Chemical Engineering Journal 313 (2017) 1509–1520

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Chemical Engineering Journal

journal homepage: www.elsevier.com/locate/cej

Review

A comprehensive review of micro-distillation methods

Ruey-Jen Yang a, Chan-Chiung Liu b, Yao-Nan Wang c, Hui-Hsiung Hou a, Lung-Ming Fu d,e,⇑
a
Department of Engineering Science, National Cheng Kung University, Tainan 701, Taiwan
b
Department of Food Science, National Pingtung University of Science and Technology, Pingtung 912, Taiwan
c
Department of Vehicle Engineering, National Pingtung University of Science and Technology, Pingtung 912, Taiwan
d
Graduate Institute of Materials Engineering, National Pingtung University of Science and Technology, Pingtung 912, Taiwan
e
Department of Biomechatronics Engineering, National Pingtung University of Science and Technology, Pingtung 912, Taiwan

h i g h l i g h t s

 Distillation is a powerful technique for separating from a miscible fluid mixture.

 Distillation is of importance in many microfluidic applications.
 Various methods for separating fluid mixtures at the microscale have been proposed.

a r t i c l e i n f o a b s t r a c t

Article history: Distillation is a powerful technique for separating the component substance from a miscible fluid mixture
Received 11 August 2016 by means of selective evaporation and condensation. Distillation is of importance in many microfluidic
Received in revised form 12 October 2016 applications, including food processing, gas/liquid separation, and biochemical. However, at the micro-
Accepted 6 November 2016
scale, surface tension forces exceed gravitational and hydrodynamic forces, and hence traditional
Available online 8 November 2016
gravity-based distillation methods have only a limited efficiency. Consequently, various alternative
methods for separating miscible fluid mixtures at the microscale have been proposed in recent years
Keywords:
based on techniques such as vacuum forces, capillary forces, centrifugal forces/gravity effect, other types,
Micro-distillation
Microchannel
and so on. The main developments in the micro-distillation field are introduced and discussed in the pre-
Evaporation sent review.
Membrane Ó 2016 Elsevier B.V. All rights reserved.

Contents

1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1510
2. Various distillations methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1510
2.1. Vacuum distillation [33–51] . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1510
2.2. Capillary force distillation [52–62]. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1513
2.3. Centrifugal force/gravity effect distillation [63–66] . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1514
2.4. Other types [67–72] . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1515
3. Concluding remarks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1518
Acknowledgement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1519
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1519

⇑ Corresponding author at: Department of Biomechatronics Engineering, National

Pingtung University of Science and Technology, Pingtung 912, Taiwan.
E-mail address: loudyfu@mail.npust.edu.tw (L.-M. Fu).

http://dx.doi.org/10.1016/j.cej.2016.11.041
1385-8947/Ó 2016 Elsevier B.V. All rights reserved.
1510 R.-J. Yang et al. / Chemical Engineering Journal 313 (2017) 1509–1520

1. Introduction

The term distillation refers to a general class of methods used to

separate components from a mixture based on a difference in their
volatilities [1–3]. In general, a distillation process involves heating
the liquid mixture to the vapor state so as to enable the selective
condensation and withdrawal of the component(s) of interest.
When the vapor and liquid phases flow in a concurrent direction,
the separation efficiency is limited to a single ideal stage [4]. If a
higher separation efficiency is required, the liquid and vapor are
brought into counter-current contact. This method is referred to
as fractional distillation, and is one of the most commonly used
separation methods in the chemical process industry [5].
In distillation processes, the extent of separation is governed by
thermodynamic equilibrium, whereas the rate of separation is
determined by the mass transfer [6]. Miniaturizing the separation
process has the advantage of improving the mass transfer perfor-
mance through the production of large gradients and high
surface-to-volume ratios. However, many common chemical sepa-
ration processes, including distillation, absorption and stripping,
rely on mass transfer across a gas-liquid interface, and establishing
such an interface in microchannels represents a significant chal- Fig. 2. Variation of absorbance value with SO2 concentration for standard H2SO3
lenge [7]. solutions (control group) and H2SO3 solutions obtained using proposed micro-
distillation system (experimental group). (Reprinted from Ref. [33] with permission
Distillation plays an essential role in many chemical processes
of Royal Society of Chemistry.)
and operations. Various large-scale distillation methods are avail-
able, including heat integrated distillation column (HIDC) [8,9],
membrane distillation (MD) [10–13], cyclic distillation [14,15], pensating for heat losses increases. This problem is compounded
cryogenic distillation [16,17], reactive distillation column (RDC) by the high surface temperature of the column together with the
[18–22], and others [23–25]. Membrane distillation involves the high surface-to-volume ratio of the channels. Consequently, in
thermal, vapor-driven transportation of the miscible fluid mixture ensuring the steady and efficient operation of micro-distillation
through a micro-porous hydrophobic membrane [26,27]. Of the systems, it is important that the heat balance be properly evalu-
various distillation techniques in common use, membrane distilla- ated and effective temperature control strategies devised.
tion has many practical advantages, including a low equipment The present paper provides a comprehensive review of recent
cost, good energy efficiency, and a low feed water pretreatment proposals for four common microfluidic distillation techniques,
requirement. As a result, it is widely used in industry for such namely vacuum force distillation, capillary force distillation, cen-
applications as environmental waste cleanup, food processing, trifugal force/gravity effect distillation, other types distillation.
and so on [28–31]. The use of membrane distillation in small- For each technique, the main principles of the associated method
scale commercialized plants is well documented in the literature are introduced and discussed and the corresponding experimental
[32]. However, with the maturation of microfluidics technology, and numerical results described. The review concludes with a brief
the application of membrane distillation at the microscale has also summary of the main challenges faced by the micro-distillation
attracted growing interest in recent years [1,2]. field together with the likely direction of future developments.
At micron scales, the significance of gravitation is reduced in
lieu of surface forces. Thus, to realize microscale distillation
requires the use of novel column designs and packing materials. 2. Various distillations methods
However, as the characteristic scale reduces, the problem of com-
2.1. Vacuum distillation [33–51]

