US3155608A - Process for reducing metals content of catalytic cracking feedstock - Google Patents

Process for reducing metals content of catalytic cracking feedstock Download PDF

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Publication number
US3155608A
US3155608A US72998A US7299860A US3155608A US 3155608 A US3155608 A US 3155608A US 72998 A US72998 A US 72998A US 7299860 A US7299860 A US 7299860A US 3155608 A US3155608 A US 3155608A
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Prior art keywords
hydrogen
stage
catalytic cracking
reactor
catalyst
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Expired - Lifetime
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US72998A
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Inventor
Jack R Hopper
Jr George P Reynolds
William B Franklin
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ExxonMobil Technology and Engineering Co
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Exxon Research and Engineering Co
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Priority to NL271102D priority Critical patent/NL271102A/xx
Application filed by Exxon Research and Engineering Co filed Critical Exxon Research and Engineering Co
Priority to US72998A priority patent/US3155608A/en
Priority to GB36799/61A priority patent/GB960440A/en
Priority to DE1961E0021880 priority patent/DE1470533A1/de
Priority to FR880547A priority patent/FR1369969A/fr
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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
    • C10G65/00—Treatment of hydrocarbon oils by two or more hydrotreatment processes only
    • C10G65/02—Treatment of hydrocarbon oils by two or more hydrotreatment processes only plural serial stages only
    • C10G65/04—Treatment of hydrocarbon oils by two or more hydrotreatment processes only plural serial stages only including only refining steps
    • 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
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/10—Feedstock materials
    • C10G2300/107—Atmospheric residues having a boiling point of at least about 538 °C
    • 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
    • C10G2400/06—Gasoil

