Fuel Processing Technology 92 (2011) 2024–2029

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Fuel Processing Technology

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Separation of some paraffin wax grades using solvent extraction technique

Magdy T. Zaky ⁎, Nermen H. Mohamed, Amal S. Farag
Petroleum Refining Division, Egyptian Petroleum Research Institute (EPRI), Nasr City, P. O. Box: 11727, Cairo, Egypt

a r t i c l e i n f o a b s t r a c t

Article history: Solvent extraction technique has been used to separate paraffin wax grades; with different characteristics;
Received 14 December 2010 from El-Ameria light, middle and heavy slack waxes. The wax deoiling has been done by solvent extraction at
Received in revised form 30 May 2011 different extraction temperatures and different solvent feed ratios (S/F by weight). The extraction solvents
Accepted 1 June 2011
used are furfural, N-methyl-2-pyrrolidone (NMP) and N, N, dimethylacetamide (DMA). The wax products are
Available online 28 June 2011
evaluated according to TAPPI-ASTM equation and petroleum wax specifications. The data revealed that DMA
Keywords:
and NMP are suitable extracting solvents for isolating of semi- and scale-refined grades of paraffin waxes from
Paraffin waxes light and middle slack waxes. But furfural solvent can separate only semi-microcrystalline waxes from heavy
Solvent extraction slack wax.
Slack waxes © 2011 Elsevier B.V. All rights reserved.
Semi-refined waxes
Scale refined waxes

1. Introduction
Paraffin waxes constitute the major bulk of petroleum waxes due
to the high market demand all over the world and to their applications
especially for household chemicals, pharmaceutical, cosmetic and
industrial fields [1–5].
Generally, paraffin waxes are derived from low-boiling wax distillate
fractions (light and middle ones). They consist mainly of n-paraffins
ranging from C16–C30 and possibly higher. Varying proportions of
slightly branched-chain paraffins (C18–C36) and naphthenes are present.
Fully, semi- and scale refined paraffin waxes are produced from
slack waxes. Slack waxes separated from lubricating oil feedstocks in
dewaxing operation, usually contain from 2 to 45% oil content. Low oil
content wax with a specific melting point and penetration is produced
by selective removal of the oil and low melting waxes from the slack
waxes. This process is called deoiling or wax fractionation.
The commercial wax fractionation processes are the wax sweating,
the re-crystallization, the warm-up and the spray de-oiling ones.
Generally petroleum refiners have been used wax re-crystallization
(fractional crystallization) technique which is the most predominant
process and was developed as a replacement for the wax sweating
process. It is sometimes called wax fractionation process and can be
used to refine or de-oil all types of slack waxes to produce different
grades of paraffin wax [1,6]. Our previous study revealed that some
grades of paraffin waxes can be produced by fractional crystallization of
light, middle and heavy slack waxes at ambient temperature by using
⁎ Corresponding author. Tel.: + 202 22745902; fax: + 202 22747433.
E-mail address: magdytadrous@hotmail.com (M.T. Zaky).
different solvents. Also, the most suitable solvents for separating
paraffin waxes are ethyl and butyl acetates, MIBK and the mixture of
MEK, B & T (60:20:20 by weight, respectively) [7]. In another research,
the differentiation between fractional crystallization and solvent
percolation technique was studied for separation of paraffin waxes
from light, middle and heavy slack waxes. The study indicated that,
fractional crystallization technique is more suitable for deoiling the
heavy slack wax than the percolation technique. While, percolation
technology is a preferable technique for separation of paraffin waxes
from light and middle slack waxes [8].
But fractional crystallization and solvent percolation techniques
need long experimental time for separation the waxes. Therefore,
solvent extraction technique was taken into our consideration for this
purpose. Solvent extraction is the most widely used process for refining
lubricating stocks. Extraction is described as a procedure for separating a
homogeneous mixture of two or more substances into its components
or groups of components by creating a two-liquid phase system with the
help of an auxiliary liquid. The extract phase which consists chiefly of
solvent in which are extracted the undesirable bodies such as aromatics
while the raffinate phase consists mainly of saturated hydrocarbons
with little solvent. In the process of refining of lubricating oil base stocks,
the well known industrially applied solvents are furfural, phenol and
NMP. More recently refiners have found that NMP is one of the more
desirable solvent for lube oil refining as it exhibits better solvent power,
better chemical and thermal stabilities and lower toxicity than either
furfural or phenol [6,9].
Thus the present study is an attempt to use solvent extraction
technique instead of both fractional crystallization and solvent
percolation techniques for saving time, to extract the oily constituents
which are mainly aromatics and low melting point waxes from light,
middle and heavy slack waxes to separate different paraffin wax grades.

