JP6042560B2 - 炭素体及び強磁性炭素体 - Google Patents
炭素体及び強磁性炭素体 Download PDFInfo
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- JP6042560B2 JP6042560B2 JP2015547247A JP2015547247A JP6042560B2 JP 6042560 B2 JP6042560 B2 JP 6042560B2 JP 2015547247 A JP2015547247 A JP 2015547247A JP 2015547247 A JP2015547247 A JP 2015547247A JP 6042560 B2 JP6042560 B2 JP 6042560B2
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Description
実施例1(比較):未処理の活性炭押出成形物
未処理の活性炭押出成形物(JECカーボン 1.8mm SHIRASAGI C2x8/12 ヤシ殻系ペレット活性炭)の微小孔構造、及び黒鉛の存在が、N2吸着測定及びXRDでそれぞれ測定された。
活性炭押出成形物(JECカーボン 1.8mm SHIRASAGI C2x8/12 ヤシ殻系ペレット活性炭)が窒素雰囲気下で、1時間800℃で加熱処理された。分析内容は、実施例1と同じものであり、下記表1で見ることができる
本発明による強磁性炭素体は、250mLのフラスコに40gの活性炭押出成形物(JECカーボン 1.8mm SHIRASAGI C2x8/12 ヤシ殻系ペレット活性炭)を置くこと、及び真空下(40 mbar)で少なくとも30分回転させることにより調製された。58重量%の硝酸鉄(III)九水和物の水溶液37mLが、真空下で炭素押出成形物上にスプレーされた。押出成形物は真空下40℃で一晩乾燥された。真空を解放して、35gの鉄が含浸された炭素押出成形物が固定床上に置かれ、400ml/分の窒素流の下、5℃/分の速度で800℃まで加熱される。3時間の等温処理の後、材料は室温まで冷やされ、調製された試料を安定化するために空気がゆっくりと加えられた。収量は、22gの黒い炭素押出成形物であった。微小孔構造及び黒鉛の存在はそれぞれ、N2吸着測定及びXRDで測定された。
実施例2の5.0gの試料が、4MのHCl 15mLで処理され、2時間撹拌され、濾過され、再び4MのHCl 10mLで処理された。それから、濾過され、水で洗浄され、110℃で一晩乾燥された。収量は、4.2gの黒い押出成形物であった。分析内容は、実施例1のものと同じであり、下記の表2aで見ることができる。
実施例2で述べたものと類似の工程が実施例3に対して実施されたが、実施例3は、150gの活性炭押出成形物及び58重量%の硝酸鉄(III)九水和物溶液140mLを用いている。加熱処理は、800℃の代わりに1000℃で実行された。微小孔構造及び黒鉛の存在はそれぞれ、N2吸着測定及びXRDで測定された。
実施例2で述べたものと類似の工程が実施されたが、実施例4は代わりに、押出成形物の代わりに50gの炭素顆粒及び58重量%の硝酸鉄(III)九水和物溶液47mLを用いている。加熱処理は、800℃の代わりに1000℃で実行された。収量は、21gの黒い炭素顆粒であった。微小孔構造及び黒鉛の存在はそれぞれ、N2吸着測定及びXRDで決定された。
実施例4の試料5.0gが、4MのHCl 15mLで処理され、2時間撹拌され、濾過され、再び4MのHCl 10mLで処理された。それから、濾過され、水で洗浄され、110℃で一晩乾燥された。収量は、3.9gの黒い顆粒であった。分析は、実施例1に対して述べられたものと同じであり、その結果は下記の表4aで見ることができる。
25gの活性炭押出成形物(JECカーボン 1.8mm SHIRASAGI C2x8/12 ヤシ殻系ペレット活性炭)にわたって、(250gの脱塩水に300.3gのクエン酸鉄アンモニウムが溶解された)5.1mlのクエン酸鉄(III)アンモニウム溶液をスプレーボトルでスプレーすることにより、本発明による強磁性炭素体が調製された。試料は、大気条件(約760mmHgの圧力)の下、110℃のストーブ内で、45分の間乾燥された。その後、5.5mlのクエン酸鉄(III)アンモニウム溶液が、炭素押出成形物にわたってスプレーされた。試料は、大気条件の下、110℃のストーブ内で一晩乾燥された。疎な粒子は、ふるいによってその後除去された。その後、含浸された球は、石英管炉(Thermolyne 21100 furnace)内で、滞留窒素ガス雰囲気で、熱処置することにより熱分解された。加熱速度は5℃/分であり、球は800℃で3時間保たれた。
