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Solvent Extraction Technology

for Used Oil Treatment

Solvent Extraction Technology

for Used Oil Treatment

Prepared for

Recycling Technology Assistance Partnership (ReTAP)

A program of the Clean Washington Center,
a division of the Pacific Northwest Economic Region (PNWER)
2200 Alaskan Way, Suite 460
Seattle, Washington 98121

December 1995

Prepared by

AERCO, Inc., P.S.

18503 - 71st Avenue West
Lynnwood, Washington 98037

This recycled paper is recyclable

Copyright 1995 by Clean Washington Center

Report No. O-95-1



TABLE OF CONTENTS ................................................................................... i
ABSTRACT....................................................................................................... 1
1.0 PROJECT OVERVIEW............................................................................ 2
1.1 THE USED OIL INDUSTRY............................................................... 2
1.3 THE SOLVENT EXTRACTION TECHNOLOGY .............................. 5
1.4 PROJECT OBJECTIVES ..................................................................... 6
2.0 LITERATURE SEARCH FINDINGS....................................................... 8
3.0 PILOT PLANT DESIGN........................................................................... 9
3.1 DESIGN ASSUMPTIONS ................................................................... 9
3.2 DESIGN DOCUMENTS .................................................................... 11
4.0 FURTHER DEVELOPMENT OF TECHNOLOGY.............................. 16
4.1 PILOT SCALE ................................................................................... 16
4.2 FULL SCALE..................................................................................... 17
4.3 SUMMARY........................................................................................ 17
5.0 ACKNOWLEDGMENTS........................................................................ 19
6.0 REFERENCES......................................................................................... 20

Figure 1 - Simplified Process Flow Diagram .................................................... 6
Figure 2 - Process Flow Diagram .................................................................... 14
Figure 3 - Piping And Instrumentation Diagram........................................... 15
Figure 4 - Appendix A, Equipment List ......................................................... 22

Solvent extraction, an innovative adaptation of existing crude oil refining technology, is being
studied for its potential to upgrade used oils produced by small-scale oil treatment facilities. This
report presents the design for a pilot-scale treatment plant using solvent extraction technology to
produce an improved fuel product.

The solvent treatment technology presented in this report, either alone or in combination with
existing used oil dehydration facilities, has the potential to significantly reduce the impurities in
the product oil currently produced by used oil processing or treatment companies. This product
oil could be used for higher value fuels without attempting to meet all the stringent specifications
and requirements that would accompany the production of lubrication stocks. The technology has
already been used successfully in Europe as a unit process on a larger scale to produce lubrication
stock from used oil. The technology also has the potential to produce a higher quality fuel than
the heavy cutter stock currently being produced for blending into marine diesel fuel.

This report presents the design and supporting documents for the construction of a pilot scale
solvent treatment plant. Observations and discussion regarding the project and the design
assumptions are presented along with the design. The objectives for the design phase of the
project were as follows:

Determine key process parameters to guide the design of the pilot plant;

Design a pilot scale plant that produces sufficient quantities of used oil for product

This report also recommends the future construction of a pilot scale solvent treatment plant by
interested parties to allow refinement of the design, testing with a wide variety of used oil
streams, treatment cost evaluation, and production of sufficient quantities of product oils and
asphalt bottoms to allow acceptance testing with customers of these products.



Solvent extraction, an innovative adaptation of existing crude oil refining technology, is being
studied for its potential to upgrade used oils produced by small-scale oil treatment facilities. This
report presents the design for a pilot-scale treatment plant using solvent extraction technology to
produce an improved fuel product.


Used oils are by-products of oil use in vehicles and machinery. Lubricating oils must be replaced
on a regular basis in all operating equipment due to contamination from dirt, water, salts, metals,
incomplete products of combustion, antifreeze, or other materials. Additives to lubricating oils
may also break down under use, adding contamination.

Once replaced by new lubricants, used oil becomes a significant management challenge. Without
access to suitable recycling or waste-to-energy options, used oil tends to be disposed in ways that
can degrade the environment: as road oil for dust control; illegally dumped into waterways; or
disposed on land or in landfills where groundwater contamination can result.

