J. Inst. Eng. India Ser.
E
https://doi.org/10.1007/s40034-019-00143-3
ORIGINAL CONTRIBUTION
Hydrodynamic, Mass Transfer and RTD Studies of Fluid Flow
in a Spiral Microreactor
Urvashi Bhivgade1 • Yadagiri Maralla1 • Bharat A. Bhanvase2 • Shirish Sonawane1
Received: 2 March 2017 / Accepted: 4 June 2019
Ó The Institution of Engineers (India) 2019
Abstract In this article, the spiral microreactor made of
copper tube with U-junction, mixing region, was used to
study the reactor performance on sodium hydroxide-n-
butyl acetate system. The internal diameter of microreactor
is 1.5 mm and length is 2 m. The performance of spiral
microreactor was studied considering hydrodynamic flow,
mass transfer characteristics, RTD and computational
analysis of fluid flow using n-butyl acetate and sodium
hydroxide system. Pressure drop was estimated in spiral
geometry using dean number and compared with simula-
tion results for laminar flow. The volumetric mass transfer
coefficient obtained was in the range of 0.02–0.37 s-1. The
dispersion number calculated from the RTD study was
equal to 0.0526 indicating the plug flow conditions.
Keywords Spiral microreactor  U-junction 
Hydrodynamics  Mass transfer characteristics  RTD
Introduction
Microreactor is one of the efficient tools for optimizing
reactor design for continuous flow synthesis of chemicals,
nanoparticles, organic compounds and industrial pharma-
ceutical products. The characteristic microscale leads to
higher volume-to-surface ratio, higher overall heat transfer
& Shirish Sonawane
shirish@nitw.ac.in
1 silicon. The copper tubes are available at low cost, and
Department of Chemical Engineering, National Institute of
Technology, Warangal, Telangana State 506004, India
2 stainless steel tubes and other materials. So, an attempt was
Department of Chemical Engineering, Laxminarayan
Institute of Technology, Rashtrasant Tukadoji Maharaj
Nagpur University, Nagpur, MS 440033, India
coefficients and the minimum mass transfer pathway [1, 2].
It is essential to develop novel microreactors with con-
trolled characteristics to get new reaction pathways in
continuous flow chemical manufacturing [3]. In order to
scale up of continuous flow microreactor, it is very much
essential to first understand the factors that are associated
with it, such as effect on mass transfer rate by changing in
configuration, hydrodynamics of flow, residence time dis-
tribution and flow regimes, which depends on geometry
and mixing pattern of a microreactor. Burns and Ramshaw
[4] have obtained mass transfer performance data for acetic
acid extraction from kerosene that was performed by using
chip-based design of glass microreactor of width 380 lm
per channel. The obtained data were compared with other
inter-phase contacting techniques. Further, Burns and
Ramshaw [4] have concluded that for 15% acetic acid
extraction, the value of Fo (Fourier number) obtained is
0.02 and for 62% extraction, Fo obtained is 0.30 [4]. Yue
et al. [5] have also explored hydrodynamics and mass
transfer characteristics experimentally for a rectangular
microchannel oriented horizontally having a hydraulic
diameter of 667 lm. The reported volumetric mass transfer
coefficient was 21 s-1, and interfacial area was 9000 m2/
m3 [5]. To obtain volumetric mass transfer coefficients, the
saponification method was successfully adopted by
researchers Ghaini et al. [6] and Plouffe et al. [7].
There are many reports on glass microreactor, stainless
steel and other materials. The reason to use copper material
in microreactor is because of ease of fabrication of
microreactor using copper materials rather than the steel or
making U-junction is also very easy as compared to
made to study the performance of copper microreactor for
the reaction. While the reaction was carried out at room
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 J. Inst. Eng. India Ser. E

temperature in the copper microreactor and it was con- Table 2 Physical properties of n-butyl acetate and NaOH at room
firmed that chemicals used in diluted solutions were not temperature
reacting with copper. In the present work, U-junction spiral NaOH Density Viscosity Interfacial tension
copper microreactor was designed and studied the hydro- concentration (kg/m3) (Pa s) 9 10-3 (mN/m)
dynamics, interfacial mass transfer performance and resi-
0.2 M NaOH 1007 1.05 –
dence time distribution for the system of n-butyl acetate
0.3 M NaOH 1012 1.13 –
and sodium hydroxide.
0.4 M NaOH 1016 1.22 –
n-Butyl acetate 882 0.70 25.3