Ju et al. [33] proposed a novel microfluidic distillation system

for SO2 detection comprising a polymethylmethacrylate (PMMA)
substrate patterned with a serpentine channel, a heating zone, a

(i) 60 mm (ii) (iii)

6 mm

150 mm

Fig. 1. Photograph and schematic illustration of fully-assembled microfluidic

distillation device. (Reprinted from Ref. [33] with permission of Royal Society of Fig. 3. Schematic diagram of continuous laminar evaporation microdevice.
Chemistry.) (Reprinted from Ref. [34] with permission of Royal Society of Chemistry.)
 R.-J. Yang et al. / Chemical Engineering Journal 313 (2017) 1509–1520
buffer zone, a cooling zone and a collection tank (see Fig. 1). The
feasibility of the proposed device was demonstrated by measuring
the absorbance values of five standard (i.e., non-distilled) H2SO3
solutions with known SO2 concentrations ranging from
100500 ppm. The corresponding results are presented in Fig. 2
(labeled as the control group). It was shown that the absorbance
value (Y) and SO2 concentration (X) were related as follows:
Y = 0.0001947X + 0.4946. Moreover, the correlation coefficient
was found to be R2 = 0.9991. The absorbance values were then
measured for five distilled H2SO3 samples with the same SO2 con-
centrations (labeled as the experimental group in Fig. 2). The mea-
sured absorbance values were found to be related to the SO2
concentration as Y = 0.0001977X + 0.4916, with a correlation coef-
ficient of R2 = 0.9981. The good agreement between the correlation
coefficients for the control and experimental data was taken to con-
firm the general feasibility of the proposed device. The practical
applicability of the device was demonstrated by comparing the
SO2 concentration measurements obtained for two commercial
red wine samples with those obtained using a large-scale con-
denser system. The two sets of results were found to deviate by
no more than 8.6% over three repeated measurements for each
sample.
Wootton and deMello [34] reported a method based on laminar
evaporation for the continuous purification of volatile liquids using
the microfluidic system shown in Fig. 3 consisting of three sections,
namely (i) a heating section; (ii) a condensation section; and (iii) a
separation section. As in a standard distillation process, the pro-
posed arrangement allowed a mixture of volatiles to be separated
in accordance with their vapor pressures. The performance of the
proposed device was demonstrated using a 50:50 mixture of ace-
tonitrile and dimethylformamide (DMF). It was shown that the
device achieved a nine-fold increase in the acetonitrile concentra-
tion in a single distillation process.
Huang et al. [35] and Tegrotenhuis and Stenkamp [36] pre-
sented a field-deployable process for the generation of clean desul-
furized fuel from JP-8 feedstock. In the proposed system, a
microchannel distillation unit was placed upstream of the fuel
reformer; thereby allowing a lower feed fraction of JP-8 to be pro-
cessed and hence improving the performance of the subsequent
hydrodesulfurization unit in reducing the sulfur content. The
results obtained in a 100-h continuous distillation test showed that
the system reduced the sulfur content of the original JP-8 sample
from an initial 329 ppmw to less than 0.5 ppmw and comprised a
catalysted bed volume of 100 cm3 at a standard conditions.
Chueachot and Chanthai [37] presented a method for determin-
ing trace amounts of cyanide in fruit wines based on the absor-
bance of the catalytic reaction of ninhydrin. The calibration curve
for the proposed method was shown to be broadly linear over
the range of 40160 lg/L, with a correlation coefficient of
r2 > 0.99. Moreover, a total cyanide recovery performance of
Fig. 4. Distillation column: (1) connections on top of column; (2) connections on
side of column. (Reprinted from Ref. [38] with permission of Elsevier.)
1511
76.894.8% was obtained for standard wine samples, with a detec-
tion limit of 6 lg/l and a reproducibility of less than 4.44%.
Sundberg et al. [38–42] developed a small-scale distillation unit
based on the planar distillation column shown in Fig. 4. The
