JP2009505830A - 石油留分の水素化転化のための触媒組成物を調製する方法 - Google Patents
石油留分の水素化転化のための触媒組成物を調製する方法 Download PDFInfo
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- JP2009505830A JP2009505830A JP2008528970A JP2008528970A JP2009505830A JP 2009505830 A JP2009505830 A JP 2009505830A JP 2008528970 A JP2008528970 A JP 2008528970A JP 2008528970 A JP2008528970 A JP 2008528970A JP 2009505830 A JP2009505830 A JP 2009505830A
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 84
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- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
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- 239000011591 potassium Substances 0.000 description 1
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- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
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- 230000035484 reaction time Effects 0.000 description 1
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- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical compound C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 description 1
- 229940081974 saccharin Drugs 0.000 description 1
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- 239000000901 saccharin and its Na,K and Ca salt Substances 0.000 description 1
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- 238000003756 stirring Methods 0.000 description 1
- 125000000446 sulfanediyl group Chemical group *S* 0.000 description 1
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- 238000012360 testing method Methods 0.000 description 1
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- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
11.93gのヘプタモリブデン酸アンモニウム[(NH4)6Mo7O24]、21.18gの硝酸ニッケル[Ni(NO3)2.6H2O]、及び0.33gの臭化セチルトリメチルアンモニウム(CTAB)が、150mlの脱イオン水内で溶解される。4〜6のpHを有する緑色の結晶溶液が得られ、その後、28容積%水酸化アンモニウム、約125mlが、8〜10のpHに達するまで添加され、溶液は、結晶性を残し、その色が、緑から青に変わる。その後、溶液は、79〜90℃に加熱され、過剰の水(125ml)の蒸発及び緑の沈殿物の形成が可能になる。形成された懸濁液は、7.3のpHを呈する。得られた材料は、ろ過され、豊富な量の脱イオン水で洗浄され、18時間の間、120℃で乾燥される。
触媒組成物内に残渣炭素前駆体として添加された界面活性剤の影響を評価するために、実施例1で調製された材料は、空気雰囲気内で400℃の温度で焼成された。得られた材料の酸化相は、その形態が、ニッケルモリブデン混合酸化物のナノ粒子からなる、β−NiMoO4相及び少量のα−NiMoO4相に相当する結晶構造を呈し(図1(b)を参照されたい)、また、105m2/gのBET表面積、0.18cm3/gの平均孔容積、及び6.9nmの平均孔直径を呈した。
この実施例は、実施例1に述べる同じ方法に従う。この実施例では、材料は、炭素前駆体有機成分の添加無しで調製された。この実施例で使用される塩の量は、界面活性剤としてのCTABの添加の無い実施例1の場合と同じであった。得られた沈殿物は、ろ過され、豊富な量の脱イオン水で洗浄された。