Experimental Procedure
using syringe pumps through a U-junction mixing element.
The experiments were carried out using a U-junction An aqueous solution containing NaOH of known concen-
copper spiral microreactor as shown in Fig. 1, and speci- tration was prepared. The concentration of n-butyl acetate
fications are given in Table 1. A U-junction was attached to transferred into aqueous phase was measured using
a spiral coil (internal diameter = 1.5 mm and length = 2 saponification method. Concentration of NaOH was mea-
m) and employed as mixing region. Coils were made from sured by titrating with HCl by using phenolphthalein as an
initially straight tubes of copper and then bent into coil indicator. In each series of experiments, the flow rates were
considering the circularity. The n-butyl acetate and sodium varied to study the characteristics of microreactor. The
hydroxide were used for carrying out the experiments with ratio of aqueous to organic phase was maintained con-
AR grade of 98% purity. Deionized water was used for all stantly at 1:1 [8–11].
the experiments. The physical properties of chemicals, at For computational analysis of the three-dimensional U-
room temperature, used in the experiments are reported in junction helix–spiral microreactors, geometry was devel-
Table 2. oped in COMSOL v5.0b. The finalized geometry has 7
The aqueous phase carries sodium hydroxide, and domain, 39 boundaries, 67 edges and 36 vertices. For this
organic phase carries saturated n-butyl acetate. The fluid flow study, ‘laminar flow’ was selected under ‘single-
experimental procedure includes the aqueous phase and phase fluid flow’ of the model. The flow in the microreactor
organic phase introduced into the spiral microreactor by is laminar and given by the Navier–Stoke equations as
follows:
   2 
qðu  rÞu ¼ r  pI þ l ru þ ðruÞT  lðr  uÞI
3
þF
ð1Þ
and the continuity equations as follows:
r  ðquÞ ¼ 0 ð2Þ
where q is the density of the fluid (kg/m3), l is the viscosity
of the fluid (Ns/m2), u is the velocity vector (m/s), I denotes
Fig. 1 An U-junction copper spiral microreactor the identity matrix, F is the volume force vector (N/m3), T
is the absolute temperature (K) and p is the pressure (Pa).
Table 1 Specifications of spiral microreactor This equation is applicable for incompressible as well as
Specification Value compressible flows where the density varies. The boundary
conditions imposed on the momentum balance are no slip
ID 1.5 mm at the microreactor walls:
ID of U-junction 3 mm
u¼0 ð3Þ
U-junction length 25 mm
U-junction gap 60 mm The inlet boundary condition was
Length 2m u ¼  U0 n ð4Þ
Axial pitch 10 mm
Radius of curvature 30 mm The outlet boundary conditions describing the fluid flow
Number of turns for sweep 12 at an outlet at an atmospheric pressure and no viscous
stress

