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ORNLCOPY
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1623 9
-’
I
TESTS OF VARIOUS PARTICLE FILTERS FOR REMOVAL~OF OIL MISTS AND BYDROCARBONVAPOR i
B, F, Hitch,
R. G. gross, Ii. F: McDuffie
ABSTRACT '."' Various filter and adsorbent materials were examined for .'*e possible use in the removal of oil mists and hydrocarbon vapors; A controlled flow of oil was injected into a heated nickel reaction Helium Vessel to cause vaporizationand some cracking of the oil. ~flowing through the reactionvessel carried the oil mist .and hydroFilter effectiveness was 'carbon-vapor through a filter system. determined by the use of a Perkin-Elmer Hydrocarbon Detector, ._, and gas--chromatographic analysis-~ Good gravimetric analysis, removal of mists was achieved by the use of a combination of felted metal fibers and ceramic fibers-in a configuration proposed c for use in the MSRE. Granulated charcoal removed hydrocarbon manner consistent with the established vapors (C, and above)ina adsorption isotherms for this material. j tEGA1 NOTICE t
NOTICL ! /
-a. Ih~s to
,
_ con -tains information documenr I-?-*--ror ~n~wllal use at the Oak revisio #n or correction and therefore
prima,ily
of a preliminary nature and Ridge National Laboratory. does not represent a final
! !
was prepared It is subject report.
i
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report
was prepared
as an accost
of Government
nor the Commission, nor any person acting A. Makes any warranty 01 representation. completeness, w any information, privately B. As
usefulness
of the
apparatus. owned rights; or
method,
NOTICE sponsored
work.
on behalf of the Commission: expressed or implied, with information or process
contained disclosed
in this in
this
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to the accuracy,
report,
or that
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may
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use of
not infringe
Assumes any liabilities with respect to the use of, or for damages resulting from the use of any information, apparatus, method. or process disclosed in this report. used in the above, “person acting on behalf of the Commission*’ includes any employee or
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to the extent
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such employee
disseminates, or the Commission,
CONTENTS Page ABSTRACT.
. . . . . . .
. . . . . . . . .
1.
INTRODUCTION.
. . . . . . . .
2.
PROCEDURE . . .- . . . . . . . . . . .
3.
OIL
MIST FILTERS.
. . . .
Description
. .
. . . . . .
1 4
. .
4
. . . . . .
7
3.1.
General
. . . . . .
3.2.
Experimental
Data
3.3.
Experimental Oil Injection
Data After Altering . . . . . . . . . . .
. . . .
. .
7
. . . . .
7
2
4.
CHARCOAL TRAP EFFICIENCY.
; . . . .
4.1.
with
4.2, 5.
6.
Charcoal
Saturation
. . .
Hydrocarbons
13
Temperature Dependence of Hydroi ‘carbon Adsorption on Charcoal . . .
TESTING
OF MSRE PARTICLE Drop
Data.
FILTER'.
5.1..
Pressure
5.2,
Pressure Drop Data of Felt at.Elevated Temperatures.
ACKNOWLEDGEMENTS. s c. . .
. .
. . . .
. . . '. .
.
Metal . .
. .
23
. . . . . .
. .
25
l
r
,
4
_-. w; :
1. ' INTRODUCTION
3 One of the problems of power operation that
of the Molten
some valves
plugged.
encountered
and filters
The plugs
during
Salt
the early
Reactor
in the off-gas
were analyzed
stages
Experiment
was
system became-
and found
to be of organic
composition. One possible
source
of organic
to lubricate
the salt
circulating
were leaking
oil
the pump bowl,
leakage
filter
experiment
was.designed
maximum expected and adsorbent
hydrocarbon
oil
materials
vapors
A complete
under
flow
to simulate
for
these
removal
Gulfspin-
is used to lubricate
was injected tube
same oil by a motor
to a heated
was 0,.67 cc,per Simulating
passed through vessel
is shown in'
the Molten
Salt
was used in our experiments. driven
syringe
reaction
vessel.
connected
I‘
The
by-a
The injection
hour.
MSRE off-gas
flow
conditions,
the system at 4 liters temperature
The gas effluent
and
PROCEDURE
la.
pump; this
mist
conditions.
as Fig.
oil
the consequences
of oil
1 and a picture
reaction
the pump
and to testvarious
of the apparatus
capillary rate
indeed
diagram
Reactor oil
If
the maximum credible
leakage
-2.
Fig.
pump-.
used
would be in the range of 15 to 20 cc per day.
