JP2022506608A - 特定形状の触媒を用いる固定床接触改質方法 - Google Patents
特定形状の触媒を用いる固定床接触改質方法 Download PDFInfo
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G35/00—Reforming naphtha
- C10G35/04—Catalytic reforming
- C10G35/06—Catalytic reforming characterised by the catalyst used
- C10G35/085—Catalytic reforming characterised by the catalyst used containing platinum group metals or compounds thereof
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/02—Boron or aluminium; Oxides or hydroxides thereof
- B01J21/04—Alumina
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/42—Platinum
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/128—Halogens; Compounds thereof with iron group metals or platinum group metals
- B01J27/13—Platinum group metals
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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Abstract
Description
接触改質により石油留分の評価ランクを向上させることが可能になる。接触改質ではリフォーメートが生じ、これは主に、C5+化合物(少なくとも5個の炭素原子を含有する化合物)で構成される。
接触改質方法ではまた、水素リッチなガス、燃焼ガス(C1-C2化合物によって構成される。)、及び液化ガス(C3-C4化合物によって構成される。)が生じる。最終的にはコークスが生じ、これは、とりわけ芳香環の縮合によるものであって、固体、即ち、触媒の活性部位上に析出する炭素リッチな生成物を形成する。
C1-C4化合物(C4とも称される。)とコークスとを生じさせる反応は、リフォーメート収率及び触媒の安定性に対して、悪影響を与える。触媒の強い活性は、可能な限り高い選択性と結び付けられなければならない。即ち、1~4個の炭素原子を含有する軽質な生成物(C4)に至る分解反応は、制限されなければならない。
しかしながら、今日にいたるまで、触媒の形態により、その安定性がもたらされるという利点に関して、その優越性が明らかにされてこなかった。驚くべきことに、出願人は、テトラローブ状の押出物、即ち、四つ葉状の断面を有する押出物の形態の触媒を用いると、固定床改質方法において、円柱状の触媒、或いは他の形状、特にトリローブ状の押出物形状を有する触媒の性能と比較して、活性に関して良好な性能を保持しつつ、安定性に関して向上した性能を得ることが可能になることを発見した。
以降、化学元素の族は、CAS分類(CRC Handbook of Chemistry and Physics, CRC Press, Editor in Chief D.R. Lide, 81st edition, 2000-2001)に従って与えられる。例えば、CAS分類によるIB族は、新IUPAC分類による第11列の金属に対応する。
本発明を実施するべく、異なる実施形態を示す。それらは単独で或いは互いに組み合わせて用いてよい。また、組合せには、何ら制限がない。
本発明による方法に関連して用いられる、炭化水素をベースとする供給原料は、n-パラフィン系炭化水素、イソパラフィン系炭化水素、ナフテン系炭化水素及び芳香族系炭化水素を含有しており、それらは一分子当たり5~12個の炭素原子を含む。かかる供給原料は、就中、密度と、重量による組成とによって定義される。
多孔質担体は、押出物の形態である。その断面形状はテトラローブを含み、好ましくはテトラローブよりなる。押出物の断面(押出の軸に対して垂直)は対称ローブであってよい。限定されない一例として、図2a及び2bは、対称テトラローブ状の押出物(四つのローブは同一形状である。)を示す。押出物の断面(押出の軸に対して垂直)は、非対称ローブ状であってよい。図3a~4bは、非対称ローブを有するテトラローブ状押出物(即ち、少なくとも一のローブの形状が他のローブとは異なる。)の一例を示すが、非限定的である。
