JP2006528547A - 脱硫およびそのための新規なプロセス - Google Patents
脱硫およびそのための新規なプロセス Download PDFInfo
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- JP2006528547A JP2006528547A JP2006521156A JP2006521156A JP2006528547A JP 2006528547 A JP2006528547 A JP 2006528547A JP 2006521156 A JP2006521156 A JP 2006521156A JP 2006521156 A JP2006521156 A JP 2006521156A JP 2006528547 A JP2006528547 A JP 2006528547A
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- 238000000034 method Methods 0.000 title claims abstract description 119
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- 239000011593 sulfur Substances 0.000 claims abstract description 71
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- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 2
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 claims description 2
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Abstract
Description
炭化水素ストリームの脱硫に有用な組成物を生成する新規な方法を提供することが望ましい。
また、炭化水素ストリームからの硫黄を除去するプロセスであって水素消費ならびに同ストリームに含有されるオレフィン類および芳香族類の飽和を最少に留めるプロセスを提供することが望ましい。
a):1)液体、2)亜鉛含有化合物、3)シリカ含有物質、4)アルミナおよび5)促進剤を混合してそれらの混合物を形成する工程;
b):上記混合物を乾燥して乾燥混合物を形成する工程;
c):上記乾燥混合物を焼成して焼成混合物を形成する工程;
d):上記焼成混合物を適切な還元剤を用いて適切な条件下で還元して、原子価が低下した促進剤を含有する組成物を生成する工程;および
e):上記組成物を回収する工程。
a):1)液体、2)金属含有化合物、3)シリカ含有物質、4)アルミナおよび5)第一促進剤を混合してそれらの混合物を形成する工程;
b):上記混合物を乾燥して乾燥混合物を形成する工程;
c):上記乾燥混合物の上あるいは中に第二促進剤を添加して促進剤添加混合物を形成する工程;
d):上記促進剤添加混合物を乾燥して乾燥促進剤添加混合物を形成する工程;
e):上記乾燥促進剤添加混合物を焼成して焼成促進剤添加混合物を形成する工程;
f):上記焼成促進剤添加混合物を適切な還元剤を用いて適切な条件下で還元して、原子価が低下した促進剤を含有する組成物を生成する工程;および
g):上記組成物を回収する工程。
a):脱硫された炭化水素ストリームおよび硫化された組成物を生成するために炭化水素ストリームを第一あるいは第二の態様で得られた組成物と脱硫ゾーン内で接触させる工程;
b):上記の脱硫された炭化水素ストリームと硫化された組成物を各々から分離して脱硫炭化水素ストリームと硫化組成物を形成する工程;
c):分離された上記硫化組成物の少なくとも一部を再生ゾーン内で再生することにより同組成物の中および/あるいは上に存在する硫黄の少なくとも一部を除去して再生組成物を形成する工程;
