0071455914_ar038

CHAPTER 10.2THE ROSE PROCESS

Tayseer Abdel-Halim and Raymond FloydKellogg Brown & Root, Inc. Resid Upgrading Technology

Houston, Texas

BACKGROUND

The Residuum Oil Supercritical Extraction (ROSE™) process is the premier deasphaltingtechnology available in industry today. This state-of-the-art process extracts high-qualitydeasphalted oil (DAO) from atmospheric or vacuum residues and other feedstocks.Depending on solvent selection, the DAO can be an excellent feedstock for catalytic crack-ing, hydrocracking, or lube oil blending. The asphaltene product from the ROSE processis often blended to fuel oil, but can also be used in the production of asphalt blending com-ponents, solid fuels, or fuel emulsions. Other possible options for the asphaltenes includeuse as feedstock to conversion processes such as partial oxidation, coking, or visbreaking.

The ROSE process was originally developed and commercialized by Kerr-McGeeCorporation and first licensed by the company in 1979. In 1995, KBR (Kellogg Brown &Root, Inc.) acquired the ROSE process from Kerr-McGee. To date, 33 ROSE units with atotal capacity of over 600,000 BPSD have been licensed and/or designed. All these unitsutilize supercritical fluid technology. KBR is responsible for the design or revamp of morethan 400,000 BPSD of this total capacity, including the conversion of the world’s largestsolvent deasphalting facility for Chevron in Richmond, California, to a 50,000 BPSDROSE unit.

ADVANTAGES

Processing residues in a ROSE unit merits serious consideration for today’s refiner. A pro-cessing scheme utilizing a ROSE unit offers several operational and economic advantagesover competing schemes. These advantages include

● Increased yield and improved quality of valuable DAO product compared to other dea-sphalting processes

● Significantly reduced fuel oil production for refineries blending vacuum residue to fuel● Flexibility to process atmospheric/vacuum residues from varying crude sources with lit-

tle difficulty

10.15

Source: HANDBOOK OF PETROLEUM REFINING PROCESSES

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● State-of-the-art supercritical solvent recovery that significantly reduces operating costscompared to other solvent deasphalting processes

● Significantly lower capital and operating costs compared to other upgrading processes

ROSE DAO YIELD AND QUALITY ADVANTAGE

ROSE technology offers significant DAO yield and quality advantages compared to othertechnologies. Superior process performance is ensured by utilizing state-of-the-art asphal-tene and DAO separator internals (ROSEMAX).

Achieving the maximum yield and quality benefits from countercurrent extractionrequires that limits to mass transfer be minimized. The capacity of the separator vesselsmust be maximized for a given size for economical design. These issues are addressed bythe new generation of ROSE separator internals. A brief discussion of the ROSEMAXinternals is provided in the next few paragraphs.

A commitment to enhance performance of the asphaltene and DAO separators for twoROSE licensees prompted KBR to consider significant design improvements to the previ-ous Kerr-McGee internals design. KBR and Koch Engineering formed a team to identifydesign improvements and to quantify potential benefits. A significant amount of engineer-ing analysis, pilot-plant testing, and computer flow modeling was done to support designchanges that would significantly improve performance. A major advance resulting fromthese efforts was the development of our new proprietary ROSEMAX separator internalsthat are now available to all ROSE licensees.

New packing capacity correlations were developed based on laboratory and pilot-planttest work done by Koch and KBR for both liquid-liquid and supercritical service. Thesecorrelations can be used for both structured and random dumped packing. The correlationswere verified for the conditions found in the ROSE separators, i.e., very high phase rates,low interfacial tension, and near-critical and supercritical conditions. These correlationsprovide improved understanding of how the packing crimp size, crimp angle, and surfacetreatment affect extraction capacity and efficiency and coalescing capacity and efficiency.A complete understanding of how to vary packing parameters to achieve desired perfor-mance is required for proper selection of packing size and arrangement.

The use of ROSEMAX internals allows the ROSE separators to operate at about twicethe phase rates of conventional separators and provides about twice the mass-transfer effi-ciency of conventional extraction contacting devices.