0378-3820/$ – see front matter © 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.fuproc.2011.06.002
 M.T. Zaky et al. / Fuel Processing Technology 92 (2011) 2024–2029
2. Experimental
2.1. Materials
Light, middle and heavy slack waxes obtained from El-Ameria
Refining Company were used. Furfural, dimethylacetamide (DMA)
and N-methyl-2-pyrrolidone (NMP) were used as extracted solvents
to deoil the slack waxes.
2.2. Solvent extraction technique
The three slack waxes were subjected to a bench scale extraction
with the desired solvent under study.
A jacketed mixer settler apparatus was used. The extraction
temperatures were adjusted to an accuracy of ±1 °C by using an ultra
thermostat. The feed and the solvent were kept in good contact by
continuous agitation for 45 min. After agitation, the phases were left
to settle for 45 min and then separated. The solvent was removed
from the raffinate phase (hard wax) by washing six times with hot
distilled water. The raffinate was then dried over anhydrous calcium
chloride. The solvent was removed from the extract phase by
distillation under reduced pressure.
The extraction variables studied were extraction temperature (70
to 90 ° C), (80 to 100 ° C) and (100 to 110 ° C) for light, middle and heavy
slack waxes, respectively and solvent feed ratio (ranging from 2:1 to
5:1 by weight).
2.3. Determination of critical solution temperature (CST)
In order to find the applicable extraction temperatures, mis-
cibilities and critical solution temperatures (CSTs) were measured for
the three slack waxes with furfural, DMA and NMP solvents by using
equal weights of wax and solvent. The wax and solvent were
introduced in a sealed tube and stirred while the tube was heated
gradually in a temperature regulated oil bath. The miscibility
temperature was marked as the point at which the turbidity of the
mixture disappeared and the two phases became completely miscible.
The heating was then stopped and another reading taken when the
solution had cooled and become turbid, indicating the beginning of
phase separation. The two readings were within 1 ° C difference. The
critical solution temperature was marked as the highest temperature
of a given solvent-to-feed ratio (S/F by weight). The chosen extraction
temperature for a given S/F ratio must be lower than its CST [10].
2.4. Method of analysis
The feed stocks and the isolated paraffin waxes were physically
characterized according to ASTM standard methods [11]. The
standard methods for analysis are, congealing point (ASTM D-938),
kinematic viscosity (ASTM D-445), refractive index (ASTM D-1747),
density (ASTM D-1418), mean molecular weight (ASTM D-2502), oil
content (ASTM D-721), cone penetration (ASTM D-937), needle
penetration (ASTM D-1321), color (ASTM D-1500), n-d-M analysis
(ASTM D-3238), and sulfur content by using X-ray fluorescence sulfur
meter (ASTM D-4294).
Their total aromatic content was determined using liquid solid
column chromatography technique. A 1.3 cm diameter and height of
130 cm column packed with activated (60–200 mesh) silica gel was
used. The column was then moistened with 100 ml of n-hexane to
dissipate the heat of adsorption. A 10 gram sample of the wax
dissolved in few milliliters of n-hexane were transferred to the
column. The column was then eluted with 300 ml of n-hexane
followed by 200 ml benzene and finally 100 ml of a 1:1 mixture of
absolute methanol and benzene. Fractions of 25 ml were taken from
the column, the solvent distilled off and the refractive index of each
fraction was determined. According to the refractive index data at
2025
20 0 C, eluates were combined into saturates, mono-, di- and poly-
aromatics. The saturate hydrocarbons have refractive indices not