Most used oil in the U.S. is treated or re-refined, restoring the used oils to a usable state. But,
meeting fuel or lubrication performance specifications entails a higher level of processing than
decanting, settling, or filtering. The large number of contaminants potentially contained in used
oil complicates the selection of appropriate treatment methods. A number of technologies of
varying complexity have been proposed, or are currently in use, throughout the used oil industry.
These technologies include variations of acid/clay or other chemical treatments, various
distillation processes, cracking, hydrotreating, solvent treatment, and blending/compounding.
Combinations of these treatment technologies with decanting, settling, and filtering are required
to produce higher value oils.

The degree and complexity of used oil treatment varies with the intended use of the end products.
Producing a clear, light-colored lubrication stock that meets a variety of different machinery

manufacturers service requirements generally requires more complex treatment and blending than
producing a used oil fuel. Capital costs usually increase the more sophisticated the treatment
technology, but may be offset to some degree by higher-valued end products.

As reported by the Clean Washington Center in its 1994 report Used Oil to Diesel, An
Alternative Technology,1 an estimated 80% of used oil collected in Washington State is blended
into heavy bunker fuels for use by ocean-going vessels; 14% is burned in land-based facilities.
The remainder of the used oil collected is recycled into lubricants or finds other uses. The
primary purchaser of used oil products in Washington state is Sound Refining Company, Inc. of
Tacoma, a small refinery which produces asphalt and marine diesel products. Other significant
purchasers include asphalt batch plants, sewage sludge dryers, and some industrial boilers.

The current saturation of the Pacific Northwest heavy fuel oils market has resulted in depressed
prices for used oil fuels.2 The lingering perception that used oil fuels are inferior products to fuels
from virgin crude sources further complicates this segment of the petroleum market. With
improved treatment, used oil could potentially be blended into higher-value, lighter fuel oils,
perhaps resulting in an improved market price.

The used oil treatment industry in the U.S. is characterized by numerous small operators
struggling to survive and a small number of large re-refining facilities. Factors such as the wide
dispersal of used oil sources, the aggressiveness of virgin oil marketers (major oil companies and
their distribution channels), tax and environmental regulations, and technological changes in oil
products have hindered the development of the used oil industry over the last twenty years. Small
business lack the ability to respond to these unfavorable conditions because of their lack of

Most used oil companies in Washington State are small, poorly capitalized, marginally profitable,
and staffed by personnel with relatively modest levels of technical education or expertise.
Consequently, the challenges for Washingtons used oil industry are to find better treatment
alternatives that are on a scale commensurate with the resources available to these businesses,

that produce affordable and safe, higher-value end products, and that are operable using
available expertise. Technologies that allow used oil to be upgraded to lighter, higher value fuels
rather than to lubricants may be the optimal alternative.



Historically, the most successful technology for treating used oils was the acid-clay process. This
process is capable of producing good quality lubrication stocks, but also produces large volumes
of petroleum-contaminated acid clay sludge. With the passage of the Resource Conservation and
Recovery Act (RCRA) and later legislation, the sludge was classified as a hazardous waste
requiring proper management and disposal. Consequently, the acid-clay process technology
became uneconomic because of the high cost of managing the residues and is no longer used in
Washington State.

Used oil treatment using simple dehydration and volatiles removal through low temperature
distillation (less than 300 Fahrenheit, 149 Celsius) is adequate to allow the sale of the treated oil
as cutter stock for blending with heavy bunker oils. While this technology can significantly
reduce water, antifreezes, and solvents in the used oil, it is limited in its ability to significantly
reduce ash and other residues, seriously limiting product marketability. Along with settling,
decanting, and filtering, low temperature distillation is used to treat used oils in most small-scale

In Used Oil to Diesel, An Alternative Technology, the Clean Washington Center considered a
high temperature (over 650F, 343 C) cracking/distillation technology manufactured by Utopia
Fabricating Ltd., Pennfield, New Brunswick, Canada (the Shurtleff Waste Oil Handling System).
While achieving a degree of success in producing No. 2 and No. 3 diesel fuels, units produced by
this firm are reported to have experienced severe operating problems. The company has
reportedly gone into bankruptcy.3 Another company producing a unit utilizing similar high
temperature cracking/distillation technologies, Green Oasis Environmental, Inc., Charleston, SC,
manufactured and sold several production units but has also reportedly gone into bankruptcy.3

