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Project Report
On
EXPERIMENTAL INVESTIGA
TIGATION OF LIQUID LIQUID FLOW IN MICROCH
CHANNELS
Guided by:
Submitted
itted by :
2011UCH1034
2011
(Assistant Professor)
Jitendra Singh
2011UCH158
2011
2011UCH1587
201
Amandeep Yadav
2011UCH1004
20
Submitted
In partial fulfilment
ent of the requirements of the degree of Bachelor
lor of
o
Technology
In
Chemical Engineering
Depart
partment of Chemical Engineering
Malaviyaa Na
National Institute of Technology, Jaipur
DEPARTMENT OF CHEMICAL
ENGINEERING
MALAVIYA NATIONAL INSTITUTE OF TECHNOLOGY
JAIPUR (302017) INDIA
CERTIFICATE
This is to certify that the project report entitled, EXPERIMENTAL
INVESTIGATION OF LIQUID LIQUID FLOW IN MICRO
CHANNELS has been completed and submitted by the VIII Semester
students Mukesh Kumar Yadav (2011uch1034), Jitendra
Singh(2011uch1583), Mahendar Kumar Meena(2011uch1587),
Amandeep Yadav(2011uch1004) under my guidance.
DECLARATION
We hereby declare that the work proposed in the B.Tech Project Report entitled
EXPERIMENTAL INVESTIGATION OF LIQUID LIQUID FLOW IN MICROCHANNELS in partial
fulfillment of the requirement for the award of the degree of B.Tech in Chemical Engineering
submitted to the Department of Chemical Engineering , MALAVIYA NATIONAL INSTITUTE OF
TECHNOLOGY, JAIPUR, is an authentic of my carried out from July 2014 to June 2015 under the
supervision and guidance of Dr. U. K. Arun Kumar, Assistant Professor, Department of Chemical
Engineering, MNIT, Jaipur. Information used from literature and other sources in the present
thesis has been duly acknowledged by giving references at the appropriate places.
The matter embedded in this thesis has not been submitted by
(Jitendra Singh)
(Amandeep Yadav)
Date:
The present work is an authentic carried out by these students refer my supervision. Try the
best of my knowledge, the matter embedded in this work has not been submitted in any other
University or Institute for the award of any Degree or Diploma.
ACKNOWLEDGEMENT
We wish to express our deep sense of gratitude to our guide Dr. U.K. Arun Kumar, Assistant
Professor,Chemical Engineering, Malaviya National Institute of Technology, Jaipur who inspired
us to undertake this challenging project.
We would also like to express sincere gratitude to Dr. Suja George, Head of the Department,
Chemical Engineering and Prof. I.K. Bhatt,Director, Malaviya National Institute of Technology,
Jaipur for all the facilities provided in the department.
Finally we would like to thank all those people who directly or indirectly were responsible for
making our project a successful endeavor.
Jitendra Singh
Amandeep Yadav
TABLE OF CONTENTS
Page no.
1. INTRODUCTION
1.1) Introduction
1.2) Conventional Contactors used for Liquid-Liquid extraction
1.3) Advantages of Micro Structured Reactors over conventional reactors
1.4) Application of Microfluidics
1.5) Governing Dimensionless Numbers in micro channel
1.6) Governing Equations in micro channel
1.7) Mechanism of Mass Transfer in Slug Flow
7
8
11
11
12
13
14
2.
LITERATURE REVIEW
15
3.
OBJECTIVE
19
4.
EXPERIMENTAL SECTION
20
5.
21
6.
CONCLUSION
24
6.
REFERENCES
25
ABSTRACT:
The hydrodynamics and the pressure drop of liquidliquid slug flow in round micro capillaries
are studied. Here the liquid liquid flow system is Toluene water. The slug lengths of the
alternating continuous and dispersed phases were measured as a function of the slug flow rate
(0.2 3ml/min.), the toluene to water flow ratio (0.1 3), and the micro capillary internal
diameter (0.5mm, 0.8mm, 1mm). We found the slug flow distribution is uniform throughout the
length of capillary.
