JP2013066890A - 都市スラッジ、産業スラッジ、コンポストおよびタバコ廃棄物から得られる触媒作用性吸着媒、およびその製造方法 - Google Patents
都市スラッジ、産業スラッジ、コンポストおよびタバコ廃棄物から得られる触媒作用性吸着媒、およびその製造方法 Download PDFInfo
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- JP2013066890A JP2013066890A JP2012276759A JP2012276759A JP2013066890A JP 2013066890 A JP2013066890 A JP 2013066890A JP 2012276759 A JP2012276759 A JP 2012276759A JP 2012276759 A JP2012276759 A JP 2012276759A JP 2013066890 A JP2013066890 A JP 2013066890A
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- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28059—Surface area, e.g. B.E.T specific surface area being less than 100 m2/g
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/42—Materials comprising a mixture of inorganic materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
Abstract
【解決手段】産業廃棄物由来吸着媒を、下水スラッジ、金属スラッジ、廃油スラッジおよびタバコ廃棄物をいくつかの組み合わせで熱分解させることによって得た。この物質を、水分の存在下室温で硫化水素を除去するための媒体として用いた。初期吸着媒、および破過試験後の消尽吸着媒を、窒素の吸着、熱分析、XRD、ICP、および表面pH測定を用いて特性評価した。タバコとスラッジを混ぜると強い相乗作用をもたらし、吸着媒の触媒特性を向上させる。熱分解の際に新規な鉱物相が、各スラッジ成分間の固相反応の結果として生成する。高温の熱分解は、炭素質相の活性化が増大され、無機相が化学的に安定化されるので、吸着媒に対して効果がある。低温で得られたサンプルは水に対して感受性があり、これは、その触媒中心を非活性化する。
【選択図】図1
Description
用語「吸着」とは、気体または液体環境からの分子の濃縮物が固体の表面に蓄積される現象を言う。
表3に掲載されているように廃棄物スラッジの均質混合物を調製し、120℃で乾燥させた。次にこの乾燥サンプルを押しつぶして、950℃の水平式炉の中で30分間熱分解した。温度勾配は10度/分であった。不活性雰囲気は、10mL/分の窒素流によって供給した。物質の収率、アッシュ含量および密度を表3に掲載してある。
表8に掲載されているように、廃棄物スラッジの均質混合物を調製し、120℃で乾燥させた。次にこの乾燥サンプルを押しつぶして、650℃の水平式炉の中で30分間熱分解した。温度勾配は10度/分であった。不活性雰囲気は、10mL/分の窒素流によって供給した。物質の収率、アッシュ含量および密度を表8に掲載してある。
表12に掲載されているように、廃棄物スラッジの均質混合物を調製し、120℃で乾燥させた。次にこの乾燥サンプルを押しつぶして、950℃の水平式炉の中で60分間熱分解した。温度勾配は10度/分であった。不活性雰囲気は、10mL/分の窒素流によって供給した。物質の収率および密度を表12に掲載してある。
標準的な粉末回折法を用いて、X線回折の測定を、WO、SS、MS、WOSSおよびWOSSMSの吸着媒サンプルに対して行った。吸着媒は、小さなメノウ乳鉢中でメタノールを用いて粉砕した。吸着媒を手によって粉砕すると、5〜10μmの粒子サイズが保証され、これは、回折ピークの線が広くなることを防ぐ。混合物は、Philips標本ホルダーのゼロバックグラウンド石英窓にスミア法で取り付け、空気乾燥させた。サンプルは、Phillips XRG 300 X-ray回折計で発生させたCu Kαradiationにより分析した。機器のふらつきを調べるために、また2θピークの正確な位置を得るために、石英製標準スライドを試した。
