WO2002026628A1 - Procede pour la production selective d'olefines c3 selon un procede de craquage catalytique fluide - Google Patents
Procede pour la production selective d'olefines c3 selon un procede de craquage catalytique fluide Download PDFInfo
- Publication number
- WO2002026628A1 WO2002026628A1 PCT/US2001/016036 US0116036W WO0226628A1 WO 2002026628 A1 WO2002026628 A1 WO 2002026628A1 US 0116036 W US0116036 W US 0116036W WO 0226628 A1 WO0226628 A1 WO 0226628A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- zone
- catalyst
- olefins
- stream
- propylene
- Prior art date
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F10/00—Homopolymers and copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F110/00—Homopolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F110/04—Monomers containing three or four carbon atoms
- C08F110/06—Propene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F210/00—Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F210/04—Monomers containing three or four carbon atoms
- C08F210/06—Propene
-
- 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
- C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
- C10G2400/20—C2-C4 olefins
-
- 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 for producing propylene from a naphtha stream.
- a problem inherent in producing olefins products using FCC units is that the process depends on a specific catalyst balance to maximize production of light olefins while also achieving high conversion of the 650°F + ( ⁇ 340°C) feed components.
- olefin selectivity is generally low because of undesirable side reactions, such as extensive cracking, isomerization, aromatization and hydrogen transfer reactions. Light saturated gases produced from undesirable side reactions result in increased costs to recover the desirable light olefins. Therefore, it is desirable to maximize olefin production in a process that allows a high degree of control over the selectivity of C 3 and C 4 olefins.
- One embodiment of the present invention is a process for producing polypropylene comprising the steps of (a) feeding a naphtha stream comprising from about 10 to 30 wt.% paraffins and between about 15 to 70 wt.% olefins and co-feeding a stream comprising C 4 olefins to a process unit comprising a reaction zone, a stripping zone, a catalyst regeneration zone, and a fractionation zone; (b) contacting the naphtha stream with a fluidized bed of catalyst in the reaction zone to form a cracked product, the catalyst comprising a zeolite having an average pore diameter of less than about 0.7 nm and wherein the reaction zone is operated at a temperature from about 500° to 650°C, a hydrocarbon partial pressure of 10 to
- the catalyst is a ZSM-5 type catalyst.
- a C 5 fraction rich in olefins is also recycled.
- the feedstock contains about 10 to 30 wt. % paraffins, and from about 20 to 70 wt. % olefins.
- reaction zone is operated at a temperature from about 525°C to about 600°C.
- Feedstreams that are suitable for producing the relatively high C 2 , C 3 , and C 4 olefin yields are those streams boiling in the naphtha range containing from about 5 wt. % to about 35 wt. %, preferably from about 10 wt. % to about 30 wt. %, and more preferably from about 10 to 25 wt. % paraffins, and from about 15 wt. %, preferably from about 20 wt. % to about 70 wt. % olefins.
- the feed may also contain naphthenes and aromatics.
- Naphtha boiling range streams are typically those having a boiling range from about 65°F to about 430°F (about 18°C to about 225°C), preferably from about 65°F to about 300°F (about 18°C to about 150°C).
- the naphtha can be a thermally cracked or a catalytically-cracked naphtha.
- the naphtha streams can be derived from the fluid catalytic cracking (FCC) of gas oils and resids, or they can be derived from delayed or fluid coking of resids.
- FCC fluid catalytic cracking
- the naphtha streams used in the practice of the present invention derive from the fluid catalytic cracking of gas oils and resids.
- FCC naphthas are typically rich in olefins and/or diolefins and relatively lean in paraffins. It is within the scope of the instant invention to feed or co-feed other olefinic streams that are not catalytically- or thermally-cracked naphthas into said reaction zone with the primary feed. It is believed that this will increase the yield of propylene.
- a C 4 olefin stream containing n-butenes is co-fed with the naphtha feed.
- the C 4 olefin stream may come from suitable sources such as conventional FCC units, coker units, steam crackers and other process units that produce C 4 olefins streams that can be recycled to the cracking unit.
- the C olefin stream may be a raffinate from a methyl-tert-butyl-ether (MTBE) process.