Chapter 1
1.1 Introduction
Microfluidics is the field of science that deals with technology and systems that can be used for
the handling or processing of very small amount of fluids in the range of 10-9 to 10-18 liters. It is
an interdisciplinary field which include engineering, chemistry, physics, nanotechnology,
biochemistry and biotechnology. In microfluidics channels in the size range of ten to several
hundred micrometer size is used. It mainly exploits the miniaturized size of the channels. It has a
wide future applicability in the field of chemical and biotechnology to synthesize chemicals and
separation process. Microfluidics emerged in the beginning of 1980s principally with the
development of inkjet print heads. The principle of process intensification which aims to use
green technology such as small, compact, energy efficient processes has led to the interest in
micro-fluidics. In the recent years more interest in micro structured devices are shown which are
expected to replace the existing manufacturing and separation processing in chemical and
pharmaceutical industries (1).
Liquid-liquid extraction is a commonly used separation techniques used in refinery,
pharmaceutical and chemical industries. Separation by Extraction contains three important
stages. In the first stage two liquids which are partially or completely immiscible are mixed
together in which emulsion drops are formed. The second is settling stage in which the liquids
separate into two layers and form two clear layers. The final stage involves decanting of
individual layers, separation of solute from the solvent and solvent recycle (2).
Mixer-Settler
Centrifugal extractors
Columns
In a mixer-settler aqueous and organic liquids are made to contact with each other in a mixer
with agitation and it is allowed to settle in a settler with a shallow basin where liquids separate
into two different layers and are decanted separately. In a centrifugal extractor, the immiscible
liquids are mixed in an annular space between a stationary housing and a rotor. Centrifugal
forces are used for separation of the two immiscible liquids. Columns can be divided into two
categories- static columns and agitated columns. Packed column, sieve plate column and spray
column are the example for static columns, whereas rotating disk contactor, Karr column, Kuhni
column, Scheibel column and pulsed columns are example for agitated columns. The advantages
and disadvantages of conventional contactors are listed in Table 1. A common disadvantage of
these conventional equipment is non uniformity that occur due to the difficulties of the
fundamental hydrodynamics (3).
Advantages
Better contacting
Low maintenance
Simplicity
Disadvantages
Mixer Settler
Investment cost is high
Operation cost is high
Centrifugal Contactors
Liquids with low density difference can be Scaling up is difficult
used
Only small volume of solvent is required
Mechanical complexity
Rapid mixing can increase quality and Maintenance cost is high
product recovery
Advantages
Disadvantages
Static Columns
Easy operation
Lower cost
Contactor
Centrifugal extractors
850-2600
Impinging streams
280
175-250
Mixer Settler
150-250
35-1500
9
0.5-190
0.2-20
Figure 1.. B
Benchmarking of micro-structured reactors
A (m2/m3)
kLa (s
( -1)
Agitated Contactor
32-311
(48-83)
3)10-3
80-450
(3.4-5)
5) 10-3
Contactor
Intalo
talox
10
RTL extractor
(Grasser raining bucket)
Air operated two impinging jets
reactors
Two impinging jets reactor
90-140
(0.6-1.3) 10-3
350-900
0.075
1000-3400
0.28
Extraction
Chemical Reactions
Polymerase Chain
Nano particle crystallization
Protein folding
Bio-process optimization
Cell analysis
Drug screening
Clinical diagnostics
11
Capillary Number=
=
Weber Number=
Equation of continuity:
+ . (
)=0
(1)
Equation of motion:
(
+ . (
) = -" + . [ $( +
&
)] + ' + (
(2)
+ .,
=0
(3)
With
=
$=
Where, , , V, p and F denote the mixture density, the mixture viscosity, the mixture velocity
field, the pressure and the source term that represents the surface tension force, respectively.
12
For Micro Structured Reactors two immiscible phases are required. The two phases can be either
Liquid-Liquid or Gas-Liquid. As the feed are in the immiscible form, the product formed will
also be in an immiscible form making separation easy. Water and kerosene are examples for
inorganic and organic phases. The parameters that define the hydrodynamics of two phase flow
are
Viscosity of fluid.
14
Chapter 2
Literature Review
2.1 Literature Review
J.R Burns et al (2001) separated acetic acid from kerosene using slug flow. The experiments
were conducted in a micro channel reactor made of glass material in a 380 m in width. Acid
and base reaction were used as the basis of the study. Aqueous solution of KOH and NaOH with
phenol red as pH indicator was used as the base having concentration ranging from 0.1 to 0.4
mol/L. Organic phase was prepared by mixing acetic acid in kerosene using Sudan III(red) and
Sudan IV (blue). The aqueous Phase was comprised of KOH and NaOH solution. Both the
organic and aqueous were made to flow in micro channel. Color change was used as the
indicator for the completion of the reaction. It is reported that 97 % of acetic acid is separated.