column was packed with porous open-cell metal foam and was
operated in a horizontal orientation with the ends carefully regu-
lated to the boiling point temperatures of the pure compounds.
The distillation unit was designed for operation at extremely low
mass fluxes and achieved a highly stable performance given an
appropriate control of the flow rate and heat losses. To reduce
the energy consumed in heating the feed flow to the bubble point
temperature, the liquid entering the distillation column was pre-
heated using the flat-channel heater system shown in Fig. 5. The
efficiency of the distillation system was evaluated using two binary
systems (n-hexane + cyclohexane and methyl formate + methanol)
and one ternary system (2-methylbut-2-ene + ethanol + 2-ethoxy-
2-methylbutane). For all three samples, a good agreement was
observed between the measured concentration profiles and the
simulated values.
Mansfeldt and Biernat [43] used a micro-distillation system
originally intended for analyzing aqueous samples to detect the
cyanide (CN) content in soil samples. As shown in Fig. 6, the main
components in the system included the sample vessel, a heater, a
capillary, an adsorption vessel, a cooler and a protective hood.
Experiments were performed using soil samples taken from former
gas works and blast furnace sludges with cyanide concentrations
ranging from <1 to approximately 10,000 (mg kg 1 CN ). The cya-
nide detection results were shown to be in close agreement with
those obtained using the macro-distillation method prescribed in
the related German standard (r = 0.997, p < 0.001%, n = 20).
Wang et al. [44] proposed an integrated microfluidic distillation
chip for separating a mixed ethanol-methanol-water solution into
its constituent components. The chip comprised a serpentine chan-
nel, a boiling zone, a heating zone and a cooled collection chamber
filled with de-ionized (DI) water (see Fig. 7). In performing the dis-
tillation process, the ethanol-methanol-water solution was driven
through the serpentine channel and into the collection chamber
by means of a nitrogen carrier gas. The results showed that the pro-
posed system achieved an average methanol distillation efficiency
of 97%. Moreover, the results obtained for the methanol concentra-
tions of two commercial fruit wines were shown to be in good
agreement with those obtained using a macro-scale technique.
Cypes et al. [45] Sotowa and Kusakabe [46] presented a micro
single stage distillation device consisting of a silicon plate pat-
terned. In those proposed device, the feed was heated and partly
evaporated, and the resulting vapor–liquid mixture and ethanol–
water mixture was flowed into an assembly of capillary channels,
where the liquid phase was separated from the saturated vapor
under the effects of capillary forces.
Liu et al. [47] presented a micro-distillation system for
formaldehyde concentration detection in food products. As shown
in Fig. 8, the system consisted of a micro-distillation device, a
micro-condenser, a micro-distillation chip, a high-pressure steam
tank, a temperature controller, and a cooling system. In performing
the distillation process, the sample was injected into the distilla-
tion chip and a high-pressure steam supply was used to vaporize
the formaldehyde and carry it to the condenser region of the chip.
The vapor condensed under the effects of the low-temperature
cooling channel and was then transported to the collection region
of the device. The results obtained using standard formaldehyde
samples showed that the distillation efficiency reached as much
as 98% given a steam pressure of 4 bar. In addition, a good agree-
ment was observed between the results obtained using the pro-
posed micro-distillation system for 18 commercial Chinese herb
samples and those obtained using a commercial macro-scale
system.
1512 R.-J. Yang et al. / Chemical Engineering Journal 313 (2017) 1509–1520

Fig. 5. Configuration of heater and heat exchangers: (1) position of electrical heating cartridges; (2) reboiler and pre-heater; (3) heat exchanger; (4) process fluid channel.
(Reprinted from Ref. [38] with permission of Elsevier.)

