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Nile Blend Crude Oil: Wax Separation Using MEK-Toluene Mixtures

Article in Arabian Journal for Science and Engineering · January 2009

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 ‫‪Amel A Nimer,, Abdelshakour A. Mohamed and Ali A. Rabah‬‬

‫‪NILE BLEND CRUDE OIL: WAX SEPARATION USING‬‬

‫‪MEK-TOLUENE MIXTURES‬‬

‫* ‪Amel A Nimer, Abdelshakour A. Mohamed and Ali A. Rabah‬‬

‫‪Department of Chemical Engineering, University of Khartoum‬‬
‫‪P.O. Box 321, Khartoum, Sudan‬‬

‫اﻟﺨﻼﺻـﺔ‪:‬‬
‫ﺗﻘﺪم هﺬﻩ اﻟﻮرﻗﺔ اﻟﻈﺮوف اﻟﺘﺸﻐﻴﻠﻴﺔ ﻹﻧﺘﺎج اﻟﺸﻤﻊ ﻣﻦ ﻣﺰﻳﺞ اﻟﻨﻴﻞ ‪ ,‬وﻳﻌﺪ اﻟﺰﻳﺖ اﻟﺴﻮداﻧﻲ زﻳﺘًﺎ ﺣﻠﻮًا ﺑﻨﺴﺒﺔ ﻋﺎﻟﻴﺔ ﻣﻦ ﻣﺤﺘﻮى اﻟﺸﻤﻊ )‪25.87 %‬‬
‫ﺑﺎﻟﻮزن(‪ .‬وﻗﺪ ﺗﻢ ﻋﻤﻞ ﻃﺮﻳﻘﺔ اﺳﺘﺨﺪام اﻟﻤﺬﻳﺐ ﺑﺎﺳﺘﺨﺪام ﺧﻠﻴﻂ اﻟﺘﻮﻟﻴﻦ ﻣﻴﺜﻴﻞ اﻳﺜﻴﻞ آﻴﺘﻮن )‪ .(MEK‬وﻗﺪ ﺷﻤﻠﺖ اﻟﺪراﺳﺔ ﻣﺠﻤﻮﻋﺔ واﺳﻌﺔ ﻣﻦ درﺟﺎت ﺣﺮارة‬
‫اﻟﺨﻠﻂ )‪ (28-70C‬ووﻗﺖ اﻹﻗﺎﻣﺔ )‪30-5‬دﻗﻴﻘﺔ( وﻧﺴﺒﺔ اﻟﻤﺬﻳﺐ إﻟﻰ اﻟﺰﻳﺖ ) ‪16:1‬إﻟﻰ ‪ (32:1‬وﺗﺮآﻴﺒﻪ اﻟﻤﺬﻳﺐ )‪.(50-100%MEK‬‬
‫وﻗﺪ اﻇﻬﺮت اﻟﻨﺘﻴﺠﺔ ان ‪ 92 %‬ﻣﻦ اﻟﺸﻤﻊ اﻟﺨﺎم ﻳﻤﻜﻦ اﺳﺘﺨﺮاﺟﻬﺎ ﺑﺨﻠﻴﻂ ‪75V%MEK‬ﻋﻨﺪ درﺟﺔ ﺣﺮارة اﻟﺨﻠﻂ ‪ 50C‬وزﻣﻦ إﻗﺎﻣﺔ ‪ 20‬دﻗﻴﻘﺔ‬
‫وﻧﺴﺒﺔ اﻟﻤﺬﻳﺐ إﻟﻰ اﻟﺰﻳﺖ ‪20:1‬ﻋﻨﺪ درﺟﺔ ﺣﺮارة اﻟﺘﺮﺷﻴﺢ ‪.17C0‬‬
‫وﻳﺘﻤﻴﺰ ﻣﻨﺘﻮج اﻟﺸﻤﻊ ﺑﻤﻠﻤﺲ دهﻨﻲ ﺧﻔﻴﻒ ﻗﺎﺑﻞ ﻟﻠﺬوﺑﺎن ﻓﻲ اﻟﻨﻔﺜﺎ‪ ,‬وﺗﻮﻟﻴﻦ ‪ ,‬واآﺴﻴﻠﻴﻦ‪ ,‬وآﻴﺮوﺳﻴﻦ ‪ ,‬وﺑﻨﺰﻳﻦ ‪ ,‬واﻳﺜﻴﻞ اﻟﻜﺤﻮل ‪ ،‬واﻳﺴﺘﻮن ‪ ,‬وراﺑﻊ آﻠﻮرﻳﺪ‬
‫اﻟﻜﺮﺑﻮن ‪.‬‬
‫وﻗﺪ اﻇﻬﺮت ﺗﺤﺎﻟﻴﻞ اﻟﻤﻄﻴﺎف أن اﻟﻤﻨﺘﺠﺎت اﻟﺨﻔﻴﻔﺔ )‪ (C10-C16‬ﺗﺤﺘﻮي ﻋﻠﻰ ‪ 6%‬ﻣﻦ اﻟﺸﻤﻊ اﻟﻤﻨﺘﺞ و ‪ C45+‬ﻳﺸﻜﻞ ‪.10%‬‬

