Sulfur Elimination Through Hydrodesulfurization

This article discusses the process of diesel hydrodesulfurization, which is used to eliminate sulfur from petroleum fuels. It explains the chemical reactions involved and the challenges faced in this process. The article also highlights the importance of reducing sulfur content in fuels for environmental reasons.

Running head: DIESEL HYDRO DESULFURIZATION
Sulfur Elimination Through Hydrodesulfurization
Name of Student
Institution Affiliation

DIESEL HYDRO DESULFURIZATION 2
Executive summary
Growth of industries is the basis of trend in most countries in the world, industrialization
contributes to the development of the state in terms of infrastructure and raising the living
standards of the natives through employment opportunities that come with the development of
industries. Development of industries leads to an equivalent increase in power production to run
heavy machines in plant operations. This result in growing hydroprocessing, to achieve this
combustion of petroleum fuels to provide the driving energy for the industries. Combustion of
petroleum fuels if not properly regulated and monitored can lead to detrimental effects on the
environment [1].
In line with this aspect, Ministry of Petroleum and natural gas allowed a maximum of
0.25 wt. % of sulfur from 1 wt % can be present in petroleum fuels [2]. This regulation demands
that all the refineries construct desulfurization facilities for diesel with the principal aim of
eliminating sulfur content and other petroleum fuels to ensure that their use is environmentally
friendly. This process involves hydro sulfurization, hydro nitrification and olefins, and aromatic
saturation, where these reactions are conducted in bi-functional catalysts. Reactor effluents are
divided into liquid and gas in a chamber known as a separator.
Table of Contents
Executive summary.........................................................................................................................2
Introduction......................................................................................................................................5

DIESEL HYDRO DESULFURIZATION 3
Literature Review............................................................................................................................7
Chemical Synthesis......................................................................................................................7
DIESEL HYDRO DESULFURIZATION..................................................................................7
Hydro Desulfurization.............................................................................................................8
The main purpose of this process is to:..................................................................................9
Chemical reaction mechanism.................................................................................................9
Hydrogenation reactions..........................................................................................................9
Refining reactions..................................................................................................................10
Catalytic hydrotreating..............................................................................................................12
The process....................................................................................................................................13
Reactions and chemical equations.............................................................................................13
DESIGN.........................................................................................................................................17
Workings....................................................................................................................................17
Implementation..........................................................................................................................18
Results............................................................................................................................................22
Challenges..................................................................................................................................25
Recommendations/Future Work)...................................................................................................25
Conclusion.....................................................................................................................................25
References......................................................................................................................................27

DIESEL HYDRO DESULFURIZATION 4
Introduction
Petroleum has been essential to humans as it is used in one way or another to aid daily
operations. Petroleum contains hydrocarbons as the main component with some considerable
amount of nitrogen, sulfur, trace metals and oxygen [5]. From petroleum, fuels are derived such
as diesel among many which are comprised of approximately 0.25 aromatic hydrocarbons and
0.75 saturated hydrocarbons[5]. In diesel sulfur makes the main contaminant ranging between
0.1% and 0.5%, this is undesirable to the environment since it increases the polarity of the fuel,
poison catalysts enhance emulsion stability and confer color [7]. During combustion of diesel
fuel, sulfur oxides may be released into the environment either as gaseous or particulate solid
matter. Gaseous discharge of burning sulfur include Sulfur oxide (SO2) and (SO3), these causes
great damage to the atmosphere and environment [11]
The target of international and domestic environment agencies has always been to control
and lessen the use of sulfur fuels to a level of environment-friendly. In situations where sulfur
related fuels are commonly used, the concentration of sulfur is also high to about 300ppm. The
objective of these agencies is to reduce this concentration level to about 100ppm. [6]
For effective and efficient removal of this sulfur from diesel fuels desulfurization process is most
ideal. With the current fast-growing of the automobile industry and industrialization leads tom
high demand for crude oil and diesel fuel as the operating fuel [4]. These lead to a corresponding
increase in the amount of sulfur released to the environment. Thanks to the endless efforts geared
towards achieving the lowering of sulfur content in these fuels through various processes.
Desulfurization is used by refiners in the context of eliminating production onboard
transportation fuels due to high compliance expenses to the set regulations [8]. Advanced
technologies have been established to obtain the most viable and economical methods of sulfur