実施例3で得られた乾燥材料は、実施例2に述べる同じ手順に従って空気雰囲気内で焼成された。酸化相では、材料は、実施例2で報告された同じ結晶構造を呈した。しかし、BET表面積は92m2/gであり、孔容積は0.132cm3/gであり、平均孔直径は5.1nmであった。酸化形態の材料は、硫化処置を受ける。硫化処置を受けるために、材料は、100ml/分の窒素流量を使用して石英管内で、400℃に達するまで4℃/分の速度で加熱される。400℃に達すると、窒素流は、10容積%のH2S及び90容積%のH2からなるガスの混合物に変更され、2時間の間維持される。粉末形態(80:100 Tyler mesh)の硫化材料の一部分は、実施例1に述べる手順及び条件によって、考えられる最大限、環境に対する暴露を回避しながら、ジベンゾチオフェン(DBT)の水素化脱硫反応において評価された。
この例では、触媒は、粘結剤又は結合剤の存在下でのニッケルモリブデン混合オキシ水酸化物の沈殿によって調製された。243m2/gの表面積、0.336cm3/gの平均孔容積、及び5.54nmの平均孔直径を有するベーマイト相のアルミナが使用された。このために、ちょうど実施例1と同様に、11.93gの硝酸ニッケル、21.18gのヘプタモリブデン酸アンモニウム、及び0.33gの界面活性剤(CTAB)が、150mlの水内に溶解された(pH=5)。溶液は、緑色を取得し、その後、この溶液は、90℃に加熱され、125mlの水酸化アンモニウム(pH=10)が添加され、結晶溶液は青色を取得した。この溶液は、90℃に加熱しながら、30分間維持され、その後、68.25gのベーマイト(Catapal)が添加された。蒸発によって水を除去するために、ベーマイトを添加された溶液は、青から緑、その後、浅緑への色の変化が認められるまで、先に示した温度で約3時間の間、加熱し続けた。得られた沈殿物は、室温で冷却されたままにされ、蒸留水で4回、洗浄ごとに600mlで洗浄された。最後に、得られた生成物は、18時間の間、120℃の温度で乾燥された。その後、材料は、実施例1で述べた手順に従って焼成された。酸化相では、材料は、ガンマ−アルミナに特有の回折パターンを示す。酸化相の触媒は、16.4重量%のMoO3、7.17重量%のNiO、及び76.4重量%のAl2O3を含有する。この材料は、271m2/gの窒素吸着によって測定された比面積、0.31cm3/gの孔容積、及び4.5nmの孔直径を示す。
実施例6は、実施例5に述べる方法に従って実施された。この場合、ヘプタモリブデン酸アンモニウム塩及び硝酸ニッケル溶液の調製中に、界面活性剤は添加されなかった。結晶化は、粘結剤、実施例5で使用されるものと同じ粘結剤の存在下で実施された。
この例は、水素化脱硫触媒のために従来のアルミナ上に担持された本発明の目的である触媒組成物と同じ金属に基づく、市販の触媒の触媒活性の評価に相当する。触媒活性の評価は、実施例1に述べた手順に従ってDBT水素化脱硫反応において実施された。
実施例1に述べる方法に従って、ニッケル塩をコバルト塩で置換して、材料が調製された。こうするために、11.93gのヘプタモリブデン酸アンモニウム、21.18gの硝酸コバルト[Co(NO3)2.6H2O]、及び0.33gの臭化セチルトリメチルアンモニウム(CTAB)が使用された。
材料は、実施例1に述べる手順に従って調製された。こうするために、同じ量のヘプタモリブデン酸アンモニウム(11.93g)が使用され、第2金属塩の量が、2つの、10.6gの硝酸ニッケルと10.6gの硝酸コバルトに分割された。同じ方法に従って、コバルト、ニッケル、及びモリブデンの混合硝酸塩の一貫した沈殿物が得られた。沈殿物は、実施例1と同様に、洗浄され、乾燥された。
合成中に添加された界面活性剤の濃度の影響を観測するために、以下の2つの例では、組み込まれる界面活性剤の量を変えた。材料は、実施例1で述べた手順に従って調製され、同じ量の前駆体塩及び溶媒の量を使用し、1.65gのCTABである添加される界面活性剤の量だけが変わった。沈殿は、実施例1と同様に洗浄され、乾燥された。
実施例1で述べた同じ手順に従って、また、実施例10の場合と同じ目的で、界面活性剤の量は、この実施例では、実施例1の場合と同じ量の塩と溶媒を使用して、3.3gのCTABまで増加した。
触媒組成物は、実施例1で述べる手順に従って調製された。得られた沈殿物、ニッケル−モリブデンオキシ水酸化物は、触媒組成物の総重量に基づいて20重量%のアルミナベーマイト(alumina boehmite)を混合された。その後、蒸留水内に溶解された3重量%の硝酸の水性溶液が、ペーストが得られるように添加された。湿潤ペーストが、閉じた容器内に溜まる(left to stand)ように放置され、その後、成形された。得られる成形品は、実施例1で述べる手順に従って120℃で乾燥された。
Claims (38)
- 溶媒内で完全溶解状態にある、少なくとも1つの第VIII族非貴金属及び少なくとも1つの第VIB族金属、並びに、炭素前駆体としての有機化合物で構成される触媒組成物を調製するプロセス。
- a)水、メタノール、エタノール、プロパノール、ブタノール、及び/又は水−アルコール混合物などのアルコールでよい溶媒内で前記前駆体塩を溶解し混合する工程と、
b)溶媒内に有機成分及び/又は界面活性剤を溶解する工程と、