Other technologies such as hydrotreating, cracking, high temperature/pressure distillation, and

blending/compounding are technically sophisticated and generally not economic, safe, or available
at the small scale (relative to virgin oil refineries) at which Washington States used oil businesses



The solvent extraction technology has the potential to produce oil products that are superior to
those produced by the low-temperature distillation process currently in use. Figure 1 presents a
simplified, conceptual process flow diagram for the solvent extraction technology. Used oil is
mixed in the Reactor Column with an aliphatic solvent such as liquefied propane (butane, heptane
or hexane may also be used). In this unit, the solvent acts selectively, dissolving the oil fraction
and leaving the less soluble impurities. The oil-laden solvent is transported from the top of the
Reactor Column to the Solvent Still (a distillation column) where the solvent fraction is separated
from the oil for recycling within the process. The impurities (bottoms) slowly settle and coalesce
in the bottom of the Reactor Column where they are pumped to the Bottoms Still (a second
distillation column). Residual solvent is also separated in this unit. The recovered solvent is
liquefied through a compressor and cooling system and reinjected into the Reactor Column
through the Solvent Recycle Tank to repeat the cycle.

While the solvent extraction process described here has been employed in some virgin crude oil
refineries for refining of vacuum gas oils4,5, these units are not of a scale and simplicity of
operation suitable for the used oil recycling industry. As part of complex lubrication stock rerefineries in Europe, solvent extraction has been successfully applied on a relatively large scale (30
million gallons, or 114 million Liters, per year).6,7 Several patents were issued on the technology
as it was applied to asphaltic oils in refineries and to used oil recycling.8,9,10 These patents have
now expired. Although more complex than the simple distillation technology discussed above,
solvent extraction processes have the potential to be adapted for use at a scale and simplicity of
operation consistent with the capabilities of Washington States used oil businesses.

Solvent Still

Waste Oil





The potentially improved oil products produced by the solvent extraction technology could be
successfully blended into more valuable lighter diesel or heating fuel products, or into certain
lubricating oil stocks. Because the solvent extraction technology separates a greater fraction of
the impurities from the used oil than do existing low-temperature distillation technologies, fewer
contaminants are burned when the products are used as fuel. The bottoms from the solvent
technology, which resemble a light asphalt product, may also be a marketable product for such
uses as the manufacture of asphalt shingles.



This report presents the initial design and supporting documents for the construction of a pilot
scale solvent treatment plant. The objectives for the project were as follows:

Determine key process parameters to guide the design of the pilot plant;

Design a pilot scale plant that produce sufficient quantities of used oil for product

Subsequent phases of the project, subject to available funding and interested parties, will include
the construction of a pilot unit. Upon construction, the projects objectives should expand to
focus on demonstrating the technology, including:

Testing of the pilot plant under varying operating parameters, such as different used
oil sources, different solvents (propane and butane), different throughput rates, and
varying quantities of water and ash.

Testing the physical and chemical characteristics of the oil product output.

Determination of market acceptance of the products by providing interested

customers with test quantities.

Designing a full-scale facility.



An initial review of the literature was made prior to conducting the design phase of the work. The
findings are summarized here.

Much of the work on technologies for reprocessing of used oils was performed
during the 1960s and 1970s. Many reprocessing plants were severely affected by
hazardous waste regulations promulgated in the late 1970s and early 1980s,
resulting in the permanent shutdown of large segments of the industry. Most of the
used oil reprocessing that has survived appears to be based upon the low
temperature (less than 300F or 149C) distillation technology.7

At least two plants operating in Europe (Italy and the former Yugoslavia) in the
1970s used the solvent extraction process. No facility based on solvent extraction
technology has apparently been constructed in the U.S. other than a pilot scale unit
constructed by the Interline Corporation in Salt Lake City. 11

The Institut Francais du Petrole (IFP) process, a solvent treatment technology

developed in France, was reportedly successful in treating used oils to acceptable
levels. Key operating parameters are reported in the literature.4

Based on discussions with a retired Shell Oil chemical engineer with propane
extraction plant experience, the solvent de-asphalting process used by the
petroleum refining industry is very successful in removing heavy compounds from
oil.12 However, the virgin oils treated by this process (vacuum gas oils) tend to be
much heavier than used oils. The vacuum gas oils treatment plants operate at
temperatures up to 400 F (204 C) and at much higher propane pressures than
those that are suitable for small-scale facilities. Because of the difference in
operating conditions and feedstocks for used oil, it did not seem appropriate to
further research the de-asphalting process as used by the petroleum refining
industry in the U.S.