Volumetric mass transfer coefficient were reported in the order of 0.510-4 s-1
Kashid et al (2007) performed experiments on Liquid-Liquid Slug flow in a capillary along with
wettability based flow splitter and showed that these are better than conventional contractors.
LLE of 3 non reacting systems were used by them i) iodine in aqueous solution and kerosene ii)
succinic acid in aqueous solution and n-butanol iii) acetic acid in kerosene and distilled water.
0.5, 0.75 and 1 mm capillary sizes were used. Capillary contactor was made of PTFE. The
splitter worked on the principle of preferential wettability of a liquid on a solid material. Mass
transfer co-efficient and extraction efficiency were used as the parameters for evaluating the
performance of capillary contactor. They studied the effect of flow rates, capillary sizes and flow
ratio on the liquid-liquid slug flow system as well as the Y splitter. They also compared the
results with conventional contactors. They showed that with increase in the flow velocity for a
given capillary, the extraction efficiency decreases. The extraction efficiency increases with
decrease in solvent flow rates. An extraction efficiency of more than 90 % were achieved in all
the cases. Specific interfacial area was found to be 4500-4800 m2/m3 and volumetric mass
transfer co-efficient kLa (10-4 1/s) was found to be 0.31-0.98 for system (i) and ID=0.5 mm.
Dessimoz et al (2008) used two rectangular glass capillaries with an equivalent diameter of 269
& 400 m. Deionized water, hexane and dyed toluene was used as the immiscible fluids. T and
15
Y junctions were studied. Volumetric flow rates of both the fluids were in the range 1 and 6
ml/hr. The formation mechanism of slug and parallel flow and compared the mass transfer
performances of two flow patterns. Slug flow and parallel flow were used for extraction and it
was reported that slug flow contributes determined the mass transfer coefficients for parallel and
slug flow using instantaneous neutralization (acidbase) reaction. The two flow patterns showed
the same global volumetric mass transfer coefficients in the range of 0. 20. 5 s1.
Raimondi et al (2014) performed experiments of mass transfer with liquid-liquid slug flow in
square micro channels. They carried out experiments in two micro reactors having square section
of 0.21 and 0.30 mm width and were made from silicon and glass. The manufacturing technique
used was photolithographic technique. High-aspect-ratio micro channels were fabricated in a
silicon wafer by plasma etching using the deep reactive ion etching (DRIE) technique and the
Bosch process. The introduction of the fluids were performed by syringes with stainless steel
needles. A high-speed camera coupled with a binocular enables the visualization of the flow in
the micro channel. Water/acetone/toluene two-phase system were used. Acetone was the solute
which transfers from toluene (dispersed phase) to water (continuous phase).The concentration of
acetone in the continuous phase is determined using secondary channels to extract this phase. In
order to analyze continuous phase samples representative of this phase in the micro channel, half
of its flow rate is constantly extracted. There were five secondary channels per micro reactor
located at a distance of 2.4mm, 7.8mm, 17.6mm, 32.2 mm and 48.8 mm from the middle of the
T-shape droplets generator. The total length of the main channel in which mass transfer occurs is
50.6 mm (from the droplets generator to the main outlet). The concentration of acetone in the
continuous phase was determined by UV-spectrophotometry measurements. They measured
droplet side mass transfer coefficient from the experimental concentration profiles. Volumetric
mass transfer coefficient ranges from 0.72 to 8.44 s-1. The higher values are obtained for the
higher droplets velocities, around 0.3 ms-1, most of the values are of the order of magnitude of 2
s-1 for droplets velocity ranging from 0.025 to 0.08 m s-1. They also performed interfacial area
modelling.
Xu et al (2013) studied alkaline hydrolysis reaction by generating slug flow in micro channel.
They extracted sodium hydroxide in water into n-butyl acetate. Interfacial area by snapshot
method. They studied the effect of various parameters on slug length, mass transfer coefficient
16
and overall volumetric extraction rate quantitatively. They found a decreasing trend of
volumetric mass transfer coefficient along the length of the channel. It was correlated volumetric
mass transfer coefficient with different channel length. Specific interfacial area reported to be
4000-2250 m2/m3 and the volumetric mass transfer co-efficient, kLa (10-4 1/s) 0.05-0.35 in a 0.6
mm capillary.
