China Petroleum Processing and Petrochemical Technology

Review December 30, 2010

Progress in the Technology for Desulfurization of Crude Oil

Liu Lin; Lü Hong; Qian Jianhua; Xing Jinjuan
(Liaoning Province Key Laboratory for Synthesis and Application of Functional Compounds,
Bohai University, Jinzhou 121013)

Abstract: The poor quality of crude oil obviously leads to high sulfur contents of oil products, and the technology for
desulfurization of crude oil is urgently needed so that the sulfur contents in petroleum product could be reduced from the
root. This paper describes the progress in technology for desulfurization of crude oil. The present technologies for
desulfurization of crude oil include caustic washing, dry gas desulfurization, hydrodesulfurization (HDS), etc. The new
combined technologies for desulfurization of crude oil being studied are: biodesulfurization (BDS), hydrogenation-
bacterial catalysis, the microwave-catalytic hydrogenation, the BDS-OD-RA desulfurization and oxidative desulfuriza-
tion in electrostatic fields, and the ultrasonic/microwave-catalytic oxidation applied in our lab, with their development
trends being also discussed.
Key words: crude oil; desulfurization; development progress

1 Introduction 2 Current Technologies for Desulfurization of Crude Oil

The poor quality of crude oil currently can obviously re- 2.1 Caustic washing method for oil desulfurization
sult in the high sulfur contents of oil products, which can
Caustic washing method is mainly aimed at removing the
lead to corrosion, catalyst poisoning, environmental pol-
sulfides from the crude oil by using the caustic solution. At
lution and other negative consequences[1-4] (Figure 1)[5].
present, this method is widely used in the oil industry. The
The treatment of high-sulfur crude oil is becoming the fo-
advantage of this method is that the process is simple and
cus of research in China’s oil refining industry[6]. The con-
the cost is lower. But this method contains many defects
ventional equipment cannot deal with the high-sulfur crude
such as the poor quality of oil products and lower effi-
oil during petroleum refining processes. The increasing
ciency of desulfurization. However, this method can’t re-
sulfur content of crude oil also results in an increase in
move all sulfur compounds from the crude oil, especially
sulfur content in automotive gasoline, diesel fuel, and jet
the organic sulfides. At the same time, it brings too much
fuel. To meet the needs for producing clean fuels, decreas-
sulfide-containing wastewater, which greatly pollutes the
ing the sulfur content of crude oil becomes an urgent task.
environment. So, it is urgent to improve this method or find
Studying new desulfurization technology and raising the
a better way to reduce the sulfur contents in petroleum
efficiency of desulfurization processes are the keys to bring-
products.
ing more profits to the oil refining companies[7].
2.2 Dry gas desulfurization method

According to the report[8], the first equipment in China for

treating heavy crude oil through dry gas desulfurization
method has been used in the No.3 joint oil gathering sta-
tion at Tahe Oilfield of the Northwest Oilfield Branch
Company. The cost of this equipment is about 500 million
RMB, and it is the first time in China to use this dry gas
treatment method at the crude oil desulfurization system in
reality. This dry gas desulfurization system works as follows.
Figure 1 Global trend on crude oil quality[5] Corresponding author: Dr. Liu Lin, Telephone: +86-416-
—API gravity; —Sulfur content, m% 3400328; E-mail: liulinln@163.com