more than 1.48. The mono-cyclic, bi-cyclic and poly-cyclic aromatics
have refractive indices from 1.48 to 1.53, 1.53 to 1.59 and higher than
1.59, respectively [12].
Their n-paraffin content was determined using gas chromatography
technique (GC). The GC apparatus used was Perkin Elmer (Clarus 500),
equipped with a hydrogen flame ionization detector and fused silica
capillary column (60 m length × 0.32 mm i.d), packed with poly
(dimethyl siloxane) HP-1 (non-polar packing) of 0.5 μm film thickness.
In the chromatograph, the injector was heated at 350° C. The column
temperature was programmed from 100 to 300° C at a fixed rate of 3° C/
min, and nitrogen (oxygen-free) was used as a carrier gas with flow
rate of 2 ml/min. The detector was heated at 350°C, and operated with
a hydrogen flow rate adjusted to optimize the detector sensitivity. The
sample was melted and 0.1 μl of it was introduced into the injector. A
mixture of pure n-paraffins was used as standard. The peak area of each
resolved component (consisting of either n- and iso-paraffin) is
determined individually. However, the unresolved complex mixtures
(humps); composed of non n-paraffins presumably mainly cyclo-
paraffins and aromatics with long side chains; were determined only as
a total.
The type of the isolated paraffin wax was carried out according to
TAPPI-ASTM equation to classify the waxes as macro-crystalline
(Paraffin), semi-microcrystalline and microcrystalline waxes. The
distinction between these groups is made on the basis of viscosity. The
proposal is as follows:
210BF
nD = 0:0001943 t + 1:3994
where t is the congealing point temperature in °F.
A paraffin wax is characterized by refractive index less than that
obtained by the above equation and by a viscosity at 210 °F of lower
than 7.4 cSt. A semi-microcrystalline wax is characterized by
refractive index higher than that obtained by the above equation
and by a viscosity at 210 °F of less than 10 cSt. A microcrystalline wax
is characterized by refractive index higher than that obtained by the
above equation and by a viscosity at 210 °F of 10 cSt or higher [13,14].
The degree of branching (% CH3 content) of the slack waxes and
isolated paraffin waxes was determined using proton nuclear magnetic
resonance (Varian Mercury H-NMR Spectrometer-Danemark) at
300 MHz in deutrated chloroform. The relative proportions of methyl
groups to methylene and methine groups (% CH3 content) were
calculated from a third of the integrated area under the methyl region
(from about 0.5 to 1.0 ppm) and a half of the integrated area under the
methylene and methin regions (from about 1.0 to 1.7 ppm) [15].
3. Results and discussion
3.1. Characterization of crude waxes
The physical characteristics, carbon distribution analysis and the
molecular type composition for the three crude waxes are repre-
sented in Table 1.
Data indicate that the heavy slack has the highest oil content,
penetration value and aromatic content as compared with the light
and middle ones. These aromatic constituents are mainly mono-
aromatic ones into which some di-aromatics are present, while the
light and middle slack waxes contain none of the latter. Data of sulfur
content and color values are parallel to the above findings. Also,
carbon distribution spectrum confirm the previous results as the
heavy slack wax show relatively higher percentage of aromatic
carbons (%CA = 10.46%) than those of the light and middle ones (5.93
and 8.41%, respectively).
The carbon number distribution of light, middle and heavy slack
waxes (C16–C37, C19–C38 and C21–C41, respectively) increases by
2026 M.T. Zaky et al. / Fuel Processing Technology 92 (2011) 2024–2029