DIESEL HYDRO DESULFURIZATION 5
removal from petroleum fuels. Through the major source of sulfur pollution, petroleum refining
industries, both direct and indirect motor fumes, are in the front line for the struggle to achieve
environment-friendly and sustainable operation.
Problem statement
The increased concerns in the petroleum refining industry concerning the quality of air
has resulted in the urge to eliminate the heteroatoms which contain molecules from the products
of gasoline, diesel and their major products. Despite various efforts aimed at reducing the
contents of sulfur in the diesel oil, the quality of fuel, as well as the regulations, is deemed to be
affected. Various options have also indicated improvements in one sector while giving rise to
environmental and sustainability concerns. It is for this note that this design will be of great
significance in attempting to create a balance for both the factors.

DIESEL HYDRO DESULFURIZATION 6
Literature Review
Chemical Synthesis.
Chemical synthesis is the process that involves the disorientation of the already existing
chemical bonds that both hold molecules or compounds together and form new bonds in
molecule or compounds that are more valuable than the existing ones. Synthesis of more
complex molecules at times involve quite a number of individual reactions that eventually
undergo sequential reaction from available initial materials to the desired final product with each
step involving reaction at the only single chemical bond in the molecule [2]. This process
requires planning and analysis of the route of chemical reactions, this demands that the chemists
have to visualize the end product and develop a backward work formula towards increasingly
simpler compounds. These are often used depending on many other factors such as availability
of starting material together with their costs [5], amount of energy required to start and sustain
these reactions and separating costs and purification of the end product.
DIESEL HYDRO DESULFURIZATION
The issue of desulfurization is gaining a lot of focus since crude oil is getting higher in
sulfur content. In order to control the level of sulfur in hydrocarbon fuels for fuel use and
protection of the environment, diesel hydrodesulfurization of the model duel and real fuel are
studied by Selective absorption for removing Sulfur (SARS) process using appropriate adsorbent
[6], examining the temperature during the desulfurization process. In regard to technology
availability, the current hydrodesulfurization is hard to control the sulfur concentration in diesel
fuels below 50 ppm since the remaining sulfur concentration in commercial diesel fuels are 4-

DIESEL HYDRO DESULFURIZATION 7
methyldibenzothiophene, 4, 6-dimethyl dibenzothiophene and other alkyl dibenzothiophenes
which are quite difficult to eliminate.
In recent research, the process of sulfur removal from transportation fuels has become of
great importance to every organization and nations worldwide due to heightened interest to have
clean air in the atmosphere hence increasingly stringent laws and regulations for sulfur fuels to
the environment [8]. The high demand for ultra-low sulfur fuels for fuel cells with modern
automobiles that are much more efficient and friendly to the environment [11]. Liquid
hydrocarbon fuels are on the rise due to the fact that they are a promising ingredient because of
their high energy density, storage, and transportation safe [7]. Automotive fuel cells, for
example, the developing PEFC and SOFC auxiliary power units in vehicles diesel and gasoline
are the most preferred fuels since they are easily available and ease in their production, storage,
and delivery. However, gasoline and diesel fuels contain a significant amount of sulfur ranging
from 300 to 450 ppm [9]. The sulfur content in fuel and hydrogen sulfide H2S produced by these
fuels are very poisonous to catalysts both electrode catalysts and in hydrocarbon fuel processor
catalysts. Thus for fuel cell application in industries and in automobiles, the sulfur content in the
fuels needs to be maintained at the lowest level possible [5]
Hydro Desulfurization
This is referred to a catalytic chemical reaction process where sulfur is eliminated or
removed from petroleum fuels such as petrol, diesel fuels, jet fuels, kerosene and natural gas [2].
The process is usually used in advancing the rating of octane in naphtha streams. Fuels obtained
through this process reduce sulfur and its oxide emission in vehicles, train, power plant, aircraft,
residential furnace, and industrial furnaces and other fuel combustion forms. [8]

