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Maki-Arvela
Abstract
The European oil rerefining industry is comprised of 28 plants treating waste oil, which represent one-third in volume of the
total European market for lubricants. The biggest European rerefineries with capacity greater than 40 000 tons/year apply
various technologies for recycling of used oils from different sources. Used oil recycling technology has undergone significant
changes over the past decade. With the newly developed rerefining technologies it is possible to produce higher quality
base oil compared with the traditional and old acid clay methods. Currently in Europe the following re-refining methods are
widely used: solvent extraction (N-methyl-2-pyrrolidone (Germany), Interline process (United Kingdom, Spain)); combined
vacuum distillation and solvent extraction (Vaxon process (Denmark, Spain); hydroprocessing (Hylube process (Germany));
combined thin film evaporation and hydrofinishing (CEP process (Finland)); combined thermal de-asphalting and hydrofinishing
(Revivoil process (Italy, Poland, and Spain)). The majority of applied technologies in Europe is appropriate for rerefining of
synthetic lubricating oils, which currently are replacing the conventional mineral lube oils due to their enhanced performance
characteristics. However, for the rerefining technologies applying alkaline treatment (CEP, Vaxon) and hydrofinishing step
(Cyclon, Snamprogetti, Revivoil) the amount of synthetic or semi-synthetic oils based on esters in the feedstock should be
eliminated, since these oils are less stable under alkali and hydrofinishing conditions.
c 2013 Society of Chemical Industry
Keywords: solvent extraction; hydrofinishing; used oil rerefining; base oil; thin film evaporation
INTRODUCTION
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Table 1. Overview of European lube consumption, used oil collection and recycling industry8
Country
Lubricants
consumption 2006,
tons103 /year
Germany
1174
45
798
United Kingdom
France
Spain
800
765
545
44
30
29
50*
125
184
Italy
542
40
303
Poland
351
22
Netherlands
Belgium
Greece
Finland
Denmark
252
142
100
79
68
20
42
36
29
30
Collected
used oil 2006, %
Total used
oil capacity
2010, tons103
88*
170
40
52
60
40
Applied technologies
Hylube
MRD process
Acid/clay treatment
and others
Interline
Ecohuile process
Interline
Vaxon
Revivoil
and others
Revivoil
Snamprogetti
Acid/clay
and others
Revivoil
and others
Propak thermal cracking process
Cyclon and others
CEP process
Vaxon
Products
base oils + by-products; fuels
*2009
with virgin base oils. The principle of refining waste oils utilizes the
following four steps: dewatering and defueling, de-asphalting,
fractionation and finishing process.16,17 The rerefining process is
depicted schematically in Fig. 1.
As mentioned earlier, the majority of collected lube oils in
Europe is automotive oils. The main functions of lubricating oils
include reducing friction, carrying away heat, protecting against
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Compound
Base oil
Viscosity index improvers (polyisobutylene,
polymethacrylate)
Oxidation inhibitor (zinc dialkyl, dithiophosphate)
Detergent (barium and calcium sulphonates or
phenates)
Multi-functional additives (dispersant, pour point
depressant)
86
5
1
4
4
Sulfur, wt%
I
II
III
IV
V
Saturates, wt%
Viscosity index
<90
80119
90
80119
90
120
All polyalphaolefins (PAOs)
All others not included in Groups I, II, III or IV
>0.03
0.03
0.03
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Water content, %
Density at 15 C, kg m-3
Kinematic viscosity at 40 C, mm2 s-1
Flash point, C
Total acid number, mg KOH g-1
Sulfur content, mg kg-1
Zinc content, mg kg-1
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Used oil
10
900
80
>60
<2.4
4000
650
Rerefined oil
light
heavy
light
<1
<1
<1
215
4.0
4000
650
154
1.5
3000
<1
193
0.5
3000
<1
182
0.01
600
<1
210
0.01
600
<1
heavy
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855
215
12
29.5
5.2
115
100
90
860
228
12
58
8.4
116
100
90
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Hylube process
Germany is the leader both in lubricants consumption and
rerefining according to the European Re-refining Industry section
of the Independent Union of the European Lubricants Industry
(GEIR) data (Table 1). About 44% of the total used oil capacity goes
to base oil production; the remainder is used for other products
including fuels, transformer oils, gasoil, etc. The Hylube process
allows production of mainly base oils.