This of this
into
was the oil
material
was about
from the filters
helium
per minute.
was ' The nickel
600°C. A, D, C, D, and E
.
ORNL DWg. 66-9447 i
Fig.
1.
Oil
Injection
and Filtering
s-2
Apparatus
“” __ .
1””
.
.
.”
.
._~...
-
..I.
_
..-..
..-----
.
.
..._.“.
b
_.I..t
Fig.
la.
Picture
of Oil
Injection
and Filtering
Apparatus
/ ’
7 passed through
two,,charcoal traps filled with PCB 6X16 P... / I A Perkin-Elmer 213 Hydrocarbon Detector, provided
charcoal:.
by the Analytical hydrocarbon the flow
Chemistry
Division,
was used to measure the
at three
positions
(S-l,
levels
diagram.
same three
Gas samples were taken
positions
Pressure manometers.
for
drop measurements Readings
filter Materials wool,
tested
into which
General
to those
Supreme #00 steel line
nickel
wool,
Ultra
Pyrex
showed an appreciable
the glass
U-tube
tightly
'However,
long fiber 3.2.
coarse
easily
wool,
Supreme #l steel
glass
wool,
of 8 psig, Fiberfrax\
two experiments
wool in trap
B and C.
The data
of
obtainable.
pressure
Experimental
nickel
assembly
the investigation
Fiberfrax
drop when packed
This was the short \ when loading the traps.
tested.
The first
hour.
traps.
drop was. in excess
3.2.1.
Hg and'H,O
Filter.
Fiberfrax
packed very
analysis.
Description
confined
pressure
traps
each half
that
were coarse
and a M-S-A air
at these
chromatographic
necessitated
materials'be
shown on
OIL MIST FILTERS
3.1. time
S-3)
periodically
were made using
were taken 3.
Limited
subsequent
S-2,
this
fiber
material
proved
removed 55% of the total
was not
Data were ,performed
iniTable oil
Because the
to be satisfactory.
A, and Supreme ,#l steel summarized
variety
injected
using wool in
1 show this into
:
the
trap
Table 1.
";;"
E"-;
1,2
6
Efficiency
of Filter.Materials
Tested
Trap B Filter wt. of Oil Removed Material
Trap C Filter wt. of Oil Material Removed
Coarse Ni wool (1)
0.690
0.878
#I Supreme steel wool
0.501
2.069
3.740
55
1.735
#l Supreme steel wool (2) #OO Supreme steel wool
3.428
*OO Supreme 0.749 steel wool
5.912
7.410
80
3
13
Coarse Ni wool
4
18
5*
23.5
6A*
22.6
6B*
31.6
71
88
Coarse Ni 3.749 Pyrex glass 5.440 wool wool #00 Supreme 5.341 Pyrex glass 3.792 steel wool wool #00 Supreme 4.929 Pyrex glass 4.188 steel wool wool Pyrex glass 5.374 X00 Supreme 6.892 steel wool wool Trap A, B, and C replaced by MSAUltra Filter 7930 cartridge
Total Oil Removed (d
Total Oil Injected (B)
w-w--
Trap A Filter wt. of Oil Material Removed
Per Cent of Oil Trapped
(3)
*These runs (1) Surface (2) Surface (3) Surface
were area area area
made with of 0.016 of 0.032 of 0.047
011 being injected into square meters per gram. square meters per gram. square meters per gram.
Pyrex wool Pyrex wool Pyrex woo1 Pyrex wool using
glass
0.000
9.189
10.090
91
glass
0.278
9.411
13.400
70
glass
0.123
9.240
12.882
72
glass
0.001
12.267
18.012
68
47.486
50.160
95
47.486
co r’
I
dip-leg.
-.
, -.
I
\
.
.
, , c I
) 0
T
.
.h
\ %b
‘9
* reaction the oil
'z
However,
vessel.
was probably
3.2.2.
A.
steel
Eighty
wool.
removed with
and Pyrex
perc,ent
duration trap
3.2.4.
with oil
of
lines.
the same coarse
nickel
Supreme #00
injected
nickel
was
ones,
Ninety-one
per cent
C.
trap
wool in trap
Although
B and C.
than previous
The following
retained
1 through
a portion
of exit
of the total
wool in traps
was removed by this
oil
#3 utilized
traps. .* Experiment #4 used coarse
was found'in
\
up on the walls
Traps 3 and C were filled
glass
of greater
few runs
these
3.2.3.