Definitions

  • the present invention deals with the hydroclesulfurization of a feed stock for a catalytic cracking process.
  • the present invention deals with the preparation by hydrodesulfurization of a catalytic cracking feed stock which is substantially sulfur free and is low in contaminating metals content and aromatic compounds.
  • the catalytic cracking of petrolernum hydrocarbons is a accomplished by the use of a catalyst either in a fixed bed or in the fluidized state.
  • the reaction takes place in the vapor phase, at temperatures in the range of about 900 F. to about 1000 F.
  • a silica-alumina catalyst which is sensitive to sulfur and to certain metallic elements is normally used.
  • Contamination of the catalyst in the catalytic cracking operation shifts the reaction toward the production of normally gaseous hydrocarbons which are unsuitable as motor fuel; toward the production of unsaturated hydrocarbons which are unstable in storage and are less suitable for motor fuel in some instances than the saturated hydrocarbons; and in the production of coke which represents a net loss of feed stock, as well as increasing the heat load on the regenerator of the catalytic cracking unit and the cooling system for the regenerator.
  • the feed stock to a catalytic cracking unit is treated to remove the sulfur compounds therein by splitting off the sulfur from the organic molecule and forming a gaseous hydrogen sulfide (which is easily separated from the normally liquid hydrocarbon product) and adding hydrogen to the molecule to replace the sulfur which has been removed.
  • the sulfur compounds normally present are thiophenic, but other sulfur compounds are also removed by hydrodesulfurization, as is well known in the art.
  • the amount of metal contaminants present in the hydrocarbon feed stock are reduced. These metallic contaminants normally are present as organo-metallic compounds which are soluble in the hydrocarbon stream, and ordinarily are not removed by sedimentation or filtration.
  • the metals which contaminate the catalytic cracking catalyst and which are partially removed by the practice of the present invention comprise nickel, vanadium, and iron. Still further, by the alsasas Patented Nov. 3, 1964 practice of the present invention, a significant portion of the heavy aromatic compounds in the oil are hydrogenated either completely or partially to naphthenic compounds.
  • the hydrodesulfurization is accomplished in two reactors: a first-stage reactor 10 and a second-stage reactor 12.
  • the fresh charge is introduced into the system by way of line 14.
  • a hydrogen-rich gas is mixed with the charge by means of line 16 from a source later to be discussed.
  • the combined charge and hydrogen-rich gas are introduced into the first-stage reactor 10 by means of line 13.
  • hydrodesulfurization is accomplished under relatively severe conditions and the hydrodesulfurized product is discharged through line 20 and is cooled in cooler 22 from whence it is dicharged by way of line 24 into a separator 26. Within the separator 26 the light gases which have been carried from the first-stage desulfurization are discharged overhead through line 28.
  • These gases comprise light hydrocarbons and hydrogen sulfide formed in the reactor, as well as the unreacted hydrogen and light hydrocarbons which are introduced to the reactor through line 16.
  • the liquid product is discharged from separator 26 through line 30 and is pumped by means 32 via line 34 to the second-stage reactor 12.
  • the liquid product of the first-stage hydrodesulfurization is mixed with a fresh hydrogen gas which is introduced in the heated state by way of line 36.
  • the mixed stream is introduced into reactor 12 by means of line 38.
  • the reaction is carried on at relatively mild conditions and the product is withdrawn by way of line 40 and introduced into a separator 42 wherein the liquid product is separated and removed from the system as a gas-oil product which is substantially sulfur free and which has had the metallic contaminants and aromatic ring compounds substantially reduced.
  • a portion of the gaseous phase which is discharged from separator 42 is carried by way of line 16, as previously discussed, for admixture with the fresh charge. If desired, a part of the gaseous phase may be discharged from the system via line 44 controlled by valve 46.
  • the liquid phase discharged from separator 42 is carried by line 48 to a catalytic cracking unit 50, which may be of a fluidized bed or fixed bed type. 7
  • the second-stage reactor would operate at 50 to 150 p.s.i. lower pressure than the first-stage reactor.
  • the severe hydrodesulfurization conditions comprise a temperature within the range of 730 F. to 800 F. at a pressure of 650 to 3000 p.s.i.g.
  • the space velocity utilized in the first-stage reactor is between 1.0 and 4.5 volumes of charge per volume of catalyst per hour.
  • the hydrogen-treat rate in this first-stage reactor suitably is between 350 and 1500 standard cubic feet per barrel of charge with the hydrogen concentration in the feed gas normally being between 65% and by volume, but may be as low as 60%.
  • the hydrogen consumed in this operation ranges between and 250 standard cubic feet of hydrogen per barrel of gas-oil charge.
  • the sulfide concentration in the feed stock at this stage normally is between /2% and 3% by weight.
  • a relatively mild hydrodesulfurization is accomplished at a temperature ranging between 600 F. and 725 P. which is approximately 50 F. to 150 F. lower than the temperature in the first stage.
  • the pressure in the second stage is about 70 to 125 p.s.i.g. higher than that used in the first stage, ranging bet-ween 750 and 3000 p.s.i.g.
  • the space velocity in the secondstage reactor suitably is identical to that in the first stage.
  • the hydrogen-treat rate in the second-stage reactor may be between 400 and 1500 standard cubic feet per barrel of charge at a hydrogen concentration about 5% to 15% tigher than in the first stage, preferably in the range of 70% to 90%.
  • the hydrogen consumed in the second stage may range between 20 and 120 standard cubic feet per barrel of charge.
  • the lesser amount of hydrogen here consumed is a result of the prior treatment in the first stage wherein the bulk of the hydrodesulfurization takes place.