- MTBE units typically feed a mixture of methanol and C 4 olefins. Only the iso-butylene reacts with the methanol to yield MTBE, leaving a significant amount of C 4 olefins, including n- butenes, in the MTBE raffinate.
- the C 4 olefin stream preferably comprises at least about 75 wt.% n- butenes, more preferably greater than about 90 wt.% n-butenes. Streams containing lower amounts of n-butenes are also acceptable, such as where a stream containing a significant amount of diolefins, such as butadiene, is employed.
- the C 4 olefin stream is injected into the reaction zone along with the naphtha feed, the C 4 olefins undergo rapid disproportionation reactions with other olefins in the naphtha feed, followed by cracking reactions. These reactions increase propylene yields.
- the process of the present invention is performed in a process unit comprising a reaction zone, a stripping zone, a catalyst regeneration zone, and a fractionation zone.
- the naphtha feed is fed into the reaction zone where it contacts a source of hot, regenerated catalyst.
- the hot catalyst vaporizes and cracks the feed at a temperature from about 500°C to about 650°C, preferably from about 525°C to about 600°C.
- the cracking reaction deposits coke on the catalyst, thereby deactivating the catalyst.
- the cracked products are separated from the coked catalyst and sent to a fractionator.
- the coked catalyst passes through the stripping zone where a stripping medium, such as steam, strips volatiles from the catalyst particles.
- the stripping can be preformed under low-severity conditions to retain a greater fraction of adsorbed hydrocarbons for heat balance.
- the stripped catalyst is then passed to the regeneration zone where it is regenerated by burning coke on the catalyst in the presence of an oxygen containing gas, preferably air. Decoking restores catalyst activity and simultaneously heats the catalyst to a temperature from about 650°C to about 750°C.
- the hot regenerated catalyst is then recycled to the reaction zone to react with fresh naphtha feed. Flue gas formed by burning coke in the regenerator may be treated for removal of particulates and for conversion of carbon monoxide.
- the cracked products from the reaction zone are sent to a fractionation zone where various products are recovered, particularly a C 3 fraction, a C 4 fraction, and optionally a C 5 fraction.
- the C 4 fraction and the C 5 fraction will typically be rich in olefins.
- One or both of these fractions can be recycled to the reactor. They can be recycled to either the main section of the reactor, or a riser section, or a stripping section. It is preferred that they be recycled to the upper part of the stripping section, or stripping zone. Recycling one or both of these fractions will convert at least a portion of these olefins to propylene.
- C 4 olefin stream may also be desirable to inject a C 4 olefin stream into the stripper section.
- a C 4 olefin stream (not to be confused with a C 4 fraction recycled from the cracked products of the cracking process) would be derived from one or more suitable sources such as conventional FCC units, coker units, steam crackers and other process units that produce C 4 olefins streams that can be recycled to the cracking unit.
- the C 4 olefin stream may be a raffinate from a methyl-tert-butyl-ether (MTBE) process as previously described.
- MTBE methyl-tert-butyl-ether
- the C olefin stream injected into the stripper section also preferably comprises at least about 75 wt.% n-butenes, more preferably greater than about 90 wt.% n-butenes.
- Streams containing lower amounts of n-butenes are also acceptable, such as where a stream containing a significant amount of diolefins, such as butadiene, is employed.
- the reaction zone is operated at process conditions that will maximize C 2 to C 4 olefins (particularly propylene) selectivity with relatively high conversion of C 5 + olefins.
- Suitable catalysts used with the present invention contain a crystalline zeolite having an average pore diameter less than about 0.7 nanometers
- said crystalline zeolite comprising from about 10 wt. % to about 50 wt. % of the total fluidized catalyst composition. It is preferred that the crystalline zeolite be selected from the family of medium-pore size ( ⁇ 0.7 nm) crystalline aluminosilicates, otherwise referred to as zeolites. Of particular interest are the medium-pore zeolites with a silica to alumina molar ratio of less than about 75 : 1 , preferably less than about 50:1, and more preferably less than about 40:1, although some embodiments may incorporate a silica to alumina ratio greater than 40:1.
- the pore diameter also referred to as effective pore diameter, is measured using standard adsorption techniques and hydrocarbonaceous compounds of known minimum kinetic diameters. See Breck, Zeolite Molecular Sieves, 1974 and Anderson et al., J. Catalysis 58, 114 (1979), both of which are incorporated herein by reference.