ROSE OPERATING COST SAVINGS

ROSE utility costs (steam, power, fuel, and cooling water) are typically 40 to 70 percentof the costs associated with a conventional solvent deasphalting process. These savings areprimarily a result of recovering over 90 percent of the extraction solvent as a supercriticalfluid. Other processes remove the solvent from the DAO by flashing at low pressure. Thesolvent is then compressed and condensed before being reused in the process.

These utility savings can play a significant role in minimizing total project costs asso-ciated with conversion of an existing solvent deasphalting unit to ROSE technology or fora grassroots installation.

Conventional versus Supercritical Solvent Recovery

Figure 10.2.1 illustrates the energy requirements to recover the solvent in the DAO for con-ventional solvent recovery processes. All the solvent exits the extractor as a solution of

10.16 SEPARATION PROCESSES

THE ROSE PROCESS



THE ROSE PROCESS 10.17

DAO and solvent at a relatively low-temperature and high pressure (point A). The streamis heated and flashed at some higher temperature and reduced pressure (point E). At thiscondition the majority of the solvent flashes from the solution and is condensed. The DAOand the remaining solvent are further heated and enter the product stripper (point F) at agreatly reduced pressure, where the remaining solvent is recovered. In this scheme, all thesolvent is vaporized and condensed prior to being recycled to the extraction conditions.The energy requirements for this path are proportional to the quantity of solvent that fol-lows each course.

Figure 10.2.2 illustrates the energy requirements to recover the solvent in the DAO fora supercritical solvent recovery processes. All the solvent exits the extractor as a solutionof DAO and solvent at approximately the same relatively low temperature and high-pres-sure conditions as the conventional scheme (point A). The DAO solvent solution flowsthrough the ROSE exchanger, gaining heat from the recycled supercritical solvent (pointB). The solution is further heated by gaining heat from the stripped DAO product and

SupercriticalFluidA

Liquid

Vapor

F

Increasing Enthalpy

Increasing Pressure

A - ExtractorE - FlashF - Stripper

E

Isotherms –

Increasing T

FIGURE 10.2.1 Conventional solvent recovery.

SupercriticalFluid

A

Liquid

Vapor

F

Increasing Enthalpy

Increasing Pressure

A - ExtractorB - Heater InletC - DAO SeparatorD - Solvent CoolerE - FlashF - Stripper

E

CB

D

Isotherms –

Increasing T

FIGURE 10.2.2 Supercritical solvent recovery.

THE ROSE PROCESS



steam or hot oil in the DAO separator preheater (point C). At point C, 85 to 93 percent ofthe solvent is recovered as a supercritical solvent. The supercritical solvent provides themajority of the heat for the DAO solvent solution (point A to point B) as it is cooled frompoint C to point D. The solvent is cooled to the temperature required for the extraction(point A) in a solvent cooler.

The residual solvent in the DAO product exiting from the DAO separator is recoveredby flashing and stripping. In the supercritical solvent recovery scheme, only 7 to 15 per-cent of the extraction solvent is heated to points E and F, compared to 100 percent of thesolvent in the conventional scheme.

Since the horizontal distances in Figs. 10.2.1 and 10.2.2 are proportional to the changein the solvent’s enthalpy and in both schemes the same amount (about 0.5 percent) mustbe stripped from the DAO product (point F), the energy requirement for the supercriticalsolvent recovery scheme is only 34 percent of the heat energy requirement for single-effectevaporative solvent recovery.

PROCESS DESCRIPTION

Summary

In the ROSE process, DAO product is extracted from the vacuum residue (feed) with alight solvent such as n-butane or n-pentane. Asphaltene is produced as a by-product. Theasphaltene product can be used as a blend component in the production of some grades ofasphalt cement or in fuel oil. The asphaltenes can also be further processed by visbreak-ing, coking, or partial oxidation to recover additional products.

Figures 10.2.3 through 10.2.6 and the process description that follows detail a two-stageROSE unit producing DAO and asphaltene products only. The process flows for two-stageand three-stage ROSE units are very similar. The three-stage unit contains an additional trainof resin product recovery equipment similar to the product recovery equipment for the DAOand asphaltene products. Detailed process design is normally performed to identify opportu-nities for heat integration within the resin product recovery system.

