Available online at http://ijcpe.uobaghdad.edu.iq and www.iasj.net
Iraqi Journal of Chemical and Petroleum
Engineering
Vol.21 No.1 (March 2020) 9 – 41
EISSN: 2618-0707, PISSN: 1997-4884
Corresponding Authors: Name: Bariq Bahmman Jima, Email: drbarikbahman93@gmail.com , Name: Najwa Saber Majeed, Email:
majeednajwa@gmail.com
IJCPE is licensed under a Creative Commons Attribution-NonCommercial 4.0 International License.
Oxidation Desulphurization of Heavy Naphtha Improved by
Ultrasound Waves
Bariq Bahmman Jima and Najwa Saber Majeed
University of Baghdad, Chemical Engineering Dept.
Abstract
The oxidation desulphurization assisted by ultrasound waves was applied to the desulphurization of heavy naphtha. Hydrogen
peroxide and acetic acid were used as oxidants, ultrasound waves as phase dispersion, and activated carbon as solid adsorbent. When
the oxidation desulphurization (ODS) process was followed by a solid adsorption step, the performance of overall Sulphur removal
was 89% for heavy naphtha at the normal condition of pressure and temperature. The process of (ODS) converts the compounds of
Sulphur to sulfoxides /sulfones, and these oxidizing compounds can be removed by activated carbon to produce fuel with low
Sulphur content. The absence of any components (hydrogen peroxide, acetic acid, ultrasound waves and activated carbon) from the
ODS process leading to reduce the performance of removal, hydrogen peroxide was the most crucial factor. The ultrasound waves
increase the dispersion of carbon, water and oil phase, promotes the interfacial mass transfer, and this leads to accelerates the
reaction. The ultrasound waves did not affect the chemical or physical properties of the fuel. The chemical analysis of treated fuel oil
showed that <1% of the hydrocarbon fuel compounds were oxidized in the ODS process. In this work, desulphurization by oxidation
is the main mechanism was tested with several parameters that effects desulphurization efficiency such as sonication time (5-40) min,
activated carbon (0.01-0.5) gm, hydrogen peroxide (1-30) ml, and acetic acid (1-15) ml. It was found that the hydrogen peroxide
amounts lead to increase oxidation rates of Sulphur compounds so, the desulphurization efficiency increases. The optimum amounts
of oxidants are 10 ml hydrogen peroxide per 100 ml of heavy naphtha. Increasing the amount of acid catalyst lead to increase
Sulphur removal, it was found that7.5 ml acid per 10 ml oxidant was the optimum amount. Activated carbon as a solid adsorbent and
reaction enhancer with 0.1gm weight was found as the optimum amount for 100 ml heavy naphtha. Increasing sonication time lead to
increase desulphurization rate, it was found that (10 min) is the optimum period. By applying the optimum parameters 89% of sulfur
can be removed from heavy naphtha with 598.4 ppm Sulphur content.
Keywords: Ultra-low Sulphur fuel, Oxidative desulfurization, ultrasonic waves, hydrogen peroxide, acetic acid
Received on 23/04/2019, Accepted on 03/09/2019, published on 30/03/0220
https://doi.org/10.31699/IJCPE.2020.1.0
1- Introduction
Sulphur compounds in oil fractions are the main reason
for many environmental pollution and equipment failure.
The presence of Sulfur compounds with a high
concentration in oil fraction lead with time to damage
industrial equipment by causing corrosion effect [1].
Sulfur compounds are poison metals and catalysts used
in industrial processes such as catalytic cracking and
catalytic reforming by precipitation on the catalyst surface
and close its pores [2].
Burning of oil fractions that contain a high
concentration of Sulphur compounds lead to releases of
Sulphur oxides gases (SOx) which cause smog and acid
rains so that for environmental protection called for
diminishing Sulphur compounds content to minimum
concentration as much as probable by using suitable
desulfurization processes [3].
Hydrodesulphurization (HDS) is the conventional
desulphurization process, it is a familiar practice in the
refinery for several years and has the dominance of pre-
existent in the infrastructure of the refinery, but this
process required high pressure and temperature [4].
Seek for preference way to sulphur component removal
has been increased in the past years [5].
The selective oxidation of organic sulphur compounds
at ambient pressure and room temperature in the process
of oxidation desulphurization (ODS), permit the utilize of
inexpensive adsorbents to get low sulphur content [6].
The challenge in oxidation desulphurization (ODS) is to
recognize the conditions that perform ultra-deep
desulphurization without using expensive catalysts or
auxiliary chemicals and keep high fuel oils recovery [7].