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J. Inst. Eng. India Ser. E

   2  0.0035
nT pI þ l ru þ ðruÞT  lðr  uÞI n ¼ ^
p0
3 ð5Þ 0.003

p^0  p0 ; 0.0025

0.002
The flow of fluids in the microreactor occurred as a

Ca
0.0015
result of pressure drop. The inlet pressure, p, is greater than 0.2 NaOH
outlet atmospheric pressure. The outlet has no viscous 0.001
0.3 NaOH
stress condition [12]. 0.0005 0.4 NaOH
Mesh was completed using a free triangular mesh on the
0
remaining domains with general dynamics, with 648,857 0 20 40 60 80 100 120 140
tetrahedral elements, 199,434 triangular elements and Re
24,904 edge elements. Here the system considered was
Fig. 2 Reynolds number (Re) versus capillary number (Ca)
sodium hydroxide-n-butyl acetate for equal flow rate. The
inlet velocity was varied from 0.0094 to 0.0754 m/s using
parametric sweep in time-dependent study. The mesh size Table 4 Comparison of Re, De and (D/RC)0.5
settings are given Table 3.
(D/RC)0.5 Re De De/Re = (D/RC)0.5

0.2236 15.2199 3.40318 0.2236

Results and Discussion 0.2236 30.6018 6.84256 0.2236
0.2236 45.8217 10.2457 0.2236
Flow Regimes Study Using Dimensionless Numbers 0.2236 61.0417 13.6489 0.2236
0.2236 76.4235 17.0883 0.2236
It has been reported that in the literature, if aqueous phase 0.2236 91.6435 20.4915 0.2236
has higher contact angle than organic phase, the slug flow 0.2236 106.863 23.8947 0.2236
formation took place instead of droplet flow in a microre- 0.2236 122.083 27.2978 0.2236
actor [13]. In the present work, the slug flow was formed in 0.2236 137.465 30.7372 0.2236
the copper spiral microreactor. To define the slug flow 0.2236 152.685 34.1404 0.2236
quantitatively, the capillary number (Ca = vl/c) and the
Reynolds number (Re = dvq/l) were determined. Due to
low flow rates and micro-size of the reactor, it was Reynolds number is linear that is De = Re (D/RC)0.5, as
obtained the low Reynolds numbers which indicates that flow rate increases the Reynolds number increases which
the viscous force is dominating over inertial force. The low leads to increase in the Dean number. Hence, the ratio of
value of capillary number and Reynolds number indicated the Dean number (De) to Reynolds number (Re) is always
that the flow inside the spiral microreactor was slug flow constant and is equal to (D/RC)0.5.
[14, 15]. Figure 2 shows the relationship between Re and In this case, (D/RC)0.5 = (1.5 mm/30 mm)0.5 = 0.2236.
Ca, and it is observed that the properties of both phase, Hence, De/Re = 0.2236, and it is constant for all the flow
velocity and the interfacial tension are influencing the flow rate, see the following Table 4.
patterns.
For the spiral/helical coiled microstructured capillary Estimation of Mass Transfer Coefficient
reactor, the relation between the Dean number and

Caq is the concentration of n-butyl acetate which is trans-
Table 3 Mesh size settings ferred from organic phase to aqueous phase. To study the
performance of the spiral microreactor, volumetric mass
Description Value
transfer coefficient was used which was derived from mass
Maximum element size 0.978 transfer rate relations as shown in Eq. (6)
Minimum element size 0.02
!

1 Caq  Caqi
Curvature factor 0.5 KL a ¼ ln  ð6Þ
s Caq  Caqo
Resolution of narrow regions 0.6
Maximum element growth rate 1.45 where Caqi and Caqo represent the amount of n-butyl acetate
Triangular elements 199,434 at the inlet and at the outlet, respectively, for aqueous
Tetrahedral elements 648,857 phase. The s is the residence time of the system in the
microreactor, which was obtained by dividing the reactor