Table 1 3.2. Solvent extraction

Physical characteristics, carbon distribution analysis and molecular type composition of
slack wax crudes.
Wax deoiling has been done by solvent extraction at different
Characteristics Slack waxes extraction temperatures and solvent feed ratios (S/F).
Light Middle Heavy
3.3. Critical solution temperature (CST)
Congealing point, °C 48 59 62.5
Kinematic viscosity, 98.9° C, cSt 3.04 4.30 6.00
Refractive index, 98.9° C 1.4224 1.4270 1.4402 Solvent feed miscibility temperature data are the prime require-
Density, 70° C 0.7920 0.8035 0.8107 ments for fixing solvent extraction operation. Data are represented in
Mean molecular weight 384 446 477 Table 2. It can be noticed that critical solution temperature of each slack
Oil content, wt.% 5.32 6.23 23.05
Cone penetration, 25° C 17 13 28
wax decreases in the following order: furfuralN DMA N NMP i.e. the
Needle penetration, 25° C 43 40 59 selectivity of the solvents decreases in the same order and consequently
Sulfur content, wt.% 0.09 0.10 0.22 the solvent power increase in the following order: furfural b DMA b NMP.
Color (ASTM D-1500) 1.0 1.5 3.0
3.4. Effect of extraction temperature
Carbon distribution analysis (n-d-M analysis)
% CA 5.93 8.41 10.46
% CN 12.85 14.20 29.44 Extraction temperature is considered as one of the main factors of
% CR 18.78 22.61 39.90 extraction variables. It is obviously advantageous to determine
% CP 81.22 77.39 60.10 experimentally the convenient temperature taking in consideration
Molecular type composition
both the yield and the quality of the refined product (raffinate). The
Total saturates, wt.% 97.63 96.97 86.18 yield and the physical characteristics of the isolated waxes are
n-Paraffins content, wt.% 74.71 62.89 35.07 represented in Tables 3–5.
Iso- and cyclo-paraffins content, wt.% 22.92 34.08 51.11 The wax yield decreases on increasing the extraction temperature
Total aromatics, wt.% 2.37 3.03 13.82
due to the increase of the solvent power of the solvents on raising the
Mono-aromatics, wt. 2.37 3.03 11.52
Di-aromatics, wt.% – 2.30 extraction temperature.
Solvent extraction of each light, middle and heavy slack wax with
%CA: Percentage of aromatic carbon per average molecule.
%CN: Percentage of naphthenic carbon per average molecule = %CR – %CA.
furfural solvent, at a given temperature, gives the highest wax yield
%CR: = %CN + %CA. with highest oil content and needle penetration value and lowest
%CP: Percentage of paraffininc carbon per average molecule = 100–%CR. congealing point. Meanwhile solvent extraction with DMA solvent
gives the lowest wax yield with lower oil content and needle
penetration and higher congealing point than those obtained by
furfural solvent. NMP solvent gives intermediate wax yield with
lowest oil content and needle penetration and highest congealing
point. It can be concluded that furfural has the lowest solvent power
increasing the boiling point range and/or the mean molecular weight and DMA has the highest solvent power while NMP has high solvent
of the slack wax (Fig. 1 and Table 1). Meanwhile, their normal paraffin power and high selectivity (Tables 3–5).
contents (74.71, 62.89 and 35.07 wt.%, respectively) decrease by The effect of increasing the extraction temperature upon the isolated
increasing the boiling point range and/or the mean molecular weight. wax quality is reflected by a decrease in the refractive index, oil content
Data of the percentage of paraffinic carbon per average molecule (% and needle penetration and increase in the congealing point and mean
CP = 81.22, 77.39 and 60.10% for light, middle and heavy slack waxes, molecular weight of the waxes extracted from the three slack waxes by
respectively) are parallel to the previous results (Table 1). using furfural, DMA and NMP solvents (Tables 3–5). It can be noted that
Generally, according to paraffin wax specifications and molecular as the extraction temperature is raised from 90 to 100 °C for extraction
type composition, paraffin wax can be derived from the three slack the light slack with DMA and NMP solvents, a slight increase in the
waxes as their characteristics are in the range of paraffin wax refractive index and viscosity of the separated waxes EL6 and EL9,
specifications and their n-paraffin contents are higher than the limit respectively are observed (Table 3). It may be related to the decrease of
of n-paraffin content of paraffin wax crude [6]. n- and/or iso-paraffin constituents of lower refractive indices, melting
points and mean molecular weights.
It is interest to note that the quality of the isolated waxes has been
greatly improved in terms of oil content, needle penetration and
14 congraling point by using DMA and NMP solvents. This may be due to
Light slack wax
Middle slack wax
Heavy slack wax the well known high solvent power of DMA and NMP solvents
12
n-Paraffin content, wt. %

