WO2000072967A1 - PRETREATMENT OF A Pt/Sn-BASED CATALYST - Google Patents
PRETREATMENT OF A Pt/Sn-BASED CATALYST Download PDFInfo
- Publication number
- WO2000072967A1 WO2000072967A1 PCT/NO2000/000175 NO0000175W WO0072967A1 WO 2000072967 A1 WO2000072967 A1 WO 2000072967A1 NO 0000175 W NO0000175 W NO 0000175W WO 0072967 A1 WO0072967 A1 WO 0072967A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- catalyst
- dehydrogenation
- oxidation
- reduction
- effected
- Prior art date
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C5/00—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms
- C07C5/32—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by dehydrogenation with formation of free hydrogen
- C07C5/321—Catalytic processes
- C07C5/324—Catalytic processes with metals
- C07C5/325—Catalytic processes with metals of the platinum group
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/12—Oxidising
- B01J37/14—Oxidising with gases containing free oxygen
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
- B01J37/18—Reducing with gases containing free hydrogen
-
- 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
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/04—Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst
- B01J38/12—Treating with free oxygen-containing gas
-
- 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
- B01J23/007—Mixed salts
-
- 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
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/62—Platinum group metals with gallium, indium, thallium, germanium, tin or lead
- B01J23/622—Platinum group metals with gallium, indium, thallium, germanium, tin or lead with germanium, tin or lead
- B01J23/626—Platinum group metals with gallium, indium, thallium, germanium, tin or lead with germanium, tin or lead with tin
-
- 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
- B01J23/90—Regeneration or reactivation
- B01J23/96—Regeneration or reactivation of catalysts comprising metals, oxides or hydroxides of the noble metals
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2521/00—Catalysts comprising the elements, oxides or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium or hafnium
- C07C2521/02—Boron or aluminium; Oxides or hydroxides thereof
- C07C2521/04—Alumina
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2521/00—Catalysts comprising the elements, oxides or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium or hafnium
- C07C2521/10—Magnesium; Oxides or hydroxides thereof
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2523/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00
- C07C2523/14—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of germanium, tin or lead
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2523/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00
- C07C2523/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of noble metals
- C07C2523/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of noble metals of the platinum group metals
- C07C2523/42—Platinum
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Definitions
- the present invention relates to a process of a pre-treatment activation of a Pt/Sn based catalyst and a catalyst activated by such a pre-treatment.
- catalysts are permanently deactivated due to poisoning and sintering and have to be replaced at given time intervals, generally after 1 to 5 years in operation depending on feedstreams and reaction conditions.
- the catalysts have to be treated according to a special pre-treatment procedure before the catalyst can operate at optimum performance (see e.s. WO 92/06784 where conditions for optimal reduction of a cobalt catalyst is described).
- WO 92/06784 where conditions for optimal reduction of a cobalt catalyst is described.
- catalysts have to be replaced at short intervals it is of major importance to reduce the pre-treatment time.
- the lifetime of a typical Pt/Sn based dehydrogenation catalyst is up to 3 years.
- the catalyst used in the STAR process has an expected lifetime of 1 to 2 years in commercial operation, while the catalyst used in the Oleflex process (Pt/Sn/Cs on Al 2 0 3 ) has an expected lifetime of 1 to 3 years [Catalytica (1993)].
- Significant losses in alkene production can be foreseen if a long activation period is needed after each catalyst replacement.
- Such catalysts, or variations thereof, can also be used for a number of chemical processes that involve mainly or partly dehydrogenation or hydrogenation steps. A long activation period is also a disadvantage connected to unexpected stops and experimental development in the laboratory.
- the alkane dehydrogenation is effected at temperatures in the range of 500 to 700 °C .
- the oxidation/regeneration is preferable effected at temperatures in the range of 500 to 700 °C .
- Equally the reduction by H 2 is preferable effected in the range of 500 to 700 °C .
- the chemical process is dehydrogenation performed on a lower alkane.
- More preferably propane is dehydrogenated.
- the oxidation is effected by a gaseous O 2 /N 2 mixture gradually increasing the O 2 content.
- the final part of the oxidation is effected in air.
- this is preferably effected in H 2 in a temperature range of 500 to 700 °C .
- dehydrogenation time this is less than half of the dehydrogenation time during normal dehydrogenation process conditions.