‫_______________‬
‫‪*Corresponding Author:‬‬
‫‪E-mail: rabahss@hotmail.com‬‬
‫________________________________________________________________________________________________________‬
‫‪Paper Received May 14, 2009; Paper Revised September 10, 2009; Paper Accepted October 12, 2009‬‬

‫‪October 2010‬‬ ‫‪The Arabian Journal for Science and Engineering, Volume 35, Number 2B‬‬ ‫‪17‬‬
 Amel A Nimer,, Abdelshakour A. Mohamed and Ali A. Rabah

ABSTRACT
This paper presents the operational conditions for wax production from Nile Blend; a Sudanese oil, characterized
as sweet oil with a high level of wax content (25.87 wt%). The method of solvent extraction was employed using a
Methyl Ethyl Ketone (MEK)- Toluene mixture as a solvent. The study covered a wide range of mixing temperatures
(28 to 70 oC) and residence time (5 to 30 minutes), solvent to oil ratio (16:1 to 32:1), and solvent compositions (50-
100%MEK). The result showed that 92% of the wax in the crude can be extracted with a mixture of 75v% MEK at a
mixing temperature of 50 oC, residence time of 20 minutes, and solvent to oil ratio of 20:1 at a filtration temperature
of -17 oC. The wax produced is characterized by a slightly greasy feel and is soluble in Naphtha, Toluene, Xylene,
Kerosene, Benzene, Ethyl Alcohol, Acetone, and Carbon Tetra Chloride. The gas chromography analysis showed
that the light products (C10-C16) constitute 6% of the produced wax and C45+ is 10%.
Key words: Nile blend, dewaxing, MEK-Toluene mixtures

18 The Arabian Journal for Science and Engineering, Volume 35, Number 2B October 2010
 Amel A Nimer,, Abdelshakour A. Mohamed and Ali A. Rabah