Solvent extraction is reported to be well suited for re-refining multigrade motor oils
formulated with high concentrations of pour point improvers, viscosity index
improvers, and other additives; and containing large amounts of varnish, gums, and
other asphaltic compounds generated by heat and friction in their use. The solvent
removes the mineral portion (phase) of the detergent present and precipitates water
which is loosely bound chemically and contained in the detergent and the
metalloorganic compounds. The solvent solubilization of the hydrocarbon phase
also disassociates it from the deteriorated portion of the antioxidant compounds
allowing the heavier antioxidant groups (also containing heavier metalloorganic
compounds) to precipitate. Similarly, solubilization of the hydrocarbon phase of
other additives such as the viscosity index improvers, the polar organic rust
inhibitors, and the pour point depressants causes a similar disassociation of the
deteriorated portion of these additives from the oils.7




This section of the report outlines the assumptions particular to the proposed host plant, Vintage
Oil Inc., Anacortes, WA. The Vintage Oil facility treats approximately 3,000,000 gallons
(11,350,000 Liters) per year of used oil by a process based on decanting, filtering, blending, and
low-temperature distillation. Vintage Oil is therefore able to provide a feed oil to the pilot plant
with no water, light ends (gasoline or light aliphatic solvents) or significant settleable solids.
Vintage Oil will also provide in-kind project contributions specific to project requirements such as
a secondary containment structure, electrical power, tankage, and other equipment.

Because the Vintage Oil plant has the capability of providing a relatively consistent feed
composition over a run period ranging from hours to days, a continuous process flow scheme was
adopted for the pilot plant design rather than the batch process that was initially considered. A
batch system would be advantageous for smaller or less complex systems, or where wide

variations in feedstocks could be expected. A continuous system allows for (optimally) adjusting
the process variables to make small changes in product oil composition.

Because of the pilot scale, the estimated nature of the input parameters, and the funding resources
involved, rigorous calculations and computer modeling were not employed in the design. A target
rate of 2,000 gallons (7,570 Liters) per day (approximately 730,000 gallons, or 2,760,000 Liters,
per year) used oil feed was employed, with actual feed rate to be determined under live test
conditions. The target rate is sufficient to produce the quantities of product needed for test
marketing, but less than the economically efficient scale typical of a used oil recycling facility
(typically over 2 million gallons, or 7,570,000 Liters, per year).

The operating parameters for the primary Reactor Column were determined by the literature,
primarily from the IFP process.6,9 An operating temperature of 120 F (49 C) and operating
pressure of 230 pounds per square inch gauge (psig or 1586 kPa gauge) were selected as within
the range quoted for the IFP process. Because of non-linear viscosity reducing effects, higher
operating temperatures positively affect the ability of the Reactor Column to separate impurities
from the oil (at the cost of higher resulting operating pressures and more complex process
control). The lower end of the pressure and temperature operating regime was selected for the
Reactor Column as a tradeoff between process efficiency and available vessel characteristics.

Water in the used oil influent stream was assumed to be negligible (less than 2.0% by volume) as a
design choice because of the pre-processing (dehydrating) capability of the proposed site. The
literature indicates that solvent extraction technology should be capable of treating oils with
significant water content (at least 10% by volume); however, higher oil treatment rates can be
achieved by treating dried oil. In addition, the downstream separation of bottoms from water is
simplified as well.

A key parameter to be measured during pilot testing is the solvent-to-oil ratio. The literature
indicates that a ratio of 1:1 is too low to be efficient in achieving good separation of bottoms. A
ratio of 20:1 was reported as yielding good lubrication base stock.7 Since the pilot plant was


being designed for fuel oil production, a lower ratio seemed appropriate. A nominal selection of
ratios in the range of 3:1 to 5:1 was targeted. Higher solvent to oil ratios reduce the oil
throughput and increase the solvent recovery requirements.