Feed System

Vacuum residue is pumped to the feed surge drum. Feed from the drum is charged to theunit by the feed pump. The feed pump boosts the vacuum residue to a sufficiently highpressure to feed the asphaltene separator. The incoming feed is mixed with a portion of thesolvent and is cooled against asphaltene solvent from the bottom of the asphaltene separa-tor in the asphaltene/feed exchanger. The cooled feed is mixed with a second portion of thesolvent prior to entering the top distributor of the asphaltene separator.

Asphaltene Separator

The feed/solvent mixture feeds the top distributor of the asphaltene separator. Additionalsolvent required for the extraction enters the bottom distributor of the asphaltene separa-tor, providing countercurrent flow.

Asphaltenes are insoluble in the extraction solvent at the extraction conditions andtherefore drop out of solution and exit through the bottom of the asphaltene separator.Slightly less than one volume of dissolved solvent per volume of asphaltenes exits as an


THE ROSE PROCESS



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THE ROSE PROCESS



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THE ROSE PROCESS



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10.21

THE ROSE PROCESS



asphaltene/solvent solution. This asphaltene/solvent solution flows to the asphaltene strip-ping section where the dissolved solvent is stripped from the asphaltene product.

The lighter DAO is soluble in the solvent at the extraction condition. This DAO/solventsolution, containing the majority of the solvent, exits the top of the asphaltene separator asrich solvent.

Operating temperature, solvent composition, solvent/oil ratio, and, to a lesser extent,pressure in the asphaltene separator affect product yield and quality. Since certain primaryprocess parameters (i.e., solvent/oil ratio, solvent composition, and operating pressure) arefixed or set at relatively constant values, the asphaltene separator operating temperature isused as the primary performance control variable.

The DAO yield is effectively controlled by the asphaltene separator operating temper-ature. Higher operating temperatures result in less DAO product extracted overhead.Lower operating temperatures produce more DAO, but of a poorer quality. The solventcooler controls the asphaltene separator overhead temperature, thereby controlling theDAO yield.

ROSE Exchanger and DAO Separator

The asphaltene separator overhead DAO/solvent solution (i.e., rich solvent) is heatedabove the critical temperature of the pure solvent by exchanging heat with recovered leansolvent in the ROSE exchanger, with DAO product in the DAO/DAO solvent exchanger,


MAKE UPHOT OIL

LC

TC

TRACINGOIL

FUEL

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29 7 22211514

Equipment List

7 DAO Separator Preheater14 DAO Stripper Heater15 Asphaltene Flash Heater21 Asphaltene Stripper Heater22 Steam Heater28 Hot Oil Surge Drum29 Hot Oil Furnace30 Hot Oil Circulation Pump

FIGURE 10.2.6 ROSE unit hot oil system.

THE ROSE PROCESS



and with hot oil in the DAO separator preheater. The rich solvent then enters the DAOseparator.

Increasing the temperature of the solvent above its critical temperature takes advantageof the solvent’s low-density properties in this region. As the temperature increases abovethe critical point, the density of the solvent significantly decreases to values approachingthose of dense gases. At this increased temperature, the DAO is virtually insoluble in thesolvent, and a phase separation occurs. Approximately 90 percent of the solvent from therich solvent stream is recovered by this supercritical phase separation.

Supercritical phase separation in the DAO separator and subsequent heat recovery inthe ROSE exchanger provide significant energy savings over conventional deasphaltingprocesses. The conventional processes have substantial energy requirements to vaporizeand condense subcritical solvent in the solvent recovery system.

The DAO phase, containing slightly less than one volume of dissolved solvent per vol-ume of DAO product, is withdrawn from the bottom of the DAO separator. This DAO/sol-vent solution flows to the DAO stripping section where the remaining solvent is strippedfrom the DAO product.

The DAO separator operating conditions are set to achieve the density difference need-ed for good separation. Pressure is controlled by adjusting recycle solvent flow to the high-pressure system from the recycle solvent pump. Temperature is controlled by adjusting thehot oil flow to the DAO separator preheater.