c)工程(a)及び(b)で得られた溶液を混合する工程と、
d)5〜14、好ましくは、8〜12を包含するpHで、溶液(c)に塩基性水酸化物溶液及び/又は炭酸アンモニウムを添加する工程と、
e)工程(d)で得られた溶液についての温度を、50〜200℃、好ましくは、60〜100℃を包含する温度に増加させる工程と、
f)工程(e)の溶液を均質化する工程と、
g)工程(f)で得られた溶液を、溶媒の蒸発によって結晶化する工程と、
h)蒸発が終了しなかった場合に、結晶を分離し、母液を回収するために、工程(g)で得られた結晶化懸濁液をろ過又は遠心分離する工程と、
i)工程(h)で得られた固形物を、十分な脱イオン水及び/又は水/アルコール混合物で洗浄する工程と、
j)50〜300℃、好ましくは、80〜150℃を包含する温度で、工程(i)で得られた固形物を乾燥する工程と、
k)200〜1000℃、好ましくは、300〜600℃を包含する温度で、窒素、ヘリウム、アルゴンなどのような不活性雰囲気内で、工程(j)で得られた固形物を熱処理する工程と、
l)工程(i)か、又は、工程(j)のいずれかで得られた材料を、10容積%硫化水素で構成されたガス流内で、又は、少なくとも0.2重量%の硫黄を含有する炭化水素留分と、200〜600℃、好ましくは、250〜500℃を包含する温度で、かつ、1〜100Kg/cm2を包含する圧力の水素流を用いて硫化するステージとからなる請求項1に記載の調製プロセス。 - 第VIII族金属及び第VIB族金属前駆体塩は全て、溶媒として使用される液体内で完全に溶解する請求項1に記載の調製プロセス。
- 完全に溶解された前駆体塩は、有機化合物を含有する溶液と混合される請求項1に記載の調製プロセス。
- 使用される溶媒は、水及び/又はアルコール及び/又はアルコール−水混合物を有する請求項1に記載の調製プロセス。
- 添加される有機化合物は、塩化物、臭化物、フッ化物、水酸化物などの形態であってよい、カチオン系界面活性剤、アニオン系界面活性剤、又は中性界面活性剤、或いは第4級アンモニウム塩(R4N+)などの界面活性剤を有する請求項1に記載の調製プロセス。
- 第VIII族非貴金属は、ニッケル、コバルト、及び/又は鉄、或いは、これらの金属の混合物を含む請求項1に記載の調製プロセス。
- ニッケル及び/又はコバルトは、酸化物として計算された、第VIII族非貴金属の100重量%に相当する請求項7に記載の調製プロセス。
- 第VIB族金属は、モリブデン及び/又はタングステン及び/又はクロムを含む請求項1に記載の調製プロセス。
- モリブデンは、選択される第VIB族金属の少なくとも50重量%に相当し、第VIB族金属の、好ましくは少なくとも80重量%、より好ましくは、100重量%は、モリブデンである請求項1及び9に記載の調製プロセス。
- pHを、5〜14、好ましくは、8〜12に維持するために、水酸化物及び/又は炭酸アンモニウム及び/又は尿素又は第4級アンモニウム塩から選択されてもよい塩基性溶液を添加する工程を有する請求項2に記載の調製プロセス。
- 溶液を均質化する工程は、選択された前駆体塩が全て、完全溶解状態にあるような、温度及びpHで起こる請求項2に記載の調製プロセス。
- 溶液を均質化する工程は、5分〜24時間、好ましくは、5分〜10時間を包含する時間で起こる請求項2に記載の調製プロセス。
- 溶液を結晶化する工程は、結晶槽に対して溶媒を部分的に蒸発させることによって、かつ/又は、蒸発器内で溶媒を完全に蒸発させることによって実施される請求項2に記載の調製プロセス。
- 溶液を結晶化する工程は、80〜200℃を包含する温度で、溶媒を蒸発させることによって実施される請求項2に記載の調製プロセス。
- 母液をろ過し、かつ/又は、遠心分離し、回収し、及び再循環させる工程は、蒸発及び/又は結晶化が終了しなかった場合に含まれる請求項2に記載の調製プロセス。
- 不活性雰囲気内で熱処理する工程は、200〜1000℃、好ましくは、300〜600℃を包含する温度で、窒素、ヘリウム、アルゴン、又はそれらの混合物の流れの中で、少なくとも0.01L/g分の流量(flow)で実施される請求項2に記載の調製プロセス。
- 熱処理は、どんな理由であっても、酸化雰囲気内で実施されるべきでない請求項2に記載の調製プロセス。
- 硫化する工程は、いずれの以前の熱処理も無い状態で、直接に乾燥材料に関して実施される請求項2に記載の調製プロセス。
- 硫化する工程は、請求項17に記載の不活性雰囲気内で、熱処理された材料に関して実施される請求項2に記載の調製プロセス。
- 硫化する工程は、大気圧で、200〜600℃、好ましくは、250〜500℃を包含する温度で、硫化水素(H2S)、二硫化炭素(C2S)、二硫化ジメチル(DMDS)、チオフェンなどと水素の混合物で構成されたガス流内で、乾燥材料か熱処理された材料のいずれかに関して実施される請求項2に記載の調製プロセス。
- 硫化する工程は、少なくとも0.1重量%の硫黄を含有する炭化水素液体留分及び200〜600℃、好ましくは、250〜500℃を包含する温度で、かつ、1〜100Kg/cm2を包含する圧力の水素の存在下で、乾燥材料か熱処理された材料のいずれかに関して実施される請求項2に記載の調製プロセス。