- a typical dehydrogenation time is 2 hours.
- the reduction in H 2 is particularly effected for about 2 hours.
- a further object of the present invention is a catalyst activated by the pre-treatment set forth above.
- the objective of this invention is to define a pretreatment procedure which decreases the time required to reach an optimum conversion level in an alkane dehydrogenation unit, using a Pt/Sn/Mg(AI)O catalyst described in patent NO 179131.
- a pre-treatment procedure which led to an optimum dehydrogenation activity of a Pt/Sn/Mg(AI)0 catalyst obtained by impregnating Pt and Sn on a pre-calcinated Mg(AI)O carrier material.
- the pre-treatment procedure used in the previous invention consisted of in situ reduction, followed by oxidation and a new reduction period (ROR).
- the ROR pre-treatment procedure did not lead to an optimum dehydrogenation activity.
- the conversion level after the first regeneration was higher than the initial conversion level after the ROR. After the next test cycle the conversion level was even higher.
- a stable catalyst performance was not obtained before after 300h on stream, when the catalyst had been subjected to 9 cycles consisting of a dehydrogenation period followed by regeneration and reduction.
- a pre-treatment procedure for the catalyst that dramatically decreased the required time to obtain optimum conversion level in dehydrogenation of propane was developed.
- the catalyst was prepared according to a slightly modification of the procedure described in patent NO 179131 , using a water based acidic solution in the deposition of platinum and tin on hydrotalcite or precalcined hydrotalcite.
- the catalysts used in the examples have an Mg/AI-ratio of 4.8.
- the content of platinum and tin are ca. 0.25 and 0.5 wt% respectively.
- the catalyst was calcinated at 560°C after the impregnation.
- the catalyst was pressed to tablets, crushed and sieved to a pellet size of 0.64-1.0 mm prior to testing.
- the reactor temperature was regulated to 600°C at a distance of 1/3 of the total catalyst bed-length from the top of the catalyst bed, while the temperature at the bottom of the catalyst bed, measured at a distance of approximately 1/3 of catalyst bed length from the bottom of the catalyst bed, was in the range of 590 to 615°C.
- the GHSV was 1000h "1 based on propane, and the reaction gas contained 4.5% hydrogen, 32% propane and rest steam on mole basis.
- the dehydrogenation periods usually lasted approximately 20 hours and were followed by a regeneration of the catalyst.
- the conversion levels were calculated from on-line GC analysis. The analysis were taken with approximately 1 hours intervals. The conversion levels presented were obtained after 5h in the dehydrogenation period.
- the regeneration of the catalyst was done by burning of the formed coke using air diluted with nitrogen.
- the content of oxygen was initially reduced to approximately 2% and was stepwise increased to a final level of 21 % where pure air was used.
- the regeneration period was followed by catalyst reduction using hydrogen. Both the regeneration and the reduction of the catalyst were done at 600°C.
- the catalyst was subjected to a pre-treatment procedure consisting of the following steps:
- the catalyst was subjected to a pre-treatment procedure consisting of the following steps:
- the catalyst is first pre-treated according to the ROR-procedure described in Example 1.
- Step 2 to 5 was repeated 9 times, when no further increase in the conversion level of propane in the PDH period was observed.
- the results from the subsequent propane dehydrogenation test are shown in Figure 1 and Table 1.
- the catalyst was subjected to a pre-treatment procedure consisting of the following steps::
- Step 3 to 5 are repeated 12 times.
- the results from the following PDH conversion tests are shown in Figure 1 and Table 1.
- the catalyst was subjected to a pre-treatment procedure consisting of the following steps:
- the catalyst is first pre-treated according to the ROR-procedure described in Example 1.
- Step 2 to 5 was repeated 6 times, when no further increase in the conversion level of propane in the PDH period was observed.
- the results from the subsequent propane dehydrogenation tests are shown in Figure 1 and Table 1.
- Example 5 R-(PDH-OR)*X
- the catalyst was subjected to a pre-treatment procedure consisting of the following steps:
- Step 3 to 6 were repeated 5 times, when it was found no further increase in conversion level in the PDH period (Step 3) are observed.
- the results from the subsequent propane dehydrogenation test are shown in Figure 1 and Table 1.
