such as water vapor, carbon dioxide, air, and ammonia.
Activation treatment is performed at 700-1200℃.
賦活処理は、ロータリー・キルン、流動層炉、
浮遊流動炉、多段床炉等を用いて行うことが出来
る本発明の方法によれば、繊維の形態を保持した
活性炭を、安価に製造することが可能となり、本
発明によつて得られる繊維状活性炭は、ガス吸着
に適した細孔構造を有し、前述のように紙状に成
形出来る他、シート状物にプリント出来、紙状な
いしはシート状の吸着材を得ることが出来る。こ
のようなシート状吸着材は種々の形状に賦形して
処理流体をハニカムのセルに平行に導き吸着せし
める吸着装置とすることが出来る。 Activation treatment is performed using rotary kiln, fluidized bed furnace,
According to the method of the present invention, which can be carried out using a floating fluidized furnace, a multi-stage bed furnace, etc., activated carbon that retains the fibrous form can be produced at low cost, and the fibrous Activated carbon has a pore structure suitable for gas adsorption, and in addition to being moldable into paper as described above, it can also be printed into a sheet-like material to obtain a paper-like or sheet-like adsorbent. Such a sheet-like adsorbent can be formed into various shapes to form an adsorption device that guides and adsorbs the processing fluid in parallel to the cells of the honeycomb.
実施例 １
化学パルプ（木材パルプ）200ｇを水溶液中、
家庭用ミキサーにより分散後、ガラスフイルター
上で、水を流出させた。Example 1 200g of chemical pulp (wood pulp) in an aqueous solution,
After dispersion using a household mixer, the water was drained off on a glass filter.
上記木材パルプに、アセトン500mlを滴下さ
せ、木材パルプに含まれている水分を除去した。
平均繊維長は2m／ｍ、嵩密度は0.1ｇ／c.c.であつ
た。該分散木材パルプ繊維に燐酸を含浸後風乾
し、窒素ガス気流中、700℃で不融化、炭化処理
を施した。収率は30％であつた。該炭化繊維を、
石英管状炉で900℃で、水蒸気を導入することに
より、活性化処理を施した。賦活収率40％で、沃
素吸着量1000mg／ｇの繊維状活性炭が得られた。 500 ml of acetone was dropped onto the wood pulp to remove water contained in the wood pulp.
The average fiber length was 2 m/m, and the bulk density was 0.1 g/cc. The dispersed wood pulp fibers were impregnated with phosphoric acid, air-dried, and infusible and carbonized at 700° C. in a nitrogen gas stream. The yield was 30%. The carbonized fiber,
Activation treatment was carried out in a quartz tube furnace at 900°C by introducing steam. Fibrous activated carbon with an activation yield of 40% and an iodine adsorption amount of 1000 mg/g was obtained.
該繊維と、木材パルプから、湿式抄紙法によ
り、50ｇ／m2のペーパーをつくり、ハニカム状に
成型した後、有機溶剤含有ガスをハニカムに通し
たところ、従来の活性炭法より低圧損で溶剤を吸
着する。ガス濃縮器が得られた。 A paper weighing 50 g/m 2 was made from the fibers and wood pulp using a wet paper-making method, formed into a honeycomb shape, and then an organic solvent-containing gas was passed through the honeycomb. Adsorb. A gas concentrator was obtained.
実施例 ２
機械パルプをハンマー・ミルにより開繊し、嵩
密度が0.05ｇ／c.c.平均繊維長1.5m／ｍの木材パル
プ繊維を得た。該繊維に燐酸−メタノール溶液を
噴霧した後、乾燥した。Example 2 Mechanical pulp was opened using a hammer mill to obtain wood pulp fibers having a bulk density of 0.05 g/cc and an average fiber length of 1.5 m/m. The fibers were sprayed with a phosphoric acid-methanol solution and then dried.
該繊維を、空気中、300℃に加熱して不融化処
理を施した。収率は50％であつた。 The fibers were heated to 300° C. in air to make them infusible. The yield was 50%.
該繊維を850℃の温度、炭酸ガス気流中で、活
性化処理を施したところ沃素吸着量900mg／ｇの
繊維状活性炭が得られた。 When the fibers were activated at a temperature of 850° C. in a carbon dioxide gas stream, fibrous activated carbon with an iodine adsorption amount of 900 mg/g was obtained.
上記繊維50部と、木材パルプ50部とから、湿式
抄紙法により容易に、繊維状活性炭含有ペーパー
が得られた。 Fibrous activated carbon-containing paper was easily obtained from 50 parts of the above fibers and 50 parts of wood pulp by a wet papermaking method.
比較例 １
NBKPパルプ・ミートを家庭用ミキサーで、ス
ラリー化後、濾過、乾燥し、嵩密度が0.8ｇ／c.c.