The HyLube process is a proprietary process developed by
Universal Oil Products (UOP) for the catalytic processing of used
lube oils into rerefined lube base stocks for reblending into saleable
lube base oils.23 This is the first rerefining process in which as
received used oil is processed, without any pretreatment, in a
pressurized hydrogen environment.
A typical HyLube process feedstock consists of a blend of used
lube oils containing high concentrations of particulate matter such
as iron and spent additive contaminants such as zinc, phosphorous,
and calcium.21
A HyLube process unit has been successfully commercialized
by Puralube GmbH located in Elsteraue / Zeitz, Germany, using
technology licensed to Puralube by UOP LLC. A simplified block
diagram of the process is shown in Fig. 3. The first part of
the process involves separation of the lube range and lighter
components of the feed from the non-distillable residue portion.
After the separation step the light feed is flowed through the
so-called guard reactor where metal-containing compounds and
other impurities are accumulated in the large pore size catalyst.
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lube oil recovery from the lube boiling range hydrocarbon in the
feedstock.
Raffinerie Dollbergen (MRD) solvent extraction
Mineralol
process using N-methyl-2-pyrrolidone
Mineralol-Raffinerie
is the best known and largest rerefinery in
Germany, located near Hanover in an area with a distinctly rural
character. This technology has been processing and recycling
used oil and oily liquids since 1955. Today, the refinery has the
capacity to process 230 000 tons/year of used oil and oil-containing
liquids. Of these, 120 000 tons/year are used as feedstock for the
production of 70 000 tons/year of new base oils.26
The applied oil rerefining process is based on a patent held
by AVISTA OIL.27 The Enhanced Selective Refining process uses
solvent N-methyl-2-pyrrolidone (NMP), which is commonly used
in the petroleum refining industry. NMP is a powerful, aprotic
solvent with low volatility, which shows selective affinity for
unsaturated hydrocarbons, aromatics, and sulfur compounds. Due
to its relative non-reactivity and high selectivity, NMP finds wide
applicability as an aromatic extraction solvent in lube oil rerefining.
The advantages of NMP over other solvents are the non-toxic
nature and high solvent power, absence of azeotropes formation
with hydrocarbons, the ease of recovery from solutes and its high
selectivity for aromatic hydrocarbons. Being a selective solvent
for aromatic hydrocarbons and PAH, NMP can be used for the
rerefining of waste oils with lower sludge, carbonaceous particles
and polymer contents, such as waste insulating, hydraulic and
other similar industrial oils.28
The MRD solvent extraction process uses the liquidliquid
extraction principle. Figure 4 provides the flow chart of the
process. Vacuum distillates from the flash distillation are used
as feed. These distillates are processed in a production cycle which
can be adjusted to the quantity to be processed. Before the
distillate enters the extraction column, any residues of dissolved
oxygen in the distillate are removed in an absorber using steam.
Properties
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Figure 4. Block flow diagram of the MRD Solvent extraction process using
N-methyl-2-pyrrolidone adapted from Ref 26.
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Density at 15 C, kg m-3
Flash point, C
Pour point, C
Kinematic viscosity at
40 C, mm2 s-1
Kinematic viscosity at
100 C, mm2 s-1
Viscosity index
Sulfur content, wt%
852856
>220
12
2226
857860
>230
9
3236
860865
>230
9
4046
4.44.9
5.55.6
6.47.1
108112
0.25
110115
0.25
110115
0.25
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Figure 5. Vaxon process block flow diagram adapted from Refs 1,15, 31.