6
held
Experiment
wool in trap
in the first
this
no increase of the oil
A
run was in weight injected
assembly. summary indicates
per gram of filter
material
the amount of
used in experiments
4.
r; Trap A
Trap B
Trap C
1 and 2
,020
. 066
.048
3
. .049
.244
. 078
4
.106
.754
Expt.
3.3.
#
Experimental
To obtain vessel‘was
better
altered.
Data After cracking,
0 Altering
the oil
In experiments
Oil entry
1 through
Injection to the reaction 4 the oil
entered
p as shown on the flow diagram in Fig. 1. This entry . entered directly was changed to point P' so that the'oil
at point point into
the stream
of flowing
helium
reaction vessel. Using this method of injection, b
and down the dip-leg the hydrocarbon
of the level
at
10
the three
analysis
points
ten times
previous
levels.
had occurred carbon
Expt.
-5
Traps
for
Supreme #00 steel traps trap
B and C. .assembly.
experiments
recovery
recovery.
of these
a small
reached
runs trap
3.3.2. commercial
only
as shown in Fig.
a large
is equipped
with
It
that
of the adsorbable
with
surface. through
-
this
resulted
be noted
in each oil
mist
the efficiency line
of a
Ultra
Filter
filter
glass
element
microfibers
The cartridge which
added holder
liquids
can be
removed periodically. The M-S-A filter replacing This material
traps
assembly
was installed
in our apparatus,
A, B, and C.
filter
assembly
tested,
retaining
c c
The particulate
plug
wool in
of the oil
A M-S-A air
capturing
glass
from 68% to 72% for
should
portion
matrix
a drain
285 ppm
cracking
2 was used.
is molded of a cellulose to present
ranged
assembly.
hydro-
5, 6A, and 6B contained
C as * shown in Table 1. Experiment 7 investigated filter
*
mm
22
A, and Pyrex
More efficient
in a decreased'oil
cracking
Analysis Point S-3
.360 ppm
wool in trap Oil
n
The average
35 mw
715 ppm
; 3.03.1.
4.
Analysis ' Point S-2
75 PPrn
- 7
much less
to about
below:
Analysis Point S-l
#
and S-3 rose
1 through
are summarized
1 -4 /
S-2,
Obviously,
in experiments
levels
id
S-l,
was the most efficient 95% of' the oil
injected
filter into
the
11
Fig.
2.
'M-S-A Air
Line Ultra
Filter , ?
12 reaction
All
vessel.
in the filter
of the trapped
element,
no liquid
oil
mist
was retained
was present
inthe
cartridge
holder. 3.3.3. mist
The following
retained Expt.
per gram of filter
#
material
the grams of oil tested.
Trap A
Trap B
Trap C
5
0.319 gm
1.365
0.049 gm
6A
0.295
1.243
0.023
6B
0.412
0.925
no wt.
7
1.700
The charcoal glass
gm
:
gain
--
--
CHARCOALTRAP EFFICIENCY
4.
I.D.
summary indicates
traps
Pyrex pipe
used in ourI experiments were l-in. packed with about 12 inches of PCB
6X16 charcoal. Under reactor is expected
conditions,
to raise
the temperature
the above dimensions traps
were kept
the decay of fission
to about
of a charcoal
100째C.
at a temperature
products trap
Consequently,
of 100째C during
of
charcoal our experi-
ments. A point necessary Data for the filter
of interest
to saturate this
a known amount of charcoal
investigation
material
Charcoal
was the amount of hydrocarbons
trap
amount of charcoal.
tests
were obtained previously
#l shown in Fig. Sample points
at 100째C.
simultaneously
with
described. 1 was filled S-l,
S-2,
with
a known
and S-3 were
monitored 5:
with
the hydrocarbon
_ assumed when the hydrocarbon,level the 'level
\
at S-2 started
Figure The first
Charcoal
Saturation
3 summarizes experiment
of charcoal
approaching
The weight
trap.
6.0 grams per inch.
tion
at a total
6 inches
ppm (C!& eq.)
time
of charcoal
The hydrocarbon
level
trap
carried
of charcoal
The first
out.
to trap
was analyzed
after
of satura-
in about
and S-2 averaged
prior
was
A second test
of 30 hours.
at S-l
3 inches
evidence
reached'saturation
respectively
The 3-in.
Hydrocarbons
made use of a packed bed‘of-about
in a glass
occurred
with
the two experiments
approximately
about
was
of S-l. 4.1.
r
Saturation
detector.
with
60 hours.
700 ppm and 425
saturation. it
became saturated
i
and the results that
are shown in 'Table 2.
as the heavier
hydrocarbons
"Breakthrough"~
to the bottom. carbons before
were forced Andy after
,4.2. /
of charcoal
trap
E
ent to the trap'was
Pu
the original i
adsorbed were forced
when the Cb hydro-
3 contains
gas samples taken.