1
 December 30, 2010 Liu Lin, et al. Progress in the Technology for Desulfurization of Crude Oil
Firstly, the sulfur compounds are removed from the crude
oil; and secondly, after settling treatment and dehydration
of crude oil, the sulfur compounds are removed again so
that corrosion of the process equipment and the pipelines
will be minimized to secure better working conditions and
avoid accidents.
Gas stripping process can reduce significantly the H2S con-
tent in crude oil. But this method has its disadvantage be-
cause the efficiency of desulfurization will change with the
water content in the feedstock. Sulfate-reducing bacteria
(SRB) can convert a part of organic sulfides into inorganic
sulfides, causing the H2S content to increase in the next
phase of desulfurization[9]. And the rate for removal of other
sulfur-containing compounds is very low.
2.3 Hydrodesulfurization (HDS)
Hydrodesulfurization is one of the catalytic desulfuriza-
tion processes, which aims at turning organic sulfur com-
pounds into H2S using H2 as the reactant in the presence of
metal catalysts operating at high temperature and pressure.
The resultant hydrogen sulfide is then removed from the
system[10]. This method is widely used in oil industry in
China since 1955. However, the HDS process features a
complicated procedure, high production cost and high
materials consumption. With an increasing ratio of heavy
crude oil supply to the oil refinery, the sulfur content in
crude slate is growing, which leads to a shortened catalyst
life at the refinery. Furthermore, the HDS process needs
more H2, so the production cost will increase a lot[11].
2.4 Biodesulfurization (BDS)
BDS is a new bio-catalytic desulfurization method, which
has been applied since the 1980s. According to the prin-
ciple of enzyme catalysis for implementing the specific
reaction for C—S bonds cleavage performed by micro bio-
logical flora, sulfides in crude oil can be turned into el-
emental sulfur that can be removed. In the process of
desulfurization, the sulfur containing pollutants are trans-
formed into sulfides and H2S by biological reduction, and
the elemental sulfur can be removed via the process of bio-
logical oxidation. Normally we use photosynthetic bacte-
ria and colorless sulfur bacteria in the BDS process, and
crude oil should stay a few days in the system to be treated
by the BDS method[12].
2
There are two disadvantages associated with this method.
Firstly, this process is not very efficient. Secondly, one kind
of bacteria can only remove one or few sulfides[13]. We are
now focusing on developing new bacterium, preparing new
biocatalysts, improving the capability of the desulfuriza-
tion technology. The efficiency of biocatalysts and envi-
ronmental adaptability are the important factors in com-
mercialization of the desulfurization technology[14-16]. Other
factors to be assessed include the location of refineries and
the biological treatment costs.
According to a report, Iran’s Sharif University of Technol-
ogy has used the bacterial desulfurization process to treat
heavy and sour crude oils in place of the existing refinery
desulfurization process. The bacteria can remove 65%—
76% of total sulfur from heavy crude oil extracted from two
different oilfields, while this desulfurization process is car-
ried out at a temperature below 30 [17-18]
.
The HDS process and the BDS process have different
characteristics, they can complement with each other. Now
some researchers are trying to use both HDS and BDS to-
gether for processing the high-sulfur crude oils under high
pressure and at low space velocity during hydro-upgrading
process. On the other hand, researchers are making strenu-
ous efforts to manufacture cheaper H2 product, and when
the technology continues its development, it is possible to
combine the two technologies in the near future[19-21].
3 New Combined Technologies for Desulfurization of
Crude Oil
The currently available desulfurization technologies are
not perfect, and their disadvantages loom more clearly.
The current technologies for desulfurization of crude
oil cannot be suited to the market needs obviously. All
domestic and foreign researchers have been doing a lot
of effective work to reduce or eliminate the pollution
resulted from processing of sour crude oils. Many new
combined technologies for desulfurization of crude oil
are being studied, such as the biodesulfurization (BDS)
process, the hydrogenation-bacterial catalysis method,
the microwave-catalytic hydrogenation method, the
BDS-OD-RA desulfurization process, the oxidative des-
ulfurization in electrostatic fields, and the ultrasonic/
microwave-catalytic oxidation method that has been
applied in our lab.
 China Petroleum Processing and Petrochemical Technology

3.1 Hydrogenation-bacterial catalytic desulfurization respectively[24].

Leshchev S. M.[22] invented the hydrogenation-bacterial 3.3 BDS-OD-RA three-step integrated desulfurization
catalytic process. This method involves two steps: firstly, process
hydrogenation of the crude oil is carried out in order to
The BDS-OD-RA method is a three-step integrated process.
remove unstable organic sulfides contained in the crude
Desulfurization of high-sulfur crude oil by BDS needs
oil, then an artificial culture of organic sulfur compounds
anaerobic conditions, combined with oxidation and ad-
with selective bacteria named Rhodococcus rhodocrous is
sorptive desulfurization to make this process viable. Des-
used in the desulfurization process. During the biological
ulfurization of low-sulfur crude oil by BDS needs aerobic
oxidation process, organic sulfides (such as dibenzothio-
conditions, combined with oxidation and adsorptive des-
phene series) are subjected to C—S bond cleavage reaction
ulfurization (as shown in Table 2)[25]. So this combined
and turned into inorganic sulfides. Hence this method can
technology for crude oil desulfurization is an important
remove sulfur compounds from oil products efficiently.
development trend.
3.2 Microwave- catalytic hydrogenation process for
desulfurization 3.4 Oxidative desulfurization in electrostatic fields