(Tables 3 and 4).

Data of molecular type composition confirm the previous results as
10
the iso- and cyclo-paraffins content and consequently the iso- and
8 cyclo-paraffins to n-paraffins ratio for the waxes separated at extraction

Table 2
4
Critical solution temperatures of light, middle and heavy slack waxes with different
solvents.
2
Feed Critical solution temperatures, °C
0
15 20 25 30 35 40 45 Furfural DMA NMP
Carbon number distribution Light slack wax 149 117 115
Middle slack wax 154 127 124
Heavy slack wax 154 133 128
Fig. 1. Carbon number distribution of slack wax crudes versus n-paraffin content.
 M.T. Zaky et al. / Fuel Processing Technology 92 (2011) 2024–2029 2027

Table 3
Effect of extraction temperature on the physical characteristics and type of waxes isolated by solvent extraction of light slack wax using different solvents at S/F of 3:1.

Characteristics Light slack Wax fractions isolated by using different solvents at different extraction temperatures, °C
wax
Furfural DMA NMP

70 90 100 70 90 100 70 90 100

EL1 EL2 EL3 EL4 EL5 EL6 EL7 EL8 EL9

Yield on crude, wt.% 100 93.62 87.68 84.68 81.22 67.56 58.12 85.36 72.24 62.22
Congealing point, °C 48 49 50 50.5 50 51 52 50.5 51.5 52.5
Kinematic viscosity, 98.9°C, mm2/s 3.04 3.05 3.07 3.07 3.06 3.08 3.10 3.08 3.09 3.12
Refractive index, 98.9°C 1.4224 1.4214 1.4210 1.4203 1.4210 1.4183 1.4192 1.4210 1.4185 1.4194
Mean molecular weight 384 393 395 395 395 397 400 397 400 406
Oil content, wt.% 5.32 3.98 3.38 3.02 3.11 2.20 1.83 2.73 1.62 1.17
Needle penetration, 25°C 43 39 35 33 31 23 22 30 22 21
Color (ASTM-D 1500) 1.0 1.0 0.5 0.5 0.5 0.0 0.0 0.5 0.0 0.0
Refining effectiveness number (REN) – 1.60 1.54 1.53 1.57 1.62 1.99 1.13 1.32 1.72
Refractive index by TAPPI-ASTM equation – 1.4228 1.4231 1.4233 1.4231 1.4235 1.4238 1.4232 1.4236 1.4240
Type of wax – Macro-crystalline

Table 4
Effect of extraction temperature on the physical characteristics and type of waxes isolated by solvent extraction of middle slack wax using different solvents at S/F of 3:1.

