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TECHNO FEASIBILITY FOR REFINING OF USED LUBRICATING OILS AS A

VALUE ADDITION STRATEGY

Conference Paper · July 2015

DOI: 10.13140/RG.2.1.4634.0569

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 TECHNO FEASIBILITY FOR REFINING OF USED LUBRICATING OILS AS A
VALUE ADDITION STRATEGY
1
T. O. Nengiwa and 2*M.M. Manyuchi
1
Department of Chemical & Process Systems Engineering

Harare Institute of Technology, Box BE 277, Belvedere, Harare, Zimbabwe

tatendanengiwa@gmail.com
2
Department of Chemical & Process Systems Engineering

Harare Institute of Technology, Box BE 277, Belvedere, Harare, Zimbabwe

mmanyuchi@hit.ac.zw

ABSTRACT
Refining is a process of refurbishing used oil to high-quality base oil by removing
contaminants, water and spent additives. The study involves refining of 1tonne per day used
lubricating oil to produce 0.75 tonnes per day refined oil with 80% plant utilization. The
process involved dehydration, solvent extraction, hydro-treating and agitated thin film
evaporation. Process conditions were experimentally determined. Optimum conditions of 4:1
solvent ratio and 4 mBar evaporation pressure produced refined oil of 24% ash content, 98cP
viscosity, -11oC pour point, 180oC flash point and specific gravity 0.909. Detailed major
equipment design of an agitated thin film evaporator, its process control and HAZOP was
done.

Keywords: refining, used oils, lubricating oil, agitated thin film evaporation

1. INTRODUCTION
Huge amounts of used lubricating oils from automotive sources are being disposed of as
harmful waste into the environment and the cost and availability of oil and its products is
significantly impacting quality of life, thus; environmental stability, health of national
economies and even relationships between nations. Thus there is need to refine used
lubricating oil. Used lubricating oil is generated mainly from the transport sector, with its
disposal polluting the environment and also its combustion as a low grade fuel causing air
pollution. The disposal of oil does not only have a negative impact on the environment but a
waste of a valuable resource. Waste oil from the engines gets contaminated but does not lose
its original properties, thus it can be refined to retain its initial characteristic for re-use.

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 2. MATERIALS AND METHODS

Virgin oil was purchased from the local market and used oil was collected from different
garages. The used oil mixture was stirred for 5 minutes before use to insure homogeneity. All
experiments were carried out with used oils taken from this mixture. Methyl ethyl ketone
(MEK) used was of 98% purity obtained from the HIT laboratory. This study used methyl
ethyl ketone (MEK) as solvent for treatment instead of butyl alcohol and isopropyl alcohol.
This choice was due to the ease of recovery, low boiling point and low cost of the MEK and
its capability as a solvent to separate contaminants from used oil is closely related to its
solubility parameters

Apparatus

The vacuum distillation apparatus consisting of heating metal, vacuum pump, divider,
condenser and receiver, solvent extraction-settler mixer tank were used.

Experimental Procedures

The used lubricating oils were collected from various automobiles garages around Harare
CBD. The used oil mixture was then stirred for 5 minutes before use to insure homogeneity.
All experiments were carried out with used oil samples taken from this mixture.

Determination of the optimum pressure for oil dehydration

The dehydration of used lubricating oil was performed in a simple batch vacuum distillation.
Water and oil were separated by dehydration. The amount of used oil was 500ml and heat
rate was fixed at 600W. Three different vacuum pressures were investigated, 4, 8 and 12
mBar. Distillation was carried out until no further distillate was produced. The dehydrated
used oil was then collected for the next step of solvent extraction.