CEP process
The process was designed by Chemical Engineering Partners (CEP),
a process technology company offering a range of products and
services for rerefining waste lubricating oils. The CEP process is
located in Hamina, Finland and has a capacity of 60 000 tons/year
with base oil production of 42 000 tons/year.
The process combines thin film evaporation and hydroprocessing (Fig. 6). The used oil is chemically pretreated to avoid
precipitation of contaminants which can cause corrosion and
fouling of the equipment. The pretreating step is carried out
at temperatures from 80170 C. The chemical treatment compound comprises sodium hydroxide, which is added in a sufficient
amount to give a pH about 6.5 or higher.32 The pre-treated used
oil is first distilled for separation of water and light hydrocarbons.
Water is treated and sent to a waste water treatment facility. Light
hydrocarbons are used at the plant as fuel or sold as a product.
Thereafter, free-of-water oil is distilled under high vacuum in a thin
film evaporator for separation of diesel fuel, which can be used at
the plant or sold as fuel. Heavy materials such as residues, metals,
additive degradation products, etc. are passed to a heavy asphalt
flux stream.
The distillate is hydropurified at high temperature (315 C) and
pressure (90 bar) in a catalytic fixed bed reactor.37 This process
removes nitrogen, sulphur, chlorine and oxygenated organic
components.
In the final stage of the process, three hydrotreating (Hydrofinishing) reactors are used in series to reduce sulfur to less than
300 ppm and to increase the amount of saturated compounds to
over 95%, in order to meet the key specifications for API Group II
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Mineralol-Raffinerie
Dollbergen GmbH in Dollbergen, Germany,
Dansk Olie Genbrug A/S in Kahlundborg, Denmark and the North
Refining and Trading N.V., Netherlands. Furthermore, Avista Oil
holds a majority holding of about 75% in the Dutch rerefining
market since August 2012. In connection with this fact, the lube
distillate obtained from the Vaxon process (Denmark) or North
Refining (Netherlands) are precursors for the Avista Oil base, the
properties of which are listed in Table 6.
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base oil (Table 7). The final step is vacuum distillation to separate
the hydrotreated base oil into multiple viscosity cuts in the
fractionator.
Hydroprocessing technology is one of the most widely used
distillation processes to eliminate undesirable components such
as sulphur, nitrogen, metals or unsaturated hydrocarbons. The
yield of base oils is about 70%.34
Ecohuile process
Ecohuile claims to rerefine about 125 000 tons of used oil annually
on the Lillebonne site, recycling 45% of the used motor oils
collected in France. The recycled oil corresponds to 10% of the
base oil market in France.
The rerefining process was based on vacuum distillation and
acid-clay treatment steps until the end of 2000.35 Clay adsorption
was banned on 1 January 2001 and the plant was modified and
upgraded to the Sotulub process.36 Moreover, the addition of
injection facilities of so-called Antipoll-additive (13 wt% of pure
sodium hydroxide) has been provided and has allowed solving the
following basic problems:
corrosion of dehydration column and cracking column top
section due to the organic acidity of the used oil;
plugging of equipment and piping due to polymer formation in
the cracking section;
high losses of base oil in the oily clay due to the high
consumption of clay.
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Figure 7. Block flow diagram of the Sotulube process adapted from Ref 1.
Properties
Flash point, C
Pour point, C
Kinematic viscosity at 40 C, mm2 s-1
Metal contents, ppm
>200
<6
2733
<0.5 each
Heavy grade
SN 400
>230
<6
7685
<0.5 each
Cyclon process
The process licence belongs to Kinetic Technology International
(KTI).38 The industrial plant to implement the KTI Relube process
was built in Greece for LPC in 1982.35 Greek Cyclon Hellas Company
currently uses this technology with an annual capacity of 40 000
tons.