Characteristics Middle slack Wax fractions isolated by using different solvents at different extraction temperatures, °C
wax
Furfural DMA NMP

80 90 100 80 90 100 80 90 100

EM1 EM2 EM3 EM4 EM5 EM6 EM7 EM8 EM9

Yield on crude, wt.% 100 96.22 93.96 91.16 85.48 71.20 69.36 86.68 80.02 77.84
Congealing point, °C 59 59.5 60 60.5 60.5 61.5 62 61 61.5 62.5
Kinematic viscosity, 98.9°C, mm2/s 4.3 4.30 4.28 4.25 4.28 4.26 4.19 4.29 4.26 4.20
Refractive index, 98.9°C 1.4270 1.4265 1.4263 1.4259 1.4259 1.4252 1.4240 1.4255 1.4247 1.4244
Mean molecular weight 446 448 450 452 452 455 461 454 455 463
Oil content, wt.% 6.23 3.98 3.18 2.02 2.13 1.79 1.16 1.99 1.64 0.95
Needle penetration, 25°C 40 36 33 30 30 26 22 29 25 22
Color (ASTM-D 1500) 1.5 1.5 1.5 1.0 1.0 0.5 0.0 1.0 0.5 0.0
Refining effectiveness number (REN) – 0.95 0.86 0.88 1.45 2.06 1.70 1.21 1.33 1.23
Refractive index by TAPPI-ASTM equation – 1.4264 1.4266 1.4268 1.4268 1.4271 1.4273 1.4270 1.4271 1.4275
Type of wax – Semi⁎ Macro-crystalline
⁎ Semi-microcrystalline.

temperature of 90 and 100 °C from light and middle slack waxes, of branching decreases in the following sequence furfuralN DMA N NMP
respectively are decreased in the following sequence: furfural N due to the decrease of iso-paraffin constituents and removal of mono-
DMA N NMP and the mono-aromatic constituents are completely aromatic components with very long side chain (Tables 6 and 7).
disappeared by using DMA and NMP solvents. Moreover, the degree
3.4.1. Isolated wax type
Table 5
Examining the isolated wax type on the basis of TAPPI-ASTM
Effect of extraction temperature on the physical characteristics and type of waxes equation; it can be noticed that all the waxes separated from light and
isolated by solvent extraction of heavy slack wax using two different solvents at S/F of middle slack waxes at all extraction temperatures by using furfural,
3:1. DMA and NMP solvents lie in the category of macro-crystalline waxes
Characteristics Heavy Wax fractions isolated by using two as they characterized by refractive indices lower than those obtained
slack different solvents at different extraction by the equation and by viscosities at 98.9 °C lower than 7.4 cSt, except
wax temperatures, °C

Furfural DMA Table 6

100 110 100 110 Molecular type composition and degree of branching of waxes isolated by solvent
extraction of light slack wax using different solvents at extraction temperature of 90 °C
EH1 EH2 EH3 EH4 and S/F of 3:1.
Yield on crude, wt.% 100 91.22 88.40 66.42 52.26
Characteristics Light Waxes isolated by using
Congealing point, °C 62.5 63 63.5 63.5 64.5
slack different solvents
Kinematic viscosity, 98.9 °C, 6.00 5.99 5.90 5.85 5.70
wax
mm2/s Furfural DMA NMP
Refractive index, 98.9 °C 1.4402 1.4392 1.4384 1.4380 1.4377
EL2 EL5 EL8
Mean molecular weight 477 506 508 512 515
Oil content, wt.% 23.05 8.51 7.55 7.10 6.15 Molecular type composition
Needle penetration, 25 °C 59 40 37 34 31 Total saturates, wt.% 97.63 98.90 100 100
Color (ASTM-D 1500) 3.0 2.0 1.5 1.5 1.0 n-Paraffins content, wt.% 74.71 76.20 78.79 79.94
Refining effectiveness – 0.46 0.53 1.34 1.71 Iso- and cyclo-paraffins content, wt.% 22.92 22.70 21.21 20.06
number (REN) Iso- and cyclo-paraffins/n-paraffins ratio 0.31 0.30 0.27 0.25
Refractive index by TAPPI- – 1.4277 1.4279 1.4278 1.4282 Total aromatics, wt.% 2.37 1.1 0.0 0.0
ASTM equation Mono-aromatics, wt. 2.37 1.1 0.0 0.0
Type of wax – Semi-microcrystalline Degree of branching (% CH3 content) 12.52 12.33 10.99 10.82
2028 M.T. Zaky et al. / Fuel Processing Technology 92 (2011) 2024–2029