  • the amount of sulfide present in the feed stock to the second-stage reactor is between 0% and 2% by weight, depending on the desulfurization accomplished in the first stage.
  • the prior art has utilized a parallel or once-through hydrodesulfuriz-a-tion wherein the admixture of hydrogen and hydrocarbon charge is passed through the reactors in one pass.
  • the present invention Ofi ers a substantial improvement over this once-through hydrodesulfurization.
  • the feed stock used in the above experiments was prepared by blending process gas oil and deasphalted oil to provide a mixture which is representative of the type of feed stock normally encountered in this type of process.
  • the "feed stock had an average boiling point of 865 F., a gravity of 22.4 API, and a sulfur content of 1.78% by weight.
  • the metals content of the charge was 0.65 ppm. nickel, 0.88 ppm. vanadium, and 0.55 ppm. iron.
  • the aromatic ring content was about 12.3 weight percent.
  • the hydrogen input into the second stage was about 98+% pure and was introduced into the unit at 800 psig
  • the sulfur content above referred to was induced in the feed stock by metering hydrogen sulfide into the gas-oil charge stream, in order to simulate plant conditions.
  • the catalyst used in these experiments was employed in the form of A3" extruded pellets.
  • the catalyst is cobalt molybdate upon an inert carrier, having a composition T able II SULFUR LEVEL OF FINAL PRODUCT (WT. PERCENT) Yield Percent Period Feed 1 2 3 4 Avg. Desulturization Parallel 1.78 Series:
  • a B O NICKEL CONTENT (PARTS PER MILLION) Yield Percent Period 1 Feed 1 2 3 4 Avg. e;
  • AROBIATIC RING CONTENT (WT. PERCENT) 1 For Series: Denotes yield periods of second pass.
  • the percent desulfurization obtainable by the practice of the present invention is above in the two completed runs shown (i.e., in Series A and Series C), amounting to 92.1% desulfurization at the lowest.
  • the amount of carhon-forming compounds which have been reduced during the hydrodesulfurization is also shown to be quite good, amounting to a minimum of 58.3%.
  • the reduction of nitrogen has been shown to be substantial, within the range of 29.3% to 42.1% reduction.
  • the metallic contaminants in the cracking operation consist of nickel, vanadium and iron. Since it was known that vanadium and iron are reduced in a relative proportion to the amount of nickel removed, the nickel analysis is representative of the other metal analyses. Hence, the selection of the best operation for reduction of metal con tarninants is based on the reduction of nickel. It should be noted that in the A series operation, 87.7% of the nickel has been removed whereas in the C series operation, 83.8% of the nickel has been removed, as compared to 78.5% reduction in the parallel reactors. In this regard, it should be noted that the analysis of .24 ppm. in the first yield period of the A series operation was disregarded in the average because the time allowed before taking the reading may have been insufiicient to obtain good distribution of the oil on the catalyst.
  • the reduction of aromatic ring compounds in the feed stock has also been shown to be quite good, amounting to between 20.1% and 26.9%.
  • the advantage shown in the C series operation in the reduction of these aromatic ring compounds is thought to be due to two reasons. First, the rate limitations had been decreased because the sulfur removal in the first pass had decreased the competition for catalyst surface in the second pass. Secondly, since the rate limitations have been decreased, greater conversions are possible because the lower temperature used in the C series favors the equilibrium in hydrogenating the polycyclic aromatics.
  • the taromati'c ring content of the feed stock likewise, has bwn shown to be reduced in greater measure by the practice of the present invention as compared to the prior art parallel system of hydrodesulturization. Therefore, it is obvious that the practice of the present invention offers a substantial benefit as compared to the parallel operation previously used.
  • the unexpected and unobvious advantage is due to the employment of higher temperatures n the first-stage hydrodesulifurizer which favor the removal of sulfur compounds by hydrogenolysis.
  • the removal of the majority or hydrogen sulfide and light bydrocarbons between stages raises the hydrogen partial pressure and lowers the hydrogen sulfide partial pressure in the second stage reactor, thus improving the equilibrium conversion of sulfur, nitrogen, condensed ring aromatics and other deleterious compounds in the oil.
  • the equilibrium for the hydrogenation reaction is t'avored.
  • the feed stock which may be suitably treated by the present process is not limited to the specific blend stocks disclosed above, but generally is a hydrocarbon stream having an API gravity within the range of about 9 to 30 API, and boiling within the range of 400 F. to 1300 F.
  • a suitable feed stock could be, for example, a mixture of 6 product gas oil (PGO) boiling within the range of 400 F. to 1050 F. and a deasphalted oil (DAO, produced, for example, by propane extraction of crude residua) to produce a hydrocarbon stream boiling within the range of 750 F. to 1300 F.
  • the vacuum flashed crude residuum can also be washed with light catalytic cycle oil prior to hydrodesulfurization to lower the metal contamination thereof.
  • the mixture of gas oil to deasphalted oil may be in a ratio within the range of 1.521 to 5:1. Boiling ranges of the product gas oil and deasphalted oil, along with two exemplary feed stock blends of the two, is given below:
  • the catalysts used in the practice of the present invention can be any of the Well-known hydrodesulfurization catalysts besides the cobalt molybdate catalysts mentioned herein. These catalysts include nickel-tungsten sulfide, molybdenum sulfide, and nickel sulfide. It should be understood that the hydrogen purity ranges stated herein are not critical and, further, that the purity of the hydrogen stream introduced into the first-stage reactor may suitably be controlled by the conditions in the separator 42 as well as being affected by the purity of the fresh hydrogen stream which is introduced into the second-stage reactor 12.
  • a suitable source of hydrogen for introduction into the second-stage hydrodesulfurization reactor is found in the net hydrogen-make stream of a catalytic reformer. This efiiuent gas may suitably be composed as tabulated below:

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
US72998A 1960-12-01 1960-12-01 Process for reducing metals content of catalytic cracking feedstock Expired - Lifetime US3155608A (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
NL271102D NL271102A (xx) 1960-12-01
US72998A US3155608A (en) 1960-12-01 1960-12-01 Process for reducing metals content of catalytic cracking feedstock
GB36799/61A GB960440A (en) 1960-12-01 1961-10-13 An improved process for purifying a gas oil
DE1961E0021880 DE1470533A1 (de) 1960-12-01 1961-10-28 Verfahren zur Entschwefelung von hochsiedenden fluessigen Kohlenwasserstoffen durch weitstufige Behandlung mit Wasserstoff
FR880547A FR1369969A (fr) 1960-12-01 1961-11-30 Procédé d'hydrodésulfuration d'hydrocarbures destinés au craquage catalytique

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Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3340178A (en) * 1964-08-25 1967-09-05 Air Prod & Chem Process for catalytically cracking pyrolysis condensates
US3349027A (en) * 1965-02-08 1967-10-24 Gulf Research Development Co Multi-stage hydrodesulfurization process
US3860510A (en) * 1973-08-22 1975-01-14 Gulf Research Development Co Combination residue hydrodesulfurization and zeolite riser cracking process
US3905893A (en) * 1973-08-22 1975-09-16 Gulf Research Development Co Plural stage residue hydrodesulfurization process
US3907667A (en) * 1973-08-22 1975-09-23 Gulf Research Development Co Process for producing a lubricating oil from a residue feed
US3926784A (en) * 1973-08-22 1975-12-16 Gulf Research Development Co Plural stage residue hydrodesulfurization process with hydrogen sulfide addition and removal
US3936370A (en) * 1973-08-22 1976-02-03 Gulf Research & Development Company Process for producing a zeolite riser cracker feed from a residual oil
DE2831061A1 (de) * 1977-07-15 1979-02-01 Chiyoda Chem Eng Construct Co Verfahren zur hydrodesulfurierung von schwerem kohlenwasserstoffoel
FR2513653A1 (fr) * 1981-09-28 1983-04-01 Chevron Res Procede d'hydrotraitement d'une charge hydrocarbonee
US4801373A (en) * 1986-03-18 1989-01-31 Exxon Research And Engineering Company Process oil manufacturing process
US5459122A (en) * 1992-12-04 1995-10-17 Exxon Research & Engineering Co. Aromatic oil pesticide adjuvant
US6325918B1 (en) 1996-06-28 2001-12-04 Exxonmobile Research And Engineering Company Raffinate hydroconversion process
US6454934B2 (en) * 1997-09-11 2002-09-24 Jgc Corporation Petroleum processing method
US6592748B2 (en) 1996-06-28 2003-07-15 Exxonmobil Research And Engineering Company Reffinate hydroconversion process
US6974535B2 (en) 1996-12-17 2005-12-13 Exxonmobil Research And Engineering Company Hydroconversion process for making lubricating oil basestockes
EP2165664A2 (en) 2008-09-23 2010-03-24 Ethicon Endo-Surgery, Inc. Motor-driven surgical cutting instrument
CN101434866B (zh) * 2007-11-15 2012-09-12 中国石油化工股份有限公司 一种重质馏分油加氢处理与催化裂化组合方法
CN101434865B (zh) * 2007-11-15 2012-12-26 中国石油化工股份有限公司 重质馏分油加氢处理与催化裂化联合方法

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0128250A1 (en) * 1983-06-08 1984-12-19 Mobil Oil Corporation Catalytic dewaxing process
JPH06299168A (ja) * 1993-02-15 1994-10-25 Shell Internatl Res Maatschappij Bv 水素化処理法

Citations (8)

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Publication number Priority date Publication date Assignee Title
US2760907A (en) * 1953-09-01 1956-08-28 Union Oil Co Hydrocarbon conversion process and catalyst
US2769754A (en) * 1954-05-03 1956-11-06 Exxon Research Engineering Co Process for hydrodesulfurization of coker products
US2771401A (en) * 1954-08-05 1956-11-20 Exxon Research Engineering Co Desulfurization of crude oil and crude oil fractions
US2889264A (en) * 1954-12-27 1959-06-02 California Research Corp Hydrocarbon conversion process
US2901417A (en) * 1954-05-17 1959-08-25 Exxon Research Engineering Co Hydrodesulfurization of a coked hydrocarbon stream comprising gasoline constituents and gas oil constituents
US2917448A (en) * 1956-11-15 1959-12-15 Gulf Research Development Co Hydrogenation and distillation of lubricating oils
US2937134A (en) * 1957-10-28 1960-05-17 Socony Mobil Oil Co Inc Cascaded pretreater for removal of nitrogen
US3071542A (en) * 1958-07-16 1963-01-01 Socony Mobil Oil Co Inc Two-stage pretreatment of reformer charge naphtha

