Petroleum Science: Jing Tan, Ya-Ni Ji, Wen-Sheng Deng, Yue-Feng Su

Petroleum Science 18 (2021) 1203e1218
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Petroleum Science
journal homepage: www.keaipublishing.com/en/journals/petroleum-science
Review Paper
Process intensification in gas/liquid/solid reaction in trickle bed

reactors: A review
Jing Tan a, *, Ya-Ni Ji a, Wen-Sheng Deng a, Yue-Feng Su b
a
School of Chemistry and Chemical Engineering, Beijing Institute of Technology, Beijing, 100081, China
b
School of Material Science and Engineering, Beijing Key Laboratory of Environmental Science and Engineering, Beijing Institute of Technology, Beijing,
100081, China
a r t i c l e i n f o a b s t r a c t
Article history: As an important form of reactors for gas/liquid/solid catalytic reaction, trickle bed reactors (TBRs) are
Received 8 December 2020 widely applied in petroleum industry, biochemical, fine chemical and pharmaceutical industries because
Accepted 26 January 2021 of their flexibility, simplicity of operation and high throughput. However, TBRs also show inefficient
Available online 8 July 2021
production and hot pots caused by non-uniform fluid distribution and incomplete wetting of the catalyst,
Handling Editor: Kun Ma which limit their further application in chemical industry. Also, process intensification in TBRs is
Edited by Yan-Hua Sun necessary as the decrease in quality of processed crude oil, caused by increased exploitation depths, and
more restrictive environmental regulations and emission standards for industry, caused by increased
Keywords: environment protection consciousness. In recent years, lots of strategies for process intensification in
Trickle bed reactor TBRs have been proposed to improve reaction performance to meet the current and future demands of
Process intensification chemical industry from the environmental and economic perspective. This article summarizes the recent
Gas/liquid/solid catalytic reaction progress in techniques for intensifying gas/liquid/solid reaction in TBRs and application of intensified
Petroleum industry TBRs in petroleum industry.
© 2021 The Authors. Publishing services by Elsevier B.V. on behalf of KeAi Communications Co. Ltd. This
is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/
4.0/).
1. Introduction et al., 2015; Kim and Ihm, 2011; Mudliar et al., 2010), electro-
chemistry (Abdullah and Xing, 2017) and fine chemical industry
Gas/liquid/solid multiphase reaction plays an important role in and pharmaceutical industry (Bonrath, 2014; Zhang et al., 2015),
chemical reaction engineering and has been regarded as one of with the targets of conversing unsaturated organic compounds into
main conference topics in important international conferences, saturated products, upgrading petroleum raw materials and in-
such as International Symposia on Chemical Reaction Engineering termediates as well as conversing undesirable by-products into
(ISCRE) and International Symposia on Catalysis in Multiphase environmentally acceptable and recyclable products (Fig. 1). In
Reactors (ISCMR). As an most important type of multiphase re- recent years, requirements of stringent environmental laws and
actors, trickle bed reactors (TBRs) show advantage in flexibility, regulations have necessitated the in-depth processing. For
simplicity of operation, large annual throughputs and are exten- example, in deep hydrodesulfurization of diesel fractions, TBRs
sively applied in chemistry industry, including petroleum refining become a potential type of reactors, which remove a few parts per
(Yuan et al., 2020; Behnejad et al., 2019; Kaiser, 2017; million of refractory sulfides.
Ghassabzadeh et al., 2020; Liu et al., 2011; Chi et al., 2013), petro- TBRs are employed for gas-liquid-solid reactions, in which liquid
chemical industry (Dashliborun et al., 2016; Gorshkova et al., 2012), and gas phases flow (either countercurrently or concurrently)
biochemical engineering (Devarapalli et al., 2016; Karimi et al., through a fixed bed of catalyst particles, where reactions take place
2009), environmental engineering (Rachbauer et al., 2016; Üresin (Fig. 2). Plug flow is nearly achieved in TBRs because of the
motionless catalyst bed, and in this regard, they are superior to
other gas/liquid/solid three-phase reactors where catalyst is either
fluidized or slurried. TBRs show high catalyst loading per unit
* Corresponding author.
volume of liquid and low energy dissipation rate and thus have the
E-mail address: tanjing@bit.edu.cn (J. Tan).
https://doi.org/10.1016/j.petsci.2021.07.007
1995-8226/© 2021 The Authors. Publishing services by Elsevier B.V. on behalf of KeAi Communications Co. Ltd. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
J. Tan, Y.-N. Ji, W.-S. Deng et al. Petroleum Science 18 (2021) 1203e1218
Fig. 1. Application examples of TBR.
Fig. 2. Schematics of TBRs. (a) Cocurrent downflow; (b) cocurrent upflow; (c) Countercurrent flow.
advantage of massive production compared with slurry reactors. Process intensification techniques, characterized by significantly
Based on different gas and liquid flow rates, fluid properties and improving process efficiency, that is, reducing energy consumption,
bed characteristics, four flow regimes exist: trickle flow, pulse flow, by-product formation and equipment size, considerably contribute
spray flow and bubble flow. Trickle flow, characterized as small to sustainable development in chemical engineering. Methods of
liquid flow rates and low or moderate gas flow rates, is the most improving reaction performance in TBRs through process intensi-
routine operation regime applied in industrial processes. However, fication (Fig. 3) have drawn great attention from researchers.
drawbacks in TBRs, such as uneven gas-liquid distribution and low In this article, strategies and mechanisms in process intensifi-
catalyst wettability, cause uncontrollable reaction process, lower cation of gas/liquid/solid catalytic reaction in TBRs over the last
yield, more by-products and hot spots for highly exothermic reac- decade from different methods are summarized, including oper-
tion and thus lead to the limitation in their application. Enhance- ating methods and techniques, solvent, catalyst, reactor structure
ment in reaction performance of TBRs is necessary for their efficient as well as alternative energy sources, and their advantages as well
application and for meeting the requirements of green chemistry in as disadvantages are discussed accordingly.
chemical industry. Moreover, any advancement of TBRs, even if is
very small, brings considerable cost saving and economic benefits.
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Fig. 3. Process intensification techniques. Reprint permission obtained from Stankiewicz (2003).
2. Process intensification techniques Cycle mode (Matthischke et al., 2018; Urme s et al., 2020) is an
unsteady state operation mode, in which reaction performance is
A series of mass transfer and reaction processes (Fig. 4) are enhanced by periodically changing operating conditions such as
involved in gas/liquid/solid three-phase reaction in TBRs. Reaction reaction temperature, gas flow rate, liquid flow rate, reactant con-