The process flow diagram of the Cyclon process is illustrated
in Fig. 8. Used oils taken from storage tanks are dewatered and
the light hydrocarbons are removed by distillation. The heavier
fraction is sent to high vacuum distillation, where the majority of
base oil components are evaporated from the heavy residue. The
oils in the residues are extracted with propane in the de-asphalting
unit and sent to the hydroprocessing unit where the other oils are
processed. Then they are treated with hydrogen and fractionated
based on the desired base oil features.
The rerefined base oil products have high quality due to the
hydrogenation.39,40 Information on the physical properties of the
obtained oils is not available in the literature.
Revivoil process
The Revivoil process was developed jointly by Axens and
Viscolube41 in Viscolube facilities. Currently the Revivoil process is
applied in the following locations:
a 130 000 tons/year plant in Italy (Pieve Fissiraga);
a 80 000 tons/year plant in Poland (Jedlicze);
a 59 000 tons/year plant in Spain (Huelva).
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Light
grade
Density at 15 C, kg m-3
852
16.5
Kinematic viscosity at 40 C, mm2 s-1
3.6
Kinematic viscosity at 100 C, mm2 s-1
Viscosity index
101
Sulfur content, wt ppm
<300
Medium
grade
853
30.6
5.3
106
<300
Heavy
grade
858
55.2
7.8
107
<300
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Properties
Flash point, C
Pour point, C
Kinematic viscosity at 100 C, mm2 s-1
Viscosity index
Saturates, %wt
Figure 11. Block flow diagram the Interline process adapted from
Refs 1, 21, 42.
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The Interline process is depicted in Fig. 11. The used oil is pretreated with a basic solution containing ammonium hydroxide
and/or potassium hydroxide for neutralization of undesirable
compounds. Pre-treated in this way, oil is mixed with propane,
which has a high selectivity for hydrocarbons, and then sent to the
solvent mixing and extraction vessel. Most of the additives, water
and other insoluble compounds are separated from the propanebase oil mixture. The solids and water settle to the bottom and
enter the residuewater separator where water is separated from
a tar-like material which goes to the asphalt blending tank. In this
tank, the tarlike material is blended with the vacuum distillation
residue to produce an asphalt extender-modifier product. The
water is purified and returned to the environment. The solventoil
mixture is pumped to an oilsolvent separation system. The
propane is re-condensed with cooling water and returned to the
solvent vessel. Solvent-free oil is then stripped to remove light
hydrocarbons and the remaining propane. The flash adjusted
oil is then directed to a traditional vacuum distillation column.
The distilled lubricant oil product is a base oil (Table 10), which
is classified as group I according to API Publications, although,
by saturates content (9192%) and viscosity index (>100), the
product oil could be considered in group II (Table 4).47
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235
9
5.05.5
>100
>91
Heavy grade
SN-300
245
9
7.58.0
>100
>91
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Figure 13. A block flow diagram the typical solvent extraction unit adapted
from Ref. 53.
Figure 12. Block flow diagram the Propak thermal cracking process
adapted from Refs 1, 21.
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Figure 14. Flow diagram of hydrofinishing unit adapted from Ref 53.
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The drawback of solvent extraction technology is the dependence of the product oil quality on the quality of the feedstock,
since this process is a physical one and does not involve any
chemical reactions with formation of the desired hydrocarbon
structures. The process leads to diminishing concentrations
of polychlorinated biphenylenes, aromatic compounds and
specifically polycyclic aromatic hydrocarbons, which were formed
during the oil use. Thereby the solvent extraction technology
allows the production of the re-refined oil bases of the same but
not superior quality to the feedstock base oils.
The MRD process belongs to the new generation processes,
where NMP is applied as a solvent instead of propane as used
in the Interline process. NMP has a lower toxicity and a higher
selectivity to the undesired species than propane. Moreover NMP
can be used at lower solventoil ratios, saving energy, thus, the
MRD process can be more economically attractive than Interline.