d):上記再生組成物を還元ゾーン内で還元して、原子価が低下した促進剤を含有する還元組成物を生成する工程−同還元組成物は炭化水素ストリームと接触した際に同ストリームから硫黄を除去する;そしてそれに続く
e):上記還元組成物の少なくとも一部を脱硫ゾーンに循環させる工程。
本仕様書で使用される「ガソリン」という用語は、沸点が約37.8〜260°Cの範囲内にある炭化水素の混合物、あるいはそのような炭化水素の留分(種類は問わない)を指す。適切なガソリンの例としては、ナフサ、直留ナフサ、コーカー・ナフサ、接触分解ナフサ、ビスブレーカー・ナフサ、アルキル化ガソリン、異性化ガソリン、改質ガソリン等およびこれらのブレンドといった製油所で生産される炭化水素ストリームが挙げられるが、これらに限られない。
a):1)液体、2)金属含有化合物、3)シリカ含有物質、4)アルミナおよび5)第一促進剤を混合してそれらの混合物を形成する工程、
b):上記混合物を乾燥して乾燥混合物を形成する工程、
c):上記乾燥混合物の上あるいは中に第二促進剤を添加して促進剤添加混合物を形成する工程、
d):上記促進剤添加混合物を乾燥して乾燥促進剤添加混合物を形成する工程、
e):上記乾燥促進剤添加混合物を焼成して焼成促進剤添加混合物を形成する工程、
f):上記焼成促進剤添加混合物を適切な還元剤を用いて適切な条件下で還元して、原子価が低下した促進剤を含有する組成物を生成する工程、および
g):上記組成物を回収する工程。
a):脱硫された炭化水素ストリームおよび硫化された組成物を生成するために炭化水素ストリームを第一あるいは第二の態様で得られた組成物と脱硫ゾーン内で接触させる工程、
b):上記の脱硫された炭化水素ストリームと硫化された組成物を各々から分離して脱硫炭化水素ストリームと硫化組成物を形成する工程、
c):分離された上記硫化組成物の少なくとも一部を再生ゾーン内で再生することにより同組成物の中および/あるいは上に存在する硫黄の少なくとも一部を除去して再生組成物を形成する工程、
d):上記再生組成物を還元ゾーン内で還元して、原子価が低下した促進剤を含有する還元組成物を生成する工程−同還元組成物は炭化水素ストリームと接触した際に同ストリームから硫黄を除去する、そしてそれに続く
e):上記還元組成物の少なくとも一部を脱硫ゾーンに循環させる工程。
ニッケルを促進剤として含有する酸化亜鉛/アルミナ/真珠岩組成物を調製した。56gのアルミナ(Vista Dispal)を118.43gの脱イオン水に添加し、20分間混合した。次いで、43.6gの担体(真珠岩を硝酸で処理し、次いでアルミナ、酸化亜鉛およびカオリン粘土を添加して調製)を上記の水/アルミナ混合物に5分間かけて添加し、更に5分間混合した。この混合物を混合物#1と称する。
実施例Iで調製した組成物の脱硫活性を以下の手順でテストした。10gの調製された同物質を、1/2インチ径、12インチ長の石英管に入れた。同管には同組成物層を保持するための不活性充填物としてのガラス・フリットを下部1/3の部分の上側に配した。
ニッケルを通常の湿式含浸法を用いて70gの担体(真珠岩を硝酸で処理し、次いでアルミナ、酸化亜鉛およびカオリン粘土を添加して調製)に2段で含浸した。各段での含浸は74.3gの硝酸ニッケル六水和物と7gの脱イオン水の混合物を用いて実施した。第一段の含浸が完了後、同組成物を150°Cの温度で1時間乾燥し、次いで第二段の含浸が完了後、同組成物を150°Cの温度で1時間乾燥し更に635°Cの温度で1時間焼成した。これにより生成した組成物のDI値は12.2であった。
実施例IIIで調製した組成物の脱硫活性を実施例IIに記載される手順でテストした。同組成物を2反応サイクルでテストし、その結果を表IIに示す。同表において、1,2,3および4時間処理後の生成物の硫黄濃度を質量ppmで示している。
ニッケルを通常の湿式含浸法を用いて85gの担体(実施例IおよびIII記載)に1段で含浸した。含浸は74.3gの硝酸ニッケル六水和物と7gの脱イオン水の混合物を用いて実施した。同含浸組成物を150°Cの温度で1時間乾燥し、635°Cの温度で1時間焼成した。これにより生成した組成物のDI値は14.7であった。