rate is restricted by hydrodynamics, mass and heat transfer centration and catalyst activity, by improving the competition be-
composed of gas-to-liquid (Tadepalli et al., 2007), liquid-to-solid tween the gas and liquid phases in supplying reactants to reactors,
and inside solid phase steps and intrinsic kinetics, which are as well as the complex interactions between hydrodynamics and
influenced by operating parameters, liquid holdup, wetting effi- reaction. In this mode, catalyst surface is renewed periodically and
ciency, intraparticle diffusion, axial dispersion and catalyst-bed interaction between gas and liquid phases is enhanced, thereby
structure. Conventional techniques in enhancing reaction perfor- effectively improving both wetting and flow distribution
mance in TBRs are mainly realized by increasing temperature to (Dashliborun et al., 2016). Dietrich et al. (2012) proposed a reliable
enhance catalytic activity, increasing operating pressure to improve periodically operating effective assessment method, in which
gas solubility or increasing concentrations of reactants, catalysts improved local liquid distribution is demonstrated by visualization
and co-catalysts within the operating ranges. In this article, process technology of Nuclear Magnetic Resonance tomography (NMR-to-
intensification by applying novel operating methods, solvent, mography). Hamidipour et al. (2013) successfully predicted the
catalyst, reactor structure and alternative energy sources are hydrodynamics of TBRs by Computational Fluid Dynamics (CFD)
mainly discussed. simulations and verified the model by Electrical Capacitance To-
mography (ECT) imaging under different cyclic operation condi-
2.1. Operating methods and techniques design tions. Wongkia et al. (2013) demonstrated increased conversion in
TBRs under unsteady operation. Although the merits of unsteady
TBRs are usually operated at low gas/liquid flow rates, in which operation praised in the literature as one of the process intensifi-
interaction between gas and liquid is quite poor. Researchers have cation strategies advocated for TBRs, there is still reluctance to
been trying to improve catalytic performance by adopting novel implement it in industrial. It can partly be ascribed to the lack of
operating methods and techniques, taking cycle and upflow modes hydrodynamics studies relevant to complex nonlinear behavior of
as typical examples, which are both effective for increasing fluid cyclic operating mode (Atta et al., 2014), engineering data relevant
distribution uniformity and improving wetting. to the elevated temperature and pressure characterizing industrial
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Fig. 4. Determination of reaction control steps.
processes and research relevant to the effect of reactor scaling-up such as elevated-temperature and high-pressure conditions,
on periodic operation performance. Therefore, more flow visuali- uniqueness of bed structure, complexity of reaction and hydrody-
zation should be directed to hydrodynamics studies for different namics phenomena. Therefore, studies have been carried out to
operations. More unsteady state CFD models need to be developed understand and quantify hydrodynamics of TBRs. Advanced tech-
involving all possible parameters for extensive research, which lay niques such as computed tomography (CT) (Johnson et al., 2017),
the foundations for industrial scale-up. wire mesh sensor (WMS) (Schubert et al., 2010), magnetic reso-
Upflow provides better axial and radial mixing than downflow nance imaging (MRI) electrical resistance tomography (ERT) (Singh
mode, with significant advantages in terms of liquid distribution, et al., 2019), electrical capacitance tomography (ECT) (Hamidipour
selectivity, temperature control and scaling-up. Moreover, increase et al., 2009) and X-ray digital industrial radiography technique
in liquid holdup as well as long residence time eliminates genera- (DIR) (Salleh et al., 2014) have been used to obtain internal struc-
tion of hot spots. Wu et al. (1996) systematically analyzed the ture of catalyst bed and gas-liquid distribution under actual oper-
research results under different operating modes and proposed ating conditions. The combination of the above advanced
reasonable approaches to adapt different operating modes. techniques and computational fluid dynamics (CFD) provides a
Houwelingen and Nicol (2011) found a greater conversion in powerful tool for studying fluid flow phenomena as an alternative
upflow within trickle flow operation than downflow. There are also to empirical models.
deficiencies in upflow, mainly includes increased liquid film In the current study, most TBR simulation (Fig. 5) focus on mass
thickness and pressure, both caused by increased holdup. The and heat transfer model, multiphase flow model, porous media
former one causes increased external mass transfer resistance from model and drag force model. In most cases, reactions in TBRs are
gas phase to catalyst surface, when the latter one leads to ther- limited by mass transfer because of poor interaction between gas
modynamic instability. and liquid phases and low mass transfer rate compared to other
As the strong interaction between gas and liquid phases and 4 heterogeneous catalytic reactors with intense mixing process.
times higher mass transfer rate compared to trickle regime in pulse Therefore, developing mass transfer models is necessary for better
regime, pulse flow operation mode has become a new enhance- understanding TBRs (Table 1). Also, establishing suitable heat
ment method. Inclined rotating tubular fixed bed reactor transfer models and accurately estimating heat transfer rate are
(Dashliborun et al., 2017) is considered to be a new and effective important in reactor design and scale-up for avoiding thermal
pulse flow regulation method, which can effectively suppress hot runaway caused by low heat transfer rate and a large amount of
spots because of the periodic renewal of liquid on catalyst surface, heat released by reactions. Mass and heat transfer are affected by
extend catalyst lifetime because of uniform utilization of catalyst momentum transfer involving flow velocity and distribution of gas
bed and flexibly adjust liquid residence time by controlling the tilt and liquid phases, which makes it important to study momentum
angle and rotation speed. Ha €rting et al. (2015a, b, c) showed that transfer model. Among them, multiphase flow model includes
reaction performance in the above novel reactor increased by 2 Euler-Lagrange and Euler-Euler methods, the former of which is
times in comparison to that in traditional TBRs. applied to discrete phase and the latter is applied to continuous
In addition, reactor performance is also influenced by factors phase. The Euler-Euler method is the most widely used in the
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Fig. 5. Numerical simulation of TBRs in literature.
Table 1
Mass transfer correlations used in some systems.
System Correlations Conditions Reference
T, K P, uG/Qm,G /SV uL/Qm,L Catalyst

