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WO1999031199A1 - Procede d'adsorption selective destine a une valorisation de residus - Google Patents

Procede d'adsorption selective destine a une valorisation de residus Download PDF

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Publication number
WO1999031199A1
WO1999031199A1 PCT/US1998/026608 US9826608W WO9931199A1 WO 1999031199 A1 WO1999031199 A1 WO 1999031199A1 US 9826608 W US9826608 W US 9826608W WO 9931199 A1 WO9931199 A1 WO 9931199A1
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WO
WIPO (PCT)
Prior art keywords
adsorbent
oil
solvent
metals
feedstream
Prior art date
Application number
PCT/US1998/026608
Other languages
English (en)
Inventor
Martin Leo Gorbaty
David Thomas Ferrughelli
William Neergaard Olmstead
Sabato Miseo
Stuart Leon Soled
Winston Karl Robbins
Original Assignee
Exxon Research And Engineering Company
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Exxon Research And Engineering Company filed Critical Exxon Research And Engineering Company
Priority to CA002313217A priority Critical patent/CA2313217A1/fr
Priority to EP98963928A priority patent/EP1062296A4/fr
Publication of WO1999031199A1 publication Critical patent/WO1999031199A1/fr

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Classifications

    • 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
    • C10G25/00—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents
    • C10G25/003—Specific sorbent material, not covered by C10G25/02 or C10G25/03
    • 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
    • C10G25/00—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents

Definitions

  • the present invention relates to the refining of hydrocarbon feedstocks. More particularly, this invention concerns the segregation and removal of coke precursors and metals from atmospheric and vacuum residua, and deasphaltened vacuum residua.
  • Hydrocarbon feedstocks are composed of hydrocarbons and heteroatom containing hydrocarbons which differ in boiling point, molecular weight and chemical structure.
  • High boiling, high molecular weight heteroatom-containing hydrocarbons weight e.g. asphaltenes
  • coke precursors metals and carbon forming constituents
  • lower boiling naphtha and distillate fractions because coke precursors form coke during thermal processing (such as is employed in a modem refinery), it is desirable to remove (or at least segregate) the heteroatom containing hydrocarbons containing the metals and coke precursors, thereby facilitating further processing of the more valuable fractions of the feedstock.
  • the present invention is a process to remove a major portion of metals and coke precursors from a hydrocarbon or heteroatom- containing hydrocarbon feedstream.
  • the feedstream is contacted with an adsorbent that adsorbs the metals and coke precursors.
  • the feedstream effluent is transferred to another vessel.
  • the metals and coke precursors are then removed from the adsorbent by a suitable solvent.
  • Figure 1 shows a schematic diagram of the process of one embodiment of the present invention, illustrating how metals and coke precursors would be removed from deasphaltened oil (DAO), the product from a solvent deasphalter.
  • DAO deasphaltened oil
  • Figure 2 shows a schematic diagram of another embodiment of the present invention illustrating upgrading a residuum from either atmospheric or vacuum distillation.
  • the present invention is an adsorption process to remove a significant amount of metals and coke precursors from a hydrocarbon feedstream, and to render that stream more valuable as a fuel or as feed to a catalytic cracker.
  • Any hydrocarbonaceous liquid containing metals and coke precursors may be used for the feedstream of this invention.
  • These may include atmospheric and vacuum residua, vacuum gas oils, solvent deasphalting (SDA) fractions with and without resins, and even whole crude oils, particularly those containing high levels of nickel and vanadium such as found in Venezuela tars for example. While any of these liquids may be used as a feedstock if the results are economically justified, particularly useful feedstreams for this invention are atmospheric and vacuum residua.
  • the effluent from the feedstieam will then provide a clean cat cracker feed.
  • the adsorption process uses a hydrocarbon insoluble adsorbent material, which has a high capacity for adsorbing metals and coke precursors, and which can be easily regenerated by washing with relatively polar solvents or solvent mixtures, or by other processes including those with pyrolysis or combustion steps.
  • FIG. 1 shows a schematic diagram of one embodiment of the process of the present invention aimed at upgrading a solvent deasphalted heavy oil.
  • the effluent from a solvent deasphalter (SDA), composed of a deasphaltened oil (DAO) in about 4-6 volumes of deasphalting solvent, such as pentane at about 120-160°C is passed into a vessel containing the adsorbent.
  • the adsorbent may be a fixed bed.
  • the reactor effluent is transferred to another vessel labeled "CSR", where the deasphalting solvent (e.g., pentane) is removed and recycled to the SDA, while the product, an upgraded deasphaltened oil, is an acceptable cat cracker feed ( ⁇ about 4 ppm metals and ⁇ about 4 wt% coke precursors).
  • the upgraded deasphaltened oil is sent to a cat cracker to be fed directly or blended with conventional vacuum gas oil (VGO).
  • VGO vacuum gas oil
  • the swing reactor configuration in Figure 1 is set up such that one vessel is set up for adsorption, while the other is set up for adsorbent regeneration.
  • regeneration is carried out by using solvents such as toluene, toluene-methanol, or other appropriate solvents available in a refinery environment.
  • solvents such as toluene, toluene-methanol, or other appropriate solvents available in a refinery environment.
  • the metal containing and coke precursor molecules are washed off the adsorbent, the solution containing these impurities is stripped in the box labeled "SEP'N", the solvent recycled and the impurities stream sent to a coker, partial oxidation unit or other disposal technique.
  • FIG. 2 shows a schematic diagram of a second embodiment of the process of the present invention aimed at upgrading a residuum from either atmospheric or vacuum distillation.
  • the residuum is passed into a vessel containing the adsorbent. After contacting the adsorbent for an appropriate time, the effluent is an upgraded residuum with lowered metals and coke precursor content.
  • the upgraded residuum flows on to further refining processing, such as cat cracking, where it is treated either directly or blended with other refinery streams, such as conventional vacuum gas oil (VGO).
  • VGO vacuum gas oil