一実施形態によると、アルミナをベースとする多孔質担体は、アルミニウムアルコキシドの加水分解によって得られるベーマイト粉末から調製される。アルミニウムアルコキシドの加水分解によって調製されるベーマイト粉末の例は、仏国特許FR1391644又は米国特許US5,055,019に見いだせる。このベーマイト粉末は、例えばコンパウンディング及び押出によって成形される。1回以上の熱処理を施すことにより、アルミナが得られるに至る。好ましくは、熱処理は、乾燥空気中、540℃~800℃の温度下での焼成によって行う。
別の実施形態によると、アルミナをベースとする多孔質担体は、アルミニウム塩からの沈殿反応によって得られるベーマイト粉末から調製される。ベーマイト粉末は、例えば、アルミニウム塩の塩基性水溶液及び/又は酸性水溶液を沈殿させることにより得てもよい。沈殿は、pH調整や、当業者に知られた任意の他の方法によって生じさせ得る。得られたゲルは、例えばコンパウンディング-押出によって成形する。次いで、成形物に対して一連の熱処理を行うことにより、アルミナを得るに至る。この方法は、“Handbook of Porous Solids”(F. Schueth, K.S.W. Sing J. Weitkamp, Wiley-VCH, Weinheim, Germany, 2002)の、“Alumina”(P. Euzen, P. Raybaud, X. Krokidis, H. Toulhoat, J.L. Le Loarer, J.P. Jolivet and C. Froidefond著)と題する章にも記載されている。
1) アルミナをベースとする多孔質担体を調製する;
2) 場合により、前記多孔質アルミナ担体に、塩素前駆体を含有する溶液を含浸させる;
3) 工程1)又は2)で得られた前記アルミナ担体に、少なくとも一種の白金前駆体の少なくとも一種の溶液を含浸させる;
4) 先行する工程で得られた前記担体に、少なくとも一種のプロモータ金属前駆体の少なくとも一種の溶液を含浸させる;
5) 先行する工程で得られた前記担体に、少なくとも一種のドーパントの少なくとも一種の溶液を含浸させる(この工程は任意である);
6) 工程4)又は5)で得られた前記担体を焼成して、酸化物形態の触媒を得る;
7) 先行する工程で得られた酸化物形態の触媒を、高純度の水素中、例えば100~600℃の温度で、30分~6時間にわたり還元して、還元された触媒を得る;
8) 先行する工程で得られた、還元された触媒を、少なくとも一種の、硫黄をベースとする前駆体と、例えば450°~580℃の温度で少なくとも1時間にわたり接触させる。
アルミニウムアルコキシドの加水分解反応に由来する市販のベーマイト粉末を水と混合し、次いで直径2mmの円柱状ダイに通して押出を行い、740℃で焼成した。この担体20gを、0.2gの塩素を含む塩酸の水溶液100cm3と3時間にわたり接触させた。次いで、含浸溶液を取り除いた。このようにして得られた固体を、120℃で1時間にわたり乾燥させ、次いで450℃で2時間にわたり焼成した。次いで白金0.07gを含むヘキサクロロ白金酸の水溶液100cm3を、先行する工程の終わりに得られた担体と、3時間にわたり接触させた。最終触媒において塩素含有量を1.1重量%とするために、塩酸の量を調整した。次いで、含浸溶液を取り除いた。次いで過レニウム酸アンモニウムの形態で導入されたレニウム0.09gを含む水溶液60cm3を、先行する工程の終わりに得られた担体と、3時間にわたり接触させた。次いで、含浸溶液を取り除いた。このようにして得られた触媒を、120℃で1時間にわたり乾燥させ、520℃で2時間にわたり焼成し、次いで520℃で2時間にわたり水素中で還元した。次いで触媒を、520℃で9分間にわたり、水素/H2S混合物(1体積%のH2S)で硫化した(流量:標準の温度及び圧力の条件下、0.15リットル/分)。
最終触媒は、触媒の全重量に対して、0.25重量%の白金、0.25重量%のレニウム、及び1.1重量%の塩素を含んでいた。
押出をトリローブ状のダイを通して行うとともに、最大直径「D」を2mmにしたことを除き、実施例1と同一の手順に従い、触媒を調製した。
押出を(図2aに示すような)対称なテトラローブ状のダイを通して行うとともに、最大直径「D」を2mmにしたことを除き、実施例1と同一の手順に従い、触媒を調製した。
以下の特徴を有する、石油の蒸留に由来するナフサタイプの、炭化水素をベースとする供給原料の転化について、触媒A~Cを試験した:
15℃での密度: 0.761kg/dm3
パラフィン/ナフテン/芳香族: 44.1/38.7/17.2体積%
全圧: 1.2MPa
供給原料の流量: 時間当たりかつ触媒の重量(kg)当たり4.8kg
リサーチオクタン価: 102
炭化水素をベースとする供給原料に対する、再循環された水素のモル比: 2.5
Claims (15)
- 固定床を用いる、炭化水素系供給原料の接触改質方法であって、
炭化水素系供給原料はn-パラフィン系、ナフテン系及び芳香族系の炭化水素であって一分子当たり5~12個の炭素原子を含み、