実施例Vで調製した組成物の脱硫活性を実施例IIに記載される手順でテストした。同組成物を2反応サイクルでテストし、その結果を表IIIに示す。同表において、1,2,3および4時間処理後の生成物の硫黄濃度を質量ppmで示している。
ニッケルを促進剤として含有する酸化亜鉛/アルミナ/真珠岩組成物を調製した。685gの蒸留水を1007.5gの硝酸ニッケル六水和物と混合した。次いで、146gのアルミナ(Condeal Disperal)を上記混合物に添加した。一方、150gの真珠岩(Silbrico Sil−Kleer#27−M)を575gの酸化亜鉛と混合した。この混合物を上記のアルミナ含有混合物に添加した。その結果生成した組成物を上記実施例に開示される手順で乾燥し焼成した。
Claims (46)
- 以下の工程を包含する、組成物の製造方法:
(a):1)液体、2)亜鉛含有化合物、3)シリカ含有物質、4)アルミナおよび5)促進剤を混合してそれらの混合物を形成する工程;
(b):上記混合物を乾燥して乾燥混合物を形成する工程;
(c):上記乾燥混合物を焼成して焼成混合物を形成する工程;
(d):上記焼成混合物を適切な還元剤を用いて適切な条件下で還元して、原子価が低下した促進剤を含有する組成物を生成する工程;および
(e):上記組成物を回収する工程。 - 該組成物が炭化水素ストリームと脱硫条件下で接触した際にそれから硫黄を除去するように該焼成混合物を該工程(d)で還元することを特徴とする請求項1記載の方法。
- 該促進剤がニッケル、コバルト、鉄、マンガン、銅、亜鉛、モリブデン、タングステン、銀、錫、アンチモン、バナジウム、金、白金、ルテニウム、イリジウム、クロム、パラジウム、チタン、ジルコニウム、ロジウム、レニウムおよびこれらの任意の二種類以上の組み合わせからなる群から選ばれる金属を含有していることを特徴とする請求項1記載の方法。
- 該促進剤がニッケルを含有していていることを特徴とする請求項3記載の方法。
- 該シリカ含有物質が粉砕された発泡真珠岩の形をしていることを特徴とする請求項1記載の方法。
- 該工程(a)からの混合物が湿状、練状、ペースト状あるいはスラリー状の形をしていることを特徴とする請求項1記載の方法。
- 該工程(a)からの混合物がスラリー状の形をしていることを特徴とする請求項6記載の方法。
- 該工程(a)からの混合物を該工程(b)に送る前に粒状化することを特徴とする請求項1記載の方法。
- 該工程(a)からの混合物を該工程(b)に送る前に顆粒形状、押出形状、錠剤形状、球形、ペレット形状あるいは微小球形のいずれかの形状に粒状化することを特徴とする請求項1記載の方法。
- 該工程(a)からの混合物を該工程(b)で噴霧乾燥により該乾燥混合物を形成することを特徴とする請求項1記載の方法。
- 該混合物を該工程(b)で約65.5〜550°Cの範囲内の温度で乾燥することを特徴とする請求項1記載の方法。
- 該乾燥混合物を該工程(c)で約204.4〜815.5°Cの範囲内の温度で焼成することを特徴とする請求項1記載の方法。
- 該焼成混合物を該工程(d)で約37.8〜815.5°Cの範囲内の温度、約103kPa〜10.33MPa(約15〜1500psia)の範囲内の圧力、そして原子価が低下した促進剤を生成するに十分な還元時間で還元することを特徴とする請求項1記載の方法。
- 該焼成工程(c)で該アルミナを少なくとも部分的にアルミン酸塩に転化することを特徴とする請求項1記載の方法。
- 請求項1記載の方法により製造された組成物。
- 以下の工程を包含する、組成物の製造方法:
(a):1)液体、2)金属含有化合物、3)シリカ含有物質、4)アルミナおよび5)第一促進剤を混合してそれらの混合物を形成する工程;
(b):上記混合物を乾燥して乾燥混合物を形成する工程;
(c):上記乾燥混合物の上あるいは中に第二促進剤を添加して促進剤添加混合物を形成する工程;
(d):上記促進剤添加混合物を乾燥して乾燥促進剤添加混合物を形成する工程;
(e):上記乾燥促進剤添加混合物を焼成して焼成促進剤添加混合物を形成する工程;
(f):上記焼成促進剤添加混合物を適切な還元剤を用いて適切な条件下で還元して、原子価が低下した促進剤を含有する組成物を生成する工程;および