  • the swing reactor configuration in Figure 2 is set up such that one vessel is set up for adsorption, while the other vessel is set up for adsorbent regeneration.
  • regeneration is carried out by using solvents such as toluene, toluene- methanol, or other appropriate solvents available in a refinery environment.
  • solvents such as toluene, toluene- methanol, or other appropriate solvents available in a refinery environment.
  • the metal containing and coke precursor molecules are washed off the adsorbent, the solution containing these impurities is stripped in the box labeled "SEP'N", the solvent is recycled and the impurities stream sent to a coker, partial oxidation unit or other disposal technique.
  • Suitable adsorbents for the present process include hydrocarbon insoluble inorganic and carbonaceous materials, which have surface areas greater than 100 m 2 /g and whose surfaces may be acidic.
  • Specific examples of adsorbents useful for this process include silica, silica-alumina, K-10 and similar acid-treated clays and activated carbons, with surface areas ⁇ 1000 m 2 /g.
  • a preferred feedstieam to adsorbent ratio is between 0J and 10 wt/wt.
  • the present invention shall be illustrated by examples using feedstreams of Arabian Light atmospheric residuum, effluent from solvent deasphalters and various acceptable adsorbents and process solvents.
  • ALAR is one example of a feedstieam suitable for the present process.
  • ALAR Arabian Light atmospheric residuum
  • solvent and adsorbent ratio of 4 solvent: 1 adsorbent: 1 oil
  • Solvents were used in the room temperature experiments in order to keep the viscosity within a workable range.
  • elevated temperatures e.g. 200 °C
  • solvents are not necessary for the contacting of oil with adsorbent.
  • the solvent was removed on a rotary evaporator yielding a clean oil.
  • the adsorbed material was treated first with toluene, then a 1: 1 (by volume) toluene :methanol mixture to desorb it from the adsorbent.
  • Data in Table 1 show that, compared to starting ALAR, the product oils treated by the method of this invention contained very low levels of metals and showed a significant enough reduction of coke precursors as measured by the decrease in % CCR such that the product could be fed directly to a cat cracker.
  • the adsorbents used include silica, calcined at 600°C. It has a surface area of 300 m 2 /g and a reported pore diameter of 150 A. Another is amorphous silica-alumina (87 wt% silica), whose surface area and pore diameter are 318 m 2 /g and 105 A respectively.
  • a mixture of one part by weight oil, 4 parts by weight solvent, and 1 part by weight adsorbent were combined and allowed to stir for 16 hours.
  • the adsorbent was separated by filtering through a medium porosity buchner funnel.
  • the solvent was removed from the filtrate by roto-evaporation.
  • the resulting oil was analyzed for %CCR and metals.
  • the recovered adsorbent was treated with a 25% ethanol in toluene at reflux in a Soxhlet extractor, until no further color was released.
  • the solvent was removed by roto-evaporation, and the residue analyzed for metals and CCR.
  • This example illustrates adsorbent regeneration by heating.
  • the filtered solid from Example 3 was heated to 490°C for 2h under flowing nitrogen, cooled to room temperature and the adsorption experiment described above repeated using this solid.
  • the recovered oil (90% of starting oil) had a CCR of 4.8% and contained 4.0 ppm V and 3.0 ppm Ni.
  • This example illustrates adsorbent regeneration by heating.
  • the filtered solid from Example 7 was heated to 490 °C for 2h under flowing nitrogen, cooled to room temperature and the adsorption experiment described above repeated using this solid.
  • the recovered oil (89% of starting oil) had a CCR of 3.9% and contained 3.0 ppm V and 2.0 ppm Ni.
  • the example illustrates the process without use of a solvent.
  • 60.0 g of Arabian Light Atmospheric residuum was heated to 200 °C with stirring and 30 g of a silica-alumina material designated MS-13 (containing 13% alumina), previously calcined at 600°C, was added.
  • MS-13 silica-alumina material
  • the mixture was sti ⁇ ed for 16 hours at 200 °C.
  • the oil was decanted from the solids and analyzed.
  • the treated oil had a CCR of 4.7% and contained 1 ppm V and 1 ppm Ni.
  • a fresh sample of 7.4 g of Heavy Arab Vacuum Resid (975°F+) containing a % CCR of 22.1%, 55 ppm Ni, and 190 ppm V was mixed with 30 ml o-xylene and heated to 100°C at which time 12 g of calcined (600°C) silica was added. The mixture was brought to 140°C and refluxed for 6 hours. The solvent was then removed by roto-evaporation and 100 ml pentane was added to the flask and stined for 16 hours at 25°C. The mixture was then filtered and the pentane removed by roto-evaporation to recover the pentane soluble oil (64.4%).
  • the DAO had a % CCR of 5.01% and contained 3 ppm Ni and ⁇ 1 ppm V.
  • the pentane insoluble oil (35.6%) was removed from the adsorbent with a 25% methanol/75% toluene mixture.
  • SDA also provides a feedstream for the present process.
  • Solvent deasphalting is another way of separating metals and coke precursors from residua.