- the catalyst was subjected to a pre-treatment procedure consisting of the following steps:
- Oxidation/regeneration using an O 2 /N 2 -mixture with a gradually increasing 0 2 content. (1. 5. and 10%) 1 h on each step. Different O 2 content was obtained by diluting air with N 2 . Total flow:84ml/min. T 600°C. 5. Oxidation in air. 80ml/min., 600°C, 1h.
- Step 3 to 6 are repeated 6 times, when it was observed no further increase in conversion level in the PDH period (Step 3).
- the results from the subsequent propane dehydrogenation test are shown in Figure 1 and Table 1.
- Table 1 Normalised conversion of propane with time on stream. The conversion level are obtained 5 hours after finishing the regeneration/reduction period. The results are also shown in Figure 1.
- the conversion level data for Example 1 to Example 6 are all given as normalised values, where the stabilised conversion level which are obtained on the completely pre-treated catalyst is given the value 100%.
- a typical example of the obtained conversion level of propane to propene is given in Table 2. Similar conversion levels are also obtained in the remaining examples. However, the conversion level shows small variation due to minor changes in the reaction conditions as for instance the temperature profile in the reactor and different partial pressure in the gases entering the reactor.
- a pre-treatment procedure which included the aforementioned ROR procedure followed by several cycles consisting of a short dehydrogenation period (2h, at 600°) followed by regeneration (oxidation) and reduction in hydrogen (Example 2) reduced the pre-treatment time to approximately 80h.
- the initial ROR pre-treatment could also be excluded using this kind of catalyst pre-treatment.
- a pre-treatment time of 40h was obtained using a pre-treatment consisting of an initial reduction followed by 5 cycles consisting of dehydrogenation, regeneration and reduction. A detailed description of this procedure is given in example 5.
- the catalyst operate at a conversion level of 90% of the optimum conversion level. Within two conventional 20 hours dehydrogenation periods at 600°C, the catalyst performance was at an optimum level.
- the catalyst was subjected to a pre-treatment procedure consisting of the following steps:
- the catalyst was subjected to a pre-treatment procedure consisting of the following steps:
- the catalyst was subjected to a pre-treatment procedure consisting of the following steps: 5 7. Oxidation/regeneration of the catalyst from example 8 using an 0 2 /N 2 -mixture with a gradually increasing 0 2 content. (1. 5. and 10%) 1h on each step.
- the activation period for the Pt/Sn/Mg(AI)O dehydrogenation catalyst is reduced from 300h to approximately 50 h by using the pre-treatment procedure developed in the present invention.
- the pre-treatment procedure consists of an initial reduction of the catalyst using hydrogen, followed by several cycles which includes a short
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Catalysts (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
Claims
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP00931745A EP1206319A1 (en) | 1999-05-28 | 2000-05-26 | PRETREATMENT OF A Pt/Sn-BASED CATALYST |
AU49575/00A AU4957500A (en) | 1999-05-28 | 2000-05-26 | Pretreatment of a pt/sn-based catalyst |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
NO19992582A NO310807B1 (en) | 1999-05-28 | 1999-05-28 | Catalyst pretreatment |
NO19992582 | 1999-05-28 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2000072967A1 true WO2000072967A1 (en) | 2000-12-07 |
Family
ID=19903377
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/NO2000/000175 WO2000072967A1 (en) | 1999-05-28 | 2000-05-26 | PRETREATMENT OF A Pt/Sn-BASED CATALYST |
Country Status (4)
Country | Link |
---|---|
EP (1) | EP1206319A1 (en) |
AU (1) | AU4957500A (en) |
NO (1) | NO310807B1 (en) |
WO (1) | WO2000072967A1 (en) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2002045852A2 (en) * | 2000-12-04 | 2002-06-13 | Basf Aktiengesellschaft | Regeneration of a dehydrogenation catalyst |