Solvent Cooler and Solvent Circulation Pump

The recovered solvent leaves the DAO separator as lean solvent, also known as circulatingsolvent. Heat is recovered from the lean solvent in the ROSE exchanger. The solvent isthen circulated back through the solvent cooler for temperature control of the asphalteneseparator overhead. Sufficient excess duty is available to provide cooling for swings infeed temperature.

The recycle solvent from the recycle solvent pump combines with the large volume ofcirculating solvent from the solvent cooler. The combined flow enters the solvent circula-tion pump, which boosts the pressure back to the asphaltene separator operating pressure,thus making up for the pressure drop in the circulating solvent loop. Flow valves down-stream of the pump provide adequate control for splitting solvent between the top and bot-tom distributors of the asphaltene separator.

DAO Stripping Section

The DAO/solvent solution is fed to the DAO flash drum on interface-level control from theDAO separator. At the flash drum, the pressure is reduced so that much of the solvent flash-es overhead. A temperature decrease is expected from the flash. The DAO is then fed tothe DAO stripper on liquid-level control from the DAO flash drum. Before entering theDAO stripper, the DAO solution is heated in the DAO stripper heater. The heater providessufficient heat to the system to maintain the recommended operating temperature in theDAO stripper. Heat is provided by either steam or a closed-loop hot oil system.

The DAO is contacted with superheated steam in the stripper to strip any remaining sol-vent to low levels in the product stream. Steam reduces the partial pressure of the solventin the stripper, thus allowing more solvent to vaporize from the DAO liquid. For goodstripping and to meet flash point specifications, stripping steam rates are on flow controland are usually set at 0.5 lb/h of steam per BPD of DAO product. The steam temperatureshould be at or above the recommended operating temperature of the stripper. Colder


THE ROSE PROCESS



steam can cool the DAO and impair stripping performance. Wet steam can cause foamingand operational problems.

The DAO flash drum overhead solvent vapor is condensed in the solvent condenser.The condensed solvent is stored in the solvent surge drum. The solvent is recycled to theprocess under pressure control.

The DAO stripper overhead solvent vapor and steam flow through the stripper con-denser, where the solvent and steam are condensed. The condensed solvent and water areseparated in the low-pressure (LP) solvent drum. The water is removed on level controlfrom the LP solvent drum and sent to the sour water system. The condensed solvent ispumped by the LP solvent pump to the solvent surge drum before being recycled to theprocess.

The DAO product exits the stripper bottom and is pumped on level control with theDAO pump. Heat from the DAO is then recovered in the DAO/DAO solvent exchanger bypreheating rich solvent upstream of the DAO separator preheater.

Asphaltene Stripping Section

The asphaltene/solvent solution from the asphaltene separator is heated by the feed in theasphaltene/feed exchanger and the asphaltene flash heater by either steam or a closed-loophot oil system. This heat input is required to maintain a minimum inlet temperature forasphaltene handling in the downstream asphaltene flash drum.

The hot asphaltene/solvent solution is fed to the asphaltene flash drum on interface-lev-el control from the asphaltene separator. At the flash drum, the pressure is reduced so thatmuch of the solvent flashes overhead. A temperature decrease is expected from the flash.

The asphaltene is then fed to the asphaltene stripper on liquid-level control from theasphaltene flash drum. Before entering the asphaltene stripper, the asphaltenes flowthrough the asphaltene stripper heater. The heater provides sufficient heat to the system tomaintain the recommended operating temperature in the asphaltene stripper. Heat is pro-vided by either steam or a closed-loop hot oil system.

The asphaltene is contacted with superheated steam in the stripper to strip the remain-ing solvent to low levels in the product stream. Steam reduces the partial pressure of thesolvent in the stripper, thus allowing more solvent to vaporize from the asphaltene liquid.Stripping steam rates are on flow control and are usually set at 0.5 lb/h of steam per BPDof asphaltene product for good stripping and to meet flash point specifications.