の木材パルプ繊維集合体を得た。このパルプを実
施例２と同様にして活性炭を製造したが、粉末状
の活性炭しか得られず、沃素吸着量も550゜mg／
ｇであつた。Comparative Example 1 NBKP pulp/meat was made into a slurry using a household mixer, filtered and dried, and the bulk density was 0.8 g/cc.
A wood pulp fiber aggregate was obtained. Activated carbon was produced from this pulp in the same manner as in Example 2, but only powdered activated carbon was obtained, and the amount of iodine adsorbed was 550゜mg/
It was hot at g.
この活性炭を実施例２と同様に木材パルプと混
合して抄紙を行なつたが、活性炭は有効にシート
状にならず、また抄紙後、紙から脱落しやすかつ
た。 This activated carbon was mixed with wood pulp and paper was made in the same manner as in Example 2, but the activated carbon did not form into a sheet effectively and was likely to fall off from the paper after paper making.
実施例 ３
ポリエチレン系合成パルプ（三井ガラバツク
KK商品名SWP）を水溶中、家庭用ミキサーで開
繊後、アセトン中に投入し、濾過し、嵩密度が
0.05ｇ／c.c.平均繊維長1m／ｍのポリエチレンパ
ルプ繊維を得た。Example 3 Polyethylene synthetic pulp (Mitsui Garabakku)
KK (trade name: SWP) is dissolved in water, opened with a household mixer, poured into acetone, filtered, and the bulk density is determined.
Polyethylene pulp fibers having an average fiber length of 1 m/m were obtained at 0.05 g/cc.
上記繊維を濃硫酸に投入し、200℃で１時間加
熱し、不融化された黒色繊維を得た。 The above fibers were put into concentrated sulfuric acid and heated at 200°C for 1 hour to obtain infusible black fibers.
上記黒色繊維を800℃まで窒素気流中加熱し、
炭化繊維を原繊維よりの収率50％で得た。 The above black fiber was heated to 800℃ in a nitrogen stream,
Carbonized fibers were obtained at a yield of 50% from the original fibers.
上記繊維を、900℃で水蒸気を50vol％を含んだ
窒素ガス気流中で、30分、活性化処理を施したと
ころ、沃素吸着量1000mg／ｇの活性炭繊維が得ら
れた。 When the above fibers were activated for 30 minutes at 900° C. in a nitrogen gas stream containing 50 vol % of water vapor, activated carbon fibers with an iodine adsorption amount of 1000 mg/g were obtained.
Claims (1)
かつ嵩密度が0.6ｇ／cm2以下となるように開繊さ
れたパルプを不融化処理の後350〜900℃に加熱し
て炭化し、引きつづいて活性化ガス雰囲気中で
700〜1200℃に加熱賦活化することを特徴とする
繊維状活性炭素繊維の製造法。1 The average fiber length is in the range of 0.1 to 10 m/m,
The pulp that has been opened so that the bulk density is 0.6 g/ cm2 or less is infusible, heated to 350 to 900°C to carbonize it, and then heated in an activated gas atmosphere.
A method for producing fibrous activated carbon fiber, which comprises heat activation at 700 to 1200°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9379177A JPS5428291A (en) | 1977-08-04 | 1977-08-04 | Production of fibrous activated carbon |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9379177A JPS5428291A (en) | 1977-08-04 | 1977-08-04 | Production of fibrous activated carbon |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5428291A JPS5428291A (en) | 1979-03-02 |
| JPS6131051B2 true JPS6131051B2 (en) | 1986-07-17 |
Family
ID=14092226
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9379177A Granted JPS5428291A (en) | 1977-08-04 | 1977-08-04 | Production of fibrous activated carbon |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5428291A (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62213015A (en) * | 1986-03-13 | 1987-09-18 | オリンパス光学工業株式会社 | Moisture-proof electric contact |
| US20110281063A1 (en) * | 2009-11-20 | 2011-11-17 | E. I. Du Pont De Nemours And Company | Honeycomb core based on carbon fiber paper and articles made from same |
| JP5985027B2 (en) * | 2010-10-12 | 2016-09-06 | フタムラ化学株式会社 | Method for producing pharmaceutical adsorbent for oral administration |
| JP5984352B2 (en) * | 2010-10-12 | 2016-09-06 | フタムラ化学株式会社 | Method for producing pharmaceutical adsorbent for oral administration |
| JP6637573B2 (en) * | 2017-12-18 | 2020-01-29 | フタムラ化学株式会社 | Adsorbent production method |
-
1977
- 1977-08-04 JP JP9379177A patent/JPS5428291A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5428291A (en) | 1979-03-02 |
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