MPa
Hydrogenation of a- Sh 413.15 / 0.35 m/s 3.2 102- Pd/g- Shigarov and Kirillov
¼ 0:395Re0:64
methylstyrene Sc0:33
eq 6.4 102 g/s Al2O3 (2009)
Sh 0:468Reeq
¼
Sc0:33 1:18Re0:41
eq 1:52
Sh
¼ 0:201Re0:707
eq
Sc0:33
Hydrogenation of benzene u
kLG af GS 343 1.6 5.98 109- 1.5 106- Ni/ Kallinikos and
uLS 1.12 107 m3/s 3 106 kg/s Al2O3 Papayannakos (2010)
Hydrogenation of octenes kR1 kR2 333.15 5 1 105- 1.8 103- Pd/g- Houwelingen and Nicol
kLS a,f ¼
and isooctenes kR1 =kT1 kR2 =kT2 2 103 m/s 7.5 103 m/s Al2O3 (2011)
Hydrogenation of Sh ¼ 2 þ 54:7Sc1=3 We1=2 41=10 303.15 0.1 5.67 103- 6.37 104- Pd/ Tan et al. (2012)
Ethylanthraquinone 4 ¼ QG =ðQG þ QL Þ e353.15 e0.4 2.83 102 m/s 6.37 103 m/s Al2O3
Hydrogenation of a- 0:24 0:49 343.15 1.1 0.002e1.18 m/s 5 103-102 m/s Pd/g- Langsch and Haase
uG;S uL;S
methylstyrene Sh ¼ 801 e373.15 Al2O3 (2013)
½m,s1 ½m,s1
Catalytic wet air oxidation of Sh ¼ 2:29f0:91 ðReL þ ReG Þ0:04 373.15 0.6 3 103- 5 104- Pd/ Tan et al. (2019)
phenol " !1=3 # e453.15 e1 2.5 102 m/s 4 103 m/s Al2O3
d uG;sup þ uL;sup
f ¼ i Ca0:19 1
dp L uG;sup
simulation of TBRs, which includes Eulerian model, volume of fluid structures can be avoided. In addition to multiphase flow model
model and mixture model. The Eulerian model (Jindal and Buwa, and porous media model, the drag force model is also important for
2017; Jejurkar et al., 2020), which was developed to simulate ho- the simulation of TBRs. The relative permeability model (Xiao et al.,
mogeneous and heterogeneous reactions by taking account inter- 2012), in which the concept of relative permeability was introduced
action among phases, is most widely applied in TBRs simulations. to modify the drag force expression for single phase flow, is
The VOF model (Deng et al., 2020) mainly focuses on capturing applicable for two-phases flows, although without taking into ac-
characteristics of phase interfaces. The Mixture Model is applicable count of gas-liquid interaction forces. The silt model (Iliuta and
to bubble flow. The porous media models (Lu et al., 2018; Larachi, 2009), in which fluid flow around catalyst bed is regar-
Mohammadpour et al., 2019) were developed to simulate catalyst ded as flowing through a rectangular slit, is applicable to poor
particles in TBRs, in which establishment of complex geometric interaction condition by ignoring gas-liquid interaction and taking
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into account of slip effect. The fluid-fluid interfacial force model 2.3. Catalyst design
(Hamidipour et al., 2013), in which gas-liquid interaction are
considered, can reasonably predict pressure drop and liquid holdup Catalysts vary reaction rates within 3e6 magnitude and also
under high pressure or high gas concentration. play an important role in improving overall performance of het-
erogeneous catalytic process. Catalyst design has become one of the
most important strategies to enhance catalyst activity (Comandella
et al., 2017), prolong catalyst lifetime (Davie et al., 2008), increase
catalyst mechanical strength (Zhao et al., 2019), improve product
2.2. Solvent design selectivity, reduce costs, decrease pressure drop and realize uni-
form liquid distribution (Honda et al., 2014). This section presents
During the reaction, solvent influences reactant solubility, an overview of recent work in catalyst design, mainly including the
catalyst dispersibility, adsorption and desorption behavior of shape, size, mechanical strength, main active constituents and
catalyst surface, and it also acts as a heat carrier for heat released in filling method.
exothermic reaction as well as heat supply in endothermic reaction. The shape, size and mechanical strength of catalyst particles play
Organic solvents, with great solubility, help enhance reaction rate significant roles in catalyst design for minimizing pressure drop and
in gas/liquid/solid three-phase catalytic reaction processes (Wu maximizing catalytic activity. Using irregular catalysts normally
et al., 2017) and are widely used in chemical production. In most results in under-utilizing active constituents and high pressure drop.
cases, alcohol is used as the solvent in hydrogenation reaction to Thus, commercial catalysts are commonly utilized in various phys-
improve conversion and selectivity (Table 2). Some new reaction ical forms such as pellets, granules and extrudates. Cao et al. (2016)
solvents are employed for process intensification in hydrogenation established correlations of shape-dependent structural and chemi-
reaction. For instance, Bai et al. (2019) developed a solvent mixture cal factors of catalyst with catalytic activity and selectivity.
Quintana-Solo rzano et al. (2018) refitted previous pressure drop
consisting of trimethylbenzene and water-insoluble organic het-
erocyclic bisamide for enhancing hydrogenation efficiency of 2- correlations (Harrison et al., 2013) to better describe hydrodynamics
alkylanthraquinone. Application of organic solvents significantly of reactors packed with different particles configurations. Particle-
increases cost and shows adverse effect on human health and resolved CFD simulations (Karthik and Buwa, 2020), linking
environment. In recent years, innovative solvent systems have been particle-shape effects to reactor performance, have become a special
developed for higher reaction productivity and lower environ- design method for developing optimal catalyst shapes and been
mental impact, mainly including supercritical fluids (SCFs) and validated against experimental results or correlations concerning
ionic liquids (ILs). pressure drop and bed voidage (Wehinger et al., 2017). Most vali-
SCF, as a “green” alternative to traditional organic solvents, has dation studies performed were conducted on simple particle shapes,
become more and more impactive in heterogeneous catalytic hy- including spheres, Raschig rings and cylinders. Jurtz et al. (2020)
drogenation reaction because of its high density, high diffusivity simulated hydrodynamics in the packed-bed filled with different