NILE BLEND CRUDE OIL: WAX SEPARATION USING MEK-TOLUENE MIXTURES

1. INTRODUCTION
On delivery to the refinery, the storage of waxy crude stream is difficult as it produces massive gel and sludge in
the storage tank [1]. This raises pumping expenses and cleaning costs. To overcome this problem, chemical
additives, known as pour point depressants (PPD), are state-of-the-art practice. Recent studies have indicated that
these chemicals are the prime cause of corrosion in equipment and piping systems of the refinery [2]. If the wax
could be removed prior to shipment to the internal refinery process, the problems of accumulation in storage and
piping system corrosion caused by chemical additives could be minimized. These are the justifications of this work.
Due to the fact that the commercial production of Nile Blend started in the late 1990’s, the available literature
regarding its thermodynamic characteristics are extremely limited. On the other hand, the dewaxing process is
mostly aimed at the feedstock of lube oil, the bottom product of atmospheric or vacuum distillate. Hence, the
available literature on dewaxing is mostly concerned with dewaxing of lube oil feedstock.
There are mainly two different methods for wax removal: solvent and catalytic. Solvent dewaxing is more
selective for removing both heavier normal and non-normal hydrocarbons. Catalytic dewaxing removes the normal
paraffins more evenly over the boiling range, while the light non-normal hydrocarbon are removed more selectively.
Oil obtained from solvent dewaxing has higher yield and viscosity index than that of catalytic dewaxing [3]. The
removal of wax from oil by means of solvent extraction involves mixing crude oil with solvent to form a solution
followed by cooling (chilling) the mixture (oil + solvent + wax) to form wax-crystal-lattice and, finally, separating
the crystal lattice from the solution. The dewaxing is influenced by many parameters such as type of solvents,
cooling rate, and temperature and solvent to oil ratio.
Several pure solvents or mixtures of solvents have been in use for solvent dewaxing. These include
Methylisobutylketone (MIBK), Dichloromethane, Trichlorethylene, and a mixture of Methyl Ethyl Ketone (MEK)
and Toluene and MEK/Benzene. Pure Toluene is an excellent oil solvent, and, has good solvent power for wax as
well. If it is used alone, a tight lattice of wax will form that hinders filtration [4]. In contrast, MEK shows low
solvent power to paraffinic compound (i.e., low selectivity) and as such it precipitates the wax very well. Previous
studies on Arabian light oil indicated that optimum wax separation occurs at MEK-toluene solvent composition
ranges from 40–75 v% MEK [4, 5]. Dewaxing of West Siberian crude with MEK-Toluene mixtures indicated that
with increasing MEK in the mixture, the filtration time increases (i.e., the filtration viscosity increases) and the oil
yield decreases. With increasing MEK, the viscosity of the oil index increases, but the solid point remains constant
[6].
In solvent dewaxing, most of the energy consumption goes into pumping and regeneration of solvent. Therefore,
the current trend is to use lower solvent dilution ratios and smaller amounts of solvent in washing the precipitate
(wax cake) on filters. At the other hand, an increase in solvent to oil ratio will enhance the filtration rate because
solvent prompts the crystal growth and lowers the viscosity of the mixture (oil + solvent). It also increases the
dewaxed oil yield and decreases the oil content in the wax yield. The previous literature indicates that the solvent to
oil ratio is between 16:1 to 32:1 on mass basis [7].
The rate of cooling (high or low) has a strong influence on crystal formation and particle characteristic. For
example, a high cooling rate is found to promote the formation of small crystals but they are of the needle type that
clogs the filter. Previous experiments showed that the optimum cooling rate varies between 0.56–4.4 oC per minute
depending on the type of crude oil. The chilling or filtration temperature is usually in the order of -20 oC [8].
Due to the fact that crude oil differs from place to place and as such the operation conditions for wax extraction
varies from crude to crude, the aim of this work is to study the operational conditions for wax production from Nile
Blend. The influence of solvent composition, mixing temperature, residence time, and solvent to oil ratio on wax
extraction will be studied.
2. MATERIALS AND METHODS
It has to be mentioned that all the experimental analyses were performed at the Central Petroleum Laboratory
(CPL), Ministry of Energy and Mining, Sudan. The level of accuracy of the equipment and apparatus herein
mentioned are supplied by CPL.
2.1. Materials
Two liters of Nile Blend, a grade of Sudanese crude oil, was provided by the Ministry of Energy and Mining.
Table 1 shows the result of the analysis of this sample. The analysis was performed in CPL using standard methods

October 2010 The Arabian Journal for Science and Engineering, Volume 35, Number 2B 19
 Amel A Nimer,, Abdelshakour A. Mohamed and Ali A. Rabah

as indicated in the said table. Table 2 shows the properties of MEK and Toluene used in this work. These are the
manufacturers’ data. The manufacturer for both chemicals is Fischer Scientific, UK.