species with respect to another, but simply to serve as a physical

Fig. 6. Schematic diagram of micro-distillation apparatus: (1) sample vessel; (2)
frit; (3) heater; (4) capillary; (5) absorption vessel; (6) cooler; (7) keyboard and
display; (8) protection hood; (9) syringe for reagent feeding; (10) septum.
(Reprinted from Ref. [43] with permission of Elsevier.)
Adiche and Sundmacher [48,49] proposed a novel micro-
separator (Fig. 9) combining the sweep gas membrane distillation
principle and microfluidic channels for the separation of binary
methanol-water mixtures. Notably, the membrane in the proposed
device was not intended to offer selectivity for any particular
separation between the liquid and the gas phase (see Fig. 10).
The performance of the device was evaluated experimentally using
different liquid-vapor/gas membrane contactors, methanol con-
centrations (570 wt%), feed temperatures (40–65 °C), feed flow
rates (up to 30 ml/min), and carrier gas flow rates (up to 600 ml/
min). The results showed that the temperature polarization effect
was localized in both the feed channel and the permeate channel
and was strongly related to the feed flow rate and inert gas flow
rate, respectively. The authors concluded that the proposed device
had a major advantage over existing membrane distillation pro-
cesses in that it allowed the separation of aqueous mixtures with
various methanol concentrations ranging from low to high.
Lautenschleger et al. [50] performed a numerical and experi-
mental investigation into the effects of the apparatus geometry
and operating parameters on the membrane distillation of metha-
nol and water. In calculating the fluxes through the membrane, an
average porosity, pore size, and tortuosity were assumed, and the
phase interface curvature at the entrance of the membrane pore
openings was ignored. The simulation model and associated
boundary conditions are shown in Fig. 11(a) and (b), respectively.
The effects of two different baffle arrangements on the fluid
dynamics and mass transfer were considered (see Fig. 12). The
results indicated that for the investigated process conditions, the
mass transfer in the membrane was dominated by the membrane
porosity rather than its thickness. Furthermore, it was shown that
the mass transfer could be enhanced by either reducing the chan-
nel height or introducing baffles, where the choice between the
two approaches depends on the maximal possible allowed pres-
sure drop.

(a) (b)
Back top heating layer Cooling module
Cool water
Back lower heating layer

Back cover layer Buffer zone

Microfluidic interface
Front cover layer
65 mm

Inlet
115 mm Front heating layer

Fig. 7. (a) Exploded view of micro-distillation device. (b) Schematic illustration of fully-assembled microfluidic distillation chip. (Reprinted from Ref. [44] with permission of
Elsevier.)
 R.-J. Yang et al. / Chemical Engineering Journal 313 (2017) 1509–1520
Chip holder (rapid coupler) Micro-distillation chip
High pressure steam tank 3cm
Collected area
Heater
Temperature controller Cooling system
Fig. 8. Photograph of micro-distillation system. (Reprinted from Ref. [47] with
permission of Elsevier.)
Timmer et al. [51] presented a micro-evaporation concentrator
in which a hydrophobic vapor-permeable membrane was used to
permit the passage of the gas components of the electrolyte solu-
tion under a forced convection effect, but to trap the analyte com-
ponents; thereby producing a concentration effect (Fig. 13).
Experiments were performed to investigate the effects of the con-
vective nitrogen flow velocity and residence time of the analyte
inside the concentrator on the separation performance of the pro-
posed device. The results revealed that the evaporation rate (i.e.,
analyte concentration factor) increased with both an increasing
nitrogen flow velocity and an increasing residence time. However,
it was noted that as the analyte velocity reduced (i.e., the residence
time increased), the normalized evaporation rate also reduced,
resulting in a greater vapor content in the dry nitrogen flow.
2.2. Capillary force distillation [52–62]
Ziogas et al. [52] presented a micro-rectification apparatus
(MRA) for the intermittent or continuous separation of liquid
mixtures for analytical or preparative purposes. The device
consisted of a screwed assembly containing a front housing, a
multi-layer plate column inlay and a rear housing (see Fig. 14).
The performance of the proposed device was evaluated in both a
batch mode (using Acetone/n-Butanol, Toluene/o-Xylene, and
i-Octane/n-Octane mixtures) and a continuous mode (using an
o-Xylene and p-Xylene mixture). The results showed that the
device achieved a high separation efficiency and a low height
(a)
Fig. 9. (a) Photograph of micro-distillation device. (b) Exploded view of micro-separator. (Reprinted from Ref. [48] with permission of Elsevier.)
1513
equivalent of theoretical plate (HETP) value for even difficult to
separate systems such as o-Xylene and p-Xylene.
Stanisch et al. [53] reviewed the strengths and weaknesses of
various distillation methods, including zero gravity distillation,
membrane distillation, micro-structured distillation, high gravity
distillation, and capillary distillation. The capillary module used
for distillation can provide a successful phase separation of gas-
liquid mixtures up to volume feeds of 10 mL min 1. The effects of
the process parameters (e.g., the reflux ratio, the evaporation rate,
and the choice of feed stage) on the distillation performance were
then investigated by means of numerical simulations. Finally,
experimental trials were performed to investigate the feasibility
of the various distillation methods for industrial applications.
Sahoo et al. [54] and Hartman et al. [55] presented an integrated
microfluidic platform for performing multi-step continuous-flow
micro-chemical synthesis (see Fig. 15). For the carbamate synthesis
process considered for illustration purposes, the first micro-
separator (lS1) in the proposed platform was used to realize the
separation of two immiscible liquid phases following the first reac-
tion step (a phase-transfer reaction between aqueous azide and
acid chloride) in a silicon-based micro-reactor (lR1). Isocyanate
was then formed from the organic azide in a second reaction step
conducted in a micro-reactor packed with solid acid catalyst (lR2).
The generated nitrogen was removed from the gas–liquid two-
phase flow by a second micro-separator (lS2). Finally, carbamate
was synthesized by contacting the isocyanate generated in lR2
with alcohol in a third micro-reactor (lR3). The device was oper-
ated in a continuous mode without interruption until all of the
reagents were consumed (67 days) and was found to achieve a
productivity of 80120 mg per day, depending on the particular
type of carbamate synthesized.
Hartman et al. [56] presented a multi-step chemical synthesis
platform, in which the reaction solvents were exchanged using a
micro-distillation system based on the vapor–liquid equilibrium
condition achieved under segmented flow and capillary forces
(see Fig. 16). The separation results obtained for MeOH–toluene
and DCM-toluene mixtures showed that the device performance
was equivalent to that obtained in a single-stage flash distillation
process.
Tonkovich et al. [57] proposed a compact microchannel plant
for the off-shore production of methane from natural gas via steam
reforming. The water co-produced with the methane during the
reforming process was removed by a microchannel-based distilla-
tion module operating on the capillary exclusion principle (see
Fig. 17). It was reported that the microchannel steam methane
reforming (SMR) unit achieved a methanol purity of more than
95%. Furthermore, it was predicted that the fresh water require-
(b)
Cover plate for the
permeate channel
Permeate channel
Membrane contactor
Feed channel
Cover plate for the
feed channel
1514 R.-J. Yang et al. / Chemical Engineering Journal 313 (2017) 1509–1520