Design documents prepared for the pilot scale unit are presented in Figure 2, Process Flow
Diagram; Figure 3,Piping and Instrumentation Diagram; and Figure 4, Vintage Oil Solvent
Treatment Pilot Plant Equipment List.

Used oil feedstock enters Tank T-301 from the host facility at a rate of 2 gpm (7.57 Lpm).
Within tank T-301, the used oil feed is heated to approximately 173F (78 C) by a steam-heated
coil within the tank. The feed oil is pumped through pump P-101 into the in-line mixer M-101,
where it is mixed with 3 gpm (11.4 Lpm) of solvent. This solvent is added from working storage
tank T-201 via pump P-201. The proper ratio of 5:1, solvent to oil, is maintained by monitoring
flow meters on both oil and solvent lines. The oil/solvent mixture is input to the Reactor Column
D-101 through a distribution header at a point near the midpoint on the column. Solvent at a rate
of 7 gpm (26.5 Lpm) is added at a lower point to Reactor Column D-101.
Within Column D-101, the solvent acts on the used oil to solubilize the oil fraction and allow the
less soluble contaminants (with higher densities) to settle. The propane also reduces viscosity
allowing the settling to proceed more quickly, although the degree of separation is a function of
residence time within Column D-101. Although some solvent and oil is carried with the asphalt
bottoms, there is a net upward flow of solvent/oil mixture to the top of tank D-101. Liquid
solvent and oil leaves Column D-101 and is allowed to expand through valve V-110 as it enters
the Solvent Still, Column D-102. Within Column D-102, the pressure is maintained near
atmospheric and the temperature is elevated. Pressure within the column is maintained by
evacuation of solvent vapors by compressors C-201 and C-202 and by addition of heat through
the reflux oil system. Solvent vapors removed by the compressors are first routed through an oil
overflow collection trap, S-201, to prevent liquid oil from accidentally entering the compressors.
After compression, the vapors are then routed through the solvent vapor condenser H-201 before

collection in solvent storage tank T-201 for re-use. The reflux oil system uses pump P-102 to
withdraw oil from near the bottom of Column D-102 and pump it through reflux heat exchanger
H-101 where the temperature of the oil is increased by heating with steam. The hot oil is then
sprayed over the column packing to increase surface area and promote offgassing by the oil. Oil
mist is trapped within the column by mist eliminator E-101. A sidestream of product oil, the clean
fuel oil, is removed from the bottom of column D-102 which has had the substantial portion of
solvent stripped from it.

Within column D-103, the bottoms from column D-101 are maintained at an elevated temperature
of 150F (66 C) for a prolonged period (several hours or longer) to allow efficient recovery of
solvent through valve V-117 and into the solvent recovery system. As needed, the bottoms are
removed from column D-103 through pump P-103.

As designed, the process is monitored by use of flowmeters in the input oil and input solvent lines,
the solvent/oil transfer line to column D-102, the reflux oil line, the steam flow line to reflux heat
exchanger H-101, and in the clean fuel oil product line (refer to the drawing in Figure 3, the
P&ID). Flow rate from column D-101 to D-102 is used as a control parameter for valve V-110.
Temperature is monitored at one point in the reactor column D-101 and bottoms distillation tank
D-103, but at five points vertically along flash distillation column D-102. Column D-102
temperature is used to control steam flow to the reflux heat exchanger H-101. Pressure is
monitored at one point in the reactor column D-101, bottoms distillation tank D-103, and within
the solvent storage tank T-201, and at two points vertically along flash distillation column D-102.
Emergency pressure release valves were provided on each of the main columns D-101, D-102,
and D-103.

Valves for isolation and maintenance of the major components have been provided as well as for
emptying solvent from the major vessels.

ASME specifications for pressure vessels must be followed along with good engineering practice
for LPG systems. Because of the small volumes of material transferred among the vessels and


tanks of the pilot plant, the piping was sized to be consistent with low pressure drop and to match
valves, flanges, and other provided equipment provided by Vintage Oil.

Figure 4,included as Appendix A, provides the equipment list for the pilot scale treatment plant.
Where the term project specific has been applied, the host site is to supply with existing
equipment on hand.