Table 1. Properties of Nile Blend

Property Test Method Unit Value
Salt Content ASTM D 3230 mgNaCl/L 9.12
Density at 15 oC ASTM D 5002 kg/m3 850.4
Wax Content UOP 46 wt% 25.87
o
Flash Point IP 170 C 21.5
o
Pour Point ASTM D97 C 33.0
Kinematic Viscosity at 50 oC ASTM D 445 mm2/s 22.64
Kinematic Viscosity at 80 oC ASTM D 445 mm2/s 8.884
Water Content by Distillation ASTM D 4006 v% 0.09
Ash content ASTM D 482 wt% 0.043
Asphaltene Content IP 143 wt% 0.11
Sulfur Content ASTM D4294 wt% 0.051

Table 2. Properties of MEK and Toluene (Manufacturer 's Data)

Property MEK Toluene
Molecular Formula C4H8O C7H8
Molecular Weight 72 92.1
Boiling Point oC 79.6 111
Melting Point oC -86 95
Flash Point oC -6 4
Vapor Pressure at 20 oC (mmHg) 77.5 22
Vapor Density 15 oC 2.42 3.14
Lower Explosive Limit % 2 1.2
Upper Explosive Limit % 10 77
Solubility in Water at 20 oC 27.5% Nearly Insoluble
Manufacturer Fischer Scientific, UK Fischer Scientific, UK
Purity w% 98 98
2.2. Experimental Apparatus
Figure 1 shows a schematic presentation of the dewaxing processes. These include mixing and heating, cooling
(chilling), filtration, and evaporation. The mixing and heating were carried out using a magnetic stirrer with a
hotplate. It was type Heidolph Hei-Tec Magnetic Stirrers manufactured by Brinkmann and Eppendorf. It has a speed
up to 1000 rpm. The level of uncertainty of the rotational speed is 1% of the maximum speed. The chiller is a
thermostat type FP50 (HD) manufactured by Julabo (Germany). The thermostat employes ethylene glycol and is
capable of producing cooling and heating levels in the range of -25 to 50 oC. Its highly accurate PID temperature
controller with digital readout has an accuracy of 0.02K. The filtration system consists of a Gooch crucible placed on
a flask and the flask is connected to a vacuum pump. On top of the Gooch crucible glass, wool was placed. The
vacuum pump is type N 035 AN and is capable of producing a vacuum pressure of 10-4 mbar. A rotary evaporator
type RE 100 (BIBBY) was used to evaporate the solvent and Naphtha from wax. The heating is provided using water
bath type RE 100B.

Naphtha Naphtha + traces of solvent

Solvent

Crude oil Evaporator

Mixer and heater Chiller Filtration
Wax + traces (oil)
Oil + solvent +
traces (wax)

Figure 1: Schematic of experimental setup

20 The Arabian Journal for Science and Engineering, Volume 35, Number 2B October 2010
 Amel A Nimer,, Abdelshakour A. Mohamed and Ali A. Rabah