CN104248968A (en) * | 2013-06-28 | 2014-12-31 | 中国石油化工股份有限公司 | Catalyst for preparation of propylene by direct dehydrogenation of propane and preparation method thereof |
CN111686709A (en) * | 2020-01-23 | 2020-09-22 | 中国科学院大连化学物理研究所 | Propane dehydrogenation propylene supported catalyst with specific pore structure and preparation method thereof |
CN114570364A (en) * | 2022-03-28 | 2022-06-03 | 福州大学 | Pretreatment method of Pt-based catalyst for preparing propylene by propane dehydrogenation |
WO2023018536A1 (en) * | 2021-08-13 | 2023-02-16 | Exxonmobil Chemical Patents Inc. | Processes for dehydrogenating alkanes and alkyl aromatic hydrocarbons |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3842139A (en) * | 1973-03-12 | 1974-10-15 | Gulf Research Development Co | Dehydrogenation of paraffins over a platinum magnesium aluminate spinel |
US4849092A (en) * | 1986-08-25 | 1989-07-18 | Institut Francais Du Petrole | Process for regenerating a hydrocarbon hydroconversion catalyst |
EP0557982A2 (en) * | 1992-02-26 | 1993-09-01 | Phillips Petroleum Company | Alkane dehydrogenation |
WO1996019424A1 (en) * | 1994-12-22 | 1996-06-27 | Den Norske Stats Oljeselskap A.S | A reactor for catalytic dehydrogenation of hydrocarbons with selective oxidation of hydrogen |
US5817596A (en) * | 1993-06-14 | 1998-10-06 | Den Norske Stats Oljeselkap A.S. | Catalyst, and processes for dehydrogenating dehydrogenatable hydrocarbons |
-
1999
- 1999-05-28 NO NO19992582A patent/NO310807B1/en unknown
-
2000
- 2000-05-26 AU AU49575/00A patent/AU4957500A/en not_active Abandoned
- 2000-05-26 EP EP00931745A patent/EP1206319A1/en not_active Withdrawn
- 2000-05-26 WO PCT/NO2000/000175 patent/WO2000072967A1/en not_active Application Discontinuation
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3842139A (en) * | 1973-03-12 | 1974-10-15 | Gulf Research Development Co | Dehydrogenation of paraffins over a platinum magnesium aluminate spinel |
US4849092A (en) * | 1986-08-25 | 1989-07-18 | Institut Francais Du Petrole | Process for regenerating a hydrocarbon hydroconversion catalyst |
EP0557982A2 (en) * | 1992-02-26 | 1993-09-01 | Phillips Petroleum Company | Alkane dehydrogenation |
US5817596A (en) * | 1993-06-14 | 1998-10-06 | Den Norske Stats Oljeselkap A.S. | Catalyst, and processes for dehydrogenating dehydrogenatable hydrocarbons |
WO1996019424A1 (en) * | 1994-12-22 | 1996-06-27 | Den Norske Stats Oljeselskap A.S | A reactor for catalytic dehydrogenation of hydrocarbons with selective oxidation of hydrogen |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2002045852A2 (en) * | 2000-12-04 | 2002-06-13 | Basf Aktiengesellschaft | Regeneration of a dehydrogenation catalyst |
WO2002045852A3 (en) * | 2000-12-04 | 2002-09-06 | Basf Ag | Regeneration of a dehydrogenation catalyst |
US6916756B2 (en) | 2000-12-04 | 2005-07-12 | Basf Ag | Regeneration of a dehydrogenation catalyst |
CN104248968A (en) * | 2013-06-28 | 2014-12-31 | 中国石油化工股份有限公司 | Catalyst for preparation of propylene by direct dehydrogenation of propane and preparation method thereof |
CN111686709A (en) * | 2020-01-23 | 2020-09-22 | 中国科学院大连化学物理研究所 | Propane dehydrogenation propylene supported catalyst with specific pore structure and preparation method thereof |
CN111686709B (en) * | 2020-01-23 | 2021-06-01 | 中国科学院大连化学物理研究所 | Propane dehydrogenation propylene supported catalyst with specific pore structure and preparation method thereof |
WO2023018536A1 (en) * | 2021-08-13 | 2023-02-16 | Exxonmobil Chemical Patents Inc. | Processes for dehydrogenating alkanes and alkyl aromatic hydrocarbons |
CN114570364A (en) * | 2022-03-28 | 2022-06-03 | 福州大学 | Pretreatment method of Pt-based catalyst for preparing propylene by propane dehydrogenation |
Also Published As
Publication number | Publication date |
---|---|
AU4957500A (en) | 2000-12-18 |
NO992582L (en) | 2000-11-29 |
EP1206319A1 (en) | 2002-05-22 |
NO310807B1 (en) | 2001-09-03 |
NO992582D0 (en) | 1999-05-28 |
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