The MRD process demonstrates higher yield of the product oil
of about 91% than the product yield in Interline process which
is c. 79%. The quality of MRD-product oils is slightly higher than
Interline-oils, the viscosity indexes are about 110 and 100 in MRD
and Interline processes, respectively. Since the Interline process
contains alkaline pretreatment of used oil, the amount of vegetable
and some types of synthetic oils should be eliminated due to their
instability under alkaline conditions.
Vaxon and EcoHuile (Sotulub) processes are based on the
vacuum distillation of oil cuts in thin film evaporators, which reduce
coking caused by cracking of the hydrocarbons and oil impurities
at high temperatures. Both processes apply alkaline pretreatment
of the used oils, which requires the elimination of synthetic and
vegetable oils in the feedstock. The Vaxon process has an additional
facility of solvent extraction treatment, which allows generation of
product oils with higher quality compared with Ecohuile-products.
Nevertheless, the quality of products is worse than in the above
solvent extraction processes. In order to produce high quality
base oils finishing steps should be added in these technologies,
however such revamps will increase operating and capital costs
and the processes could become less financially attractive.
Hydrofinishing processes are applied in such technologies as
Hylube, CEP, Revivoil, Snamprogetti and Cyclon processes. The
advantages of these technologies are listed below:
Hylube technology applying hydroprocessing allows production of high quality base oil products, in which viscosity index is
Feedstock
Investment costs
Product quality
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Cyclon process
Interline
1. Solvent extraction
MRD process
Technology
Residueasphalt extender.
Finishing process can be
chemical treatment or solvent
extraction
6570
72
72
Used catalyst of
hydropurification - disposed
off-site.
70
7480
85
8292
Comments
79
91
Oil yield, %
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higher than 110 and sulfur content is less than 100 ppm. The process feedstock is oils from different sources, however, a key factor
in maintaining stable Hylube catalyst activity is minimization of
the inorganic contaminants level in the reactor feed. Thus, careful
monitoring of the used oil for known catalyst poisons such as
arsenic and silicon is needed, moreover, some synthetic oils that
are unstable in hydroprocessing conditions should be eliminated.
The high quality of the products obtained is compensated by
relatively high capital investment and operating costs.
The CEP process, which is a combination of TFE and hydrofininshing step, produces high quality product oils comparable with
Hylube-products. Since this process applies caustic pretreatment
of the used oil, the amount of vegetable oils and some types of
synthetic oils should be eliminated. Off-site catalyst regeneration
causes an increase in the operating and capital costs.
The Revivoil process accepts all type of used oils. Thermal deasphalting combined with hydrofinishing allows generation of
high quality products with a yield of about 72%. The advantage of
this technology is regeneration of the used catalysts.
The advantage of processes applying solvent extraction
combined with hydrofinishing (Snamprogetti and Cyclon) is its
acceptance of all types of used oil. Similar to all technologies
applying hydroprocessing the product oil quality is high with
yields of c. 7280. Drawbacks are high operating and capital costs,
since both technologies use propane, which belongs to the old
generation of solvents. Propane requires high solventoil ratios,
which increases energy consumption; moreover losses of propane
in the Snamprogetti process are about 510%.
In terms of the qualities of the feedstock required to obtain the
desired product, high quality base oils API Group II/II+ can be
obtained by solvent extraction methods only when the reaction
mixture is homogeneous. Therefore the quality of the base oil
produced with this technology is directly related to the quality
of feedstock, while hydrofinishing technology allows base oil API
Group II to be obtained independently of the quality of the
feedstock. The major drawback of hydroprocessing is the catalyst
sensitivity and poisoning; in this regard feedstock pretreatment is
necessary to prevent catalyst deactivation. However, technologies
applying alkali treating agents (CEP, Vaxon, Ecohuile and Interline)
cannot be used for rerefining vegetable and some types of
synthetic oils. Thus, the yield and selection of the operation
conditions are strongly dependent on the composition and
properties of the feedstock.
CONCLUSIONS
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