- Medium-pore size zeolites that can be used in the practice of the present invention are described in "Atlas of Zeolite Structure Types", eds. W. H. Meier and D. H. Olson, Butterworth-Heineman, Third Edition, 1992, which is hereby incorporated by reference.
- the medium-pore size zeolites generally have a pore size from about 5A, to about 7A and include for example, MFI, MFS, MEL, MTW, EUO, MTT, HEU, FER, and TON structure type zeolites (IUPAC Commission of Zeolite Nomenclature).
- Non-limiting examples of such medium- pore size zeolites include ZSM-5, ZSM-12, ZSM-22, ZSM-23, ZSM-34, ZSM- 35, ZSM-38, ZSM-48, ZSM-50, silicalite, and silicalite 2.
- ZSM-5 which is described in U.S. Patent Nos. 3,702,886 and 3,770,614.
- ZSM-11 is described in U.S. Patent No. 3,709,979; ZSM-12 in U.S. Patent No. 3,832,449; ZSM-21 and ZSM-38 in U.S. Patent No. 3,948,758; ZSM-23 in U.S. Patent No. 4,076,842; and ZSM-35 in U.S. Patent No.
- Suitable medium-pore size zeolites include the silicoaluminophosphates (SAPO), such as SAPO-4 and SAPO-11 which is described in U.S. Patent No. 4,440,871; chromosilicates; gallium silicates; iron silicates; aluminum phosphates (ALPO), such as ALPO-11 described in U.S. Patent No. 4,310,440; titanium aluminosilicates (TASO), such as TASO-45 described in EP-A No. 229,295; boron silicates, described in U.S. Patent No. 4,254,297; titanium aluminophosphates (TAPO), such as TAPO- 11 described in U.S. Patent No. 4,500,651; and iron aluminosilicates.
- SAPO silicoaluminophosphates
- SAPO-4 and SAPO-11 which is described in U.S. Patent No. 4,440,871
- chromosilicates such as ALPO-11 described in U
- the medium-pore-size zeolites can include "crystalline admixtures" which are thought to be the result of faults occurring within the crystal or crystalline area during the synthesis of the zeolites.
- Examples of crystalline admixtures of ZSM-5 and ZSM-11 are disclosed in U.S. Patent No. 4,229,424, which is incorporated herein by reference.
- the crystalline admixtures are themselves medium-pore-size zeolites and are not to be confused with physical admixtures of zeolites in which distinct crystals of crystallites of different zeolites are physically present in the same catalyst composite or hydrothermal reaction mixtures.
- the catalysts of the present invention may be held together with an inorganic oxide matrix material component.
- the inorganic oxide matrix component binds the catalyst components together so that the catalyst product is hard enough to survive interparticle and reactor wall collisions.
- the inorganic oxide matrix can be made from an inorganic oxide sol or gel which is dried to "bind" the catalyst components together.
- the inorganic oxide matrix is not catalytically active and will be comprised of oxides of silicon and aluminum. It is also preferred that separate alumina phases be incorporated into the inorganic oxide matrix.
- Species of aluminum oxyhydroxides-g-alumina, boehmite, diaspore, and transitional aluminas such as a-alumina, b-alumina, g-alumina, d-alumina, e-alumina, k-alumina, and r- alumina can be employed.
- the alumina species is an aluminum trihydroxide such as gibbsite, bayerite, nordstrandite, or doyelite.
- the matrix material may also contain phosphorous or aluminum phosphate.
- Process conditions include temperatures from about 500°C to about 650°C, preferably from about 500°C to 600°C; hydrocarbon partial pressures from about 10 to 40 psia (about 70-about 280 kPa) to about, preferably from about 20 to 35 psia (about 140- about 245 kPa); and a catalyst to naphtha (wt wt) ratio from about 3 to 12, preferably from about 4 to 10, where catalyst weight is total weight of the catalyst composite. Steam may be concurrently introduced with the naphtha stream into the reaction zone, with the steam comprising up to about 50 wt. % of the naphtha feed.
- the naphtha residence time in the reaction zone is less than about 10 seconds, for example from about 1 to 10 seconds.