(g):上記組成物を回収する工程。 - 該第一促進剤がニッケル、コバルト、鉄、マンガン、銅、亜鉛、モリブデン、タングステン、銀、錫、アンチモン、バナジウム、金、白金、ルテニウム、イリジウム、クロム、パラジウム、チタン、ジルコニウム、ロジウム、レニウムおよびこれらの任意の二種類以上の組み合わせからなる群から選ばれる金属を含有していることを特徴とする請求項16記載の方法。
- 該第一促進剤がニッケルを含有していることを特徴とする請求項16記載の方法。
- 該焼成促進剤添加混合物が該工程(g)で炭化水素ストリームと脱硫条件下で接触した際にそれから硫黄を除去するように該混合物を該工程(f)で還元することを特徴とする請求項16記載の方法。
- 該金属含有化合物が亜鉛、マンガン、銀、銅、カドミウム、錫、ランタン、スカンジウム、セリウム、タングステン、モリブデン、鉄、ニオビウム、タンタル、ガリウム、インジウム、およびこれらの任意の二種類以上の組み合わせからなる群から選ばれる金属を含有していることを特徴とする請求項16記載の方法。
- 該金属含有化合物がニッケルを含有していることを特徴とする請求項20記載の方法。
- 該第二促進剤がニッケル、コバルト、鉄、マンガン、銅、亜鉛、モリブデン、タングステン、銀、錫、アンチモン、バナジウム、金、白金、ルテニウム、イリジウム、クロム、パラジウム、チタン、ジルコニウム、ロジウム、レニウムおよびこれらの任意の二種類以上の組み合わせからなる群から選ばれる金属を含有していることを特徴とする請求項16記載の方法。
- 該第二促進剤がニッケルを含有していていることを特徴とする請求項22記載の方法。
- 該シリカ含有物質が粉砕された発泡真珠岩の形をしていることを特徴とする請求項16記載の方法。
- 該工程(a)からの混合物が湿状、練状、ペースト状あるいはスラリー状の形をしていることを特徴とする請求項16記載の方法。
- 該工程(a)からの混合物がスラリー状の形をしていることを特徴とする請求項25記載の方法。
- 該工程(a)からの混合物を該工程b)に送る前に粒状化することを特徴とする請求項16記載の方法。
- 該工程(a)からの混合物を顆粒形状、押出形状、錠剤形状、球形、ペレット形状あるいは微小球形のいずれかの形状に粒状化することを特徴とする請求項16記載の方法。
- 該工程(a)からの混合物を該工程b)で噴霧乾燥により該乾燥混合物を形成することを特徴とする請求項16記載の方法。
- 該混合物および該促進剤添加混合物を各々該工程(b)および(e)で約65.5〜550°Cの範囲内の温度で乾燥することを特徴とする請求項16記載の方法。
- 該乾燥促進剤添加混合物を該工程(e)で約204.4〜815.5°Cの範囲内の温度で焼成することを特徴とする請求項16記載の方法。
- 該焼成促進剤添加混合物を該工程(g)で約37.4〜815.5°Cの範囲内の温度、約103kPa〜10.33MPa(約15〜1500psia)の範囲内の圧力、そして原子価が低下した促進剤を生成するに十分な還元時間で還元することを特徴とする請求項16記載の方法。
- 該焼成工程(e)で該アルミナを少なくとも部分的にアルミン酸塩に転化することを特徴とする請求項16記載の方法。
- 該工程(b)からの該混合物を該工程(c)で促進剤を添加する前の段階で焼成することを特徴とする請求項16記載の方法。
- 該乾燥混合物を約204.4〜815.5°Cの範囲内の温度で焼成することを特徴とする請求項34記載の方法。
- 請求項16記載の方法により製造された組成物。
- 以下の工程を包含する、炭化水素ストリームから硫黄を除去する方法:
(a):脱硫された炭化水素ストリームおよび硫化された組成物を生成するために炭化水素ストリームを第一あるいは第二の態様で得られた組成物と脱硫ゾーン内で接触させる工程;
(b):上記の脱硫された炭化水素ストリームと硫化された組成物を各々から分離して脱硫炭化水素ストリームと硫化組成物を形成する工程;
(c):分離された上記硫化組成物の少なくとも一部を再生ゾーン内で再生することにより同組成物の中および/あるいは上に存在する硫黄の少なくとも一部を除去して再生組成物を形成する工程;