- 前駆体塩の混合物を均質化する工程において、アルミナ、シリカ、チタニア、シリカ−アルミナ、アルミナ−チタニア、ジルコニア、ジルコニア−チタニア、ジルコニア−アルミナ、アモルファスシリコアルミネート、及び/又は結晶、粘土などのような粘結剤に似た無機酸化物を含む請求項2に記載の調製プロセス。
- 湿潤材料及び/又は乾燥材料の結晶化の工程後に、粘結剤に似た無機酸化物の添加を考慮する請求項2に記載の調製プロセス。
- 材料が、熱処理された、かつ/又は、硫化された後に、粘結剤として無機酸化物の添加を考慮する請求項2に記載の調製プロセス。
- 請求項23、24、及び25に記載の工程のうちの任意の工程において添加される粘結剤に似た無機酸化物を含有する材料の成形品の配合組成を考慮する請求項2に記載の調製プロセス。
- 少なくとも1つの第VIII族非貴金属、少なくとも1つの第VIB族非貴金属、及び炭素を含み、任意で、酸化状態にある、かつ/又は、部分的に還元される、かつ/又は、硫化されることができる粘結剤として無機酸化物を含有してもよい触媒組成物。
- 第VIII族非貴金属は、その濃度が、含まれる酸化物の全組成物の20重量%から50重量%まで変わる、ニッケル及び/又はコバルト或いはその混合物に相当する請求項27に記載の触媒組成物。
- 第VIB族金属は、好ましくは、その組成が、関係する金属の酸化物として判定される全組成物の30から50%まで変わる、モリブデン及び/又はタングステンに相当する請求項27に記載の触媒組成物。
- 第VIB族金属は、好ましくは、モリブデンである請求項29に記載の触媒組成物。
- 炭素は、アモルファス状態にあるか、又は、その濃度が、関係する酸化物の全濃度の0.05重量%から5重量%まで変わる、第VIB族金属と第VIII族金属を有するカーバイドを形成する請求項27に記載の触媒組成物。
- 第VIII族金属と第VIB族金属は、酸化物として判定される全触媒組成物の50〜100重量%を有する請求項27に記載の触媒組成物。
- 触媒組成物のX線回折パターンは、第VIB族から選択される金属がモリブデンである場合、第VIII族金属のモリブデン酸塩のアルファ相又はベータ相に、かつ/又は、選択される金属がタングステンである場合、第VIII族金属のタングステン酸塩に相当する請求項27に記載の触媒組成物。
- 触媒組成物のX線回折パターンは、第VIB族から選択される金属がモリブデンである場合、モリブデン酸塩アルファ相又はベータ相又はコバルトモリブデン酸塩又はニッケルコバルトモリブデン酸塩に、かつ/又は、第VIB族から選択される金属がタングステンである場合、タングステン酸塩又はコバルトタングステン酸塩又はニッケルコバルトタングステン酸塩に相当する請求項27に記載の触媒組成物。
- 少なくとも1つの第VIII族非貴金属の硫化物、及び、少なくとも1つの第VIB族金属の硫化物、及び/又は、第VIII族金属と第VIB族金属の混合硫化物を含む請求項27に記載の触媒組成物。
- 第VIB族金属の硫化物及び第VIII族金属の硫化物の少なくとも一部は、2の構造層から20の構造層の積層レベルを有するフラーレン微小球の形態を呈する請求項35に記載の触媒組成物。
- 炭化水素留分の水素化処理反応において、高い水素化脱硫、高い水素化、及び高い水素化脱窒素を呈することを特徴とする請求項27に記載の触媒組成物。
- 硫黄及び窒素含有量が非常に低い燃料を生産するために、水素化脱硫及び水素化脱窒素に対して高い活性を呈することを特徴とする請求項27に記載の触媒組成物。
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US (2) | US8946110B2 (ja) |
EP (1) | EP1941944A4 (ja) |
JP (2) | JP5495563B2 (ja) |
CA (1) | CA2620656C (ja) |
MX (1) | MXPA05009283A (ja) |
RU (1) | RU2417124C2 (ja) |
WO (1) | WO2007027079A1 (ja) |
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JP5495563B2 (ja) | 2014-05-21 |
MXPA05009283A (es) | 2007-02-27 |
US8946110B2 (en) | 2015-02-03 |
JP5761814B2 (ja) | 2015-08-12 |
CA2620656A1 (en) | 2007-03-08 |
WO2007027079A1 (es) | 2007-03-08 |
US20080280754A1 (en) | 2008-11-13 |
CA2620656C (en) | 2014-03-25 |
EP1941944A1 (en) | 2008-07-09 |
EP1941944A4 (en) | 2011-06-01 |
RU2417124C2 (ru) | 2011-04-27 |
JP2013018001A (ja) | 2013-01-31 |
US20150087502A1 (en) | 2015-03-26 |
RU2008112007A (ru) | 2009-10-10 |
US9776174B2 (en) | 2017-10-03 |
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