MICROWAVE HEATING AND SEPARATION
OF WATER-IN-OIL EMULSIONS
C.S. Fang and P.M.C. Lai
Laboratory and field tests showed that viscous
and stable water-in-oil emulsions can be
demulsified and separated into oil and water
layers by the combined process of microwave
heating and gravity sedimentation. The process
provides an opportunity for waste reduction and
oil recovery from waterin-oil emulsions.
The process was tested with bench-scale
experiments using laboratory samples and sludge
samples collected from a dump-site. The
laboratory samples were 50-50% and 3070%
water-in-oil emulsions. The results were
encouraging and consistent with the observation
in field tests. In some cases better than 80% of
the water in emulsion samples was separated.
Key Words:
Microwave heating, Demulsification, Separation,
Water-inoil emulsions.
ABOUT THE AUTHORS:
C.S. Fang is affiliated with Department of Chemical similar result was obtained in the field test in
Engineering, University of Southwestern Louisiana, Louisiana for 188 bbls of crude-oil/water emulsion
Lafayette, LA 70504-4130. Peter L.C. Lai is affiliated with left in a tank, which was 10 ft in diameter and 15 ft
CTCI Corporation, Taipei, Taiwan.
Manuscript received July 28, 1994. Accepted for
publication November 30, 1994.
© International Microwave Power Institute
V
iscous and stable water-in-oil emulsions are
generated in various industrial operations,
such as petroleum refining, oil and gas
production, and transportation of natural gas through
pipelines. Since it is no longer permitted by law to
discharge oil-containing emulsions to a dump site,
the present practice is to use demulsifying chemicals
to break the emulsion and separate water from oil.
After separation, water is discharged to the river or
lake. Examples of demulsifying chemicals are alkyl
substituted benzene sulfonic acids and alkyl phenolic
resins [Kermmer, 1988]. For water-in-oil emulsions
which usually have high viscosity, the required
mixing of these chemicals with the emulsion is dif-
ficult. Also when a high dosage of chemicals is used
to overcome the difficulty, it leads to a secondary
pollutant, since the separated water may contain too
much chemicals to be discharged to public water.
As an alternative, microwave heating was studied.
The concept of microwave heating of emulsions was
first suggested by Klaila [ 1983] and Wolf [ 1986] in
their patent applications. In recent years, active
research and development work on microwave
demulsification technology for applications in
chemical plants was carried out by Samardzija [ 19911.
Following his patent award, Klaila conducted
several field tests, with a 50 kW microwave
generator, which was equipped with wave guides and
a microwave power monitor. One of the tests was in
March 1984 in Coffeyville, Kansas [Fang et al,
1988; 1989] with approximately 120 bbls of slop oil
in a large storage tank that was 10 ft in diameter and
10 ft high. The slop oil was an emulsion of 50% oil,
22.5% bottom sediment and 27.5% water. After 228
kWh of microwave energy was applied continuously
at 20 kW, the temperature of the top portion of
emulsion reached approximately 100°C and the
emulsion was separated to oil and water layers. A
high. After 18.2 hours and 417.5 kWh of
microwave radiation, the emulsion was separated to
146 bbls of dehydrated oil and 42 bbls of clear water.
In parallel with the field tests, experimental tests
on the controlled emulsion samples was conducted.
These samples of known compositions were prepared
in the laboratory. The objective of the experiments
was to produce quantitative information. Viscous
samples of sludge collected from a dumpsite were
also tested to demonstrate the effectiveness of mi-
crowave demulsification technology. The results are
presented

International Microwave Power Institute 47

here with equations to calculate approximate values of temMicrowave Oven
perature increase and the rate of heat generation of irradiated TC Amplifier
emulsions.
9
Laboratory Study Thermocoupl
es
Experimental Apparatus