and low kinematic viscosity (Seki et al., 2008). Also, SCF shows complex catalyst shapes by applying particle-resolved CFD and
precise control of reaction environment and regulates the selec- validated against experimental results. The reduction of catalyst size
tivity (Gadge and Bhanage, 2016). Among all SCFs, supercritical leads to the increase in effective contact area, which improves
carbon dioxide has received widespread attention because of its catalyst activity. Nano-sized catalyst particles exhibit relatively
low cost, non-toxicity, non-flammability, green, easy disposing and higher catalytic activity compared to micron-size or milli-size par-
recycling. Catalytic hydrogenation reaction, which is diffusion- ticles for the same mass catalyst (Intanin et al., 2020) because of
limited in traditional organic solvents, can be carried out in su- increased specific surface area. For example, hybrid nanoparticles
percritical CO2. More and Yadav (2018) proved that application of (Awad et al., 2020), combining inorganic and organic components
SCF significantly increases the hydrogen concentration on catalyst on the molecular scale, provide a new idea for obtaining catalysts
surface, leading to a higher reaction rate. with excellent performance in catalytic hydrogenation; magnetic
ILs, composed of organic cations and organic or inorganic an- recyclable nanocatalysts (Jiang et al., 2017) show excellent catalytic
ions, are gradually replacing traditional organic solvents in catal- activity and reusability in catalytic hydrogenation of styrene and 4-
ysis, petrochemical industry and other chemical engineering nitrophenol. Low mechanical strength in TBRs causes large pressure
industries. ILs have received widespread attention because of their drop and uneven gas/liquid distribution, leading to low catalytic
low-cost, non-toxicity, negligible vapor pressure, high thermal efficiency or even plant shutdown, and, thus, improving mechanical
stability, high solubilizing ability for organjc and inorganic com- strength is important. Powder processing parameters (Zhao et al.,
pounds and excellent designability according to needs (Garg et al., 2019), mainly including binder and water amount as well as pH of
2020). solvent, are frequently optimized for improving mechanical
Table 2
Literature summary on solvent effect in hydrogenation reactions.
Reaction system Effect of solvent on reaction rate Effect of solvent on selectivity Catalyst Reference
Hydrogenation of Reaction rate fMolar fraction of room SelectivityfMolar fraction of room temperature ionic liquid Pt/ Khodadadi-
cyclohexene temperature ionic liquid Al2O3 Moghaddam et al.
(2009)
Hydrogenation of 2- i-PrOH > EtOH > H2O þ EtOH Toluene > hexane > heptane > octane > cyclohexane Pd/ Nikoshvili et al.
methyl-3-butyn-2- MN270 (2015)
ol
Hydrogenation of Methanol > benzene > toluene > cyclohexane Methanol > benzene > toluene > cyclohexane Co/SiO2 Segobia et al. (2015)
butyronitrile
Hydrogenation of 4- Alkanes, secondary alcohols > primary Cyclohydrogenation: alkanes; Pt/TiO2 Mcmanus et al.
phenyl-2-butanone alcohols Carbonylhydrogenation: aromatics and alcohols (2015)
Hydrogenation of Aprotic > Protic [ Apolar solvents Aprotic polar solvents (excluded tetrahydrofuran): COL (60%); Pd/C Li et al. (2018c)
cinnamaldehyde Aprotic apolar (excluded benzene), protic: HCAL (80% or more)
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stability. 3D printing, fabricating the designed product by obtaining 2017), knitted wire packing (Wen et al., 2020), corrugated sheet
a virtual design from computer-aided design (CAD) software and packings (Singh et al., 2017) and winpak (Qi et al., 2017). These new
printing layer by layer, provides a novel technique to maximize the structured packings have been proved to be feasible on the laboratory
catalytic surface and adjust manufacturing parameters for obtaining scale because of high porosity, high geometric surface area, low
excellent mechanical properties. pressure drop and better heat transfer characteristics. However,
Precious metals, such as palladium, platinum and rhodium are structured packings are still not yet commercially available because of
frequently applied as catalyst in heterogeneous catalytic reaction in the low catalyst loading and high cost.
TBRs to achieve higher conversion under mild operating conditions. The full utilization of catalyst, especially in the trickle flow
Large-scale consumption of precious metals may raise concerns regime, relies on well-dispersed liquid feed on catalyst bed, which
about sustainability of economic and environmental, and, thus, means both desired bed loading and effective liquid inlet distrib-
development of low-cost catalysts is important. Sponge metals, utors are necessary. In downflow operation mode of packed beds,
such as Raney Co (RaeCo) and Raney Ni (RaeNi), have been re- both gas and liquid enter reactor from the top through a mixer, then
ported as potential catalysts (Loos et al., 2016) for continuous cat- pass through pre-distributor and redistribute through the second
alytic reaction because of their high porosity and mechanical or principal distributor tray. Mixed liquid and gas phases are evenly
properties, low cost and pressure drop (Islam et al., 2019). Said et al. sprayed onto the catalyst bed by distributors. Distribution effect of
(2017) demonstrated high selectivity of RaeCo catalyst in catalytic distributors directly affects apparent reaction rate, product yield
hydrogenation of iodo-nitroaromatic refametinib active in- and catalyst deactivation rate in reaction process. Especially, when
termediates in TBRs. Carangio et al. (2020) demonstrated high most highly exothermic processes are carried out in TBRs, inho-
conversion of RaeNi in the reduction of aliphatic nitro and without mogeneous distribution of gas and liquid phases could be amplified
any obvious deactivation during continued operation. However, because of fast drying of catalyst. At present, there are many types
there is still safety issues need to be solved in the operation of of distributors applied in industrial TBRs, mainly including bubble