Determination of optimum solvent to oil ratio

The dehydrated used oil was prepared in amount of 50 mL (about 45 g) for each experiment.
The investigated solvent (MEK) to oil ratios were (2, 3, 4, 5 and 6). Solvent to oil ratio less
than 2 produced viscous mixture during separation. While when the ratio was higher than 6 to
1, operation was considered economically not feasible. According to these ratios the solvent
amounts added were (100, 150, 200, 250 and 300 mL). Adequate mixing of the solvent-oil
mixture was obtained by stirring for 5 minutes. The mixture was allowed to settle for 4 hours
in order to separate the extract phase (solvents and oil base dissolved) from the raffinate
phase (contaminants or sludge). Separation of the two phases was carried out in 1 liter
separating funnels. After 4 hours the extract phase was separated and turned to another

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separation funnel and allowed to settle in order to ensure that no contaminants will remain in
the solution. This experiment was repeated two times. The extract phase was subjected to
simple batch atmospheric distillation to recover the solvent from the oil by heating up to 200
°C. The produced oil was weighed and tested for ash content.

Determination of the optimum residence time

Hydro treating of extracted oil took place by feeding the sample into a trickle bed reactor
which serves for laboratory study of heterogeneous catalytic processes under pressure
occurring in liquid or gaseous phase. The reactor contains catalyst of Nickel. The process was
operated at: temperature: 350⁰C, pressure: 5 bars, residence time: 0.7 and hydrogen to oil
ratio: 300 mL/L. Hydrogen gas stream was supplied to the unit from a hydrogen cylinder
having a maximum pressure of 8 bars. The unit was first flushed with nitrogen to remove air,
and then kept for 4 hours under a hydrogen gas pressure of 5 bars to check any leakage. The
liquid feed and the hydrogen gas streams were injected under pressure at the top of the
reactor, both cross the different zones of the reactor in down-flow direction.

Determination of the optimum pressure for high oil recovery

The experiment was carried out by the evaporator apparatus. After each experiment, the
apparatus were washed with n-hexane solvent in order to remove any contaminants that
accumulated in the column, condenser and vacuum lines. The n-hexane washed the
contaminants and accumulated them at the bottom of the still pot where they can be removed.
After washing, all connections and joints were re-lubricated, and prepared for the next
experiment. The evaporator operation variable that was studied was: Vacuum pressure: 4 and
8mbars.

3. EXPERIMENTAL RESULTS
Dehydration of Lube Oils

Several experiments were carried out for the dehydration of used lubricating oil and the
amount of water removed is indicated in Fig. 1. The first experiment at 4 mbar was
considered the best dehydration condition. The presence of excessive water contamination
will affect the viscosity of the oil and this may give rise to emulsion formation and can also
lead to gear tooth and bearing problems.

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 Amount of water removed at various
pressures
30
Mass of water removed (g)

25
25

20

15 14.5
9.9
10

0
4 8 12
Pressure used (mBar)

Fig. 1: Amount of water removed at different pressures

Determination of Optimum Solvent to Oil Ratio

Fig. 2 indicates that the maximum ash reduction is achieved for solvent to oil ratio of 4:1.
The oil recovery and ash reduction for the same ratio are better than that obtained for solvent
to oil ratio of 3:1 and 2:1.

Solvent to oil ratio vs. weight percent product

100
90
80 Oil recovery (wt%)

70
Product weight %

Ash reduction (wt%)

60
Sulfur reduction (wt%)
50
40
30
20
10
0
2:1 ratio 3:1 ratio 4:1 ratio 5:1 ratio 6:1 ratio
Solvent to oil ratio

Fig. 2: Solvent -oil ratio vs. percent weight product

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Hydro-treating of the solvent treated oil to remove sulphur

Hydro-treating was done to remove sulphur. There was increasing of sulphur removal at high
reaction temperature as shown in Fig. 3.

Effect of residence time and temperature on

sulphur removal Temp=393K
85
Temp=403K
75
Temp=413K
65
% sulphur content

Temp=423K
55

45

35

25

15
1.4 2.2 3 3.8
residence time (1/hr)

Fig. 3: Effect of residence time and temperature on sulphur removal

4. DISCUSSION
Table 1 summarizes the analytical test results for the refined lube oil.

Table 1: Refined used oils physicochemical characteristics

Parameter Virgin lube oil (SN50) Used lube oil Refined lube oil

Flash point (oC) 245 120 230

Pour point (oC) - 12 -3 - 15

Specific gravity 0.9 0.93 0.909

Viscosity @ 100 oC 18.6 40 15

Viscosity Index 98 20 87

Flash point - The decrease in value of flash point for the used oil could be as result of the
presence of light ends of oils.

