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NATIONAL operated

UNION

CARBIDE

AiOMlC .c’sz:I

by

CORPORATION

for

U.f.

HELP

LABORATORY

the

ENERGY

COMfilSSlON

pBy-?S

ORNLCOPY

TMNO.

-

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

LEGAL This

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

Neither

the

respect

United

States,

to the accuracy,

report,

or that

report

may

the

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

contractor

of the

Commission,

or

l mplo~a

of such

contractor,

to the extent

that

or contractor of the Commission, OT l mployee of such contractor pwpares, provides ~cc.ss to, any information pursuant to his employment 01 contract with or his l mploynunt with such conhixtor.

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


ORNL-TM-1623