650℃、950℃で0.5時間または1時間の条件で得られた、H2S除去媒体としての吸着媒の性能を比較した。結果を表16〜18に示す。
アシッドレッドおよび塩基性フクシンの吸着についての平衡に関する検討を、293Kにあるシリーズになった100mLエルレンマイヤーフラスコ中で行った。各フラスコを、濃度が10〜1000mg/Lの染料(dye)溶液10mLで満たした。平衡化の後、サンプルを濾過し、その染料濃度を分析し、平衡吸着容量を計算した。平衡データを、いわゆるラングミュア-フロイントリッヒ単一溶質等温線にフィッティングした。結果を表19に示す。変数qmは吸着媒単位グラムあたりの吸着容量であり、Kはラングミュア型の平衡定数であり、そして指数項nはサイトエネルギーの異質性パラメータである。
サンプル多孔性に対する水への曝露の影響を調べるために、本物質を水に分散させ、室温にて24時間震盪した。表面部分を乾燥させた後、ポア体積および平均ポアサイズを測定した。結果はメソポア体積の増加を示したが、これは、無機酸化物/塩と水が反応した結果によるものである。結果を表20に示してある。Δは平均ポアサイズである。
銅の吸着についての平衡の検討を、20℃にあるシリーズになった100mLエルレンマイヤーフラスコ中で行った。各フラスコを、濃度が10〜1000mg/Lの塩化銅溶液10mLで満たした。平衡化の後、サンプルを濾過し、その銅含量を分析し、平衡吸着容量を計算した。平衡データを、いわゆるラングミュア-フロイントリッヒ単一溶質等温線にフィッティングした。結果を表21に示す。変数qmは吸着媒単位グラムあたりの吸着容量であり、Kはラングミュア型の平衡定数であり、そして指数項nはサイトエネルギーの異質性パラメータである。吸着容量、特に650℃で得られたサンプルのものは、活性炭のものよりもはるかに高かった。
各単一成分サンプル中のFe、Ca、Cu、Zn、およびMgの含量を測定し、そして混ぜ合わせたサンプルの組成に基づいて、これら元素の含量数値を求めた。結果を表22に示す。
物質
2種の産業スラッジ、すなわちNewport News Shipyardから得た廃油スラッジ(WO)および金属スラッジ(M)を、乾燥タバココンポストと混ぜ、均質化し、120℃で48時間乾燥させ、次いで水平式炉の中で窒素中650℃および950℃で炭素化した。加熱速度は10度/分で、保持時間は1時間であった。各湿潤産業スラッジ(それらには75%の水が含まれている)の重量を調整して、産業スラッジ成分が乾燥質量を基準にして10%および50%になるようにした。得られた吸着媒の名前、それらの収率、アッシュ含量および嵩密度ならびに組成を表23に集めてある。タバコ廃棄物は、TCと記載されている。
上述したように、特注設計の動的試験を用いて、ガス流からのH2S吸着に対する吸着媒性能を評価した。吸着媒サンプルを粉砕し(1〜2mm粒子サイズ)、ガラス製カラム(長さ370mm、内径9mm、ベッド体積6cm3)に充填して、湿潤空気(相対湿度25℃で80%)で1時間予加湿した。吸着された水の量は、サンプル重量の増加から推算した。0.3%(3,000ppm) のH2Sを含有する湿潤空気(相対湿度25℃で80%)を吸着媒のカラムに0.5L/分で通した。流量は、Cole Parmerの流量計を用いて制御した。H2Sの破過は、MultiRaeの光イオン化センサーを用いてモニタリングした。試験は、破過濃度100ppmで停止した。吸着媒1gあたりの硫化水素mgでの各吸着媒の吸着容量は、破過曲線より上にある面積を積分して、流入ガス中のH2S濃度、流量、破過時間、および吸着剤の質量から計算した。試験は各サンプルに対して少なくとも2回繰り返した。H2S以外に流出ガス中のSO2の含量もMultiRaeの光イオン化センサーを用いてモニタリングした。H2Sを吸着した後の消尽吸着媒は、その名前に追加の文字Eを加えることで示されている。
得られた物質に対して、ASAP 2010(Micromeritics社) を用いて、沸点にある窒素の吸着を行った。実験の前に、サンプルは、120℃で、一定真空(10〜4トール)に気体抜きをした。等温線からは、表面積(BET法)、全ポア体積(Vt)を、(相対圧力が0.99に等しいところにおける最後の等温線ポイントからは)、ミクロポアの体積(Vmic(DR))、メソポア体積Vmes、全ポア体積(Vt)を、ポアサイズ分布と並んで計算した(DFT)。
炭素質サンプル懸濁液のpHは、表面の酸性および塩基性についての情報を与える。乾燥炭素質粉末サンプル0.4gを20mLの蒸留水に加え、この懸濁液を一晩攪拌して、平衡にもっていった。その後、懸濁液のpHを測定した。