DIESEL HYDRO DESULFURIZATION 8
The main purpose of this process is to:
1. To perform desulfurization of the diesel fuels in the reactor feed to obtain the desired
specification
2. To use a catalyst to determine hydrogenation of eventual olefin structure.
Chemical reaction mechanism
1. Hydrogenation reactions
2. Refining reactions
Hydrogenation reactions.
These are processed reactions that affect directly aromatics, diolefins, and olefins and are
associated with high temperatures where olefins and diolefins are transformed into saturated
compounds with a restriction on the reaction rate of aromatics.
The feed to the diesel hydrodesulfurization unit is a merger of cracked gas oils and straight run.
These feed fuels are then filtered through a filter package to surge drum where the pressure is
maintained at a constant level through fuel gas blanketing [10].
The liquid phase feed pump is pumped underflow control by feed pump, combined with
hydrogen recycle compressor delivery stream and let in the heat exchanger train. The injection of
inhibitors that prevents polymerization at the inlet of the reactor facilitates the combining the
recycle hydrogen with feed to ensure sufficient hydrogen partial pressure. [9]
Hydrogenation of olefin compounds
RCH=CH2 + H2 RCH2 –CH3
Hydrogenation of aromatic compounds
C6H6 + 3H2 C6H12

DIESEL HYDRO DESULFURIZATION 9
The incoming hydrogen make up gas is directed via chlorine adsorbent before it is
compressed. Some portion of this gas is channeled into the reactor as quench gas. In the heat
exchanger, the combined stream is intensified before passed to the second exchanger and lastly
to the reactor heater where it's heated to the desired input temperature [8]. The temperature of the
reactor is regulated by regulating the fuel oil to fuel gas into the heater and then the stream is
then introduced to the reactor with catalysts. This is done in three beds and the temperature of
each bed is controlled by introducing cold quench hydrogen from the recycling compressor [11].
Water is let at the effluent inlet to prevent deposition of ammonium salts that might cause
corrosion of the reactor. The sour water is partly recycled since it contains ammonium salt and
can be used in washing.
Refining reactions
Denitrification- this reaction only occurs in cases of heterocyclic compounds with an
aromatic structure such as pyridine and the rate of reaction of denitrification is lower compared
to the rate of desulfurization. Denitrification leads to the establishment of ammonia gas and the
elimination of hydrogen gas[7]
Denitrification
C2H2N + 5H2 C2H2 + NH 3
Desulfurization is the reaction that involves saturated sulfides, disulfide, and aromatic
compounds. Sulfur combine in the cycle of the aromatic structure is not easy to eliminate like in
case of thiophene. This reaction leads to the formation of hydrogen sulfide and hydrogen
consumption. [5]
Desulfurization
RSH + H2 R-H + H2S

DIESEL HYDRO DESULFURIZATION 10
Diesel hydrodesulfurization is also referred as hydrotreating as it is widely used in
petroleum refineries and mining industries for the purpose of producing high-quality fuels as
well as upgrading crude oil by eliminating or lowering concentration of metal, sulfur or nitrogen.
For the design and installation of new plants [2], detailed research is of the essence to function at
optimal conditions. This involves steady-state reactor which becomes significant in the actual
process of refining. When considering light-medium reactors and because it involves probably
mixture hundreds of compounds, which not all of these compounds can be explicitly considered.
In such a case, hypothetical compounds are clearly defined to take the basis of feed. This is
followed by a characterization step of feed to obtain feed composition in reference to the
hypothetical components [8].
Some previous approach to tackle this process was by defining quasi compounds
generated as a result of true boiling. Another approach is to employ lumping of species where
various species are clustered by their chemical families with similarities in their structural and
chemical behavior [7]. Hydrotreating of diesel fuels is based in three phases that are varied
catalysis: where the model have proper consideration on how to formulate the starting points
stating all kinetics that defines the reactions, then estimate this kinetic essentials with data
obtained at pilot plant scale eventually scaling up [3]. Even though this aspect of hypothetical
considerations, it's associated by some setbacks that might arise in the refinery reactor modeling
and as new feeds which prevent the formulation of a fixed reaction set. The best way to manage
this, there should be a hydrocarbon mixture beginning with the feedstock properties where
configuration of molecular techniques have produced satisfactory outcomes. [10]