Darekar et al (2014) carried out liquid-liquid extraction experiments in two diverse types of
micro-channels using zinc sulfate, di-(2-ethylhexyl)-phosphoric-acid (D2EHPA) in dodecane
which would be a typical reactive extraction system. They used T-junction serpentine micro
channel and split and recombine micro channel. They studied the effects of organic to aqueous
ratio and residence time on overall mass transfer coefficient. They also made an attempt to
explain the L-L flow patterns with the help of high speed image acquisition system. They also
reported correlations connecting overall mass transfer co-efficient for organic to aqueous ratio
and velocity for both the micro channels. They got volumetric mass Transfer Co-efficient, kLa
(10-4 1/s) as 5.41-0.02.
Kashid and Agar (2007) studied the effect of different operating conditions on the slug size,
pressure drop, interfacial area, flow regimes gas been done. They measured the pressure drop
along the Y shaped mixing element and the length of downstream capillaries were reported.
Power required for creating interfacial area were also reported from the pressure loss over the Y
junction. The results obtained from the power requirement calculation and interfacial area
showed that the Micro Structure Reactor are much superior to conventional equipment in term of
power input and specific energy per unit interfacial area generated.
Tsaoulidius et al (2013) studied the extraction of uranium (VI) from aqueous nitric acid solution
by using tri-butyl phosphate dissolved in 1-butyl-3-methylimidazolium bis {(tri-fluoro methyl)
sulfonyl} amide. They performed the experiments on a Teflon micro channel of 0.5 mm internal
diameter. UV-Vis Spectroscopy was used to determine the concentration of dioxouranium (VI)
in the aqueous and the ionic liquid phases. They studied the effect of initial nitric acid
concentration (.01-3 M), phase flow rates and residence time and showed that extraction
efficiency followed a marginally different trend. They also showed that mass transfer co efficient
varied between 0.049 s-1 & 0.312 s-1
17
Kashid et al.,
Year System
2007
Volumetric mass
Efficiency Specific
Interfacial
Transfer Co-efficient,
Area(m2/m3)
4500-4800
0.31-0.98
film.(I.D-0.5 mm)
film.(I.D-0.5 mm)
1.Iodine in aqueous
>90 %
2001
Ramshaw
Dessimoz et
--
2008
--
10,700-11,200
Order of magnitude-0.5
--
1450-1680 (I.D-0.5
0.2-0.5
2007
Agar
Tsaoulidis et
--
into water
al.,
Kashid and
mm)
2013
al.,
Uranium(VI) from
78 %-
58%
78 %- 58%
0.312-0.132
2013
Sodium hydroxide in
--
acetate
Darekar et
al.,
2014
Sodium hydroxide in
--
2930(250 L
serpentine micro
acetate
channel)
18
5.41-0.02
Raimondi et
2014
--
toluene
al.,
4540-9600
(Square microchannel- 0.30 mm)
Objective:
To study the various parameter relations in liquid liquid flow in micro channel
Velocity distribution
Pressure drop
Flow regimes
Surface area
Different diameter
Different length
Different flow rates
19
0.72-8.44
Experimental Section:
Experimental setup:
Procedure:
Fill both the syringes up to 10ml one is with water (dye) and the other with Toluene.
Connect the syringes to capillary with the help of Teflon tubes.
Set the flow rates for both the liquids.
Then start the experiment and observe the flow pattern.
If the slugs are of uniform length then take a picture of it.
Then by changing the flow ratio take observations.
20
1
2
3
4
5
6
Pressure
drop
(N/m2)
Reynolds
no.
Weber
no.
(Capillary
no.)*10^-3
S/V
(toluene)
(m2/m3)
1640.88
2547.51
1940.72
2117.17
1061.196
1856.5
114.55
35.85
43.43
56.46
17.945
55.675
0.475
0.337
0.0447
0.095
0.00833
0.0738
3.321
0.931
1.03
1.68
0.4646
1.36
6677
5503
5492
5551
5506
5606
Pressure
drop
(N/m2)
Reynolds
no.
Weber
no.