A Kenmore domestic microwave oven (Sears

Model 566.8878611) was used in heating emulsion _to
samples. Its rated power output is 700 watts at 2450
MHz, consuming approximately 1400 watts of
electric power. A 800 ml cylindrical glass container A/D IBM PC-XT
was used as the sample holder. The top and bottom of Interfac Computer
e
the container were covered with aluminum foil, as
shown in Figure 1, so that microwaves enter only
FIGURE 1: Experimental
on the side surface of samples. The diameter and apparatus.
height of emulsion sample in the container were,
respectively, 88 mm and 132 mm, as shown in Figure
TOP
2. View
Nine J-type subminiature thermocouples
(OMEGA Model SICSS-020U-6) were inserted to
different locations of the sample body to measure
local temperatures of emulsion: three in the top layer,
three in the middle layer and three in the bottom
layer, as shown in Figure 2. The diameter of the
thermocouples was 0.010 inch. These thermocouples
were connected to thermocouple amplifiers (Cole-
Parmer No. J8109-00, Model 20B) and a data
acquisition analog/digital interface card (Cole-Parmer
No. J-8109-27, Model 134) in a desktop personal
computer. SIDE VIEW
A data logging computer program, written in
BASIC, was used to specify the interval of data
sampling and calibration constants. The overall
system accuracy in temperature measurements was
±1.5°C with 0.1°C resolution.

Sample Preparation and Procedures

Samples of water-in-oil emulsion were prepared using Golden _
State SAE-30 motor oil and distilled water. This particular 800
ml JAR
i_
motor oil was used because it contained the fewest additives. LAYERS
In many cases, emulsions in the oilfield are very stable. To TOP
assure the stability of emulsion samples prepared in the labo- ° MIDDLE
ratory, 0.95 NaOH solution was added to distilled water used Er$.7ISION
in preparation of samples. After oil had been poured into a ~l M
domestic blender (Sears, Kenmore Power 10), the blender ''
was turned on at the "3" position, which provided agitation o
and shear of liquid at 12,400 rpm. The NaOH solution was "~
added slowly to oil during agitation. After all solution was S B >30I~
added, agitation was continued until the mixture became too I
viscous for the blender to continue mixing. The pH values of
samples were measured with a Chemcadet pH meter (Cole- (DLMENSICN aI
mm) Parmer Model J-5986-60). The pH value of 50-50% emul
sion samples was 12.6 to 12.8. The 50-50% water-in-oil FIGURE 2: Locations of Thermocouples.
emulsion was prepared initially by using the same volumes 40
of oil and aqueous NaOH solution, but the actual G 120s Sample Size: 800 ml
volumetric composition when analyzed with a 3 • 1OOs
• 80s Highest Power Setting, 700
∎ 60S W
centrifuge was found to 5 • 30s
be 46.50% water and 53.5% oil by volume. The 30-70% wa- Radiation
0
a ----------------------------------120s
30 ter-in-oil emulsion was prepared with 30% aqueous 100s
solution
0

I0 9-- 60s
∎
• .-- 30s

10 20 30 40 5
Distance from Center, mm 0
FIGURE 3: Temperature
distributions of 50-50% water-
in-oil emulsion (middle layer) at
the end of microwave radiation.
100

1o Sample Size: 800 ml

Highest Power Setting, W
700
so
U 0 0
X
•
5 X
d 60 L A
Radiation
U
50
o
w • + 260s
40
30 X 240s
CL
-0
0 c ISOs
E 0 A 120s
-0 o 1005
Experimental Results Q 20 r 0 SOS
- ∎
∎ 60s
10 • 30s

0
0 10 20 30 40 15
Distance from Center, min

v
25
and 70% motor oil by volume, however the actual Composi-
tion was 22.50% water and 77.50% oil. A drop of water
soluble ink (Pelikan brand) was added to a small amount of
the emulsion sample, approximately 5 ml, in a test tube. No
dispersion of the ink was observed. Clear water droplets were
E observed when the samples were placed under a
microscope. Therefore, the continuous phase of emulsion
was oil and the sample was indeed a water-in-oil emulsion.
Microscopic examination showed the diameter of water
droplets to be in the range of 1 to 100 µm. Most were in 10
to 40 tm range.
The glass container containing 800 ml of emulsion sample
was placed in the center of a Kenmore microwave oven and
the microwave radiation was applied at the highest power
setting. Radiation time varied from 30, 60, 80, to 120 sec-
onds, or longer. After radiation, the sample was insulated with
polyurethane form and removed from the oven. Nine ther-
mocouples were inserted in the sample quickly, and the com-
puter immediately recorded the temperatures. The amount of
water separated and settled to the bottom of the container by
gravity was monitored and measured every five or ten min-
utes.
Similar temperature measurements were conducted using
distilled water. The results served as reference points for the
emulsion experiments.