Ultrasonic waves used to raise quick reactions by
dissipating the multiphase admixtures of the oil phase and
aqueous phase. The oxidation process modifies the
physical properties of organic sulphur compounds so that
these compounds can be removed by adsorption using
inexpensive adsorbent [8].
The moderates condition used in the ODS process
reduces the total energy required for sulphur removal in
comparisons with the HDS process [9].
https://doi.org/10.31699/IJCPE.2020.1.2
B. B. Jima and N. S. Majeed / Iraqi Journal of Chemical and Petroleum Engineering 21,1 (2020) 9 - 14
01
Oxidation desulphurization considered an efficient
process to remove Sulphur compounds that can't be
removed by the HDS process such as benzothiophenes
and dibenzothiophenes compounds [10].
This study is a first attempt to treat commercial heavy
naphtha supplied from Al-Doura refinery to remove
Sulphur content by the oxidation process improved by
ultrasound waves. The effect of several variables on the
process was studied, such as the effect of hydrogen
peroxide, acetic acid, sonication time and activated
carbon as adsorbent.
2- Experimental Work
2.1. Materials
Chemical materials utilized in this research are shown
in table 1, the activated carbon used in this work is of
1184.9 m2/gm surface area. Heavy naphtha of 598.4 ppm
sulphur content was derived from Al-Doura refinery with
60.7 API and a density of 0.7379 g/cm3.
Table 1. Chemical materials utilized in experiment work
chemical
materials
function
molecular
weight
Purity
%
formula company
Hydrogen
peroxide
Oxygen
source
34 50 H2O2
Hopkin and
Williams,
England
Acetic acid
Increase
oxidation
60 99 C2O2H4
Riedel-De
Haen
Activated-
carbon
Solid
adsorbent
12.01 ----- C
Jacobi
Carbons
2.2. Apparatus
The equipment used is as follows:
A-Q 500 Sonicator
Q 500 sonicator is the important apparatus employed in
these experiments, Fig. 1 ultrasound device. It is a strong
device for ultrasound wave's processor displaying
programmable action and numerical show of running
parameters. Q500 sonicator is of 20 kHz and 500 W
maximum amplitude of power ultrasound. The device is
designed and produced by the company of Materials and
Sonics, Inc. Model VX 500, Newton, United States).
Fig. 1. Ultrasound device of Q 500 sonicator
B- Hot plate magnetics stirrer manufactured by PCE
Americas Inc., USA.
2.3. Analysis
Sulphur content of heavy naphtha was obtained due to
ASTM D-7093 by utilizing the Antek-Multitek device
located in Al-Daura refinery, manufactured by (PAC LP,
Houston, Texas, USA).
2.4. Procedure
100 ml of heavy naphtha with 598.4 ppm sulphur
content put in a beaker, as oxidative agent amounts of
hydrogen peroxide(H2O2) (1-30 ml) and as a catalyst
amounts of acetic acid (1-15 ml) and activated-carbon
(0.01-0.5 gm) as adsorbent, were added to this beaker.
This beaker put in ultrasound effects for periods (5-40
min) of time with Amplitudes (20-60% Amp) of power
ultrasound.
After the sonication process, the mixture put up in a
magnetic stirrer for 1 hr. with 900 rpm to satisfy
adsorption equilibrium [11], then the oil phase and
aqueous phase separated and the oil phase went to
analysis to know Sulphur content by the Antek-Multitek
device.
3- Results and Discussion
3.1. Effects of hydrogen peroxide amount
The effects of changing hydrogen peroxide added
amount on desulphurization of heavy naphtha are shown
in Fig. 2.
Fig. 2. effects amounts of oxidant on Sulphur content for
100 ml of heavy naphtha, 10 min sonication time, 20%
Amp ultrasound power, 0.1 gm activated carbon and 1ml
acid.
Note: Amp means amplitude
As shown in Fig. 2, the desulphurization efficiency
increases with increasing amounts of oxidant hydrogen
peroxide, this is because of increasing the free radicals in
the mixture which leads to increase oxidation of Sulphur
compounds, this behavior was also pointed out by
Hosseini, 2012, [12].
B. B. Jima and N. S. Majeed / Iraqi Journal of Chemical and Petroleum Engineering 21,1 (2020) 9 - 14
00
The optimum volume of hydrogen peroxide is 10 ml,
for this reason, all subsequent experiments are selected at
hydrogen peroxide volume 10 ml hydrogen peroxide per
100 ml of naphtha.