Pour point - This decrease in pour point is because of degradations of additives, which were
present in fresh oil as pour point depressants. The decrease in pour point observed also
implies that considerable amount of paraffin responsible for the initial high pour point has

5|Page
been removed, thereby reducing the difficulty of pumping the oil to burners. These results
show that the refining method is comparatively better than other methods used in the past.

Specific gravity - The value of specific gravity of used engine oil is slightly above that of
fresh oil. It could be lower or higher than fresh engine oil depending on the nature and type of
contaminations.

Viscosity - The decrease in viscosity of used oil value is attributed to the removal of aromatic
contents that are normally responsible for the high viscosity value. The result of the viscosity
test shows that, the used lube oil has lost most of its viscosity due to contamination.
However, refining has restored most of its viscosity. This can be attributed to possible
conversion of contaminants by hydrogenation and their removal.

Table 2: SPSS analysis of dehydration results

The value R= -0.999 shows that there is a strong negative correlation between the pressure
used and the amount of water removed, thus the lower the pressure the more water removed
from the oil and R2=0.997 implies that 99.7% of the water removed is attributed to the
pressure applied thus in order to remove maximum water in the oil, pressure has to be
optimized and monitored.

SPSS analysis of solvent-oil ratio experiment

SPSS software was used to analyse the results as shown in Table 3.

Table 3: SPSS analysis of optimum solvent ratio results

Beta value for temperature is 0.058 implying temperature has no impact on the oil recovery
yield since the value is very small and that for solvent to oil ratio is 0.894. This means that
solvent to oil ratio has an impact on the oil recovered and has to be optimised in order to
recover the highest amount of oil possible.

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SPSS analysis of effect of residence time and temperature on sulphur removal

SPSS was used to analyse the correlation between the dependent (sulphur removal) and the
independent variables (temperature and residence time) as in Table 4.

Table 4: SPSS on effect between residence time, temperature on sulphur removal

Since R= 0.993, it means that there is a strong correlation between the various parameters
which were being investigated. R2 = 0.984, means that 98.4% of the changes in sulphur
content of the oil are being caused by the changes in residence time and temperature.

Table 5: SPSS analysis on the effect of residence time on sulphur removal

Beta value for temperature is 0.848 and that for residence time is -0.517. This means that
both variables have an impact on the sulphur removal with residence time having a negative
one implying that the smaller the residence time the higher the sulphur content removed.

The best oil recovery and ash reduction by extraction that were obtained using optimum
evaluated solvent to oil ratio of 4:1 were 65% ash reduction and 75 % oil recovery. On the
basis of experimental work, it was found that this method effectively removed contaminants
from used lubricating base oil and returned the oil to a quality essentially equivalent to oils
produced by fresh lube oil stocks. The results have clearly showed that during purification of
fuel oil, the sulphur content as major impurity is significantly reduced. Also, there is
improvement in viscosity, specific gravity, pour and flash points. This has shown that
aromatics, carbon residues, and ash of the oil have been reduced. Therefore, it is possible to
refine used lubricating oil.

Equipment Design

Agitated thin film evaporator spreads a thin layer or film of liquid on one side of a metallic
wall, with heat supplied to the other side. It has a vertical cylinder where the feed material is
distributed to the inner surface. As the liquid flows downward, axially arranged blades
distribute the liquid as a thin film, which is constantly mixed. This type of equipment can

7|Page
operate at very low pressure and provides minimum pressure drop. Because of low pressure
drop during gas flow inside the evaporator the boiling temperature of liquid, which is
evaporated, depends only on its composition and does not depend on liquid position in the
evaporator.

Fig 3: Agitated thin film evaporator 2D drawings

Chemical engineering design for the agitated thin film evaporator

Table 6 below shows the chemical engineering design parameters for the ATFE.