Table 7 Table 9
Molecular type composition and degree of branching of waxes isolated by solvent Effect of solvent feed ratio on the physical characteristics and type of waxes isolated by
extraction of middle slack wax using different solvents at extraction temperature of solvent extraction of middle slack wax using NMP solvent at extraction temperature of
100 °C and S/F of 3:1. 100 °C.

Characteristics Middle Waxes isolated by using Characteristics Middle Wax fractions isolated at different S/F
slack different solvents slack ratios
wax wax
Furfural DMA NMP 2:1 3:1 4:1 5:1

EM3 EM6 EM9 EM10 EM9 EM11 EM12

Molecular type composition Yield on crude, wt.% 100 87.18 77.84 69.54 62.68
Total saturates, wt.% 96.97 98.50 100 100 Congealing point, °C 49 60 62.5 63 63.5
n-Paraffins content, wt.% 62.89 63.40 68.05 69.55 Kinematic viscosity, 98.9 °C, 4.3 4.29 4.20 4.22 4.24
Iso- and cyclo-paraffins content, wt.% 34.08 35.10 31.95 30.45 mm2/s
Iso- and cyclo-paraffins/n-paraffins ratio 0.54 0.55 0.47 0.44 Refractive index, 98.9 °C 1.4270 1.4255 1.4244 1.4248 1.4250
Total aromatics, wt.% 3.03 1.50 0.0 0.0 Mean molecular weight 446 454 463 466 469
Mono-aromatics, wt. 3.03 1.50 0.0 0.0 Oil content, wt.% 6.23 2.14 0.95 0.82 0.75
Degree of branching (% CH3 content) 10.78 10.35 9.60 9.36 Needle penetration, 25 °C 40 31 22 21 20
Color (ASTM-D 1500) 1.5 1.0 0.0 0.0 0.0
Refining effectiveness – 1.42 1.23 1.60 1.87
number (REN)
the wax separated from middle slack wax EM1 using furfural at Refractive index by TAPPI- – 1.4266 1.4275 1.4277 1.4278
extraction temperature of 80 °C lies in the category of semi- ASTM equation
microcrystalline wax. Also, all the waxes isolated from heavy slack Type of wax – Macro-crystalline
wax by using furfural and DMA solvents at extraction temperatures of
100 and 110 °C; lie in the category of semi-microcrystalline waxes as
they characterized by refractive indices higher than those obtained by needle penetration up to 22 (Compare EL8 with EL6 and EL9 in Table 3
the equation and by viscosities at 98.9 °C lower than 10 cSt. and compare EM9 with EM6 in Table 4).
According to petroleum wax specifications (refractive index is
≤1.433, congealing point is between 46 and 68° C and needle penetration 3.5. Effect of solvent feed ratio
at 25° C is between 15 and 22 [6], the waxes EL6, EL8 and EL9 separated
from light slack wax and EM6 and EM9, separated from middle slack Solvent extraction was carried out for light and middle slack waxes
wax lie in the category of macro-crystalline waxes. Meanwhile the waxes with NMP solvent at extraction temperature of 90 and 100 °C,
EL1–EL5 and EL7 separated from light and EM1–EM5, EM7 and EM8 respectively and at various solvent feed ratios (2:1 to 5:1 by weight)
separated from middle slack wax give needle penetration higher than to separate different grades of paraffin waxes. Data represented in
macro-crystalline group limit 22 (Tables 3 and 4). Tables 8 and 9 indicate that the increase of solvent ratio decreases the
The solvent efficiency was measured by the refining effectiveness yield of the isolated waxes due to the increase of the solvent power
number (REN) [16]. It is defined as: and improves the isolated wax quality in terms of lowering the oil
REN = Weight percent of extract yield/Modification property by content and needle penetration and elevating the congealing point
refining which is a good measure of attainable refining effect, i.e. the and mean molecular weight.
lower REN the better is the solvent efficiency. Taking the needle
penetration change in the raffinates (paraffin waxes) as the refining 3.5.1. Isolated wax type
performance parameter and applying that to the present investiga- By examining the isolated wax type on the basis of TAPPI-ASTM
tion. It can be concluded that the most suitable solvent is NMP for equation and petroleum wax specifications, the waxes EL8, EL11 and
extraction the paraffin wax from light and middle slack waxes at the EL12 separated from light slack wax and EM9, EM11 and EM12
most suitable extraction temperatures of 90 and 100° C, respectively separated from middle slack wax; at solvent feed ratios ranged from
and solvent feed ratio of 3:1 by weight to produce paraffin wax of 3:1 to 5:1; lie in the category of macro-crystalline waxes. Meanwhile,
the isolated waxes EL10 and EM10 separated from light and middle
slack wax, respectively at solvent feed ratio of 2:1 lie in the category of
macro-crystalline waxes on the basis of TAPPI-ASTM equation but
Table 8
Effect of solvent feed ratio on the physical characteristics and type of waxes isolated by
their needle penetrations 29 and 31, respectively are higher than the
solvent extraction of light slack wax using NMP solvent at extraction temperature of macro-crystalline wax limit 22 (Tables 8 and 9).
90 °C.