3.2. Effects of Acetic Acid Amount
The effects of changing the amounts of acetic acid on
desulphurization process are shown in Fig. 3.
Fig. 3. Effects amount of acid on Sulphur content for 100
ml heavy naphtha, 10 ml hydrogen peroxide, 10 min
sonication time, 20% Amp power ultrasound and 0.1 gm
activated carbon
As shown in Fig. 3, increasing the amounts of acid
catalyst lead to increase the removal of Sulphur until 7.5
ml of acid that is because beyond this amounts adverse
reaction occurs, this behavior was due to the reaction
between oxidant and acid.
… (1)
The reaction of hydrogen peroxide and acetic acid
produces peracetic acid. this acid is a form of proxy-
carboxylic acids, that can decompose to produce hydro-
proxy radicals ( .OOH), these radicals are more effective
than hydroxyl radicals (.OH) formed from hydrogen
peroxide decomposition, so oxidation process increases.
it was found that the best Sulphur removal when utilized
7.5 ml acetic acid per 10 ml hydrogen peroxide. The
optimum ratio of acid to oxidant is 0.75, for this reason,
all subsequent experiments are selected at acid to oxidant
ratio of 0.75.
Fig. 4. The relation between Sulphur content and
sonication time for 100 ml naphtha, 10 ml hydrogen
peroxide, 7.5 ml acetic acid, 20% Amp of ultrasound
power and 0.1 gm activated carbon
As shown in Fig. 4, increasing the sonication time leads
to an increase in the oxidation of Sulphur compounds due
to increasing exposure periods of these compounds to the
oxidants, then increasing desulphurization rate.
These longer times of reaction under the energy of
ultrasound lead to strong cavitation formation that leads to
fine emulsions formation for the oxidation reaction, this
fine emulsion increase contacts and exposure of the
oxidative system to organic Sulphur compounds, so
increase desulphurization efficiency. These results are in
good agreement with that of Teng-Chien Chen., et al
2010, [13]. The optimum period of sonication time is 10
min, for this reason, all experiments are selected at 10 min
sonication time.
3.4. Effects of Activated Carbon Amounts
The results related to satisfying these effects are shown
in Fig. 5
Fig. 5. Sulphur content with different amounts of
activated carbon for 100 ml heavy naphtha, 10 min
sonication time, 20% Amp ultrasound power, 10 ml
hydrogen peroxide and 7.5 ml acetic acid
B. B. Jima and N. S. Majeed / Iraqi Journal of Chemical and Petroleum Engineering 21,1 (2020) 9 - 14
01
As shown in figure 5, the increase of activated carbon
amounts leads to increase desulphurization efficiency due
to increased oxidation rates by increase attractions the
organic Sulphur compounds to the aqueous phase where
oxidation occurs, this behavior was also pointed out by
Gonzalez., et al 2012, [8]. The optimum amount of
activated carbon is 0.1 gm so that all experiments are
selected at 0.1 gm activated carbon.
4- Conclusion
Based on the results obtained, the conclusions can be
demonstrated as follows:
It was found that increasing hydrogen peroxide amounts
lead to an increased oxidation rate, so desulphurization
efficiency increases.
The ultrasound-assisted oxidative desulphurization
process with adsorption by active carbon has high effects
on desulphurization of crude oil fractions up to 89 % for
heavy naphtha.
The amounts of acetic acid used in this process have an
optimum value, if more than the optimum value, the
adverse reaction will occur leading to decrease the
efficiency of desulphurization, 7.5 ml acetic acid per 10
ml of hydrogen peroxide is the optimum value of acetic
acid in this work.
Increasing the time of sonication lead to increase
Sulphur removal, but using too much time leads to
increase in the cost of operation, it was found that the
optimum sonication time for heavy naphtha is 10 min.
Increasing amounts of active carbon lead to increase
adsorption rate but at 0.5 gm ≥ the amount becomes too
much, so the favorite amount for 100 ml heavy naphtha is
0.1 gm. The process is done without any effects in the
chemical or physical properties of the fuel.
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02
الموجات فوق الصوتية أكسدة و إزالة الكبريت من النافتا الثقيمة المحسنة بواسطة
بارق بهمان ونجوى صابر مجيد
قسم اليندسة الكيمياويةجامعة بغداد,
ألُخالصة
تبعًا لزيادة ألطمب العالمي عمى أستخدام وقود أقل ظررًا بالبيئة وبأقل تكمفة ممكنة من ألجانب أالقتصادي,
فأن ىذا ألعمل يركز عمى عممية كفوؤة وقميمة ألكمفة من أجل إزالة ألكبريت من وقود ألنفثا ألثقيمة عن طريق
مركبات ألكبريت ألمعززة بالموجات فوق ألصوتية حيث أثبتت ىذه ألعممية كفائتيا في إزالة عميقة عممية أكسدة
لممحتوى ألكبريتي.