Dependence of Hydrocarbon on Charcoal
temperature
indicates
saturation.
of hydrocarbons
charcoal
hydrocarbons
occurred
Table
hydrocarbon
Temperature
Adsorption
booling
out,
data
were more strongly
the lighter
in the top of the tra$,
This
Adsorption
on the charcoal
as shown in Figs.
4and
is,a 5.
function Upon
#2 from 100°C to 25OC the helium lowered
hydrocarbon
to approximately
concentration.
efflu-
40 per cent
Cooling
of
from 100°C \
Fig.
3.
Hydrocarbon
Saturation
of Charcoal
Trap #-1
‘_
.
/
Table
2.
Hydrocarbons Adsorbed in Concentration,-Wt. ’
3-in. %
Charcdal
Trap
I
Depth In Inches
<c6
c6
’ 0.0 - 0.5
0.5
0.3
0.3
0.3
0.5 - 1.0
0.3
0.2
0.4
1.6
1.0 - 1.5.
0.3
0.3
1.4
4.0
4.5
3.1
13.6
1.5 - 2.0
0.2
0.8
4.2
j.3
0.6
0.3
9.4
2.0 - 2.5
0.3'
1.9
2.6
1.0
0.1
0.1
6.0
2.5 - 3:o
0.2
,2.3
1.1
0.3
0.0
0.0 -
3.9
3.0 - 3.5
0.4
2.7 s' 0.3
0.1
0.0
0.0
3.5
. c7
c8
c9
-1 0 2.1
'Cl 0 14.3.
17.8 17.5
16
Table 3. Analysis of Gas Samples Taken Before and After Hydrocarbon Saturation of-Charcoal Trap (ppm by Volume)
Components Methane
Before Sample Sample Pt. S-l Pt. s-2
After Sample Pt. S-l
Sample Pt. s-2
25
30
16
28
4
6
3
7
Ethylene
70
95
41
80
Propylene
33
40
20
41
Butene-1
7
12
7
12
Isobutylene
3
3
4
4
Cis-Butene-2
4
8
5
8
2-Me Butene-1
4
8
10
Pentene-2
1
2
2
5
1
3
3
4
37
1
1-
6
Ethane
Branched
Hexenes
Hexene-1 Isomeric
Hexenes.
,
a.
% P
. Fig.
4.
Hydrocarbon
Adsorption
on Charcoal
at 25OC and lbO째C ',
_ . - - .
- - - - . - â&#x20AC;&#x153; . . - .
Fig.
5.
Hydrocarbon Adsorption on Char&al 25OC, 75'C, and lOO?C.
at
I
19 to 75OC lowered returned
the concentration
to 100°C:-aif:ter
content
rose
sharply 5.
to 70%.
each cooling'cycle
then returned
with
with
shown in Fig.
of the Reactor
long fiber
6.
felt
metal
Fiberfrax.
filters
Pressure
the maximum AP after
filters
with
were saturated
oil
filter
mist.
of the
was prepared
The filter
were made to determine
using
level.
a prototype
This
Division.
of two Huyck stainless.steel filled
original
TESTING OF MSRE PARTICLE FILTER
filter
by personnel
was
the hydrocarbon
to its
Traps A, B, and C were replaced MSRE particle
When the trap
consisted and a chamber
drop measurements the felt
Measurements
metal were made
Hz0 and Hg manometers. A further
test
was performed
filters
were welded inside
in Fig.
7.
and tests
This
Iâ&#x20AC;&#x2DC;
5.1. Figure
filter
remained
constant
the felt
metal
at various Pressure
test.
filters,
but returned The felt
to its metal
drop across
former filters
pipe
inside
a tube furnace
drop data obtained 24 hours Attempts
level
to blow the oil
increasing
was returned in
less
than
were removed from
the- Fiberfrax
alone
from the
the pressure
were not'successful. rate
as shown
temperatures.
by suddenly
when the-flow
steel
metal
Drop Data
After
at 2.7 psig.
to 8 liters/min,
drop slightly,
pressure
was placed
8 shows the pressure
MSRE particle
of helium
a,stainless
assembly
were conducted
in which the felt
the flow
off rate
The AP would to 4 liters/min, 5 minutes. the system and a
was determined.
The
20
ORtTL IWO.
664451
TO
,
,-
Fig.
6.
Sketch
of MSRE Particle
Filter
Prototype
ORNL WG.
i
r
c
; LJ
Fig.