Microwave energy can be used as the power for regenera-
tion of the HDS catalyst. Integrating microwave,catalysis
and hydrogenation together in the desulfurization process
is more efficient than the traditional technology of des-
ulfurization as shown in Table 1[23]. And microwave in-
ducement can improve the effect of chemical desulfuriza-
tion and better desulfurizing results were gained. The des-
ulfurizing efficiencies increased from 18.6%, 21.8%,
28.5% and 24.3% to 34.7%, 33.3%, 34.5% and 43.3%,
The process of oxidative desulfurization of oil products in
electrostatic fields applied in our lab is carried out as follows.
During the pretreatment process, the desulfurizer is loaded
into the desalter drum, and the feed oil in an electric field is
heated under intensive agitation and mixed with the des-
ulfurizing agent to achieve a complete desulfurization of
the oil. Then the sulfides that are removed after desulfur-
ization reaction are discharged to the wastewater treatment
system[26-27].

Table 1 Microwave-promoted HDS using iron powder as the catalyst[23-24]

Test No. Feed oil Reaction conditions Level of desulfurization, %
1 Dibenzothiophene 50 psi H2, at 200 for 20 min 8
2 Crude oil 50 psi H2, at 200 for 20 min 25
3 Crude oil 20 psi H2, at 200 for 20 min 10
4 Crude oil No H2, at 200 for 20 min No reaction detected
5 Crude oil 50 psi H2, at 250 for 20 min 24
6 Crude oil 50 psi H2, at 200 for 30 min 27
7 Crude oil 50 psi H2, at 200 for 110 s 7
Table 2 Desulfurization of crude oils achieved through three-step integrated process[25]
Sample to be treated HCO LCO HCO LCO
S content, % 1.88 0.378 1.88 0.378
First-step treatment BDS (AN) BDS (AN) BDS (AO) BDS (AO)
S content after the first step, % 0.58 0.138 0.69 0.15
Desulfurization rate, % 69.14 63.40 63.29 61.4
Second-step treatment OD OD OD OD
S content after the second step, % 0.11 0.07 0.23 0.08
Desulfurization rate, % 94.15 81.48 87.76 78.84
Third-step treatment RA RA RA RA
S content after the third step, % 0.09 0.053 0.10 0.022
Desulfurization rate, % 95.21 85.9 94.6 94.3
Notes: HCO: heavy crude oil, LCO: light crude oil, BDS: biodesulfurization, OD: oxy-desulfurization, RA: reactive adsorption,
AO: aerobic, AN: anaerobic.