(Capillary
no.)*10^-3
S/V
(toluene)
(m2/m3)
2271.69
2582.59
1679.56
2078.87
1567.15
1842.18
2031.27
2261.46
56.847
79.867
36.75
43.935
90.195
19.65
53.49
48.28
0.0756
0.3756
0.04781
0.0678
0.08156
0.561
0.3128
0.1561
1.253
0.315
0.3186
0.1875
0.1325
0.2386
0.3175
1.6981
4752
5050
4325
4550
4223
4435
4545
4750
s. no.
1
2
3
4
5
6
7
8
21
s. no.
1
2
3
4
5
6
7
8
Water flow
Toluene flow Unit
rate(ml/min) rate(ml/min) Slug
length
(cm)
0.50
0.50
0.1782
0.30
0.30
0.2323
0.40
0.40
0.1966
0.60
0.60
0.1643
0.40
0.60
0.2725
0.40
0.80
0.2543
0.60
0.80
0.1952
0.60
0.90
0.1772
Pressure
drop
(N/m2)
Reynolds
no.
Weber
no.
(Capillary
no.)*10^-3
S/V
(toluene)
(m2/m3)
1672.515
1470.595
2018.101
1247.099
2400.667
2823.835
2436.292
2720.781
5.2019
29.277
78.47
57.135
52.12
58.88
67.28
74.84
0.0943
0.0338
0.0588
0.1368
0.092
0.132
0.182
0.208
1.808
1.1574
0.7506
2.3957
0.1325
0.2386
0.3175
1.6981
9970
9943
10157
11263
9420
9530
10700
10100
22
Sample Calculation:
Flow rate of toluene = 0.6 ml/min.
Flow rate of water = 0.3 ml/min.
23
Volume = 01 Ld
S/V for toluene = 4223 m2/m3
P(slug flow) = P(frictional) + P(interfacial)
= Pfr,c + Pfr,d + PI
Pfr,d =
456 7 8
9:
Pfr,c =
45; (< 7) 8
9:
v = (Qc + Qd)/A
PI =
=
9
cos A
Conclusion:
We have used three capillaries of different diameters (0.5mm, 0.8mm, 1mm). The S/V ratio is
achieved highest in 0.5mm capillary(about 10000 m2/m3), & lowest in 1mm capillary (about
4400 m2/m3), while for 0.8mm capillary it is about 5500 m2/m3. S/V ratio increases with slug
velocity & decreases with slug length. Pressure drop increases with slug velocity & decreases
with capillary diameter. The weber no. is about 0.4, so interfacial force is predominant over
inertial force.
24
The capillary no. is very low, thus interfacial force is predominant over viscous force.From the
results we find that the slug length is the function of slug velocity. For weber no. greater than 1,
the flow becomes annular and parallel flow. Annular and parallel flows are easily destabilized
by changing flow rates and volumetric flow ratios. Slug and drop flows are easily controllable.
The interfacial pressure drop is calculated at constant contact angle. The superficial velocity is
used to calculate frictional pressure drop. The receding & advancing contact angles can only be
assumed equal at very low velocities. The difference between them increases with the linear
velocity.
25
References
1.
G.M.Whitesides. The origins and the future of microfluidics, Nature, Vol. 442,
2006.
2.
3.
4.
5.
6.
7.
8.
9.
Bujian Xu, Wangfeng Cai, Xiaolei Liu and Xubin Zhang. Experiments of mass
transfer with liquidliquid slug flow in square microchannels, Chemical Engineering
Science, Vol. 105, pp. 169178, 2014.
10.
Mayur Darekar, Nirvik Sen, K.K. Singh, S. Mukhopadhyay, K.T. Shenoy and S.K.
Ghosh. Liquidliquid extraction in microchannels with ZincD2EHPA system,
Hydrometallurgy pp. 144145, 2014.
26
11.
Dimitrios Tsaoulidis and Panagiota Angeli. Effect of channel size on mass transfer
during liquidliquid plug flow in small scale extractors, Chemical Engineering
Journal Vol. 262, pp. 785793, 2015.
12.
13.
14.
Hemant B. Mehta and Jyotirmayi Banerjee. CFD Analysis of the Taylor slug flow in
a microchannel under microgravity condition using VOF Method, International
Conference on Fluid Mechanics and Fluid Power, 2010.
27