温度が400~700℃であり、かつ圧力が0.1~4MPaであり、かつ単位時間当たり及び触媒単位質量当たりに処理される供給原料の質量流量が0.1~10h-1であり、
前記供給原料を、少なくとも白金と、レニウム及びイリジウムからなる群より選択される少なくとも一種のプロモータ金属と、フッ素、塩素、臭素及びヨウ素からなる群より選択される少なくとも一種のハロゲンと、押出物の形態の多孔質アルミナ担体とを含む触媒と接触させることにより行い、
前記押出物の長さ「l」が1~10mmであり、断面がテトラローブを含み、かつ前記押出物の断面の最大直径「D」が1~3mmであることを特徴とする、
方法。 - 前記押出物の断面の最大直径「D」が1.1~2.2mmである、請求項1に記載の方法。
- 前記押出物の長さ「l」が2~7mmである、請求項1又は2に記載の方法。
- 前記押出物の断面が対称ローブ形状を有する、請求項1~3のいずれか1つに記載の方法。
- 前記押出物の断面が非対称ローブ形状を有する、請求項1~3のいずれか1つに記載の方法。
- 前記押出物が軸状の押出物である、請求項1~5のいずれか1つに記載の方法。
- 前記押出が、1mm当たり10~180°の回転ピッチを有する螺旋状の押出物である、請求項1~5のいずれか1つに記載の方法。
- 前記触媒の白金含有量が、触媒の全重量に対して0.02~2重量%である、請求項1~7のいずれか1つに記載の方法。
- 前記触媒のレニウム又はイリジウムの含有量が、触媒の全重量に対して0.02~10重量%である、請求項1~8のいずれか1つに記載の方法。
- 前記触媒がまた、ガリウム、ゲルマニウム、インジウム、スズ、アンチモン、タリウム、鉛、ビスマス、チタン、クロム、マンガン、モリブデン、タングステン、ロジウム、亜鉛、及びリンからなる群より選択される、少なくとも一種のドーパントを含む、請求項1~9のいずれか1つに記載の方法。
- 前記ドーパントの含有量が、触媒の重量に対して0.01~2重量%である、請求項10に記載の方法。
- 前記触媒のハロゲン含有量が、触媒の全重量に対して0.1~15重量%である、請求項1~11のいずれか1つに記載の方法。
- ハロゲンは塩素であり、その含有量が、触媒の全重量に対して0.5~2重量%である、請求項1~12のいずれか1つに記載の方法。
- 前記多孔質担体の比表面積が150~400m2/gである、請求項1~13のいずれか1つに記載の方法。
- 10ミクロン未満の直径を有する担体の細孔容積が0.2~1cm3/gであり、メソ細孔の平均直径が5~20nmである、請求項1~14のいずれか1つに記載の方法。
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2018
- 2018-11-08 FR FR1871420A patent/FR3088338B1/fr active Active
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2019
- 2019-10-21 BR BR112021004765-4A patent/BR112021004765A2/pt unknown
- 2019-10-21 US US17/292,158 patent/US20210388272A1/en active Pending
- 2019-10-21 KR KR1020217013125A patent/KR20210076028A/ko unknown
- 2019-10-21 JP JP2021524050A patent/JP2022506608A/ja active Pending
- 2019-10-21 EP EP19787286.4A patent/EP3877084A1/fr active Pending
- 2019-10-21 WO PCT/EP2019/078574 patent/WO2020094378A1/fr unknown
- 2019-10-21 CN CN201980073277.8A patent/CN113242765A/zh active Pending
Also Published As
Publication number | Publication date |
---|---|
KR20210076028A (ko) | 2021-06-23 |
FR3088338B1 (fr) | 2021-10-29 |
US20210388272A1 (en) | 2021-12-16 |
BR112021004765A2 (pt) | 2021-08-03 |
WO2020094378A1 (fr) | 2020-05-14 |
CN113242765A (zh) | 2021-08-10 |
EP3877084A1 (fr) | 2021-09-15 |
FR3088338A1 (fr) | 2020-05-15 |
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