  • DAO deasphaltened oil
  • the yield and cleanliness of DAO defined the economic limit of how much deasphalting can be done. For example, using n-pentane approximately 75% yield of DAO can be obtained from a Baytown vacuum residuum. However, this DAO contains about 11% Conradson carbon and about 70 ppm of metals.
  • propane or butane in SDA a good quality cat cracker feed stock can be obtained but in yields between 35-50%. This has the effect of limiting the amount of resid cat cracking possible by using SDA.
  • the present process provides a simple way to clean up the DAO after SDA, or the feed to SDA, or to isolate the impurities during SDA, which would remove the bottleneck and allow the use of SDA to produce high yields of DAO as cat cracker feed stock, leading to more resid conversion.
  • the effluent from SDA composed of a DAO in about 4-6 volumes of pentane, at about 120-160°C is passed into a vessel containing the adsorbent. After contacting for an appropriate time, the reactor effluent is transferred to another vessel labeled "CSR" where the pentane is removed and recycled to the SDA process, while the product, now an acceptable cat cracker feed ( ⁇ 4 ppm metals and ⁇ 4 wt% coke precursors) is sent to a cat cracker to be fed directly or blended with conventional VGO (see Figure 1).
  • the adsorbents used include silica, calcined at 600°C. It had a surface area of 300 m 2 /g and a reported pore diameterof 150 A. Another is amoiphous silica-alumina (87 wt% silica), whose surface area and average pore diameter were determined to be 318 m /g and 105 A respectively. Data for calcined silica are shown in the attached Table 2, along with a non-limiting experimental protocol. In this protocol, a DAO was combined with a solvent (ratio of 4 parts solvent: 1 DAO), heated to temperature, and the adsorbent added at a treat rate of 2: 1 adsorbent to feed oil.
  • NONANE 140 72 5.0 1.0 0.5 84.88 11.75 0.15 3.09 1.66
  • a wt% mixture of one part oil, 4 parts solvent and 2 parts adsorbent were refluxed at 140°C for 6 hours.
  • the solvent was removed by roto- evaporation.
  • Pentane was added in a ratio of 10: 1 (solvent to oil) and the mixture was stined for 16 hours.
  • the pentane soluble oil was separated by filtering through a medium porosity buchner funnel.
  • the pentane was removed from the filtrate by roto-evaporation.
  • the resulting oil was analyzed for % CCR and metals.
  • the pentane insoluble portion of the oil was removed from the adsorbent by treating with a more polar solvent or solvent mixture in a ratio of 10: 1 (solven oil).
  • the pentane insoluble oil was removed from the silica by stirring overnight at 25°C in a mixture of 25% methanol/75% toluene and filtering to recover the pentane insoluble oil (23%) and regenerated adsorbent.
  • Example 12 A fresh sample of one part Baytown DAO (see Example 12) and 4 parts nonane were heated to 100°C at which time 2 parts silica (Example 12) was added. The mixture was brought to 140°C and refluxed for 6 hours. The workup was as described in Example 12. The resulting oil had a reduced % CCR and was virtually metal free (see Table 2).
  • Example 12 A fresh sample of one part Baytown DAO (see Example 12) and 4 parts heptane were heated to 100°C at which time 2 parts silica (Example 12) was added. The mixture was refluxed at 100°C for 6 hours. The workup was as described in Example 12. The resulting oil had a reduced % CCR and was virtually metal free (see Table 2).
  • Example 16 A fresh sample of one part Baytown DAO (see Example 12) and 4 parts heptane were heated to 100°C at which time 2 parts silica (Example 12) was added. The mixture was refluxed at 100°C for 6 hours. The workup was as described in Example 12. The resulting oil had a reduced % CCR and was virtually metal free (see Table 2).
  • Example 16 A fresh sample of one part Baytown DAO (see Example 12) and 4 parts heptane were heated to 100°C at which time 2 parts silica (Example 12) was added. The mixture was refluxed at 100°C for 6 hours. The work
  • Example 12 A fresh sample of one part Baytown DAO (see Example 12) and 4 parts o-xylene were heated to 100°C at which time 2 parts of an uncalcined silica (87%)/alumina (13%) mixture was added. The mixture was brought to 140°C and refluxed for 6 hours. The workup was described in Example 12. The resulting oil (69%) had a % CCR of 3.19% and contained ⁇ 3.0ppm Ni and ⁇ 0.5 ppm V.
  • Example 19 A fresh sample of one part Baytown DAO (see Example 12) and 4 parts o-xylene were heated to 100°C at which time 2 parts of an uncalcined silica (87%)/alumina (13%) mixture was added. The mixture was brought to 140°C and refluxed for 6 hours. The workup was described in Example 12. The resulting oil (69%) had a % CCR of 3.19% and contained ⁇ 3.0ppm Ni and ⁇ 0.5 ppm V.
  • Example 19 A fresh sample of one part Baytown DAO
  • Example 12 A fresh sample of one part Baytown DAO (see Example 12) and 4 parts toluene was prepared at which time 1 part of Norit activated carbon was added. The mixture was stirred at room temperature for 16 h. The workup was described in Example 12. The resulting oil (85%) had a % CCR of 6.5% and contained 1.0 ppm Ni and 7 ppm V.