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 J. Inst. Eng. India Ser. E

Table 5 Solubility of transfer component in aqueous phase [10] 0.40

System 
Caq (kmol/m )3
0.35 0.2 M NaOH
0.3M NaOH
0.2 M NaOHaq–n-butyl acetate 0.0403 0.30 0.4 M NaOH
0.3 M NaOHaq–n-butyl acetate 0.0377 0.25

kL a (s-1)
0.4 M NaOHaq–n-butyl acetate 0.0353
0.20

0.15

volume with volumetric flow rate [6, 15]. The solubility of
transfer component in aqueous phases is reported in
Table 5.
The volumetric mass transfer coefficient (kLa) obtained
using Eq. (6) varies in the range of 0.02–0.37 s-1. The
aqueous phase’s outlet concentration of n-butyl acetate was
measured and plotted against the volumetric flow rate as
shown in Fig. 3. It indicated that the outlet concentration of
n-butyl acetate was directly proportional to the flow rate.
From the Eq. (6), it was clear that the volumetric mass
transfer coefficient was inversely proportional to the resi-
dence time, therefore directly affected by the variation in
the volumetric flow rate as shown in Fig. 4. As the volu-
metric flow rate was increasing, the interfacial mass
transfer area also increases due to the presence of internal
circulations within slug. At low flow rate, the plot shows
the straight line, while with the increase in the flow rate,
there is deviation in the graph [16]. The volumetric mass
transfer coefficient was negligibly influenced by the NaOH
concentration in aqueous phase as we did not consider the
chemical reaction occur to evaluate the mass transfer
coefficients.
Correlation of Mass Transfer Data for Physical
Mass Transfer
There was no empirical model available to estimate the
volumetric mass transfer coefficient in spiral microreactor.
Here, it was assumed that the density and the viscosity of
the fluids used were constant throughout the microreactor.
0.043
0.2 M NaOH
0.042
0.3 M NaOH
0.041 0.4 M NaOH
0.040
Caqo (M)
0.10
0.05
0.00
0 2 4 6 8 10
Q (mL/min)
Fig. 4 Variation of kLa with volumetric flow rate (Q)
Reynolds numbers and capillary numbers were employed
to estimate the volumetric mass transfer coefficient in
spiral microreactor. It was considered that the following
variables were affecting the mass transfer coefficient in the
mass transfer extraction [14]
kL a ¼ f ðRe; Ca; d; LÞ
kL a ¼ aðRe; CaÞb ðd=LÞc :
Using a least square regression analysis of the
experimental data, the correlation was developed for
volumetric mass transfer coefficient in the spiral
microreactor. By evaluating the values of ‘a’, ‘b’ and ‘c’
in order to correlate Re, Ca, diameter and length of the
spiral microreactor, the following correlation was
developed
  0:1
d
kL a ¼ 0:4617ðRe; CaÞ0:657 : ð7Þ
L
RTD Study for Spiral Microreactor
Residence time distribution (RTD) study was carried out to
identify the flow behaviour in the spiral microreactor. A
pulse of NaOH (0.2 M) aqueous solution (tracer) was
introduced into microreactor previously filled with saturate
n-butyl acetate in water with the help of the syringe pump
at a flow rate of 4.8 mL/min. The concentration of NaOH
was measured at the outlet and inlet pulse of the experi-
ment to obtain the C-curve. Figure 5 shows the C-curve for

0.039

0.038 pulse tracer experiment. The residence time distribution

0.037 (RTD) of samples was evaluated to characterize the spiral
0.036 microreactor using age distribution EðtÞ of element which
0.035
had passed through the spiral microreactor.
0.034
The calculated mean residence time is given by
0 2 4 6 8 10
R1 Z 1
tEðtÞdt
Q (mL/min) t ¼ R01 ¼ tEðtÞdt ¼ 27:493s
0 E ðtÞdt 0
Fig. 3 Variation of Caqo with volumetric flow rate (Q)

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0.20 3.5

0.16 3

2.5
0.12
C (M)

σ2
0.08
1.5
0.04
1

0.00 0.5
0 20 40 60 80
t (s)
0
0.050 0 20 40 60 80
t (s)
0.040
Fig. 6 Variation of variance with residence time
0.030
E (t)

microreactor, Da is the diffusivity. The theoretical disper-

0.020 sion was 0.0285. The dispersion number was introduced to
indicate the flow deviation from ideal plug flow. The RTD
0.010
experiment explored that the flow in spiral microreactor
0.000
was laminar with radial molecular diffusion and closely
0 10 20 30 40 50 60 70 80 matching up to a plug flow.
t (s)