Experimental results from temperature and volume in-oil emulsions is plotted against time, showing
measurements include the following: (1) temperature temperature histograms of irradiated samples at the
distributions, (2) temperature histograms, (3) No. 2 location, which is 2.5 cm from the center of the
volume rates of microwave heat generation, and (4) glass container.
separation of water from emulsion. The first three
items are presented here, while the last item is
presented in the next section.

(1) Temperature Distributions. Nine temperature

readings were obtained for each run, showing
temperature distributions for the top, middle and
bottom layers. Figures 3 and 4 show rapid
temperature rises at three locations of the middle
layer of 50-50% and 30-70% water-in-oil emulsions,
respectively, after 30, 60, 80, 100 and 120 seconds
of radiation. Similar temperature distributions were
obtained for the top and bottom layers of the same
sample.
For viscous water-in-oil emulsions, the motion of
emulsions in the horizontal direction is slow.
Therefore, horizontal-temperature distributions in
Figures 3 and 4 show that water-in-oil emulsions
were heated uniformly through the
FIGURE 4: Temperature distributions of
30-70% water-in-oil emulsion (middle
layer) at the end of microwave radiation.

body of emulsion by microwaves. This was expected,

since the dielectric loss of oil is small. The small
decline of temperature near the container wall may
be caused by the heat loss to the surrounding
atmosphere.

(2) Temperature Histograms. In Figures 5 and 6 the

temperature increase of 50-50% and 30-70% water-
 The rates of increase in temperature of irradiated
samples are shown in Table 1. These samples include
distilled water, SAE motor oil, 50-50% and 30-70%
water-in-oil emulsions. The bulk temperature of
emulsions were obtained from the average values of
nine local temperature readings. The rate of
temperature increase was calculated from
temperature increase divided by radiation time. It is
interesting to observe that the rates of temperature
increase of emulsions were not between the rates
for water and oil. The average rates of temperature hA ea A , \ ddt
increase of 50-50% and 30-70% water-in-oil T
(T-T~)+
q MW = [(T+273.16) -(Ta+273.16)'] +PCB
emulsions are 0.24 and 0.31 °C/sec, respectively. V V

The rates appear to decrease at higher temperatures.

This is believed to be the result of the decreasing
dielectric loss of water. The heat loss to the
100
2-T 2 -
M 2 -
B
80

60
Calculated
Values
40
(3) Rate of Heat Generation. The volume rate of
Sample size: 800
20 0p /W/ Location: No. 2
ml heat generation is of great interest, since it is not only
an important term in the energy balance equation, but
also a term connecting the temperature increase and
0 50 100 150 200 250 300
Time of Radiation, t, sec the dielectric property of irradiated emulsion. Based
on the assumption that the rate of heat transfer from
FIGURE 5: Temperature emulsified water droplets to the surrounding oil is so
increase of 50-50% water-in- fast that water and oil practically have the same
oil emulsion. temperature, the lumped-capacity energy balance
10 produces the following energy-balance equation:
0 surrounding is not a strong factor for this
phenomenon, based on the heat convection and The first, second and third terms in the right-
radiation calculations. hand side of Equation (1) represent, respectively,
the heat loss by convective heat transfer to the (1
surrounding air, radiative heat loss from the wall
surface, and heat accumulation in the emulsion. The
contributions of the first and second terms are much
smaller than that of the third term. The heat generated
by the glass container is assumed to be negligible,
because of its small mass and low dielectric constant.
In applying Equation (1) to the volume rate of heat
0
250 30
generation, gMW, the density (p) and heat capacity (CP)
0 50 100 150 200
Time of Radiation, t, sec
0 of emulsions are calculated by the following simple
mixing rules:
FIGURE 6: Temperature
increase of 30-70% water-in-
oil emulsion.