The steam temperature should be at or above the recommended operating temperatureof the stripper. Colder steam can cool the asphaltene product and impair stripping per-formance. Wet steam can cause foaming and operability problems.

The asphaltene flash drum overhead solvent vapor flows through the solvent condens-er and is condensed. The condensed solvent is stored in the solvent surge drum. The sol-vent is recycled to the process.

The asphaltene stripper overhead solvent vapor and steam flow through the strippercondenser, where the solvent and steam are condensed. The condensed solvent and waterare separated in the LP solvent drum. The water is removed on level control and sent to thesour water system. The condensed solvent is pumped by the LP solvent pump to the sol-vent surge drum before being recycled to the process.

The asphaltene product exits the stripper bottom and is pumped on level control by theasphaltene pump. Positive displacement pumps are usually required to handle the highlyviscous material. The operating temperature maintains the asphaltenes at a viscosity suit-able for pumping. Colder temperatures may cause pumping and handling problems. Theasphaltene product can be cooled against the asphaltene solvent before it is sent to down-stream fuel oil blending facilities or to other potential processes or markets.


THE ROSE PROCESS



The solvent recovered from the strippers is recycled to the process from the LP solventdrum. Since hydrogen sulfide (H2S) may be present in the drum vapor, noncondensablegases are purged from the drum vapor space and directed to sour fuel gas.

The solvent condenser is designed to accept additional intermittent loads from the high-pressure solvent system’s overpressure control valve. This valve opens when the DAO sep-arator pressure increases and excess solvent must be purged from the system to maintainthe proper pressure. This situation occurs primarily during start-up when charge is admit-ted to the liquid-filled system and additional solvent must be released to the solvent con-denser to compensate for the charge volume.

The 30,000 BPD ROSE unit shown in Figs. 10.2.7 and 10.2.8 was designed to useeither a mixed butane or n-pentane solvent to take advantage of seasonal and marketdemands.

PRODUCT YIELD AND QUALITIES

Many operating factors affect the DAO quality, but the two major parameters are DAOyield and extraction solvent. The highest maximum DAO yield is obtained by using n-pen-tane, the heaviest solvent tested. As lighter solvents are used, solvency is reduced and themaximum DAO yield decreases. Typical maximum DAO yield for each solvent is shownin Table 10.2.1.

For any given solvent, the DAO yield has significant impact on the DAO quality, asillustrated in Fig. 10.2.9. If a plant operates at maximum extraction using n-pentane, theDAO will have certain qualities. The other parameter that has significant impact on theDAO quality is the extraction solvent. The lighter the solvent, the less DAO is extracted,


SolventSurge

A. SeparatorA. Stripper

FlareDrum

FeedSurge

DAO Stripper

FIGURE 10.2.7 30,000 BPD ROSE unit, south side.

THE ROSE PROCESS



but the DAO is always cleaner than when produced by heavier solvents. For example, DAOproduced by n-butane will always have a higher viscosity, specific gravity, Conradson car-bon, etc., than a DAO produced at the same yield by i-butane.

A common use of DAO is as additional fluid catalytic cracking unit (FCCU) feed.Several factors could limit FCCU’s feed rate, among them feedstock quality and feed sys-tem hydraulics.

If an FCCU is feedstock-quality-limited, the optimal solvent extraction unit operationwill use a light solvent to achieve the desired quality at the highest possible yield. Forexample, n-butane would produce a more acceptable DAO than n-pentane. Obviously,using n-butane instead of n-pentane is important to a refiner because the amount of FCCUfeedstock can be increased without the detrimental effects of higher carbon and metals.

If an FCCU is operating at its hydraulic limit, the solvent extraction unit can only pro-duce a fixed amount of DAO. Even though the FCCU feedstock quality may be satisfac-tory, if it is possible to shift to a lighter solvent, the refiner will benefit by producing acleaner DAO. The cleanest DAO is produced by the lightest solvent that can achieve thedesired DAO yield.


Hot Oil Surge Drum DAO Separator

ROSE Exchangers

FIGURE 10.2.8 30,000 BPD ROSE unit, north side.