Fig. 5 C-curve and RTD curve for pulse tracer input at flow rate of Hydrodynamic of Fluid Flow Through Spiral
4.8 mL/min Microreactor

Space time (s), i.e. the volume of reactor to volumetric In this study, the pressure drop was obtained from exper-
flow rate (V/Q) is 27.5 s which was approximately equal to iments using computational analysis and compared it with
mean residence time. theoretical pressure drop. The theoretical pressure drop
The variance of the exit age distribution was estimated through a helix–spiral coil was evaluated using curve tube
and reported as shown in Fig. 6 which indicates the spread friction factor fc [20]. Further in this work, for the spiral
of element through the spiral microreactor [17] microreactor with finite pitch, the curve tube friction factor
Z 1 was calculated from the regression analysis done by
2
r ¼ ðt  sÞ2 EðtÞdt ¼ 79:536 s2 : Manlapaz and Churchill [21] for the fully developed lam-
0
D inar flow having Dean number ([Re(d/2R)0.5] C 1) was as
Dispersion number UL , from axial dispersion model, follows:
was used to characterize the spiral microreactor, where D is  
axial dispersion coefficient, L is length of the microreactor, fc ¼ fs 1 þ 0:033½log10 De4 ð10Þ
U is velocity and the relation between dispersion number,
Using the Eq. (10), the curve tube friction factor for the
mean residence time and variance is given as follows: [18]
  spiral microreactor was calculated using dean numbers and
r2 D straight tube friction factor values (fs = 16/Re). For the
¼2 : ð8Þ
t2 UL experiments carried out in this study, the dean number
obtained was in the range of 2.6–21.
Experimental dispersion number for closed system using
In order to validate results from numerical analysis, the
above equation was estimated, and the value was 0.0526
estimated results for 0.2 M NaOH had taken in Comsol
for spiral microreactor which indicates that the flow
Multiphysics model. The pressure drop and maximum
behaviour is laminar. For laminar flow in a tube having
velocities for different inlet velocities in the U-junction
Bodenstein number greater than 50, the theoretical
spiral microreactor from simulation are given in Table 6.
dispersion number was given by Levenspiel [19]
  The pressure drop contour during the fluid flow in the spiral
D Ud 2 microreactor at U = 0.0094 m/s is shown in Fig. 7.
¼ : ð9Þ
UL 192DA L The variation of the pressure drop in the spiral
microreactor was compared with theoretical results
where D is axial dispersion coefficient, L is length of the
obtained from correlation as shown in Fig. 8a. From
microreactor, U is velocity, d is inner diameter of the

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 J. Inst. Eng. India Ser. E

Table 6 Pressure drop and maximum velocities obtained from (A)

simulations 3000
P computational
U (m/s) DPComputational (Pa) Umax (m/s) 2500
P estimated
0.0094 205 0.053 2000

∆P (Pa)
0.0189 465.5 0.078
1500
0.0283 710 0.09
0.0377 963 0.11 1000
0.0472 1200 0.22
500
0.0566 1468 0.456
0.066 1740 0.75 0
0.0754 1995 0.98 0.00 0.02 0.04 0.06 0.08 0.10
U(m/s)
0.0849 2323 2.7 (B)
1.20
0.0943 2617 5.2
f computational
1.00