Besides these apparatuses, a four decimal digital balance type TOLEDO AB204S manufactured by METTLER
of Switzerland was used. It has a range of 10mg to 210 g with an accuracy of 1.0 mg. A potable platinum
thermometer is used to monitor the temperature during heating and cooling (chilling) of the mixture. The
thermometer has a level of accuracy of 0.5K. Gas Chromatography (flame ionization detector) model Chrompac CP
9001 was used for wax analysis. The GC has a column-type wall coated open tube WCOT fused silica. The column
length and inside diameter are 25m and 0.25mm, respectively. It has a retention time repeatability within 0.1 minute.
The tests were performed in accordance with ASTM D5442.
2.3. Experimental Design and Procedure
In the present work, there are eight parameters to be investigated. These are three temperatures (heating, cooling,
and evaporation), two retention times (mixing and chilling), one mixing speed, one solvent to oil ratio, and one
mixture concentration. If each parameter is varied twice in accordance with a 2k factorial method, there will be 256
experiments. With a minimum replicate of three, this will be infeasible due to high cost and time. An alternative
method of “fractional factorial designs” was used. Here, only the parameters that best describe the problem are
studied. In this process, the mixing speed, chiller and evaporator temperatures, and chiller resident time are kept
constant in this work. Each of the rest of the parameters is replicated at least three times. The number of experiments
and their procedures are given as:
1. Material preparation: 720 samples each of 2 g of crude oil are prepared. MEK - Toluene mixtures of
different concentrations (50, 75, and 100 %MEK) are prepared; a known amount of MEK is added to a
known amount of Toluene.
2. Heating and mixing: The desired amount of solvent is added to the 2 g of oil. The flask is tightly closed and
manually shaken then placed in the magmatic stirrer (the stirring ball is placed inside the flask). The mixing
is done gradually; starting at low speed and increasing towards full speed. The mixing time is varied from
5–30 minutes with 5 minute intervals (6 replicates) at a temperatures range of 28 to 70 oC [28, 40, 50, 60,
and 70 oC].
3. Chilling: After mixing and heating, the flask with its content is transferred to the chiller. It is placed in the
ethylene glycol bath of the thermostat. Since the desired chilling temperature is -17 oC, the thermostat is set
at -20 oC. This is made to reduce the cooling time (increase the cooling rate). When the bulk temperature
reaches -17 oC, the thermostat temperature is adjusted to and left for an additional 30 minutes at -17 oC. It
was observed that the bulk temperature reaches the desired level within 30 minutes. This is equivalent to a
cooling rate of up to 2.25 oC per minute.
4. Filtration: The wax formed in the mother solution was filtered under vacuum through glass wool in a Gooch
crucible. The flask containing the mother solution was rinsed with 20 ml of fresh solvent at -17 oC to ensure
that all components have been removed. The wax collected on the glass wool was washed with 100 ml of
Naphtha.
5. Evaporation: The Naphtha and the traces of solvent were driven off under vacuum evaporation. The water
bath temperature is maintained at 95 oC. The wax in the flask is then left for 24 hours in a desiccator
containing P2O5. This was made to dry the wax from the traces of Naphtha and solvent.
The produced wax is then weighed and analyzed using GC. The test method ASTM D 5442 was used. The
produced wax was subjected to touch inspection. In addition, its solubility in Naphtha, Toluene, Xylene, Kerosene,
Benzene, Ethyl Alcohol, Acetone, and Carbon Tetra Chloride was checked.
3. RESULTS AND DISCUSSIONS
The extracted wax, here called yield X, is determined as a percentage of the total wax in crude oil as
Wi
X = × 100%
WT

Wi is extracted wax in grams for experiment i, and WT is the total wax in the crude oil sample in grams. In the present
work, the total wax is 25.87 w% of the sample.
3.1. Influence of Mixing Time and Temperature
Figures 2 (a) and (b) show the wax yield at various mixing temperatures and residence times.
1. The wax yield increases along the line of isotherm with time till it reaches a point beyond which it asymptotes.
It begins to asymptote at residence time of about 20 minutes. It can be concluded that for all lines of isotherm
at different solvent to oil ratios, the residence time of 20 minutes gives the highest yield. Although there are
few cases in which the maximum yield occurs at retention time of about 25 minutes, the increase in wax yield

October 2010 The Arabian Journal for Science and Engineering, Volume 35, Number 2B 21
 Amel A Nimer,, Abdelshakour A. Mohamed and Ali A. Rabah

between 20 and 25 minutes does exceed 1 %. In turn, this does not justify the energy consumed to maintain
the mixture at the desired temperatures for the said difference in the residence times. A comprehensive
economical analysis for this study is found in [9].
2. The wax yield increases with temperature at constant residence time. This is expected since heating decreases
viscosity and enhances solvent distribution in the mixture. It can also be seen that, at residence time of 20
minutes, the difference in the wax yield at 50 oC and that at 70 oC does exceed 5%. Similar to retention time,
this relatively small increment does not justify the energy required to raise the mixture (oil, wax, and solvent)
temperature by 20 oC. It should be remembered that the mixture will be cooled again, which requires
additional energy for this purpose.

100 100
a) 75% MEK b) 50% MEK
95 95

90 90

85 85
Yield %

80 80
28 28
75 40 75 40
Temperature oC
70 Temperature oC 50 70 50
60 60
65 65
70 70
60 60
5 10 15 20 25 30 5 10 15 20 25 30
Residence Time (min.) Residence Time (min.)

Figure 2: Influence of temperature on dewaxing at solvent to oil ratio of 16:1

3.2. Influence of Solvent to Oil Ratio

Figures 3(a) and (b) show the influence of the solvent to oil ratio on wax yield. As mentioned earlier, the increase
in solvent will enhance the filtration rate because solvent prompts the crystal growth and lowers the viscosity of the
mixture (oil + solvent). The result clearly confirms these facts. However, the effect becomes almost asymptotic at a
solvent to oil ratio of 20:1.