sponge metal (Jindal and Buwa, 2017). In addition, combining a cap trays, jet distributors, perforated plate or sieve trays, chimney
small amount of precious metals and relatively inexpensive com- trays and gas assisted lift tube trays. Distributor performance could
ponents is promising for reducing costs and improving catalytic be measured by its liquid discharge pattern, liquid distribution,
efficiency. In general, compared to monometallic metal nano- pressure drop, coverage span, fouling surfaces and sensitivity to
particle catalysts, bimetallic metal nanoparticles show higher cat- tray levelness (Jain et al., 2020). Bazer-Bachi et al. (2013) gave some
alytic activity (Fulajta rova et al., 2015). Jiang and Xu (2011) guidelines for choosing distributors by comparing intrinsic per-
reviewed the latest developments in multimetallic nanoparticles formance of distribution and resistance to tray unlevelness in
for improving catalytic performance. Shesterkina et al. (2016) re- different distributors. Jain et al. (2020) developed a Eulerian two-
ported the increase in catalytic activity and selectivity in hydro- fluid model to simulate gas-liquid flow in distributors and vali-
genation of phenylacetylene to styrene by applying PdeFe/SiO2 dated it by applying high speed imagine, voidage probes and
bimetallic catalyst compared with Pd/SiO2 catalyst. pressure drop measurements. Lopes et al. (2018) developed three
Carbon, g-aluminum oxide, silica, zeolite, polymer, gel and glass novel flow distributors, evaluated their performance by varying the
fiber are frequently applied as support in heterogeneous catalytic distributor height as well as the presence or absence of internal
reaction in TBRs. For Preventing the aggregation of nanoparticles, obstacle and analyzed the phase distribution uniformity.
ligands (Moghaddam et al., 2018), ILs (Salminen et al., 2014), sur-
factants (Harraz et al., 2012), dendrimers (Bingwa and Meijboom, 2.4. Novel reactor structure design
2015), polymer (Comandella et al., 2017), periodic open cellular
structure (POCS) (La €mmermann et al., 2018), metal-organic Most heterogeneous reaction in TBRs is limited by external mass
frameworks (MOFs) (Isaeva et al., 2011) and microgel (Tan et al., transfer and heat transfer. In addition, difficulties with heat dissi-
2016) have been developed to stabilize nanoparticles and pation may lead to hot spots resulting in catalyst deactivation.
improve catalyst stability. For example, Harraz et al. (2012) re- Therefore, some new reactor structure has been proposed to
ported Pd/PEG catalyst, which exhibits excellent stability, catalytic improve the contact between phases and increase mass and heat
activity and selectivity for hydrogenation of styrene under mild transfer rate.
operating conditions in an environmentally friendly solvent sys-
tem. Zhang et al. (2014) and Li et al. (2016) reported novel MOFs 2.4.1. Microreactors
catalyst, encapsulated with precious metal nanoparticle, can Application of micro-structured devices intensifies mass and
significantly improve the stability and selectivity of the product. heat transfer of gas/liquid/solid catalytic reaction by reducing
Comandella et al. (2017) reviewed various methods for embedding diffusion time and increasing mass transfer area. They have become
palladium catalysts through polymer films to avoid catalyst deac- one of the significant methods of chemical process intensification
tivation. Yousaf et al. (2017) developed a unique structure by because of their high specific surface area, safety, waste minimi-
loading palladium nanoparticles on MnOx-CeO2 mixed oxides for zation and precise control of reaction temperature. As shown in
catalytic hydrogenation. In addition, many new carbon materials Fig. 6, microreactors mainly include micro-packed bed reactors,
are also applied as catalyst supports, including fullerene (Qu and chip-based microreactors, catalytic membrane reactors, monolithic
Chen, 2020), graphene (Wei et al., 2016) and mesoporous carbon microreactors, polytetrafluoroethylene capillary microreactors,
(Feitosa et al., 2019). In many cases, “bifunctional catalysts” (Jin falling film microreactors and so on.
et al., 2016) are applied to increase product selectivity. Micro-packed bed reactors (MPBRs) show increased product
Industrial TBRs are packed by the sock packing method, in which selectivity (Zhang et al., 2017) and faster reaction rate, and varies
particles are randomly introduced inside the packed bed, or the dense mass transfer coefficient within 2 magnitudes (Sang et al., 2020),
packing method. In the latter one the number of contact points and achieving continuous flow under fast dynamic control (Yang et al.,
pressure drop significantly increase. Many new catalyst filling 2018). Most well-known processes in chemical industry, such as
methods and packings have been proposed to improve fluid distri- hydrogenation, HDS and Fischer-Tropsch synthesis, are carried out
bution of the gas-liquid mixture on catalyst surface and increase gas- in MPBRs. There are some shortcomings in MPBRs, mainly include
liquid contact efficiency as well as mass transfer rate. For example, poor reproducibility caused by inherent randomness of catalyst
monolithic catalysts (Tsai and Ma, 2018), open-celled foams (Nie et al., distribution (Navarro-Brull and Go mez, 2018) and high pressure
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sito et al. (2019), Li et al. (2018a, b), Liu et al. (2018, 2020), Rehm et al. (2016), Sun et al. (2018), Tan et al.
Fig. 6. A variety of microreactors. Reprint permission obtained from Expo
(2019), Truter et al. (2016).
drop caused by small catalyst particles. Different designs and con- sites (Xu et al., 2013).
figurations (Faridkhou et al., 2016) are designed for reducing Catalytic membrane reactors (CMRs), combining membrane
pressure drop, such as a radial design and a cross-flow design. In separation and catalytic reaction, have become an effective way to