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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)

Abstract

La présente invention concerne un procédé d'enlèvement d'une portion majeure de métaux et de précurseurs de coke, à partir d'un courant d'hydrocarbures. Les étapes de ce procédé consistent à mettre en contact le courant d'alimentation avec un adsorbant insoluble dans des hydrocarbures, à récupérer l'huile qui ne s'adsorbe pas et à enlever les métaux et les précurseurs du coke à partir de l'adsorbant.
PCT/US1998/026608 1997-12-16 1998-12-15 Procede d'adsorption selective destine a une valorisation de residus WO1999031199A1 (fr)

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CA002313217A CA2313217A1 (fr) 1997-12-16 1998-12-15 Procede d'adsorption selective destine a une valorisation de residus
EP98963928A EP1062296A4 (fr) 1997-12-16 1998-12-15 Procede d'adsorption selective destine a une valorisation de residus

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US99127997A 1997-12-16 1997-12-16
US08/991,279 1997-12-16

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Cited By (6)

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EP2011849A1 (fr) * 2007-06-12 2009-01-07 General Electric Company Procédés et systèmes de retrait de métaux de combustible secondaire
US20140110343A1 (en) * 2012-10-22 2014-04-24 Florida State University Research Foundation, Inc. Isolation of interfacial material from organic matrices
US20150192501A1 (en) * 2012-10-22 2015-07-09 Florida State University Research Foundation, Inc. Immobilized water stationary phase
US20190161688A1 (en) * 2014-12-18 2019-05-30 Phillips 66 Company Solid adsorption process for removing particles from heavy, partially refined oils
WO2021211690A1 (fr) * 2020-04-17 2021-10-21 Saudi Arabian Oil Company Procédé de production d'huile désasphaltée et démétallisée
CN113736509A (zh) * 2020-05-28 2021-12-03 中国石油化工股份有限公司 一种用于渣油浆态床加氢残渣油的处理方法

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2011849A1 (fr) * 2007-06-12 2009-01-07 General Electric Company Procédés et systèmes de retrait de métaux de combustible secondaire
US7947167B2 (en) 2007-06-12 2011-05-24 General Electric Company Methods and systems for removing metals from low grade fuel
US20140110343A1 (en) * 2012-10-22 2014-04-24 Florida State University Research Foundation, Inc. Isolation of interfacial material from organic matrices
US20150192501A1 (en) * 2012-10-22 2015-07-09 Florida State University Research Foundation, Inc. Immobilized water stationary phase
US10315131B2 (en) * 2012-10-22 2019-06-11 Florida State University Research Foundation, Inc. Isolation of interfacial material from organic matrices
US20190161688A1 (en) * 2014-12-18 2019-05-30 Phillips 66 Company Solid adsorption process for removing particles from heavy, partially refined oils
WO2021211690A1 (fr) * 2020-04-17 2021-10-21 Saudi Arabian Oil Company Procédé de production d'huile désasphaltée et démétallisée
CN113736509A (zh) * 2020-05-28 2021-12-03 中国石油化工股份有限公司 一种用于渣油浆态床加氢残渣油的处理方法
CN113736509B (zh) * 2020-05-28 2023-06-09 中国石油化工股份有限公司 一种用于渣油浆态床加氢残渣油的处理方法

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CA2313217A1 (fr) 1999-06-24
EP1062296A4 (fr) 2003-01-22
EP1062296A1 (fr) 2000-12-27

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