100 100
a) 75% MEK a) 50% MEK
95 95

90 90
Yield %

Yield %

85 85

80 80
Solvent to Oil Ratio Solvent to Oil Ratio
75 16.1 75 16.1
70 20:1 70 20:1
28:1 28:1
65 65
32:1 32:1
60 60
5 10 15 20 25 30 5 10 15 20 25 30
Residence Time (min.) Residence Time (min.)

Figure 3: Influence of solvent to oil ratio on dewaxing at a mixing temperature of 50 oC

3.3. Influence of Solvent Compositions

Figure 4 shows the influence of solvent compositions in wax extraction. As expected, an increase in the ratio of
MEK in the solvent enhances the wax yield. Increasing MEK in the solvent from 50% to 75% enhanced wax
recovery by 3.5 to 5.0% at the same operational conditions. This is because MEK prompts the crystallization of wax
and enhances the filtration rate. At 100 wt% MEK, high wax recovery is obtained. It was observed during the
experimental run that the filtration rate is slower than that with MEK-Toluene mixtures. This is expected since pure
MEK is known to form a third phase in addition to the existing solvent/oil phase, wax/solvent phases. The new phase
consists of molecules which are insoluble in MEK that clogs the filter [4].

22 The Arabian Journal for Science and Engineering, Volume 35, Number 2B October 2010
 Amel A Nimer,, Abdelshakour A. Mohamed and Ali A. Rabah

100

95

90

Yield %
85

80 MEK content in the solvent

75 100%v

70 75%v
50%v
65

60
5 10 15 20 25 30
Residence Time (min.)
Figure 4: Influence of solvent composition on wax removal at a mixing temperature of 50oC and solvent to ratio of 20:1

3.4. Wax Characteristics

The wax produced at the operational conditions of 75% MEK solvent composition, 20:1 solvent to oil ratio, 50
o
C mixing temperature, and 20 minute residence time at -17 oC filtration temperature is inspected and found to be
slightly greasy to the touch. It is also found to be soluble in Naphtha, Toluene, Xylene, Kerosene, Benzene, Ethyl
Alcohol, hot Acetone, and Carbon Tetra Chloride. Table 3 shows the result of GC. The light hydrocarbon (nC10-
nC16) constitutes about 6% and C45+ is 10 %. The light n-paraffins may originate from the oil entrapped within the
wax.

Table 3. GC Analysis for Produced Wax

Carbon Number Mass% Carbon Number Mass %
nC10 0.225 nC28 4.957
nC11 0.633 nC29 4.445
nC12 0.994 nC30 3.349
nC13 1.257 nC31 2.705
nC14 1.380 nC32 1.945
nC15 1.474 nC33 1.493
nC16 1.575 nC34 1.073
nC17 1.986 nC35 0.810
nC18 2.190 nC36 0.650
nC19 2.968 nC37 0.496
nC20 4.354 nC38 0.398
nC21 6.279 nC39 0.299
nC22 7.104 nC40 0.228
nC23 7.805 nC41 0.174
nC24 7.115 nC42 0.184
nC25 6.853 nC43 0.165
nC26 6.232 nC44 0.137
nC27 6.045 C45+ 10.023
Total 100.000

4. CONCLUSION
This study provides experimental data on dewaxing of Nile Blend. The operational conditions for wax production
from Nile Blend are 75% MEK, 20 minute retention time, and 20:1 solvent to oil ratio at -17 oC cooling and a 30
minute cooling time. Under these conditions, the wax contains 6% of light n-paraffins (nC10-nC16) and 10% of C45+.
ACKNOWLEDGMENT
The authors acknowledge the support of the Central Petroleum Laboratory (CPL) at the Ministry of Energy and
Mining, Sudan.

October 2010 The Arabian Journal for Science and Engineering, Volume 35, Number 2B 23
 Amel A Nimer,, Abdelshakour A. Mohamed and Ali A. Rabah

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University of Khartoum, 2008.

24 The Arabian Journal for Science and Engineering, Volume 35, Number 2B October 2010

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