3
 December 30, 2010 Liu Lin, et al. Progress in the Technology for Desulfurization of Crude Oil
This method is mainly aimed at removing most of mercap-
tans and few thioethers contained in the feed oil. But with
increasing boiling points of petroleum fractions, their mer-
captans and disulfides contents drop down immediately,
and the thioethers content grows first, and then falls down,
while the content of thiophenes keeps rising. Most of sul-
fur in crude oil exists in the form of thioethers and
thiophenes in higher boiling petroleum fractions, these in-
active sulfur compounds are much more difficult to be re-
moved than active sulfides[27].
Moreover, some researches are also studying the methods for
preparation of Sb/Sn intermetallic compound with Al addi-
tion and its behavior for desulfurization of crude oil emulsions.
The desulfurization mechanism was achieved by the electro-
chemical reaction between sulfides and the Sb/Sn surface un-
der electric current induction in combination with the physi-
cal adsorption on active sites like vacancies formed by re-
moving Al atoms on the alloy surface[28].
3.5 Desulfurization process involving ultrasonic/ micro-
wave - catalytic oxidation
The SulphCo Inc. uses the ultrasonic wave to remove the
sulfur compounds from oil, and large-scale ultrasound tests
are being carried out in the EU. The company’s technology
can turn the sour heavy oil into light oil with little sulfur
content to produce more useful oil products[29].
This technology is realized by mixing the feed oil and the
water together with a small amount of oxidizing agent and
catalyst in a container, in which the mixture will react upon
each other under cavatition effects. In the course of reac-
tion the feed oil receives the energy from ultrasonic wave
to mix intensively with water, while the temperature will
raise to more than several thousand degrees of centigrade
with the pressure increasing to more than 1013.2 MPa, that
Table 3 Effects of different desulfurizers and microwave inducement on desulphurization[33]
Dosage of Mass fraction of sulfur content
Desulfurizer
desulfurizer, % after desulfurization, %
DCP 0.01 0.961 (12.6%)
BPO 0.01 0.860 (21.8%)
BBPV 0.01 0.787 (28.5%)
BPMC 0.01 0.833 (24.3%)
H 2O 2 0.05 0.962 (12.5%)
Peroxy acetic acid 0.05 0.860 (21.8%)
Formylhydroperoxide 0.05 0.895 (18.6%)
Note: The reaction was conducted at a temperature of 60 for a reaction time of 30 min.
4
may cause the formation of hydrogen peroxide in the mix-
ture to react upon sulfides that are then turned into some
sulfates, sulfoxides and few sulfones. The solvent can be
reused after regeneration, while sulfoxides and sulfates can
be used to make other products[30-31]. The ultrasonic-oxida-
tive desulfurization process has a lot of advantages such as
simple operation, lower cost, low reaction temperature, low
operating cost and high efficiency. This technology has a
bright future[32].
Using microwave in combination with the catalytic oxida-
tive desulfurization is more efficient than a single catalytic
oxidative desulfurization of crude oil as evidenced by the
results presented in Table 3.
Ultrasonic wave can become a very useful tool in the oil
desulfurization industry. Ultrasonic wave combined with
other technologies can reduce the temperature, the con-
sumption of power and solvent, the amount of waste dis-
charge and the production cost, which can also increase the
efficiency of recycling and product purity. On the other
hand, this process does not cause environmental pollution to
promise a rosy future. This method can fully apply the prin-
ciple of cavatition resulted from ultrasonic wave vibrations
to realize the function of extraction and mechanical agitation,
and the microwave power is applied to improve the pre-des-
ulfurization effect that is applied in our lab currently.
4 Prospects on Development of Crude Oil Desulfurization
At present, the commercial methods for desulfurization of
petroleum products have their own deficiencies. It is neces-
sary to improve the desulfurization process to maximize
the sulfur removal efficiency and turn the waste into trea-
sure that should be reused. The desulfurization efficiency
and economic benefits should be compatible, and the ex-
isting facilities should be fully utilized to provide quick
Mass fraction of sulfur content after desulfurization
coupled with microwave induction, %
0.856 (22.2%)
0.857 (22.1%)
0.720 (34.5%)
0.624 (43.3%)
0.914 (16.9%)
0.734 (33.3%)
0.718 (34.7%)
 China Petroleum Processing and Petrochemical Technology
returns. And it is also necessary to support the develop-
ment of appropriate technologies that can reduce low-value
products, increase high-value products, improve economic
efficiency, and enhance the competitive edge of the enter-
prise[34].
The difficulties in crude oil desulfurization are aggravated
by the existence of polycyclic aromatic hydrocarbons
(PAHs), nitrogenous compounds and H2S. Global crude oil
production has been nearly reaching the limit that technol-
ogy can hardy break through. By building new devices or
optimizing the related technologies, we can improve the
product yield and reduce the materials consumption dur-
ing oil refining, which will bring about significant eco-
nomic returns. In the near future, the key to “zero sulfur”
emissions and minimum consumption of oil that is used to
produce H2 applied in the fuel cells is how to produce
cleaner fuels by a most effective, environmentally friendly,
and economically viable way[35-36].
Removing the sulfur compounds during the pretreatment
of crude oil should be based on the forms and natures of
sulfur compounds existing in crude oil. Upon desulfuriza-
tion and desalting of crude oil, a ternary system of hydrated
liquid is injected into crude oil, which is separated from the
water by gravity under the action of a demulsifier, and after
treatment with a desulfurization agent coupled with the
ultrasonic/microwave treating in an electric field, the low-
sulfur oil can be obtained. This is the key to tackling the
problem for desulfurization of oil that can allow for reduc-
tion of the cost for processing crude oil and for the produc-
tion of clean fuels. The advanced desulfurization technolo-
gies need less investment, and are more efficient for treat-
ing the crude oils that can solve the problems of pollution,
equipment corrosion, equipment overload, and catalyst
poisoning during catalytic cracking process to ensure a
long-cycle, full-load and safe operation of the equipment.
Pretreatment of crude oil by means of desulfurization pro-
cess is the direction for development of oil refinery indus-
try to enhance its economic benefits.
Acknowledgement: The authors are grateful to financial
supports from the Science and Technology Office of
Liaoning Province (Project Number: 2008403001) and the
Liaoning Provincial Office of Education for Innovation
Team (Project Number: 2009T002).
5
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used as the solvent with the reminder routed to the waste-
water treatment system. The PTA mother liquor recovery
and utilization project was put on stream in 2008, and its
utilization rate was raised in 2009. Currently the solid recov-
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equivalent to an incremental 230 tons of PTA. A total of
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a reduction of wastewater discharge of 40 kt/a. The materials
recovered can bring about an incremental income of 1.8625
million RMB to the enterprise.