DIESEL HYDRO DESULFURIZATION 11
Catalytic hydrotreating
It refers to the hydrogenation process that is employed to eliminate environmental
pollutants such as nitrogen, metals, and sulfur from petroleum fractions such as diesel, petrol
kerosene and gasoline [4]. Elimination of these pollutants is very crucial since when they are
carelessly released to the atmosphere, they have harmful implications on the equipment's, end
products and even the catalysts. Hydrotreating is also efficient since it removes about 90% of
these contaminants from crude petroleum [9]. This process of hydrotreating is done prior to
catalytic reforming to avoid contamination of catalysts by untreated feedstock. It also comes
before catalytic cracking to boost product yield and upgrade middle distillate petroleum portions
into finished end products such as heating fuel oils, kerosene, and diesel fuels [3]. It also
enhances the conversion of aromatics and olefins to saturated compounds.
The process
Figure 1.1Schematic of hydrodesulfurization
Hydrodesulfurization is the hydrotreating that involves the removal of sulfur from diesel
fuels [8]. The process commences with the feedstock being deaerator then combined with
hydrogen which is preheated in the heater to a temperature of 8000F then charged at a pressure of

DIESEL HYDRO DESULFURIZATION 12
up to 1000 pascal via a catalytic reactor [10] [12]. The conversion of sulfur and nitrogen
compounds present in feedstock takes place to produce hydrogen sulfide H2S and ammonia NH3.
After cooling to considerably low temperature these products leaves the reactor and enters to the
gas-liquid separator. The gas rich of hydrogen is then recycled back to the feedstock while low-
pressure gas stream reaches in hydrogen sulfide H2S is directed to the gas treating unit for
removal. The clean gas is channeled to fuel refinery chamber [4], liquid stream product from
hydrotreating id sent to doffing tanks for extraction of H2S together with other unwanted
components.
Reactions and chemical equations
The removal of sulfur demands for special conditions in order to efficiently eliminate
sulfur from diesel fuels. In the case of organosulfur compounds involving reaction with hydrogen
gas producing hydrogen sulfide, this reaction requires high hydrogen pressure greater than 200
atm and temperature of 4500C [3] [11]
There are different types of catalysts that escalate various reactions depending on the
requirements for the reaction to occur. The selection is also pegged on the type of oil being
purified. The most commonly used catalysts are a combination of Mo and Co sulfides with
alumina, a mixture of Ni and Mo. There a number of models that gives a detailed clarification to
the manner thiophene moieties are oriented on the catalysts, generally, the Co-Mo-S model
developed by Topsoe. Under this catalysts are formed in a mono layer of Mos2 with Co or Ni at
the edges [6].
The coordination of thiophene Moieties occurs in a way that all the thiophene molecules,
present the sides with an increased electronic density forming the single pair of sulfur atoms and

DIESEL HYDRO DESULFURIZATION 13
the double bond within carbon atoms [9][14][16]. Some of the coordination is involved in the
hydrogenolysis process. The common coordination mode of the thiophenes is shown in figure
1.2 below.
Figure 1.2 Coordination of thiophene
In the recent research has managed to develop the first catalytic illustration of the desulfurization
of 4, 6-Me2DBT using nickel-phosphine with Grignard components to produce cross-coupled
sulfur-free fuels [17]. Catalytic desulfurization of DBT with nickel-phosphine is shown in figure
1.3 below.