addition, expanding the scale of microreactor to millimeter reactor improve fluid distribution, mass and heat transfer (Table 3). In
(Piskun et al., 2016) has also been proposed to reduce pressure CMRs, membrane could be used either as a catalytic active material,
drop. Catalytic wall reactors (Moreno-Marrodan et al., 2018), with a such as palladium membranes or as a catalyst support, such as
thin layer of catalyst coated on the inner wall, have also been palladium nanoparticle-loaded microporous ceramic. The transfer
developed to reduce random distribution of catalysts. of reactant components to reaction zone can be controlled by
Chip-based microreactors (Expo sito et al., 2019), with unique membrane to strengthen gas-liquid mass transfer (Aran, 2011),
advantages of low reactant consumption, high sensitivity, high improve product selectivity (Escola stico et al., 2016) and improve
mass transfer rate and environmental friendliness, have received system security of premixed explosion systems. CMRs show good
widespread attention. For instance, Truter et al. (2016) demon- application prospects because of the numerous advantages over
strated improved residence time control and increased yields ob- conventional catalytic and separation process. There are also some
tained in microchannel reactor. Being able to combine with shortcomings still need further studied, mainly including the
microscopic visualization is another significant advantage of chip- adsorption and diffusion of reactants, solvent and product on the
based microreactors, which makes reaction and mass transfer membrane, lack of appropriate modification methods to obtain the
phenomena more understandable. Micro-structured devices also required distribution of active catalyst components, deactivation of
help enhance chaotic convection (Martínez et al., 2017), among catalyst and blockage of membrane pores.
which embedding obstacles (Pordanjani et al., 2018) in the chip- Novel reactor structures, coupling gas-liquid microdispersion
based microreactors is simple and most widely studied methods. technique (Ji et al., 2020) (Fig. 7) with TBR, were developed to in-
However, application of the microchannel reactors is still limited in crease processing capacity and address difficulty in processing of
heterogeneous catalysis because of the lack of suitable methods for microreactors, expanding their application in industrial processes
loading various catalysts in microfluidic devices, controllability of with high throughput. Tan et al. (2012) proved that the mass
catalyst position and homogeneous distribution of catalyst active transfer coefficient in this novel reactor structure is two orders of
Table 3
Some examples of CMRs applied in catalytic reactions.
Membrane Method Activity testing Reference
Porous expanded polytetrafluoroethylene Deposited Ru catalyst particles Aqueous phase hydrogenation of levulinic Stanford et al.
(ePTFE) membrane acid (2016)
Porous ceramic alumina (a-Al2O3) hollow fiber Nickel deposition-precipitation Hydrogenation of nitrite Espinosa et al.
(2018)
Hollow fiber membrane made of corundum (a- Sputtering, microemulsion, impregnation, Situ epoxidation of trans-chalcone and phenol Pinos-Ve lez et al.
Al2O3) precipitation of Fe complex peroxidation (2019)
Commercial microfiltration ceramic membrane Impregnation Hydrogenation of 1-butyne Colli et al. (2019)
Perovskite hollow fiber membrane Conventional solid-state reaction Partial oxidation of methane Jiang et al. (2020)
1210
Fig. 7. A variety of micro-dispersion system. Reprint permission obtained from Tan et al. (2012), Tan et al. (2019), Ji et al. (2020).
magnitude higher than that of traditional TBRs by applying stain- (Table 4). It can be removed and easily replaced if needed. Advances
less steel microfiltration membrane as the dispersion medium. Our in 3D printing have allowed for flexible production of parts with
previous studies (Tan et al., 2019) have shown that disappearance specific design requirements for matching fluid properties and flow
rate of phenol in catalytic wet oxidation of phenol increased by 70% conditions as well as reduced cost by 10-to-100-fold compared to
by applying micro-dispersion device. commercial metal static mixers of similar dimensions (Avril et al.,
Monolithic microreactors (Maresz et al., 2020), integrating the 2017). Electrodeposition (EP) and cold spray (CS) have also been
active phase into a straight channel or a macroporous monolithic applied in preparation of catalyst-coated static mixers. In addition,
structure, were developed to eliminate hot spots and stagnation some novel techniques such as electron beam additive
areas. Studies (Song et al., 2016; Chen et al., 2018) demonstrated the manufacturing (EBAM) (Wanjara et al., 2019), wire arc additive
increased controllability of operating conditions, conversion and manufacturing (WAAM) (Derekar, 2018) and laser metal deposition
selectivity in above novel microreactor. (LMD) (Donadello et al., 2019) have been developed, which are
excepted to be applied to this field. Despite their improved heat and
mass transfer and reduced pressure drop, there are several chal-
2.4.2. Catalytic static mixers (CSMs)
lenges facing commercially viable conformation of CSMs, such as
CSMs (Hornung et al., 2017), constructed by retrofitting the
deposition quality and repeatability.
tubular reactor with specially designed catalytic insert, were
developed to achieve effective mixing of reactants, heat transfer
and catalytic reaction in a continuous flow chemical reactor
Table 4
Some examples of CSMs intensified hydrogenation reactions.
Reaction system Catalyst Deposition methods Reference
Hydrogenation of oleic acid, vinyl acetate, and cinnamaldehyde Ni, Pt EP and CS Avril et al. (2017)
Hydrogenation of vinyl acetate Ni, Pd EP and CS Nguyen et al. (2017)
Reductive amination of aldehydes and ketones-two-step Ni, Pd EP and CS Genet et al. (2018)
Hydrogenation of substituted nitrobenzene Pd EP Gardiner et al. (2018)
Semi-hydrogenation of alkynes Ni, Pd CS Kundraa et al. (2020)
1211
3. Alternative energy sources 3.1.3. Magnetic control