Once a pilot plant has been constructed, testing should be directed toward evaluating the
effectiveness of the solvent technology in cleaning used oils. Specifically, the improvement of
physical and chemical characteristics of the oil product as compared to the used oil feedstocks
should be evaluated for different feedstocks. Parameters to be considered during testing include:
reduction in ash content, heavy metals content, and viscosity, and increasing flashpoint
temperatures. These parameters directly affect the potential acceptance of the product oil by the
market. Sufficient quantities of product oil should also be produced to provide potential
customers for testing in their facilities.

Future system design should investigate in greater detail the potential for product oil foaming. It
is anticipated that the solvent treatment process would remove anti-foaming agents which would
ordinarily serve to limit product oil foaming. With elevated operating temperatures, this issue
may not be problematic, but should nevertheless be considered. Evaluation of this potential pipe
fouling mechanism should be evaluated during pilot plant operation.

Stripping the clean oil from the solvent following the solvent extraction step is key to process
efficiency. Under actual conditions, separation will never be perfect. There will be some solvent
that is lost in the oil. Determining acceptable solvent losses at the pilot scale is an important
design consideration for the full-scale implementation. Effective recovery of the solvent must also
be achieved to ensure that product oil will meet flash point specifications.

The effectiveness of the solvent technology in cleaning oils containing certain soaps used in
cleaning petroleum-coated parts and equipment must be evaluated at the pilot scale since there is
a significant quantity of used oil containing these materials. Some of these soaps are ether-based
and are soluble both in oil and in water. Soap materials are very effective emulsifiers and pose
challenges to the current used oil recycling methods and potentially to the solvent technology as

The question of whether raw (wet) used oil can be treated directly or whether dehydrated used oil
must be used should also be addressed in the pilot scale testing. Additionally, the effectiveness of
the solvent technology for treating synthetic oils must be evaluated at the pilot scale since these
oils appear to be a growing fraction of the used oil stream being recycled.



In the pilot plant, a single solvent still was specified. In larger implementations, multi-stage
distillation flow sheets will probably be required for improved process efficiency. With optimal
operating point selection, recovery and liquefaction of a significant fraction of the solvent may be
accomplished using cooling towers rather than compressor capacity. This can reduce energy
requirements and operating costs.

A full-scale implementation should also take into consideration asphaltic tar handling requirements
and solvent losses in the tar. Rapid depressurization of the bottoms during transfer from the
reactor column to the bottoms distillation vessel may result in frozen solids formation or freezing
of any water present. Significant quantities of pressurized solvent will be present in the bottoms.



The used oil industry in Washington State, as well as in other parts of the U.S., is in need of a
cost-effective alternative treatment technology for upgrading used oil into more refined products,
either fuel or lubrication stocks. The solvent treatment technology presented in this report, alone
or in combination with existing used oil dehydration facilities, has the potential to significantly
reduce impurities in the product oil currently produced by used oil treatment companies.

A pilot scale solvent extraction plant is needed to refine the design, test with a wide variety of
used oil streams, evaluate treatment costs, and produce sufficient quantities of product oils and
asphalt bottoms to promote acceptance testing with customers for these products.


When a pilot unit is constructed, the remaining objectives identified in Section 1.3 above can be
accomplished: testing under varying operating parameters and different sources of oil;
characterizing the physical and chemical parameters of the product oil; determining market
acceptance of the product oils; and determining the requirements for a full-scale plant.




The following organizations contributed their time, effort, support and understanding during the
conduct of this project:
1. Vintage Oil Inc., Anacortes, Washington.
2. AERCO, Inc., P.S., Lynnwood, Washington.

ReTAP is a joint venture of the Clean Washington Center, Washington States lead agency for the
market development of recycled materials, and the National Recycling Coalition, a 3,500 member
nonprofit organization committed to maximizing the benefits of recycling. ReTAP is an affiliate
of the national Manufacturing Extension Partnership (MEP), a program of the U.S. Commerce
Departments National Institute of Standards and Technology. The MEP is a growing nationwide
network of extension services to help smaller U.S. Manufacturers improve their performance and
become more competitive. ReTAP is also sponsored by the U.S. Environmental Protection
Agency and the American Plastics Council.




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10. U.S. Patent 3,870,625, Process and Equipment for the De-Asphalting of Residues from
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