Friction factor
f estimated
Fig. 8a, it could be concluded that as the velocity increases, 0.80

the pressure drop increases along the length of the spiral 0.60
microreactor. Furthermore, from Fig. 8a, it could be
observed that the computational (simulated using CFD) 0.40
and the estimated pressure drop profiles were identical. The 0.20
friction factor as function of Reynolds number is given in
Fig. 8b. From computational data, friction factor for spiral 0.00
0 50 100 150 200
microreactor was correlated with Reynolds number and is
Re
given as follows:
Fig. 8 a pressure drop variation with velocity, b the friction factor
f ¼ 10:328Re0:9 ð11Þ
variation with Reynolds number (Re)
From Fig. 8b, it was observed that as the velocity
increases, the Reynolds number increases which resulted Computational Analysis for Laminar Flow
into decrease in friction factor. Moreover, from Fig. 8b, it
could be observed that the computational and theoretical Along with pressure drop, it was important to know about
graphs were identical. fluid flow inside the spiral microreactor, and therefore, the

Fig. 7 Pressure drop contour during the fluid flow in spiral microreactor at U = 0.0094 m/s

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J. Inst. Eng. India Ser. E
Fig. 9 a skewed profile of
velocity along the arc length,
b colour visualization of
velocity variation with the
radius of spiral microreactor
(colour figure online)
Fig. 10 Velocity profile inside the spiral microreactor
velocity streamlines for single phase were evaluated at
different inlet conditions. After the simulation, it was found
that flow was laminar through out the range of inlet
velocity, i.e. 0.0094–0.0943 m/s. Non-parabolic profile of
velocity inside the helix–spiral microreactor along arc
length in x direction was observed as shown in Figs. 9
and 10, for inlet velocity of 0.0943 m/s. It indicates that
the flow in x direction was having noncircular velocity
profile. In any helical/spiral microstructured capillary
reactor, the flow is laminar and the velocity profile is non-
parabolic. From Fig. 9, it could be noticed that when fluid
flows in the spiral microreactor, the velocity was minimum
at the wall and the maximum at the centre of the spiral
microreactor for laminar flow. As velocity was minimum at
wall, the particles spend more time than centre. So, the
velocity profile in spiral coiled capillary microreactor is
skewed mean velocity profile. Continuously developing
skewed mean velocity profile would lead to control local
back mixing and the extent of back mixing, so it would
thus strongly depend upon the total length of the spiral and
the spatial increase in RC [22–26].
Conclusion
The performance of the U-junction spiral microreactor was
studied using the n-butyl acetate-sodium hydroxide
(NaOH) system. The study of flow patterns using fluid
properties of immiscible liquids was done. Flow charac-
teristics were studied by determining the dimensionless
numbers of Reynolds number and capillary number in the
spiral microreactor. The Reynolds number varied in range
of 16.47–172 indicates the flow was laminar flow inside the
spiral microreactor. The capillary number was obtained in
the range of 0.00019–0.002, which shows that the slug
formation instead of droplet flow. The mass transfer per-
formance was studied using physical extraction of n-butyl
acetate in aqueous media. The volumetric mass transfer
123

coefficient for the experiment was obtained in the range of
0.02–0.37 s-1. The volumetric mass transfer coefficient
was varied with variation in flow rate and interfacial mass
transfer area. The empirical correlation was developed
from the obtained experimental data and the volumetric
mass transfer coefficient estimated which gave good vali-
dation with experimental data. The C-curve and the E-
curve were obtained for pulse tracer input. The mean res-
idence time determined for the spiral microreactor from
experimental data was 27.493 s, which was approximately
equal to space time of spiral microreactor (27.5 s). The
experimental dispersion number obtained was 0.0526, and
the theoretical dispersion number from dispersion model
was 0.0285. The hydrodynamics of flow was studied to
estimate pressure drop inside spiral microreactor. The
results shown that with the increase in inlet velocity, there
was a gradual increase in pressure drop. The computational
study confirms that the flow was laminar flow inside the
spiral microreactor with parabolic velocity profile. The
pressure drop, maximum velocity and friction factor were
calculated for various inflow velocities from simulation.
The results were validated with estimated theoretical
values.
From the experimental studies, we concluded that the U-
junction spiral microreactor was one of the prominent and
efficient tools for process intensification of chemical
reactions.
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