Aqueous mixture nol for illustration purposes, it was shown that the concentration
of the condensed liquid in the nanopillar region reached approxi-
mately 19 wt% due to the reduction in the vapor pressure com-
pared to that achieved at a flat liquid surface.

2.3. Centrifugal force/gravity effect distillation [63–66]

p
MacInnes et al. [63] proposed a rotating spiral microchannel
Vapor + I nert distillation device, in which the liquid and vapor layers were seg-
gas regated into two parallel counter-flows along the channel under
the combined effects of centrifugal forces and the pressure gradi-
ent (see Fig. 20). The spiral channel network was formed on an
optical glass substrate with a thickness of 2.3 mm by an isotropic
wet etching process. Access holes were drilled in a second optical
Inert carrier gas + permeate glass plate (with a thickness of 1 mm), and the drilled plate was
then bonded to the patterned substrate via a thermal fusion pro-
Fig. 10. Liquid-vapor/gas membrane contactor. (Reprinted from Ref. [48] with
permission of Elsevier.)
cess to form the completed chip (see Fig. 21). The experimental
results showed that the proposed device achieved a more efficient
contact performance and a shorter separation time than other
microchannel distillation devices reported in the literature.
ment for stream reforming could be reduced by up to 65% by reus-
Seok and Hwang [64] proposed a horizontal zero-gravity distil-
ing the water captured from the SMR exhaust stream.
lation column for separating ethanol-water and methanol-water
Lam et al. [58–60] presented a multi-stage microfluidic distilla-
mixtures utilizing the heat pipe principle. The separation perfor-
tion chip (Fig. 18) based on the heat pipe principle of counter-
mance of the proposed device was improved by lining the column
current liquid and vapor flows in the presence of a temperature
with capillary wicks. A good agreement was observed between the
gradient. To prevent flooding between the two flows, micropillar
experimental and simulation results for the concentration profiles
structures were fabricated on either side of the channel. The per-
of both mixtures along the column length under various reflux
formance of the proposed device was evaluated by separating
conditions. In general, the results confirmed the feasibility of the
acetone-water and methanol-toluene mixtures, respectively. The
proposed device for performing distillation under gravity-free con-
results showed that a highly efficient (>95%) separation perfor-
ditions (e.g., material recycling in outer space applications).
mance was obtained for both samples given the use of appropriate
Kralj et al. [65] developed a microfluidic device for continuous
heating and cooling temperatures. The same authors [61] pre-
flow liquid-liquid phase separation incorporating a hydrophobic
sented an in-situ study of the separation of toluene–benzaldehyde
polytetrafluoroethylene (PTFE) membrane sandwiched between
mixtures using the micro-distillation chip shown in Fig. 19, in
two microchannels. The experimental results showed that the
which micropillars were incorporated along both sides of the ser-
device was capable of completely separating organic–aqueous
pentine microchannel in order to guide the liquid flow by capillary
and fluorous–aqueous liquid–liquid systems, even given high frac-
forces. It was found that separation occurred within a limited sec-
tions of partially-miscible compounds in the sample stream.
tion of the chip, where the length of this section was determined
MacInnes et al. [66] developed the modelling and analysis for
by the heating and cooling temperatures, respectively. It was fur-
two-phase system (including liquid–liquid or gas–liquid) contact-
ther shown that the largest value for the minimum number of
ing in an infinitely wide spiral channel. The results showed that
equilibrium stages under total reflux conditions was equal to 2.7.
the infinitely wide spiral channel model is powerful that can eval-
Hibara et al. [62] developed a micro–nano combined structure
uate nearly all aspects of performance. Finite width channels are
for performing gas-liquid separation by means of an evaporator
used in practical devices that Coriolis mixing is active. Coriolis mix-
containing hydrophilic–hydrophobic patches and a downstream
ing can increase performance but with greater flow resistance for
condensation region containing nanopillar structures with a capil-
the same channel height that need greater rotation rate and pres-
lary radius of 270 nm. Using an aqueous solution of 9.0 wt% etha-
sure gradient than for the infinite channel. The infinite channel