25gの活性炭押出成形物(JECカーボン 1.8mm SHIRASAGI C2x8/12 ヤシ殻系ペレット活性炭)が、(250gの脱塩水に300.3gのクエン酸鉄アンモニウムが溶解された)200mLのクエン酸鉄(III)アンモニウム溶液内に1分間浸漬された。試料は排水され(drained)、パッドドライされた(padded dry)。試料は、大気条件(約760mmHgの圧力)の下、110℃のストーブ内で一晩乾燥された。疎な粒子は、ふるいによってその後除去された。その後、浸漬された球は、石英管炉(Thermolyne 21100 furnace)内で、滞留窒素ガス雰囲気で、熱処理することにより熱分解された。加熱速度は5℃/分であり、球は800℃で3時間保たれた。
Claims (22)
- 部分的に黒鉛化した活性炭及び少なくとも一つの強磁性金属の金属粒子を含む強磁性炭素体であって、100nmから20mmの大きさ、200から1000m2/gの間のBET表面積、0.1から1ml/gの間の孔の全体積、及び2から10nmの間の平均孔直径を有している、強磁性炭素体。
- 前記強磁性金属は、鉄、ニッケル、及びコバルトの金属及び/または合金、及びそれらの組み合わせからなる群から選択され、前記強磁性炭素体は、10から90重量%の黒鉛状炭素を含む、請求項1に記載の強磁性炭素。
- 前記強磁性体は、20から80重量%の黒鉛状炭素を含む請求項2記載の強磁性炭素。
- 前記強磁性体は、25から70重量%の黒鉛状炭素を含む請求項3記載の強磁性炭素。
- 前記強磁性体は、30から60重量%の黒鉛状炭素を含む請求項4記載の強磁性炭素。
- 前記金属粒子は、黒鉛状炭素によって完全にカプセル化されている、請求項1または5に記載の強磁性炭素体。
- 前記強磁性炭素体は、金属及び/または金属酸化物の追加の粒子をさらに含む、請求項1から6のいずれか一項に記載の強磁性炭素体。
- 前記強磁性炭素体は、ポリマーをさらに含む、請求項1から7のいずれか一項に記載の強磁性炭素体。
- 前記強磁性炭素体は、カーボンナノチューブ及び/またはカーボンナノファイバを備えている、請求項1から8のいずれか一項に記載の強磁性炭素体。
- 請求項1から9のいずれか一項に記載の強磁性炭素体の製造方法であって、活性炭を不揮発性の金属化合物の水溶液に含浸させる段階、含浸された活性炭を乾燥させる段階、及び乾燥され含浸された活性炭を不活性雰囲気の下で熱分解し、それによって前記金属化合物を対応する金属に還元させる段階、を含む強磁性炭素体の製造方法。
- 100nmから20mmの大きさを有している強磁性炭素体の製造方法であって、活性炭粉末を不揮発性の金属化合物粉末と混合する段階、結果としての混合粉末を本体に成形する段階、及び成形された本体を不活性雰囲気の下で熱分解し、それによって前記金属化合物を対応する金属に還元させる段階、を含む強磁性炭素体の製造方法。
- 前記金属化合物は、強磁性金属及び/または合金の前駆体である、請求項10または11に記載の方法。
- 前記金属化合物は、硝酸鉄(III)またはクエン酸鉄(III)アンモニウムである、請求項12記載の方法
- 前記強磁性炭素体は、800℃より上の温度で、水素及び炭素含有化合物を含むガス流に接触される、請求項10から13のいずれか一項に記載の工程。
- ポリマーが、前記強磁性炭素体の前記黒鉛表面上へ吸着される、請求項10から14のいずれか一項に記載の方法。
- 前記強磁性炭素体は、金属及び/または金属酸化物が担持されている、請求項10から15のいずれか一項に記載の方法。
- 前記強磁性炭素体は、黒鉛状炭素層によって完全にカプセル化された強磁性金属粒子を含む、請求項16記載の方法。
- 請求項10から17のいずれか一項に記載の方法によって得ることのできる、部分的に黒鉛化された活性炭及び少なくとも一つの強磁性金属の金属粒子を含む、強磁性炭素体。
- 部分的に黒鉛化された活性炭を含む炭素体の製造方法であって、請求項1から9及び17のいずれか一項に記載の強磁性炭素体を酸に接触させ、それによって前記金属粒子を溶解させる段階、及びそれから酸処理された強磁性炭素体を液体ですすぎ、それによって前記溶解した金属粒子を除去する段階、を含む方法。
- 請求項19の方法により得ることのできる部分的に黒鉛化された活性炭を含む炭素体。
- 浄水または電気化学的応用における、吸着剤として、触媒担体として、触媒としての、請求項1から9のいずれか一項に記載の強磁性炭素体または請求項20に記載の炭素体の使用。
- 一酸化炭素を水素化することによりオレフィンを製造するのに適した触媒であって、請求項1または2に記載の強磁性炭素体を含む、触媒。
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