TA Instrument Thermal Analyzerを用いて熱分析を行った。機器の設定は、10℃/分の加熱速度、および100mL/分の流量による窒素雰囲気であった。各測定では、約25mgの粉砕吸着媒サンプルを用いた。結果の解析には、一次微分熱重量測定曲線(DTG曲線)を用いる。アッシュ含量は、800℃でサンプルを空気中で加熱した後に残っている残渣から測定した。
吸着媒中の金属含量は、LSL labs, Syracuse, NYにあるICPを用いて測定した。
X線回折測定は、標準的な粉末回折法を用いて行った。吸着媒は、小さなメノウ乳鉢中でメタノールを用いて粉砕した。吸着媒を手によって粉砕すると、5〜10μmの粒子サイズが保証され、これは、回折ピークの線が広くなることを防ぐ。混合物は、Philips標本ホルダーのゼロバックグラウンド石英窓にスミア法で取り付け、空気乾燥させた。サンプルは、Phillips XRG 300 X-ray回折計で発生させたCu Kαradiationにより分析した。機器のふらつきを調べるために、また2θピークの正確な位置を得るために、石英製標準スライドを試した。
Claims (30)
- a) 有機窒素種が組み込まれた多孔質炭素20〜30%と、
b) 無機物質70〜80%と
を含む、コンポストまたはコンポスト材料の1つとスラッジとから誘導された吸着媒であって、
該スラッジが、産業スラッジまたは都市スラッジの少なくとも1つである、吸着媒。 - 前記無機物質が、高度に分散された触媒作用性酸化物を含む、請求項1に記載の吸着媒。
- 前記触媒作用性酸化物が、酸化銅、酸化亜鉛、酸化鉄、酸化カルシウム、シリカおよびアルミナのうちの1つ以上である、請求項2に記載の吸着媒。
- 前記窒素種が、アミンまたはピリジン基を含む、請求項1に記載の吸着媒。
- 前記吸着媒の表面積が、100〜500m2/gである、請求項1に記載の吸着媒。
- 前記吸着媒の表面積が、100〜200m2/gである、請求項5に記載の吸着媒。
- 前記吸着媒がミクロポアを含み、該ミクロポアの体積が少なくとも0.03cm3/gある、請求項1に記載の吸着媒。
- 前記吸着媒のpHが10よりも大きい、請求項1に記載の吸着媒。
- 前記吸着媒のpHが7と10の間である、請求項1に記載の吸着媒。
- 前記吸着媒のpHが4と7の間である、請求項1に記載の吸着媒。
- a) コンポスト材料をコンポストにするステップ;
b) 脱水した下水スラッジを熱的に乾燥させて、粒状にした有機肥料を生成させるステップ;
c) 前記有機肥料と前記コンポストとを混合するステップ;および
d) 該混合物を600℃と1000℃の間である温度で熱分解させるステップ
を含む、吸着媒の生成方法。 - 加熱速度が5℃/分と10℃/分の間であり、保持時間が60分と90分の間である、請求項11に記載の方法。
- 前記熱分解の温度が800℃と1000℃の間である、請求項11に記載の方法。
- 前記熱分解の温度が900℃と1000℃の間である、請求項13に記載の方法。
- 前記熱分解の温度が600℃と900℃の間であり、前記吸着媒を15〜20% HClでさらに処理する、請求項11に記載の方法。
- 前記熱分解の温度が800℃と900℃の間である、請求項15に記載の方法。
- 前記混合物を約5重量%と約30重量%の間の鉱油で処理するステップをさらに含み、該鉱油が、軽質鉱油、重質鉱油、天然鉱油、合成鉱油、使用済みエンジンオイル、およびこれらの組み合わせから選択される、請求項11に記載の方法。
- 有機窒素種が組み込まれた多孔質炭素20〜30%と下水スラッジから誘導された無機物質70〜80%とを含む吸着媒を湿潤空気流れと接触させるステップと、該吸着媒に酸性ガスを吸着させるステップとを含む、湿潤空気流れから酸性ガスを除去する方法。
- 前記酸性ガスが、硫化水素、二酸化硫黄、シアン化水素、および二酸化窒素のうちの1種または複数である、請求項18に記載の方法。
- 前記酸性ガスが硫化水素であり、これが無機物質と反応して、二酸化硫黄または元素の硫黄さらにはこれらの塩の形態に酸化される、請求項18に記載の方法。
- 前記湿潤空気流れが、下水処理プラントからの放出ガス、ガス燃料、または熱水ベントからのガスである、請求項18に記載の方法。
- コンポスト材料をコンポストにするステップ;
脱水した下水スラッジを熱的に乾燥させて、粒状にした有機肥料を生成させることによって吸着媒を生成させるステップ;
前記コンポストと前記有機肥料を混合するステップ;および
該混合物を600℃と1000℃の温度で熱分解させ、前記吸着媒を湿潤空気流れと接触させて、吸着媒に酸性ガスを吸着させるステップ