(a) (b)

Gas channel
N2 Gas channel
Pore N2
Nmethnaol
qG
+Nwater Membrane
(1- )q M
TL,if = TM,iF Liquid channel:
Methanol/Water
TL,if = TG,iF Liquid channel:
Methanol/Water

Fig. 11. (a) Schematic view of energy and mass transport through membrane pore. (b) 2-D view of model domain and corresponding boundary conditions. (Reprinted from
Ref. [50] with permission of John Wiley and Sons.)
 R.-J. Yang et al. / Chemical Engineering Journal 313 (2017) 1509–1520 1515

Fig. 12. Representative section of feed channel with two different baffle arrange-
ments: (a) Arrangement A: both baffles placed in middle of channel height; (b)
Arrangement B: second baffle placed at bottom of channel. (Reprinted from Ref. [50]
with permission of John Wiley and Sons.)
Fig. 14. Exploded view of micro-rectification apparatus: (1) housing front part; (2)
housing rear part; (3) plate column inlay; (4) viewing window; (5) column bottom;
(6) column top; (7) plate; (8) holes for heating cartridges; (9) bottom outlet with
thermocouple; (10) distillate outlet; (11) vapor outlet; (12) feed; (13) reflux
condenser; (14) product condenser; (15, 16) holes for thermocouple; (17) reflux
valve head; (18) distillate valve head; (19) seals; (20) lining groove; (21) pin for
valve with O-ring; (22) hole for valve controller. (Reprinted from Ref. [52] with
permission of John Wiley and Sons.)

(a)

(b)

Fig. 15. Schematic diagram of multi-step continuous-flow microchemical platform

for carbamate synthesis. (Reprinted from Ref. [54] with permission of John Wiley
and Sons.)

Fig. 13. Schematic diagrams of: (a) evaporation enhanced by convective nitrogen
flow, (b) evaporation concentrator, comprising gas channel, electrolyte channel and
electrolyte conductivity sensor. (Reprinted from Ref. [51] with permission of
Elsevier.)

analytical model is possible carry over at least approximately to

the finite-width channels of practical devices.

2.4. Other types [67–72]

Boyd et al. [67] showed that when a small amount of heat is

added close to the liquid-vapor interface of a captive gas bubble
in a microchannel, interphase mass-transfer through the bubble
can occur in a controlled manner with only a slight change in the
temperature of the fluid. He further showed that this phenomenon
can be exploited to realize interphase chemical separation on a Fig. 16. Proof of concept device used to achieve single-stage distillation by means
microfluidic platform without the need for high temperatures, vac- of vapor–liquid equilibrium reached under segmented flow. (Reprinted from Ref.
uum conditions, or active cooling. The practical feasibility of the [56] with permission of Royal Society of Chemistry.)
1516 R.-J. Yang et al. / Chemical Engineering Journal 313 (2017) 1509–1520

Two-phase Coriolis
Mixture Vapor secondary
flows
P1 Spiral channel
Centrifugal
force
P2 Capillary
structure
P1 P2
Liquid
flow
Vapor
flow Rotation
Liquid Out axis

Fig. 17. Phase separation based on capillary exclusion effect. (Reprinted from Ref. Fig. 20. Phase contacting in rotating spiral microchannel. (Reprinted from Ref. [63]
[57] with permission of Elsevier.) with permission of Elsevier.)

14 µm Vapor channel
20 µm Contacting channel
outlet
40µm 20 µm

Junction

c (Chip) 600 µm

Fig. 18. Photograph of micro-distillation chip and magnified views of microchannel

configuration at indicated locations. (Reprinted from Ref. [57] with permission of
Royal Society of Chemistry.)