Table 6: Agitated thin film evaporator design specifications

Item Agitated Thin film Evaporator

No. required 1

Function Purification of used lube oil into base oil

Operation Continuous

Effective Heat transfer area 7.1m2

Total Heat Transfer Area 8.7m2

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 Overall heat transfer coefficient (Ua) 280 kcal/hr-m2oC

Diameter 0.5 m

Total height 2.2 m

Design pressure 6 mbar

Temperature 250 0C

Jacket Thickness 10 mm

Insulation Thickness 45 mm

Material of Construction Low carbon steel 304

Agitator Design

A 3 - level agitator was designed.

Table 7: Agitator design summary

Agitator

Number required 1

No. of blades 9

Blade Length 0.21 m

Blade Width 0.033 m

Blade Arrangement 120 0 apart

Impeller diameter 0.17 m

No. of baffles 4

Baffle height 1.6

Baffle Width 0.05 m

Agitator speed 115 rpm

Agitator Power 0.5 hp

Material of construction Low carbon steel 301

Mechanical Design

The mechanical design specifications are given in Table 8.

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Table 8: Agitated thin film evaporator mechanical specifications

Parameter Value

Stress on the walls 0.04 Pa

Weight of contents 1 774 N

Maximum tensile strength 6.72 N

Maximum compressive strength 18.962 N

Shell thickness 15 mm

Wind load 5.6 kN

Temperature Control

The temperature of the crude oil is raised from 100⁰C to 250⁰C. A Proportional Integral (PI)
controller was used. Thermocouples were used as sensing elements and were implemented in
the control architecture. The liquid temperature is maintained at 250⁰C. At this temperature
only base oil is in gas form. The flow rate of steam is manipulated to control the temperature
of the process fluid. A combination of feedback and feed-forward control schemes was used
to ensure good results.

Feed forward scheme was achieved by measuring the inlet temperature of oil and sending the
information to the PI controller. If the temperature has deviated from the set point (250⁰C)
the thermocouple sensor sends information to the transmitter. The transmitter converts the
reading from the thermocouple to a standard signal and transmits it to the PI controller. PI
control uses an algorithm that is proportional to the difference between a set point (SP) and a
process variable (PV) which in this case is temperature, and integral time-function
algorithms, which provide a continuous-control process output to meet the desired set point.
The PI controllers sends a correcting signal to a converter which converts the correction
signal to pneumatic signal and send it to an actuator. If the temperature is too hot, the control
valve was adjusted to decrease steam flow rate. If the temperature is too low the valve is
adjusted to increase steam flow rate, thus increasing the amount of heat exchanged and
temperature of the process fluid increases. Pressure is controlled as it affects relative
volatility, temperature difference as well as process safety. A vacuum pump is installed to
maintain the vacuum system needed. If there is an excessive increase in pressure the bypass
valve opens and releases pressure. The control loop is given in the Fig 4 below.

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 transmitter
TC

Convertor
actuator
converter

actuator

FC thermocouple

T
I-1
Lube oil L steam
EVAPORATOR
373K

Pressure
V-1 sensor Base Oil at 523K
V-1
actuator
PC
to vacuum pump

V-2

convertor

Fig 4: Agitated thin film evaporator process control loop

HAZOP Analysis of agitated thin film evaporator

HAZOP Analysis for the agitated thin film evaporator was done in Table 9.

Table 9: HAZOP Analysis for the Agitated thin film evaporator

Parameter Guide Possible causes Possible Action required

word consequences

Temperature More More available Product quality low PI control action

steam as residue can also

Failure of control evaporate

valve

Less Less available Low base oil yield PI control

steam Poor heat transfer
High fouling rate

Pressure High Vacuum pump Low product yield Operator alert.

valve failure Proper
maintenance.

Low Vacuum pump No separation Repair pump

failure Oil quality poor

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 5. CONCLUSION
Optimum conditions of 4:1 solvent ratio and 4 mBar evaporation pressure produced refined
oil of 24% ash content, 15cp viscosity at 100 oC, -15oC pour point, 230oC flash point,
viscosity index of 87 and specific gravity 0.909. These parameters if slightly adjusted using
additives results in refined lubricating oil grade 50.

Refining of used lubricating oils promotes sustainable development since it deals with
chemical waste management and disposal.

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