DIESEL HYDRO DESULFURIZATION 14
Figure 1.3 Catalytic desulfurization of DBT with nickel-phosphine

DIESEL HYDRO DESULFURIZATION 15

DIESEL HYDRO DESULFURIZATION 16
DESIGN
Workings
In order to proceed with the mathematical calculations, below parameters were provided
 Feed diesel flow rate: 360 m3 / hr
 Make-up H2 flow rate: 21,000 kg / hr
 Initial sulfur content present in diesel: 15,000 ppm (1.5%)
 Final sulfur content present in diesel: 300 ppm (0.03%)
 The molecular weight of diesel: 229.5
 The density of diesel: 857.393
 Spacetime: 0.9127 hr
Additionally, some of the below assumptions were made
The formula below will assist in determining the Heat of Formation calculation for
hydrodesulfurization reaction.

DIESEL HYDRO DESULFURIZATION 17
Implementation
The process of hydrotreating the diesel fuel having a 1.5% mass of Sulphur is conducted
under a laboratory catalytic equipment [18]. The set-up of the laboratory is characterized by the
condenser, vaporizer, reactor, products as well as a special metallic grid having a catalyst. The
capacity of the catalysts was measured to be 20 millimeters. Hydrogen and diesel fuel fraction
are fed subsequently at the top the reactor. Further, a high-pressure dosing pump is supplied at
the feed [19]. Using an automatic dispenser, it becomes easier to regulate the hydrogen feed.
Additionally, to ensure that the accuracy of the heat having an error is nit more than 0.5 degrees,
a thermal regulator is installed in the thermostat [11]. At the Center of the reactor is the
thermocouple which ids in determining the temperature of the catalyst. A high-pressure reducer
is then used to set the system pressure and regulate the data in the exemplary gauge.

DIESEL HYDRO DESULFURIZATION 18
The products from the reaction then flow into the water condenser, whereby the liquid
products are poured into the receiver for collection and subsequent analysis. A valve choke Is
present where the gaseous products enter through, and then discharge into the atmosphere. The
catalyst for the process is known as aluminum-cobalt-molybdenum catalyst GKD-202. This type
of catalyst is manufactured in Russia and has the shape of cylinder granules [20]. The active
metals used in the process are molybdenum and nickel, while aluminum oxide is used as a
carrier. Sample catalyst is then charged into the reactor, having the size of a granule of 2
millimeters. Prior to the use, the catalyst was the first sulfide into the reactor directly [10]. The
diesel fraction, thereafter having a mass content of 0.03 Sulphur was used. The process of
sulfidation included the below steps
I. Drying the aluminum-cobalt-molybdenum catalyst GKD-202 at a temperature of 120-
degree Celsius in a stream of nitrogen
II. Increasing the pressure of the reactor to 3.5 mpa after supplying it with hydrogen.
III. Using the feed to wet the catalyst
IV. Escalating the reactor temperature to 240 degrees Celsius
V. At a low-temperature stage, performing the sulfidation for 2 hours, at 240 degrees Celsius
temperature
VI. Thereafter increasing the temperature to 340 degrees, and then sulfiding at the high-
temperature stage for a period of 2hours
After coming up with the sulfide mixture, the sulfide mixture I fed into a reactor, having
a capacity rate of 2 h-1, and a fed rate ratio of 360 m3 / hr. The below conditions are then
utilized to conduct the hydrotreating process.

DIESEL HYDRO DESULFURIZATION 19
Feed diesel flow rate: 360 m3 / hr., temperatures of 340, 360 and 380 degrees Celsius. Make-
up H2 flow rate: 21,000 kg / hr., Initial sulfur content present in diesel: 15,000 ppm (1.5%),
Molecular weight of diesel: 229.5, Density of diesel: 857.393 and Spacetime: 0.9127 hr.
A spectral photometer is then used for the checking of concentration of the sulfur content, which
was confirmed to be 1.5% [7].
The identification of the sulfur compounds was made possible by the gas-liquid
chromatography. The carrier gas used was helium gas. A liner increase in temperature was
realized during the analysis of the sulfur compounds, from 50 to 290 degrees Celsius. The rate of
hate was set at 4 degrees every minute [21].
Qualitatively, the configuration of the sulfur compounds was arrived at by comparison of
the retention times of the singular compounds (dibenzothiophene, benzothiophene, and (hexyl
sulfide) as well as the analyzed components. By extension, data from literature was utilized
On the other hand, the quantitative composition was achieved through analysis of the space peak
areas which are obtained from the calculation in the below section.
Kinetic scheme of the dehydrogenation process
SCHEMATIC MODEL