Feed inlet

Bottom outlet
Fig. 21. Glass chip fabricated from two glass layers. Note that overall size is
40 mm  40 mm; spiral channels are 255 lm wide and 95 lm deep; and inlet and
outlet holes are 1 mm in diameter. (Reprinted from Ref. [63] with permission of
Elsevier.)

gas bubble. In the separation process, a laser with a frequency near

Fig. 19. Micro-distillation chip and its operation: (a) photograph of entire chip with
connection ports; (b) magnified image of straight channel section showing
micropillars and liquid menisci during operation. (Reprinted from Ref. [61] with
permission of Elsevier.)
so-called bubble-assisted interphase mass-transfer (BAIM) phe-
nomenon was demonstrated using the microfluidic system shown
in Fig. 22 consisting of a microfluidic channel with a quasi-ordered
array of gold nanoparticles incorporated into the base and a captive
the plasma resonant frequency of the nanoparticle array was
focused near the edge of the bubble causing it to be heated. Mean-
while, the heat from the nanoparticles was transferred by conduc-
tion and convection to the surrounding fluid; causing evaporation
from the surface near the laser and subsequent condensation on
the far surface of the bubble. The results obtained using a solution
of ethanol and Coumarin 4 buffered with HCl and tris(hydroxy-m
ethyl)aminomethane (Tris buffer) showed that the achievable mass
transfer rate was suitable for small-scale applications such as the
preconcentration of fragile biomolecules and bioproduct recovery
from single living cells, respectively.
Xin et al. [68] examined the flow and transfer characteristics in
a hydrophobic membrane pore by means of numerical simulations
using an ethyl acetate solution for illustration purposes. As shown
in Fig. 23, during the vacuum membrane distillation (VMD) pro-
cess, the membrane surface contacts the liquid feed directly and
part of the volatile components and water gasify and enter the
membrane. Given the application of a pressure difference across
the membrane, the vapor is sucked through the membrane pores
into the cold side, where it subsequently condenses. It is seen that
the concentration of ethyl acetate increases from a minimum
value of 0.14 mol/m3 at the inlet side to a maximum value of
2.38 mol/m3 at the outlet side. Overall, the simulation results
 R.-J. Yang et al. / Chemical Engineering Journal 313 (2017) 1509–1520 1517

Counter-current flow mode

Tc,o
Permeate channel Tc,j

v c,j

Th,j Membrane Mass Th,o

v h,j Feed channel

Fig. 25. Schematic diagram of simulated DCMD 2D model. (Reprinted from Ref. [71]
with permission of Elsevier.)

showed that the membrane flux increased with an increasing

Fig. 22. Schematic diagram of microchannel assembly (side view). Note that an
array of nanoparticles is placed on a glass slide, which serves as the base of the
channel. (Reprinted from Ref. [67] with permission of American Chemical Society.)
solution
membrane
vacuum
Fig. 23. Feed flow in membrane module. (Reprinted from Ref. [68] with permission
of Taylor & Francis.)
porosity, pore diameter and tortuosity, but was insensitive to the
pore length.
Zhang et al. [69,70] presented a multi-layered microchip for the
vacuum distillation of water-methanol mixtures. The polymer chip
employed a cooling channel to generate a temperature gradient
along the distillation channel, which was separated into two chan-
nels (one for liquid phase and one for vapor phase) by a micro-
porous PTFE membrane. Fig. 24(a) and (b) show an exploded view
of the microchip assembly and a schematic illustration of the
micro-distillation process, respectively. As shown in Fig. 24(b),
the portion of the horizontal channel to the left of the feed entry
serves as a rectifying section, while that to the right of the feed
entry serves as a stripping section. The chip was designed with a
high specific area so as to enhance the exchange rate between
the liquid phase and the vapor phase. Experimental investigations
were performed to examine the effects of the hotplate tempera-
ture, cooling water flow rate, feed concentration, feed flow rate,
and membrane pore size on the distillation efficiency of the pro-
posed device. The results revealed that the distillation performance
was enhanced given the use of a low feed concentration and a high
feed flow rate. Moreover, for a smaller pore diameter, a higher tem-

(a) (b)
Description / Layer
Rectifying Stripping
Cover layer to section section
mechanical support 1
Inlet of
Cooling channel layer cooling
for temperature 2 water Outlet of
gradient generating cooling Liquid contained
water Feed reduced volatile
Cover layer for 3 component in the feed
mechanical support
Liquid
Distillation channel outlet 72 µ m
layer for liquid phase 4
Membrane layer for 80 µ m
contact of liquid and 5
vapor
Vapor
Distillation channel Vapor 72 µ m channel
layer for vapor phase 6 outlet Vacuum
Substrate,
1 mm thick 7 Vapor contained
25 mm enriched volatile Heat
95 mm component in the feed

Fig. 24. (a) Exploded view of micro-distillation chip containing four microfluidic channel layers. (b) Schematic diagram of micro-distillation process. (Reprinted from Ref. [69]
with permission of Royal Society of Chemistry.)
1518 R.-J. Yang et al. / Chemical Engineering Journal 313 (2017) 1509–1520

Fig. 26. Schematic illustration of DCMD system. (Reprinted from Ref. [72] with permission of Elsevier.)