を含む、湿潤空気流れから酸性ガスを除去する方法。 - 前記酸性ガスが、硫化水素、二酸化硫黄、シアン化水素、および二酸化窒素のうちの1つ以上である、請求項22に記載の方法。
- 前記熱分解の温度が800℃と1000℃の間である、請求項22に記載の方法。
- 前記熱分解の温度が900℃と1000℃の間である、請求項24に記載の方法。
- 前記熱分解の温度が600℃と900℃の間であり、前記吸着媒を15〜20 % HClでさらに処理する、請求項22に記載の方法。
- 前記熱分解の温度が800℃と900℃の間である、請求項26に記載の方法。
- 前記吸着媒が、300〜500℃に加熱して元素の硫黄および二酸化硫黄を遊離させることによって再生可能である、請求項22に記載の方法。
- 第1のスラッジと、第2のスラッジおよびコンポスト材料のうちの少なくとも1つとを組み合わせて混合物を生成させるステップ;
該混合物を熱的に乾燥させるステップ;
該混合物を約600℃〜1100℃の温度で熱分解させるステップ;および
該熱分解のステップの間に、ウルツ鉱、フェロアン、輝銅鉱、尖晶石(スピネル)、フェロキシハイト、斑銅鉱、ヒボナイト、紅亜鉛鉱、アンケル石、クバンザクロ石、ペロホタイト、黄銅鉱、トリオライト、フェルシリサイト、サファーリン、磁赤鉄鉱、コーエナイト、ローソン石、菱亜鉛鉱、閃亜鉛鉱、針鉄鋼、ハント石、灰長石、ダイアスポア、バテライト、鱗繊石、バイヤライト、モグヘマイト、ピロホタイト、赤鉄鉱、スファレライト、鉄礬柘榴石、およびヘマタイトのうちの少なくとも1つを生成させるステップ
を含む、吸着媒の製造方法。 - 前記コンポスト材料が、タバコ廃棄物、古紙および木材炭のうちの少なくとも1つ、またはそれらの組み合わせであり、
前記第1のスラッジが、都市スラッジまたは産業スラッジであり、
前記第2のスラッジが、都市スラッジまたは産業スラッジであり、且つ第1のスラッジとは異なっている、請求項29に記載の方法。
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US20160236146A1 (en) | 2016-08-18 |
JP2014217841A (ja) | 2014-11-20 |
KR20130102115A (ko) | 2013-09-16 |
KR20080057263A (ko) | 2008-06-24 |
IL189959A0 (en) | 2008-08-07 |
CN101505855B (zh) | 2013-12-04 |
US9808761B2 (en) | 2017-11-07 |
EP1922138A4 (en) | 2013-06-26 |
CN101505855A (zh) | 2009-08-12 |
EP1922138A2 (en) | 2008-05-21 |
AU2006287450B2 (en) | 2011-12-01 |
KR101375467B1 (ko) | 2014-03-18 |
US9339806B2 (en) | 2016-05-17 |
BRPI0617033B1 (pt) | 2018-02-06 |
JP5759969B2 (ja) | 2015-08-05 |
CA2621621A1 (en) | 2007-03-15 |
IL233839A (en) | 2015-11-30 |
BRPI0617033A2 (pt) | 2011-07-12 |
IL233839A0 (en) | 2014-09-30 |
JP5508714B2 (ja) | 2014-06-04 |
WO2007030677A3 (en) | 2009-04-23 |
IL189959A (en) | 2014-08-31 |
AU2006287450A1 (en) | 2007-03-15 |
US20130102456A1 (en) | 2013-04-25 |
US20070113736A1 (en) | 2007-05-24 |
KR101393120B1 (ko) | 2014-05-08 |
WO2007030677A2 (en) | 2007-03-15 |
CA2621621C (en) | 2015-09-22 |
JP2009508666A (ja) | 2009-03-05 |
MX341219B (es) | 2016-08-10 |
US20100152038A1 (en) | 2010-06-17 |
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