(d):上記再生組成物を還元ゾーン内で還元して、原子価が低下した促進剤を含有する還元組成物を生成する工程−同還元組成物は炭化水素ストリームと接触した際に同ストリームから硫黄を除去する;そしてそれに続く
(e):上記還元組成物の少なくとも一部を脱硫ゾーンに循環させる工程。 - 該炭化水素ストリームが分解ガソリン、ディーゼル燃料およびこれらの組み合わせからなる群から選ばれる燃料から構成されていることを特徴とする請求項37記載の方法。
- 該工程(a)での脱硫を約37.8〜537.8°Cの範囲内の温度、約103kPa〜10.33MPa(約15〜1500psia)の範囲内の圧力、そして該ストリームから硫黄を除去するに十分な時間で実施することを特徴とする請求項37記載の方法。
- 該工程(c)での再生を約37.8〜815.5°Cの範囲内の温度、約68.9kPa〜10.33MPa(約10〜1500psia)の範囲内の圧力、そして分離された該硫化組成物から硫黄の少なくとも一部を除去するに十分な時間で実施することを特徴とする請求項37記載の方法。
- 該工程(c)において該再生ゾーン内で空気を再生剤として使用することを特徴とする請求項37記載の方法。
- 該工程(c)からの再生組成物を該工程(d)において該再生ゾーン内で水素を使用して約37.8〜815.5°Cの範囲内の温度、約103kPa〜10.33MPa(約15〜1500psia)の範囲内の圧力、そして該再生組成物内の促進剤の原子価を低下するに十分な還元時間で還元することを特徴とする請求項37記載の方法。
- 該工程(b)からの分離された該硫化組成物を該工程(c)に送る前にストリッピングすることを特徴とする請求項37記載の方法。
- 該工程(c)からの該再生組成物を該工程(d)に送る前にストリッピングすることを特徴とする請求項37記載の方法。
- 請求項38記載の方法で生成する分解ガソリン製品。
- 請求項38記載の方法で生成するディーゼル燃料製品。
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IN2006DE00352A (ja) | 2007-08-17 |
BRPI0412823A (pt) | 2006-09-26 |
KR20060034714A (ko) | 2006-04-24 |
CA2533485C (en) | 2010-04-20 |
US20080039318A1 (en) | 2008-02-14 |
CN100438970C (zh) | 2008-12-03 |
RU2006105627A (ru) | 2006-08-27 |
AU2004260098A1 (en) | 2005-02-03 |
JP4938448B2 (ja) | 2012-05-23 |
WO2005010124A3 (en) | 2005-07-28 |
KR101104440B1 (ko) | 2012-01-12 |
AU2004260098B2 (en) | 2009-10-08 |
CA2533485A1 (en) | 2005-02-03 |
EP1673164A2 (en) | 2006-06-28 |
EP1673164A4 (en) | 2010-06-09 |
CN1856359A (zh) | 2006-11-01 |
US7846867B2 (en) | 2010-12-07 |
ZA200600610B (en) | 2007-05-30 |
NO20060874L (no) | 2006-02-22 |
MXPA06000736A (es) | 2006-03-30 |
US7351328B2 (en) | 2008-04-01 |
BRPI0412823B1 (pt) | 2015-06-02 |
US20050020445A1 (en) | 2005-01-27 |
WO2005010124A2 (en) | 2005-02-03 |
RU2336126C2 (ru) | 2008-10-20 |
MX262567B (es) | 2008-11-27 |
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