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2760907A (en) * 1953-09-01 1956-08-28 Union Oil Co Hydrocarbon conversion process and catalyst
US2769754A (en) * 1954-05-03 1956-11-06 Exxon Research Engineering Co Process for hydrodesulfurization of coker products
US2901417A (en) * 1954-05-17 1959-08-25 Exxon Research Engineering Co Hydrodesulfurization of a coked hydrocarbon stream comprising gasoline constituents and gas oil constituents
US2771401A (en) * 1954-08-05 1956-11-20 Exxon Research Engineering Co Desulfurization of crude oil and crude oil fractions
US2889264A (en) * 1954-12-27 1959-06-02 California Research Corp Hydrocarbon conversion process
US2917448A (en) * 1956-11-15 1959-12-15 Gulf Research Development Co Hydrogenation and distillation of lubricating oils
US2937134A (en) * 1957-10-28 1960-05-17 Socony Mobil Oil Co Inc Cascaded pretreater for removal of nitrogen
US3071542A (en) * 1958-07-16 1963-01-01 Socony Mobil Oil Co Inc Two-stage pretreatment of reformer charge naphtha

Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3340178A (en) * 1964-08-25 1967-09-05 Air Prod & Chem Process for catalytically cracking pyrolysis condensates
US3349027A (en) * 1965-02-08 1967-10-24 Gulf Research Development Co Multi-stage hydrodesulfurization process
US3860510A (en) * 1973-08-22 1975-01-14 Gulf Research Development Co Combination residue hydrodesulfurization and zeolite riser cracking process
US3905893A (en) * 1973-08-22 1975-09-16 Gulf Research Development Co Plural stage residue hydrodesulfurization process
US3907667A (en) * 1973-08-22 1975-09-23 Gulf Research Development Co Process for producing a lubricating oil from a residue feed
US3926784A (en) * 1973-08-22 1975-12-16 Gulf Research Development Co Plural stage residue hydrodesulfurization process with hydrogen sulfide addition and removal
US3936370A (en) * 1973-08-22 1976-02-03 Gulf Research & Development Company Process for producing a zeolite riser cracker feed from a residual oil
DE2831061A1 (de) * 1977-07-15 1979-02-01 Chiyoda Chem Eng Construct Co Verfahren zur hydrodesulfurierung von schwerem kohlenwasserstoffoel
FR2513653A1 (fr) * 1981-09-28 1983-04-01 Chevron Res Procede d'hydrotraitement d'une charge hydrocarbonee
DE3229898A1 (de) * 1981-09-28 1983-04-14 Chevron Research Co., 94105 San Francisco, Calif. Verfahren zur hydrobehandlung eines kohlenwasserstoffhaltigen materials
US4801373A (en) * 1986-03-18 1989-01-31 Exxon Research And Engineering Company Process oil manufacturing process
US5459122A (en) * 1992-12-04 1995-10-17 Exxon Research & Engineering Co. Aromatic oil pesticide adjuvant
US6325918B1 (en) 1996-06-28 2001-12-04 Exxonmobile Research And Engineering Company Raffinate hydroconversion process
US6592748B2 (en) 1996-06-28 2003-07-15 Exxonmobil Research And Engineering Company Reffinate hydroconversion process
US6974535B2 (en) 1996-12-17 2005-12-13 Exxonmobil Research And Engineering Company Hydroconversion process for making lubricating oil basestockes
US6454934B2 (en) * 1997-09-11 2002-09-24 Jgc Corporation Petroleum processing method
CN101434866B (zh) * 2007-11-15 2012-09-12 中国石油化工股份有限公司 一种重质馏分油加氢处理与催化裂化组合方法
CN101434865B (zh) * 2007-11-15 2012-12-26 中国石油化工股份有限公司 重质馏分油加氢处理与催化裂化联合方法
EP2165664A2 (en) 2008-09-23 2010-03-24 Ethicon Endo-Surgery, Inc. Motor-driven surgical cutting instrument

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NL271102A (xx)
DE1470533A1 (de) 1969-10-23
GB960440A (en) 1964-06-10

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