49
 Pm =PWO+PO(l-0) (2)

C p,m -Cp,,o+Cp,O(1-0) (3
The volume rate of microwave heat generation of )
water, motor oil and emulsions calculated from the
temperature measurements and Equation (1) are
shown in the fourth column of Table 1. They are
considered as experimental values of the volume rate
of heat generation.

Separation of Emulsion

Temperature

The objective of heating viscous water-in-oil

emulsions with microwave radiation is to separate
water from oil. The separation involves two
processes: coalescence of emulsified water
droplets and sedimentation of coalesced water drop-
lets. Both processes are affected by temperature.
The rate of water separation in sedimentation
depends on the settling velocity of water droplets in
the emulsion. If the concentration of water droplets is
low, droplets move without interaction with others
and their settling velocity is given by Stoke's law
[Bird, et al., 19601. Otherwise, the hindered
settling velocity is given by the Richardson-Zaki
correlation
 TABLE 1
Experimental Results of Microwave Heating

Radiation Time, Temp Rate of Temp. Volume Rate of

t,sec Increase Increase Heat Generation
AT, °C dT/dt, °C/s qMW, cal/s.cm'

Water
30 4.7 0.157 0.156
60 10.0 0.167 0.167
120 20.4 0.170 0.170

180 30.7 0.171 0.171

240 39.7 0.165 0.166
300 48.1 0.160 0.162

360 56.8 0.158 0.159

SAE Motor Oil

30 1.0 0.033 0.0136
60 2.6 0.060 0.0246
90 4.4 0.0489 0.0201

120 6.6 0.055 0.0227

150 10.2 0.068 0.0282

Water-in-Oil Emulsion (50% water, 50% oil) 0.216 0.151

30 6.49 0.261 0.183
60 15.6 0.235 0.165
80 18.8
0.265 0.186
100 0.229 0.161
26.5
120 27.5

0.364 0.212
Water-in-Oil Emulsion (30% water, 70% oil) 0.320 0.186
30 10.9 0.319 0.186
60 19.2
80 25.5 0.307 0.180
0.306 0.179
too 30.7 0.293 0.173
120 36.7
180 52.7 0.289 0.172
0.287 0.171
240 69.5 0.264 0.158
260 74.7
300 79.2

50 Journal of Microwave Power and Electromagnetic Energy Vol. 30 No. 1,

1995
 Properties

[Probstein, 1989]. In both cases the settling velocity The rate of heat generated from microwave radiation
is proportional to the density difference, square of depends upon physical and dielectric properties, and
droplet diameter, and the reciprocal of oil viscosity. may be predicted from electromagnetic field theory
The viscosity of oil is very sensitive to [Johnk, 1975; Decareau, 1985; Osepchuk, 1984;
temperature, much more than density difference. Decareau and Peterson, 1986]. There are three
Therefore, as temperature increases, viscosity dielectric properties involved in microwave heat
decreases much faster than the density difference.
The results are a higher settling velocity and faster
separation of emulsified water from oil. 100.0
According to Osipow [ 1977], the rate of
90.0
(4) Radiation
Rate = Ale-8, i 80.0 n 120s
70.0 o loos
RT o
w 80s
80s
coalescence is given by: 80.0 • 30s

As temperature increases, the rate of coalescence 50.0

increases. The diameter of water droplets plays an 40.0

important role, since the settling velocity depends on 30.0

a-------------------------------------------a
the square of diameter, as indicated above. o'°
/
o 0
100.0
20.0 1