- the reaction conditions will be such that at least about 60 wt. % of the C 5 + olefins in the naphtha stream are converted to C 4 - products and less than about 25 wt. %, preferably less than about 20 wt. % of the paraffins are converted to C 4 - products, and that propylene comprises at least about 90 mol.%, preferably greater than about 95 mol % of the total C 3 reaction products with the weight ratio of propylene/total C 2 - products greater than about 3.5.
- ethylene comprises at least about 90 mol.% of the C 2 products, with the weight ratio of propylene: ethylene being greater than about 4, and that the "full range" C 5 + naphtha product is enhanced in both motor and research octanes relative to the naphtha feed. It is within the scope of this invention to pre- coke the catalysts before introducing the feed to further improve the selectivity to propylene. It is also within the scope of this invention to feed an effective amount of single-ring aromatics to the reaction zone to also improve the selectivity of propylene versus ethylene.
- the aromatics may be from an external source such as a reforming process unit or they may consist of heavy naphtha recycle product from the instant process.
- Comparison of Examples 1 and 2 show that increasing Cat/Oil ratio improves propylene yield, but sacrifices propylene purity.
- Comparison of Examples 3 and 4 and 5 and 6 shows reducing oil partial pressure greatly improves propylene purity without compromising propylene yield.
- Comparison of Examples 7 and 8 and 9 and 10 shows increasing temperature improves both propylene yield and purity.
- Example 13 shows an example where both high propylene yield and purity are obtained at a reactor temperature and cat/oil ratio that can be achieved using a conventional FCC reactor/regenerator design for the second stage.
- the cracking of olefins and paraffins contained in naphtha streams can produce significant amounts of ethylene and propylene.
- the selectivity to ethylene or propylene and selectivity of propylene to propane varies as a function of catalyst and process operating conditions. It has been found that propylene yield can be increased by co-feeding steam along with cat naphtha to the reactor.
- the catalyst may be ZSM-5 or other small or medium-pore zeolites. Table 2 below illustrates the increase in propylene yield when 5 wt. % steam is co-fed with an FCC naphtha containing 38.8 wt. % olefins. Although propylene yield increased, the propylene purity is diminished. Thus, other operating conditions may need to be adjusted to maintain the targeted propylene selectivity.
- ZCAT-40 was used to crack cat cracker naphtha as described for the above examples.
- the coked catalyst was then used to crack a C 4 stream composed of 6 wt.% n-butane, 9 wt.% i-butane, 47 wt.% 1-butene, and 38 wt.% i-butene in a reactor at the temperatures and space velocities indicated in the table below.
- a significant fraction of the feed stream was converted to propylene.
- Light olefins resulting from the preferred process may be used as feeds for processes such as oligimerization, polymerization, co-polymerization, ter- polymerization, and related processes (hereinafter "polymerization") to form macromolecules.
- Such light olefins may be polymerized both alone and in combination with other species, in accordance with polymerization methods known in the art. In some cases it may be desirable to separate, concentrate, purify, upgrade, or otherwise process the light olefins prior to polymerization.
- Propylene and ethylene are preferred polymerization feeds. Polypropylene and polyethylene are preferred polymerization products made therefrom.