بأستخدام نظام أالكسدة ألمكون من بيروكسيد ألييدروجين وحامض ألخميك كعامل مساعد من أجل أكسدة
إزالة أالخير بواسطة ألكاربون ألنشط.مركبات ألكبريت ألعضوية وتحويميا ألى سمفونات حيث تتم
ألموجات فوق ألصوتية تزيد من ألمساحة ألسطحية لتالمس نظام االكسدة مع ألطور ألنفطي في ألنظام ثنائي
ألطور وألتي تؤدي لزيادة معدل أالكسدة لمركبات ألكبريت وبالتالي زيادة كفائة أالزالة وبدون أي تأثير عمى
فيزيائية لموقود.ألخواص ألكيميائية او أل
في ىذا ألعمل ِإزالة ألكبريت بواسطة أالكسدة ىي ألعممية ألرئيسية وقد أختُبرت مع عدة متغيرات والتي تؤثر
04-04دقيقة(, مقدار طاقة ألموجات فوق ألصوتية ) 04-5في كفائة أإِلزالة وِمن ىذِه ألعوامل وقت ألتفاعل )
مل( 04-0غم(, كمية ألعامل ألمؤكِسد ىيدروجبن بيروكسيد ) 5..4-4.40%(, كمية ألكاربون ألمنشط )
مل(. 05-0وكمية حامض ألخميك )
في ما يتعمق بتأثير ألعامل ألمؤكسد فقد لوحظ أنو بزيادة كمية ألييدروجين بيروكسيد تؤدي لزيادة معدل إزالة
ن أل مل من ألنفثا 044كمية ألُمناِسبة ِلمعالجة ألكبريت نظرًا ِلزيادة ُمعدل أالكسدة ِلمركبات ألكبريت ألعظوية وا
مل من ىيدروجين بيروكسيد. 04ألثقيمة ىي
مل من حامض 5..في ما يتعمق بتأثير حامض ألخميك فقد لوِحظ ِبأنُو يجب أن تكون كميتُو ُمحددة وىي
لُمحددة تؤدي مل من ألييدروجين بيروكسيد حيُث أن زيادة كمية ألحامض أكثر من ألكمية أ 04ألخميك لكل
ِلحصول تأثير عكسي وبالتالي تُقمل ِمن كفائة أإِلزالة لمكبريت.
غم ِمن ألكاربون 4.0مل ِمن ألنفثا ىي 044ألكاربون ألمنشط كسطح ممتز وِجد أَن ألكمية ألُمناِسبة ل
ألُمنشط.
B. B. Jima and N. S. Majeed / Iraqi Journal of Chemical and Petroleum Engineering 21,1 (2020) 9 - 14
03
ِجد أنُو أفضل فترة زمنية مناسبة زيادة وقت ألتعُرض ِلمموجات فوق ألصوتية يؤدي ِلزيادة ُمعدل أاِلزالة وقد و
دقيقة( ِلُمعالجة ألنفثا ألثقيمة. 04ىي)
% من ألمقدار ألُكمي ِلطاقة 04مقدار طاقة ألموجات فوق ألصوتية مؤثر ميم في ىذه ألعممية حيث ِوجد أنُو
حالة أستخدام طاقة جياز ألموجات فوق ألصوتية ىو ألمقدار ألمناسب ِِلزالة ألكبريت ِمن ألنفثا ألثقيمة وفي
أعمى َفإن ذلك يؤدي لحدوث تأثير عكسي يؤدي ِلتقميل َكفائة إزالة ألكبريت.
% ِمن ألمحتوى ألكبريتي وذِلك عند تطبيق جميع 98عمى ُكِل حال فإنٌو أمكن ألحصول عمى إزالة تصل إلى
ق ألصوتية إِلزالة ألكبريت من النفثا ألثقيمة إن تفاُعل أالكسدة ألمعززة ِبالموجات فو ألمقادير ألِمثالية ِلممتغيرات.
ىوتفاعل من ألدرجة أِلولى.
موجات فوق الصوتية ,أالكسدة ,: إزالة ألكبريتدالةالكممات ال