Experimental Data of Separation /

90.0 0 0
0.0
80.0
0 10 20 -
A •-30•-* • • 40 50A e0
70.0
Time of Sedimentation, ts, min.
The results of separation of 50-50% and 30-70% 60.0
water-in-oil emulsions are shown, respectively, in 50.0 FIGURE 7:
Figures 7 and 8, where the percent of water Separation
separation is plotted against the time of 40.0
Radiation
sedimentation, i . The water separation in percent was
s 30.0
calculated from volume measurements as follows: 20.0/ / 0300S
A
10.0 Inr ~" 270s
0260S
• 250s
Water Separation, % = x 100%
V (5) 0.0
0
∎ 240s
5 100 150
0
0

In Figure 7, 120 seconds of microwave radiation of water from 50-

provided a significant improvement in separation of 50% water-in-oil emulsion after
50-50% emulsion over that of 30 second radiation. It microwave radiation.
took a little more radiation for 30-70% emulsion to
produce separation, according to the results shown in
Figure 8. In both cases the separation was made Time of Sedimentation, t , min. s

possible by microwave radiation. The rate of

separation increased when more microwave radiation
was applied, as shown in Figures 7 and 8. However,
i too much radiation was found to cause turbulence in
emulsion and reverse the separation process.
Experiments shown in Figures 7 and 8 were
discontinued at the onset of turbulence.
FIGURE 8: Separation of water from
30-70% water-in-oil emulsion after
microwave radiation.
ing. They are dielectric constant, dielectric loss and
loss tangent. Loss tangent is the ratio of dielectric

Theory of Microwave = 85.215 - 0.33583T (6)

Heating Dielectric = 320.658T-10268 (7)

constant to dielectric loss. Dielectric properties of

5
1
various liquids have been reported by von Hippel
[1954], Weast [19681, Tinga and Nelson [1973],
Singh and Sinha [1985], Singh et al. [1986], Ritzoulis
et al. [1986], Smyth [ 1977], Mudgett et al. [ 1974],
and Mudgett [1982].
Dielectric constant and dielectric loss of water
used in this work are given by the following two
equations:
which are the least-fit equations of the data given
by von Hippel [ 1954]. Temperature T is in °C.
Dielectric properties of various petroleum oils
also were given by von Hippel. Based on his data, the
dielectric constant and loss tangent of motor oil
used in this work were estimated and expressed in
the following equations:
c ° = 2.24 - 0.000727T (8)
tan S° = (0.527T + 4.82) x 10-4 (9)
Attenuation Factor
The Beer-Lambert's equation [Atkins, 1986] in
physical chemistry states that the loss of
electromagnetic energy, including microwaves, is
proportional to the energy intensity and pathlength.
This equation will be used to calculate the rate of heat
generation by microwave radiation. Considering that
the lost microwave energy is converted to thermal
energy (heat), the volume rate of heat generation is
given by the following equation:
tag
gMw,z4.184
= (z) h
where the local microwave flux, P(z), is given by the where the pathlength z is equal to R-r, and the
integrated form of the Beer-Lambert's equation; that quantity inside the brackets is the local microwave
is: flux at the location r. The remaining microwaves
continue to propagate the
P(z) = P(°)e-2,,z
The combination of Equations (10) and (11) gives
the local volume rate of heat generation in terms of
incoming microwave flux P(o) and the attenuation
factor of the emulsion.
The attenuation factor can be calculated from
the following equation given by the electromagnetic
field theory [von Hippel, 1954]:
ing to von Hippel [ 1954], the dielectric constant and
1/2
2itf \
ag= C°C (VI +tan2S-1I
(12)
The attenuation factor of water varies from 0.465
cm- I at 15°C to 0.085 cm -1 at 95°C. Therefore, under
52 Journal of Microwave Power and Electromagnetic
Energy
loss tangent of petroleum oils are in the ranges of 2.0
to 2.2 and 0.001 to .005, respectively. Therefore, the
following equations were developed to include the
case where microwaves may go through the entire
thickness of emulsion sample. If microwaves go
through the water-in-oil emulsion, they should reach
the other side of microwave cavity, and be reflected
back into the emulsion as shown in Figure 9. This
process of microwave propagation is repeated many
times until the radiation is discontinued. If the
emulsion is in a cylindrical glass container with its
top and bottom ends covered with aluminum foil and
the container is placed in the center of the micro-
wave oven, the volume rate of microwave heat
generation can be developed as follows. As a first
approximation, considering that microwaves
propagate only in the radial direction, in the first
forward pass of microwaves, the pathlength of
microwaves before reaching the element under
consideration is R-r (z=R-r). The volume rate of heat
generation produced by this first forward pass of
microwaves in the element is given by Equation (10)
as follows:
tag [P e-2 a F _ ( R -T)1
4.184 1R
Inner Surface of Microwave Oven
FIGURE 9: Multiple pass
propagation and absorption of
microwaves within emulsion.
Vol. 30 No. 1,
1995
the same intensity of microwave power, water generates
less heat at higher temperatures.