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AU64651/01A AU6465101A (en) | 2001-05-19 | 2001-05-19 | Process for selectively producing C3 olefins in fluid catalytic cracking process |
CA002388605A CA2388605A1 (fr) | 2000-05-19 | 2001-05-19 | Procede pour la production selective d'olefines c3 selon un procede de craquage catalytique fluide |
JP2002530418A JP2004509928A (ja) | 2000-05-19 | 2001-05-19 | 流動接触分解法においてc3オレフィンを選択的に製造する方法。 |
MXPA02000719A MXPA02000719A (es) | 2000-05-19 | 2001-05-19 | Proceso para producir selectivamente olefinas c3 en un proceso de desintegracion catalitica fluida. |
EP01939096A EP1289887A1 (fr) | 2000-05-19 | 2001-05-19 | Procede pour la production selective d'olefines c 3? selon un procede de craquage catalytique fluide |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US57426200A | 2000-05-19 | 2000-05-19 | |
US09/574,262 | 2000-05-19 |
Publications (1)
Publication Number | Publication Date |
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WO2002026628A1 true WO2002026628A1 (fr) | 2002-04-04 |
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ID=24295356
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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PCT/US2001/016036 WO2002026628A1 (fr) | 2000-05-19 | 2001-05-19 | Procede pour la production selective d'olefines c3 selon un procede de craquage catalytique fluide |
Country Status (6)
Country | Link |
---|---|
EP (1) | EP1289887A1 (fr) |
JP (1) | JP2004509928A (fr) |
CN (1) | CN1383448A (fr) |
CA (1) | CA2388605A1 (fr) |
MX (1) | MXPA02000719A (fr) |
WO (1) | WO2002026628A1 (fr) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2005082957A1 (fr) * | 2004-02-25 | 2005-09-09 | Exxonmobil Chemical Patent Inc. | Procede de production de polypropylene a partir d'un propylene de classe intermediaire |
WO2011121613A2 (fr) | 2010-03-31 | 2011-10-06 | Indian Oil Corporation Ltd | Procédé de craquage simultané de charges d'hydrocarbures légères et lourdes, et système associé |
US8940955B2 (en) | 2008-12-19 | 2015-01-27 | Uop Llc | Fluid catalytic cracking system and process |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7425258B2 (en) * | 2003-02-28 | 2008-09-16 | Exxonmobil Research And Engineering Company | C6 recycle for propylene generation in a fluid catalytic cracking unit |
CN101747129B (zh) * | 2008-11-28 | 2013-09-04 | 中国石油化工股份有限公司 | 一种催化转化生产低碳烯烃的方法 |
CN114846117B (zh) * | 2019-12-23 | 2023-12-12 | 雪佛龙美国公司 | 通过炼油厂fcc和异构化脱蜡单元将塑料废物转化为聚丙烯和润滑油的循环经济 |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1999057225A1 (fr) * | 1998-05-05 | 1999-11-11 | Exxon Research And Engineering Company | Procede relatif a la production selective d'olefines c3 dans un processus de craquage catalytique fluide |
-
2001
- 2001-05-19 MX MXPA02000719A patent/MXPA02000719A/es unknown
- 2001-05-19 CA CA002388605A patent/CA2388605A1/fr not_active Abandoned
- 2001-05-19 CN CN01801862A patent/CN1383448A/zh active Pending
- 2001-05-19 EP EP01939096A patent/EP1289887A1/fr not_active Withdrawn
- 2001-05-19 WO PCT/US2001/016036 patent/WO2002026628A1/fr not_active Application Discontinuation
- 2001-05-19 JP JP2002530418A patent/JP2004509928A/ja not_active Withdrawn
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1999057225A1 (fr) * | 1998-05-05 | 1999-11-11 | Exxon Research And Engineering Company | Procede relatif a la production selective d'olefines c3 dans un processus de craquage catalytique fluide |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2005082957A1 (fr) * | 2004-02-25 | 2005-09-09 | Exxonmobil Chemical Patent Inc. | Procede de production de polypropylene a partir d'un propylene de classe intermediaire |
US7067597B2 (en) | 2004-02-25 | 2006-06-27 | Exxonmobil Chemical Patents Inc. | Process of making polypropylene from intermediate grade propylene |
EA009877B1 (ru) * | 2004-02-25 | 2008-04-28 | Эксонмобил Кемикэл Пейтентс Инк. | Способ получения полипропилена из пропилена промежуточного сорта |
US8940955B2 (en) | 2008-12-19 | 2015-01-27 | Uop Llc | Fluid catalytic cracking system and process |
WO2011121613A2 (fr) | 2010-03-31 | 2011-10-06 | Indian Oil Corporation Ltd | Procédé de craquage simultané de charges d'hydrocarbures légères et lourdes, et système associé |
US9433912B2 (en) | 2010-03-31 | 2016-09-06 | Indian Oil Corporation Limited | Process for simultaneous cracking of lighter and heavier hydrocarbon feed and system for the same |
Also Published As
Publication number | Publication date |
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CN1383448A (zh) | 2002-12-04 |
CA2388605A1 (fr) | 2002-04-04 |
MXPA02000719A (es) | 2004-02-26 |
EP1289887A1 (fr) | 2003-03-12 |
JP2004509928A (ja) | 2004-04-02 |
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