External magnetic field is also considered as a potential method
3.1. Centrifugal control for process intensification and sustainable innovation concepts. Li
et al. (2015) demonstrated enhanced catalytic activity when the
It is one of the effective methods for process intensification by surface spin configuration of Pd nanoparticles changes from
applying a controllable external field. In most cases, increasing gas- paramagnetic-like to ferromagnetic-like configuration. Magnetic
liquid mass transfer rates can significantly improve reaction per- field has also been applied to the fluidized beds. With the devel-
formance of the reaction process limited by external mass transfer. opment of microfluidics (Yang et al., 2016), controlling the fluid in
The high gravity technology (Grob et al., 2019), realized via microfluidic channels by magnetic force has attracted lots of
generating centrifugal force at high-speed rotation, can signifi- attention because of its enhanced mixing (Boroun and Larachi,
cantly increase the gas-liquid contact area and gas-liquid mass 2020a, b) and improved mass transfer (Kumar et al., 2019). How-
transfer rate because liquid, within this process, is sheared into tiny ever, there are few reports on the enhancement of TBRs by applying
droplets, liquid film or ligaments (Yang et al., 2016). Based on this a controllable magnetic field.
concept, reactors were developed, including rotating packed beds
(RPBs) (Hacking et al., 2020), high-shear reactors (Feng et al., 2019) 3.1.4. Ultrasound
and spinning disc reactors (Martínez et al., 2017), among which Ultrasound, with high frequency and strong penetrating force,
RPBs are the most widely studied and applied reactors. could improve the reaction performance of heterogeneous catalytic
Compared with traditional TBRs, the most significant advan- reaction via created cavitation (Floris et al., 2013) and chemical
tages of RPBs are decrease in time for achieving steady-state effects (Maghami et al., 2015). Disselkamp et al. (2005) proved that
operation and feasibility for high viscosity fluids (Neumann et al., catalytic activity increased 9 times by applying ultrasound in hy-
2018). Mixing and mass transfer rates are 1e3 orders of magni- drogenation of cinnamaldehyde. In microreactors, ultrasound could
tudes higher than those in traditional reactors (Wang et al., 2019). also enhance the generalizability via enhancing mixing (Wang
However, because of multi-scale geometric characteristics of RPBs, et al., 2013), improving mass transfer (Hübner et al., 2012) and
structural characteristics of packings and flow properties of fluids, preventing blocking in the microreactor (Hartman et al., 2010).
it is difficult to obtain the flow phenomenon in reactors and Thus, it is suggested as a promising method for improving gas-
traditional packed bed models are also not suitable for RPBs. liquid mass transfer (Yang et al., 2020), with which the total mass
Therefore, more and more studies are focus on RPBs via CFD transfer coefficient increases by 3e20 times (Dong et al., 2015).
(Ouyang et al., 2019), which makes gas-liquid interaction more However, relatively high energy loss and increased temperature
understandable and lays the foundation for transitions the tech- caused by heat dissipation still need to be further addressed.
nology from lab-scale to industrial scale.
4. Application of intensified TBRs in petroleum industry
3.1.1. Microwave (MW) 4.1. Petroleum refining