Volume Rate of Heat Generation

Since the continuous phase of water-in-oil emulsion is
oil, which has a low dielectric constant and a low
dielectric loss factor, it is relatively "transparent" to
microwaves. Accord
pathlength of r + R inside the emulsion to reach the
cavity wall. After the reflection by the wall,
microwaves travel the additional pathlength of r + R
to return to the element. Therefore, the returning
microwave power reaching the element is attenuated
by the pathlength of r + R + R + r. The volume rate
of heat generated by the first backward pass of
microwaves in the element is:
2
C CE {PRe-2aF(R-r)e-2at(r+R+R+r)
4.18 4
which gives qMw to be used in Equation (1).
The volume rates of heat generation of water and
motor oil were calculated from Equations (12) and
(17), using the dielectric properties of water and oil
given by Equations (4) through (7). The results of the
calculations are shown in Table 2. The calculated
volume rates of heat generation of water are 10.9%
to 41.1 % lower than the corresponding experimental
values. The literature values of dielectric properties of
water

Similarly, the volume rates of heat generated by

the subsequent forward and reflected passes of
microwaves can be obtained. The combined volume
rate of heat generated by the i-th forward and
reflected passes is:

2a.E -2aF[R+4(i-1)R-rj + PRe -2aF[3R+4(i-

1)R+r]
gMw,i = 4.184 j PRe

(15)

The microwave intensity decreases each time

microwaves pass the element. The summation of gMw.I
given in Equation (15) over the total number of passes
gives the volume rate of heat generation for the
element at r.

The average volume rate of heat generation can

be obtained from the integration of the local volume
rate over the entire volume of emulsion. That is:

rR (17)
qMW= 1 nR2H J° 27trH~
gMW,idr

i+1

where itR H is the volume of irradiated emulsion.

2

After integration,
2aE
qMW = PR________2 2 {[l+e2a,..R(2aER-1)Je-2a,:[R+4(i-1)R]
4.184 (2aER) i=1

+[1- (2(XER+ 1)e-2a,..R Je-2a,,.[3R+4('-')R]l

5
3
at temperatures higher than the room temperature may The calculated volume rates of heat generation of
be too low. Table 2 shows that values of dielectric 50-50% and 30-70% water-in-oil emulsions are
properties of motor oil estimated from the information shown in the fourth column of Table 3. The
given in the literature are also too low. deviations of the calculated values from the
corresponding experimental values vary from -5.96%
Temperature Increase

The ability to predict the temperature increase of

irradiated emulsions is of great interest in the design
and operation of microwave heating and separation
processes. Equation (1) shows that it can be achieved
if the volume rate of heat generation is known. After
converting Equation (1) to a difference equation, the
temperature rise at a given location per unit time is
given as follows:

AT _ qMw hA
At C PP (T; - T,
Pp PpV

(18)
e (TA [(T1 + 273.2)' - (T. + 273.2)'
]
vp

where AT is Ti J+I - T, ,j and AT/At is the approximate

value
of dT/dt, which is the rate of temperature increase in
°C/s. From the rate of increase and the initial
temperature, the temperature increase, AT, is
calculated from Equation (18) and shown in Figures 5
and 6. Equation (18) appears to be able to predict the
temperature increase of 50-50% water-in-oil emulsion
reasonably well in the early stage of radiation. The
deviations between the calculated and experimental
values are in the range from -2.0% to -25.7%. For 30-
70% emulsion, the deviations vary from -27.7% to
39.9%. An alternative calculation using permittivity
data [Mudgett et al., 1974] and the mixing rule
suggested by Noguchi and Maeda [ 1973] was tried.
The differences between the calculated and
experimental values were larger than these values
indicated above.
Considering that emulsion is a heterogeneous
mixture of water and oil, and heat is generated
separately in the suspended phase (water droplets)
and continuous phase (oil), Equation (17) is applied
separately for water and oil with individual
attenuation factors. The total volume rate of heat
generation of emulsion to be used in Equation (1) is
given by:

qMW =
gMW,w`Y+gMW,o0 -
0)
 TABLE 2
Volume rates of heat generation of water and motor oil by microwave radiation.
Vol. Rate of Heat Generation,
gmw ca /s cm'
, 1 .

Radiation Ave. Temp.* Experimental Calculated Deviation

a
Time T
ave, Values Values %
t, sec Eq. (17)
Water
30 25.0 0.156 0.139 -10.9
60 27.5 0.167 0.132 -21.0
120 33.1 0.170 0.120 -29.4
180 38.9 0.171 0.110 -35.7
240 43.5 0.166 0.104 -37.3
300 47.6 0.162 0.0980 -39.5

360 51.8 0.159 0.0937 -41.1

Motor Oil
30 20.6 0.0136 0.0522 284
60 23.7 0.0246 0.0522 112
90 19.4 0.0201 0.0521 159
120 23.9 0.0227 0.0521 130

150 31.1 0.0282 0.0521 84.8

(0.142 cal/s•cm ) to -31.7% (0.127 cal/s•cm ) for 50- the emulsion from the dump-site into water, oil and
3 3

50% emulsion, and -31.6% (0.108 cal/s•cm ) to solid by microwave heating. In each run, 300 grams
3

-42.5% (0.122 cal/ s•cm ) for 30-70% emulsion.

3 of this emulsion in a glass beaker were placed in
the microwave oven for 20, 30
and 80 minutes of radiation. The microwave power
Dump-Site Sludge to the cavity was calibrated against the power level
setting. Based on this calibration and the power
Thick, viscous, brown water-in-oil emulsion was levels used, microwave energy inputs to these three
collected from a dump-site of a compressor station samples were calculated to be 58.3, 69.6 and 117.1
and tested with microwave radiation. This emulsion watt-hours, respectively. After radiation, samples
is referred to as "sludge" in the field, and its physical were placed on a bench for gravity sedimentation.
appearance and property are very similar to emulsion After a few minutes on the bench, three or more
samples prepared in the laboratory. From an analysis layers of fluid began to appear in the beaker. An
using a bench-top centrifuge, the composition of this oil layer on the top and a water layer on the bottom
dump-site sludge was found to be 21.1% oil, 76.6% were observed. One or two layers of slop were
water and 2.3% solids by weight. found between water and oil layers. A portion of oil
Three experimental runs were made to separate was believed to be evaporated during irradiation.
The water layer was removed and weighed,
while other layers were fed to a filter to separate
solids. The filtrate, after a few minutes of gravity
settling, separated into two layers again: a water
layer and slop layer. Table 4 shows the amounts and
percents of each layer obtained in these experimental
runs. The separation was accomplished without using
any chemical demulsifier.
 TABLE 3
Volume rates of heat generation of emulsions by microwave radiation.