7.
*Felt Metal Filter Assembly -Used, At Elevated Temperatures -
66-9452
ORNT.,IXJO. 66-9453
Fig.
8.
AP' Ac'ross Prototype
at MSRE Particle
Filter
c
23
pressure drop was 0.012 psig and remained constant over a 20-hr period. 5.2.
Pressure Drop Data of Felt Metal at Elevated Temperatures I
A filter assembly with the coarse and fine felt metal filters welded in a stainless steel pipe was fabricated as shown in Fig. 9 . furnace.
The assembly was placed in a 5-in. tube
It was desirable to measure the AP of the felt
metal filters at/elevated temperatures, since, during reactor operations, the decay of fission products would possibly raise the temperature of the filter assembly. Measurements at various temperatures were reproducible i
as shown in Fig, 9 . 0.45
However, the maximum aP at 25OC was
psig compared with 2 . 7 psig measured in the previous
experiment.
DOP measurements conducted by the Reactor Division on the prototype of the MSRE particle filter showed it to be 99.9870
efficient.
The welded filter assembly, when tested,
was only about 9570 efficient.
Although there was no visible
evidence, cracks may have been present in the welds of the welded filter assembly.
â&#x20AC;&#x2122;
Thirty hours at 25OC were required before the felt metal filters became saturated with oil mist.
The transition to the
maximum AP required only about one or two minutes.
Upon
reaching maximum AP at room temperature, heat was applied to the filter assembly.
At a temperature of 15OoC the AP
tb
N
1
25
- i fb
decreased
sharply,
temperature
returning
was'raised
almost
to the minimum.
to 400째C and 600째C -the aP rose slightly
in each case but gave no indication AP associated uted
with
a rise
to an increasetin
of helium
the heated
the-viscosity
reaction
vessel
Upon termination
tained
0.5 grams of dry carbon;
again no liquid
for
felt
I
into
described the reaction
The vessel
no 8vidence.of
assembly
con-
any liquid
and much assistance
Division,
who supplied assisted
and .analyzed
of-the
of many days was made possible
the evening
assignment and night
us with
many samples
by~~the gas chromatographic operation
was
and A. D.
gas analyzer,
of the results,
their
cut apart;
C. M:Boyd,
Chemistry
the hydrocarbon
through
was also
were found.
A.~ S. Meyer,
Continuous
data during
was injected
ACKNOWLEDGEMENTS
of the Analyt>cal
of gas and charcoal
section
oil
inspection.
cooperation
from Messrs.
the interpretation
-. t-u
and at 600째C is 405
the previously
filter
hydrocarbons
Excellent
and installed
period
visual
metal
6.
~6.2.
be,attrib-
was found.
The welded
6.1.
in
The viscosity
of the experiments
was cut apart
Horton,
of helium.
during
vessel
hydrocarbons
can probably
of 230 grams of Gulfspin-
experiments.
a.
in temperature
The rise
\
A total
received
of plugging.
at 25OC is 180 micropoises,
micropoises.
When the
procedure,
apparatus
over the
by the MSRE operations
of personnel shifts,
for
taking
6.3. with gation
The close
D. Scott,.
Jr.,
in directions
of fi.lters
cooperation
and frequent
were invaluable
in guiding
which were bseful
to the MSRE off-gas
for
bl(..-
discussions
â&#x20AC;&#x2DC;r
the investi-
the application
syetem.
I
27
%.
i "
\
t
DISTRIBUTION
\ 3 .
!
/
1. 2. 3. 4. 5: 6. 7, 8. 9. 10. 11. 12. 13-18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29; 30. 31. 32, 33. 34-35. 36. 37-39. 40. 41,
.
G. M; Adamson C. F. Baes, Jr. ' S. E. Beall E. S. Bettis F. F. Blankenship E. G. Bohlmann C. M. Boyd R. B. Briggs w. Il. Cook W. R. Grimes A. G. Grindell P. N. Haubenreich B. F, Hitch A. D. Horton P. R. Kasten S. S. Kirslis R. B. Lindauer H. G. MacPherson H. F. McDuffie A. S. Meyer, Jr. R. L. Moore R. J. Ross D. Scott, Jr. A. N. Smith P. G. Smith J. R. Tallackson R. E. Thoma M. E. Whatley Central Research Library Document Reference Section Laboratory Records Laboratory Records, ORNL R.C. ORNL Patent Office
28
DISTRIHJTIOIV .
42. 43-57.
Research aid Development Div., DTIE, OR
OR