Compared with external heating mode, MW radiation generates
effective internal heating by directly coupling MW energy with With continuous global oil exploitation, amount of light oils is
solvents, reagents or catalysts in reaction, especially when applying constantly decreasing and crude oil has gradually developed to-
MW absorbing materials or receptors, such as silicon carbide (Sun wards high metals content, high sulfur content and heavy quality.
et al., 2019). MW heating has already been applied widely in het- The techniques for upgrading petroleum fractions are one of the
erogeneous catalytic reaction (Li et al., 2020) because of increased most important processes in the refining industry to fulfill re-
reaction rates and selectivity, energy saving, improved process quirements of energy saving and environmental protection, as well
control, as well as reduced heat transfer limitations and reduced as to improve use performance of oil. Among the above techniques,
undesired side reaction (Sturm et al., 2014). Romano et al. (2016) hydrotreatment (HDT) shows ability in removing sulfur, metals,
demonstrated high conversion and selectivity by applying a pres- nitrogen, asphaltenes and increasing quality and quantity of refined
surized MW reactor in catalytic hydrogenation of biomass-derived petroleum products (Balasubramanian and Pushpavanam, 2008).
compounds. The combination of MW and microstructure device is HDT is usually carried out in TBRs, in which HDS, HDN, HDM,
promising for process intensification (Yesiloz et al., 2017), although HAD, and HDC are often implemented simultaneously. Therefore,
it is still yet limited inconclusive parameters caused by non- development of a detailed, easy-to-operate and highly efficient TBR
uniform thermal distribution (Durka et al., 2010) as well as scale- process model which can be used for design and optimization of
up issues such as limited penetration depth (Benaskar et al., 2011). the HDT process is practically important for improving fuel quality.
Sadighi (2016) demonstrated a two-dimensional (2D) CFD model
by using discrete lumping approach to evaluate the yield of a pilot
3.1.2. Radio frequency (RF) energy scale vacuum gas oil HDC reactor and validated it by using the re-
Compared to conventional heating method, RF heating could ported experimental data in the literature. Novaes et al. (2017)
improve heat transfer, minimize energy loss, realize a better control developed a phenomenological model to estimate the kinetic pa-
in reaction temperature and avoid hot spots caused by directly rameters of diesel HDT process, by taking axial dispersion and
transferring energy to magnetic catalyst surface (magnetic nano- effectiveness factors for both HDS and HDN reaction into account.
particles) (Houlding and Rebrov, 2012). RF heating at intermediate Dasgupta and Atta (2020) enhanced HDN process by applying pe-
frequencies is promising in some systems because of its greater riodic flow modulation in TBRs and developed an isothermal 2D
penetration in comparison to MW heating (Ye et al., 2020). axisymmtric Eulerian model to simulate the intensified HDN pro-
Chatterjee et al. (2015) developed a radio-frequency heating micro- cess. Gheni et al. (2020) developed a novel dynamics model for
trickle bed reactor for catalytic hydrogenation reaction, with which evaluating nan-catalyzed HDS process in TBRs and scaled up to a
increased total product yield is achieved. For further application of commercial scale.
TBR coupled with RF heating, issues including lack of understand- Nadeina et al. (2017) developed a novel CoMo catalyst for se-
ing on RF heating, available controllable magnetic nanoparticles lective hydrotreating of FCC gasoline, which makes it possible to
and understanding of magnetic actuation still need improved. produce a hydrotreated gasoline with sulfur content of less than
1212
10 ppm. Tian et al. (2018) studied the effect of catalyst activity on among which oxidative desulfurization (ODS) is one of the most
the energy consumption on a 900000 ton y1 gasoline-diesel HDT promising desulfurization methods.
unit by applying the integration of HDT reactor and heat exchanger ODS has received a good deal of attention in the recent years
network and identified optimal matching scheme in terms of both because of its advantages, mainly including mild reaction condi-
operating cost and capital cost. Saha et al. (2019) developed tions, absence of hydrogen and the ability of removing organosulfur
NieMo/Al2O3 and CoeMo/Al2O3 catalysts by cryochemical copre- compounds not destroyed in HDS. Nawaf et al. (2015b) developed
cipitation methods, studied their performance for HDS of diben- catalysts of Co3O4/g-Al2O3 and MnO2/g-Al2O3 for ODS of light gas
zothiophene and obtained a better performance in terms of oil containing DBT with air as oxidant, achieved complete oxidation
reaction conversion as well as regeneration. Safari and Vesali- of DBT and obtained high quality fuel for light gas oil. Zhao et al.
Naseh (2019) designed and optimized HDS of liquefied petroleum (2015) developed phthalocyanine molecular sieve catalysts,
gas (LPG) by Aspen Plus software and obtained a cleaner LPG for including Cu2(PcAN)2-W-HZSM-5 and Cu2(PcTN)2/W-HZSM-5, for
sulfur reduction to 10 ppm and eliminated all the drawbacks with ODS of fuel oil and obtained removal efficiencies for DBT of up to
current HDS of LPG in South Pars Gas Complex. 87.32%. The ultrasound-assisted oxidative desulfurization method
The average sulfur content ranges from 0.03 wt% to 7.89 wt% in has been introduced in the desulfurization process, which obtained
crude oil (Soleimani et al., 2007), whose classification is shown in higher desulfurization efficiency within a shorter reaction time
Fig. 8. Although HDS is the most common sulfur removing method, compared with conventional mixing ODS process (Jalali and Sobati,
it is difficult to remove benzothiophene (BT) and dibenzothiophene 2017).
(DBT) because of high resistance of BT and DBT in hydrogenation
process (Nawaf et al., 2015a) and required extreme operating 4.2. Petrochemical
conditions such as high pressures, high temperatures, high volume
of hydrogen and more active catalysts. Therefore, alternative deep TBRs have been extensively utilized in oxidation, hydrogenation
desulfurization processes have been developed, mainly including and hydration in petrochemical, including hydrogenation of al-
adsorption (Blanco-Brieva et al., 2010), extraction (Seeberger and kenes and alkynes, hydrogenation to alcohols, oxidation of ethanol,
Jess, 2010), oxidation (Jiang et al., 2011) and biodesulfurization, formic acid and acetic acid and organic pollutants in wastewater.
Fig. 8. Important classification of sulfur-containing compounds in crude oil.
1213
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Acknowledgements denitrogenation in a trickle bed reactor using periodic flow modulation. Chem.
Eng. Process 157, 108135. https://doi.org/10.1016/j.cep.2020.108135.
The authors gratefully acknowledge the support of National Dashliborun, A.M., Larachi, F., Hamidipour, M., 2016. Cyclic operation strategies in
inclined and moving packed beds-potential marine applications for floating
Natural Science Foundation of China (21878019) and Beijing Nat- systems. AIChE J. 62 (11), 4157e4172. https://doi.org/10.1002/aic.15327.
ural Science Foundation (2182063). Dashliborun, A.M., Hamidipour, M., Larachi, F., 2017. Hydrodynamics of inclined
packed beds under flow modulation - CFD simulation and experimental vali-
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Contents lists available at ScienceDirect

Process intensiﬁcation in gas/liquid/solid reaction in trickle bed

Fig. 1. Application examples of TBR.

Fig. 4. Determination of reaction control steps.

Fig. 5. Numerical simulation of TBRs in literature.

System Correlations Conditions Reference

T, K P, uG/Qm,G /SV uL/Qm,L Catalyst

Membrane Method Activity testing Reference

Reaction system Catalyst Deposition methods Reference

3. Alternative energy sources 3.1.3. Magnetic control

3.1.1. Microwave (MW) 4.1. Petroleum reﬁning

Fig. 8. Important classiﬁcation of sulfur-containing compounds in crude oil.

Gorshkova et al. (2012) simulated the hydrogenation process of 10.1021/acs.iecr.9b01130.

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