Vol. Rate of Heat Generation,

gMN„ca1/s.cm'
Radiation Time Ave. Temp.* Experimental Calculated
Values Values
t, sec T~Ve,
°C
Water-in-Oil Emulsion (50% water, 50% oil)
30 24.8 0.151 0.142
60 29.4 0.183 0.134

80 31.0 0.165 0.130

100 34.9 0.186 0.127

120 35.4 0.161 0.125

Water-in-Oil Emulsion (30% water, 70% oil)

30 27.1 0.212 0.122
60 31.2 0.186 0.117

80 34.4 0.186 0.115

100 36.9 0.180 0.113

120 40.0 0.179 0.112

180 47.9 0.173 0.110

240 56.3 0.172 0.109

260 59.0 0.171 0.108

300 61.2 0.158 0.108

The emulsion with 20 minutes microwave and oil layers. This method can be important for
radiation produced four layers: water layer (51.2%),separation of viscous and stable water-in-oil
liquid-solid mixture layer (12.8%), oil layer emulsions that are difficult to pump and mix with
(8.9%) and slop layer (12.5%). From material chemical demulsifiers. The microwave
balance, it is believed that 14.6%, mostly oil, is demulsification process was demonstrated by tests of
evaporated. The cases of 30 and 80 minute laboratory samples and field samples. Laboratory
radiation appeared to have excessive energy inputs, experiments under better controlled conditions
causing turbulence and mixing of water and oil. produced data that confirmed the field test findings.
The oil layer disappeared in these two cases. Small temperature gradients through the body of
irradiated emulsions prove that viscous water-in-oil
emulsions are heated more quickly and uniformly by
Conclusion microwaves than by conventional convective heating,
providing a faster water-oil separation.
Microwave heating provides a new option in breaking The temperature rise and volume rate of heat
waterin-oil emulsions and enhances gravity generation of emulsions induced by microwave
sedimentation to separate the emulsions into water radiation can be calculated from basic dielectric

55
properties, considering water-inoil emulsion as a
heterogeneous mixture of water and oil. The
calculated values using the data available in the
literature are approximately 30% lower than
experimental values.
 TABLE 4
Separation of dump-site sludge by microwave heating.

Run 1 Run 2 Run 3

Microwave Radiation Time, min. 20 30 80

Energy Input, w-hr 58.3 69.6 117.1
Water Layer, grams 153.7 159.6 146.2
(51.2%) (53.2%) (48.7%)
Solid Layer, grams 38.5 20.6 24.9
(12.8%) (6.9%) (8.3%)
Oil Layer, grams 26.8 0 0
(8.9%)
Emulsion Layer, grams 37.5 65.8 71.1
(12.5%) (21.9%) (23.7%)
Evaporation, grams 43.5 54.0 57.8
(14.6%) (18.0%) (19.3%)
Emulsion before Radiation, grams 300 300 300
(100%) (100%) (100%)

Notatio increment in radiation time,

n convective heat transfer area, tj+l - tj, sec. or min.
cm 2 loss tangent
A tans time of settling, min.
A1 constant constant
is volume of irradiated
B1 heat capacity at constant
V emulsion, Equation (1), cm3
Cp pressure, cal/g•°C 3
• volume of water separated, cm
c speed of light, cm/s Vo
• frequency of incident microwaves z
= initial volume of water in emulsion,
fo cm3
• height of container, cm
H • path length of microwave
h • convective heat transfer coefficient, Greek
cal/s•cm2•°C Letters
• microwave power flux at z = 0, aE = electromagnetic attenuation factor,
P(0)
P(z) watts/cm 2 S cm-1
• local time-average microwave power E • loss angle
PR flux, watts/cm2 = emissivity of surface
.
Er
time-average microwave power flux = relative permittivity (dielectric
at the surface of container, watts/cm2 Er" constant) = dielectric loss
qM
• average volume rate of heat P = density of emulsion, g/cm3
W 6
generation induced by microwaves, • Stefan-Boltzmann constant
gMW,r or z cal/s•cm3 local volume rate of heat
= volume fraction of emulsified water
=R generation,
cal/s•cm3
r radius of sample = the i-th step of computations in the
T container, cm
Ta radial
j= the j-th step of computation for radiation
Tav time m = mixture or emulsion o = oil
e w = water
AT
t
 Subscripts
• gas constant in Equation (4)
• radial coordinate, cm i temperature of emulsion, °C
ambient temperature, °C average temperature, °C
• temperature increase, °C
• time, sec. or min.
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