perature gradient was required to achieve micro-distillation. membrane were investigated for various CNT concentrations in
Finally, given an appropriate setting of the temperature gradient, the range of 15 wt%. It was found that an increasing CNT concen-
a total theoretical plate number of 1.8 was achieved, which implies tration resulted in a higher contact angle, a greater liquid entry
a process with close to two perfect simple distillations. pressure, and a higher flux. The authors thus concluded that the
Hwang et al. [71] performed a numerical and experimental incorporation of CNTs into superhydrophobic nanofiber mem-
investigation into the effects of the module dimensions on the per- branes is beneficial in introducing additional functionalities which
formance of a commercially available hydrophobic porous PTFE enhance the DCMD performance.
membrane for the direct contact membrane distillation (DCMD)
of salty water. Fig. 25 presents a schematic illustration of the sim-
3. Concluding remarks
ulation model, consisting of the feed channel, the membrane layer
and the permeate channel. The simulations considered three trans-
This study has presented a comprehensive review of the main
port processes, namely energy convection and conduction in all
developments in the micro-distillation field in recent years. The
three layers, momentum transport in the feed and permeate chan-
review has focused specifically on four common microfluidic distil-
nels, and mass transport in the membrane layer. The experiments
lation techniques, namely vacuum force distillation, capillary force
were performed using a PTFE membrane with a mean pore size of
distillation, centrifugal force/gravity effect distillation, other types
0.28 lm and an effective porosity value of 17,000 m 1. It was
distillation (see Table 1). In general, the reviewed studies show
found that the mass transfer coefficients increased with a higher
that micro-distillation systems offer the advantages of an efficient
operating temperature and higher flow rate. In addition, the tem-
separation performance and a short residence time (i.e., a high
perature gradient profiles in the feed side and permeate side were
throughput). However, for all of the considered methods, the distil-
found to be parallel to one another in the counter-current flow
lation performance requires a careful control of the associated pro-
mode, but to approach one another in the co-current flow mode.
cess and apparatus parameters, e.g., the temperature profile, the
Finally, the flux and vapor pressure difference reduced as the NaCl
carrier/analyte flow rates, the pressure difference, the microchan-
concentration of the feed increased.
nel height, and so on. Overall, however, the results confirm the
Tijing et al. [72] used a one-step colloidal electro-spinning pro-
applicability of micro-distillation systems for a diverse range of
cess to fabricate a superhydrophobic nanofiber membrane contain-
high-throughput and high-performance microfluidic applications.
ing carbon nanotubes (CNTs) for DCMD desalination applications
Furthermore, as the basic mechanisms and behaviors of micro-
(see Fig. 26). The mechanical and hydrophobic properties of the
distillation techniques become increasingly clear, tremendous

Table 1
Summary of micro-distillation system studies.

Refs. First author Year Type Micro-channel width Efficiency System considered Material
and height (lm)
[33] Ju 2012 Vacuum 300, 300 94.6% SO2/water PMMA
[34] Wootton 2004 Vacuum 100–500, 50 0.72 TP Acetonitrile/DMF/toluene Glass
[35] Huang 2008 Vacuum 140, 10 8.6 wt% ethanol Desulfurization of JP-8 fuel n/r
[38] Sundberg 2013 Vacuum 30 mm, 5 mm 5 cm HETP Methyl formate/methanol Metal foam
[44] Wang 2016 Vacuum 300, 300 97% Ethanol/methanol/water PMMA
[47] Liu 2016 Vacuum 3 mm, 1.5 mm 98% Formaldyhedye/water PMMA
[48] Adiche 2010 Vacuum / 677 Separation factor 5 Methanol/water Polymeric oleophobic
[50] Lautenschleger 2015 Vacuum 1 mm, 0.5 mm Separation factor 5 Methanol/water PES40, PVDF22
[52] Ziogas 2012 Capillary Gravity 35 mm, 5 mm 1.08 cm HETP Toluene/n-octane Stainless steel
[53] Stanisch 2015 Capillary 100, 10 10 wt% ethanol Ethanol/water/mixture Glass
[54] Sahoo 2007 Capillary 400, 400 1.0 TP Dichloromethane/toluene n/r
[57] Tonkovich 2008 Capillary 178, 1350 0.83 cm HETP Hexane/cyclohexane Stainless steel
[58] Lam 2011 Capillary 350, 300 4 TP Methanol/toluene Silicon wafers
[61] Foerster 2013 Capillary 350, 300 2.7 TP Benzaldehyde/toluene Silicon wafers
[62] Hibara 2008 Capillary n/r 9.0 wt% ethanol Ethanol/water n/r
[63] MacInnes 2010 Centrifugal force 250, 95 6.6 TP 2,2-Dimethylbutane/2-methyl- Glass
2-butene
[64] Seok 1985 Gravity effect / 10.5 mm 5 cm HETP Methanol/water, ethanol/water Copper
[67] Boyd 2008 Bubble 30, 5 n/r Ethanol/Coumarin 4 buffered with HCl PDMS
[69] Zhang 2010 Vacuum membrane 1000, 72 1.8 TP Methanol/water PTFE

n/r: not report.

 R.-J. Yang et al. / Chemical Engineering Journal 313 (2017) 1509–1520 1519

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