Characteristics Light Wax fractions isolated at different S/F

4. Conclusions
slack ratios
wax From the above study, it can be deduced that NMP is more effective
2:1 3:1 4:1 5:1
solvent at extraction temperatures of 90 and 100 °C for light and
EL10 EL8 EL11 EL12
middle slack waxes, respectively and at solvent feed ratios ranged
Yield on crude, wt.% 100 84.58 72.24 66.38 56.74 from 3:1 to 5:1 by weight due to the increase of the solvent power by
Congealing point, °C 48 50 51.5 52.5 53 dilution which is necessary to increase the solubility towards the
Kinematic viscosity, 98.9 °C, 3.04 3.06 3.09 3.12 3.15
mm2/s
undesired constituents.
Refractive index, 98.9 °C 1.4224 1.4212 1.4185 1.4190 1.4194 By using NMP solvent, three semi-refined grade of paraffin waxes
Mean molecular weight 384 395 400 406 412 EL9, EL11 and EL12 as their oil contents are higher than 0.5 and less
Oil content, wt.% 5.32 2.12 1.62 1.26 1.10 than 1.5 wt.% and one scale refined grade EL8 as its oil content is more
Needle penetration, 25 °C 43 29 22 21 20
than 1.5 and less than 3 wt.% [1] were extracted from the light slack
Color (ASTM-D 1500) 1.0 0.5 0.0 0.0 0.0
Refining effectiveness – 1.10 1.32 1.53 1.88 wax and three semi-refined grade paraffin waxes EM9, EM11 and EM12
number (REN) were obtained from the middle slack wax.
Refractive index by TAPPI- – 1.4231 1.4236 1.4240 1.4242 By using DMA solvent, one scale-refined grade of paraffin wax EL6
ASTM equation was obtained from light slack wax and one semi-refined paraffin wax
Type of wax – Macro-crystalline
EM6 was extracted from the middle one.
 M.T. Zaky et al. / Fuel Processing Technology 92 (2011) 2024–2029
It is interest to note that, furfural is not suitable solvent for
isolation of paraffin waxes from light and middle slack waxes as these
waxes have high oil contents and needle penetration values. While all
the waxes separated from heavy slack wax by using furfural and DMA
solvents at extraction temperatures of 100 and 110 °C and at solvent
feed ratio of 3:1 are classified as semi-microcrystalline waxes.
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