TABLE 10.2.1 Maximum DAO Yields

Solvent Max. DAO yield, wt %

n-Pentane 84n-Butane 74i-Butane 66Propane 50

THE ROSE PROCESS



Factors such as market supply and demand and technology of downstream process-es can change during the operating life of a solvent extraction unit, hence the need fora very flexible extraction unit. ROSE units are usually designed for operation over arange of solvent compositions. A light-solvent unit uses propane or i-butane while aheavy-solvent unit uses n-butane or pentane. This flexibility is made possible by thesimilarities in the product stripping section of n-pentane/n-butane units and i-butane/propane units.

The ultimate in operational flexibility is a unit that can run on all four solvents ormixtures of solvents, such as mixed butanes. This option is available at a slightly high-er cost because of the flexibility inherent in the ROSE processes supercritical solventrecovery.

Since markets and technology do not always remain the same, today’s bottom-of-the-barrel processing facilities must be flexible. This flexibility is inherent in a ROSE unitbecause of its ability to use different solvents. This flexibility, coupled with energy effi-ciency, makes the ROSE process the heavy oil processing technology of the future.

ROSE ECONOMICS SUMMARY

The estimated utility requirements for a grassroots ROSE unit are shown in Table 10.2.2.The figures provided in the table are the typical range of expected utility consumption. Theactual values obtained in the final design will depend on process battery-limit conditions,site conditions, and optimized process conditions such as separator temperatures, strippertemperatures, and solvent/oil ratio.

The estimated installed cost for a 30,000 BPSD unit is $1250 per BPSD, U.S. GulfCoast, second quarter of 2002.


% COMPONENT IN DAO

100

80

60

40

20

00 10 20 30 40 50 60 70 80 90 100

DAO YIELD, VOL %

METALS

SULFUR

NITROGEN

CCR

FIGURE 10.2.9 Typical contaminant distribution in DAO.

THE ROSE PROCESS



BIBLIOGRAPHY

Abdel-Halim, T., and P. Shah: “Refinery Residuals as a Source of Chemical Feedstock and ValueAdded Products,” APPEAL Resource and Training Consortium, Bangkok, Thailand, March 2002.

Abdel-Halim, T., R. Uppala, B. Bansal, R. Floyd, and D. Eastwood: “ROSE™ and Bottom-of-the-Barrel: A Synergistic Approach,” Second Bottom of the Barrel Technology Conference, Istanbul,Turkey, October 2002.

Nelson, S. R., and R. G. Roodman: “ROSE: The Energy Efficient Bottom of the Barrel Alternative,”1985 Spring AICHE Meeting, Houston, Tex., March 1985.

Northup, A. H., and H. D. Sloan: “Advances in Solvent Deasphalting Technology,” 1996 NPRAAnnual Meeting, San Antonio, Tex., March 1996.

Patel, V. K., E. M. Roundtree, and H. D. Sloan: “Economic Benefits of ROSE/Fluid CokingIntegration,” 1997 NPRA Annual Meeting, San Antonio, Tex., March 1997.

Sloan, H. D., H. J. Simons, J. Griffths, and D. J. Bosworth: “Solvent Deasphalting andGasification to Reduce Fuel Oil,” 1996 European Oil Refining Conference, Antwerp, Belgium,June 1996.


TABLE 10.2.2 Utilities

Process requirements per barrel of feed*

Propane Butane Pentane

LP stripping steam, lb/bbl 12 12 12Electricity, kWh/bbl 1.5–2.1 1.4–2.0 1.3–1.9Process heat,† million Btu/bbl absorbed 0.097–0.147 0.070–0.104 0.057–0.086Solvent loss, wt % of feed 0.05–0.10 0.05–0.10 0.05–0.10Initial solvent fill, bbl/bbl 0.15 0.15 0.15No other major chemicals or catalyst use is required.

*Figures provided indicate typical range of expected utility consumption. Actual values will depend on processbattery-limit conditions, site conditions, and optimized process conditions such as separator temperatures, strippertemperatures, and solvent/oil ratio.

†Process heat can be supplied by steam or hot oil.

THE ROSE PROCESS



0071455914_ar038

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