DIESEL HYDRO DESULFURIZATION 20
Mathematical model

DIESEL HYDRO DESULFURIZATION 21
Results
In the current research, programming software’s; fressbsic and freepascal are utilized to
aid in the implementation of the reverse problem that is in regards to the diesel fuel
desulfurization. The primary functions are to determine the kinematic parameters which are more
of all the overall rate constants of all the quantified process routes. The input data which is used
are the final and initial concentrations. The equations are solved by means of the quasi-
homogeneous model, which is in the form of differential equations [22].
The probable amalgamations of the rate constants k1 are included mathematically in the
cycle with various recursive steps ofܰ ൌܵ ௄. Runge Kutta technique is utilized for the test
calculation of the product concentrations. Three scan points are used for the calculation of the
chemical rate constants, i.e. Two side points and a central point. The optimal
condition is selected by the sum of the concentration differences.
Where
P – a number of concentrations

DIESEL HYDRO DESULFURIZATION 22
Cexp, i – experimental concentration
Ccalc, i – calculated concentration
The molar concentrations realized are recorded in the table below
The above graph was destined to rely on the dynamics of the sulfur compound
concentrations vis-à-vis the reactive time. From the curve, the hydrogenation process is directly

DIESEL HYDRO DESULFURIZATION 23
proportional to the concentration of the hydrocarbons. From the deigned algorithm, the effective
values for the rate constants result into the below illustrations
Challenges
Despite the low reduction of sulfur content in the overall diesel product, there still other concerns
which have sprouted, and needs to be addressed. For instance; environmental and sustainably
issues concerned with the whole process of diesel hydro desulfurization [23]. Additionally, most
of the substrates such as thiophenes which presents out as a challenge to the whole procedure.
Recommendations/Future Work).
The only probable way which remains to possible reduce the content of sulfur in diesel to
a very lower is by the complete elimination of 4,6-dimethyl dibenzothiophene (4,6-DMDBT).
However, its hydrodesulfurization does not take place via the direct methodology of
desulfurization [25]. Hence, the reactivity needs to be enhanced, either by converting it into a a
highly activated molecule via isomerization, hydrogenation, c-c bond scission, as well as
demethylation or by enhancing the degree of direct desulfurization. In the past, there have been

DIESEL HYDRO DESULFURIZATION 24
various attempts which have been undertaken to improve the catalysts. For instance; fluorine,
phosphorus zeolite, lanthanum, Titania and zirconia [5]. More research needs to be done on
these additives to help enhance the catalysts. Additionally, system modification for purposes of
better energy savings improved performance is also significant and more research needs to be
undertaken in the area.
Conclusion
Petroleum and petroleum products have played a significant role in our daily life, by
aiding the daily activities. However, it has been associated with environmental issues due to the
contaminants which it contains such as sulfur. In diesel, sulfur makes the main contaminant
ranging between 0.1% and 0.5%, this is undesirable to the environment since it increases the
polarity of the fuel, poison catalysts enhance emulsion stability and confer color. During
combustion of diesel fuel, sulfur oxides may be released into the environment either as gaseous
or particulate solid matter. Gaseous discharge of burning sulfur include Sulfur oxide (SO2) and
(SO3), these causes great damage to the atmosphere and environment.
This report has looked into a methodology of diesel hydrodesulfurization, with the aim of
reducing the concentration of sulfur content in the overall diesel product. A mathematical has
also been developed, having various algorithms which have validated the process of
hydrodesulfurization. Despite the reduced concentration of sulfur, much still needs to be done.
For instance, enhancing the reactivity of the desulfurization of 4,6-dimethyl dibenzothiophene
(4,6-DMDBT), or the addition of various additives to the catalyst can be imperative to ensuring
quality products.

DIESEL HYDRO DESULFURIZATION 25
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