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Патент USA US2410633

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NOV- 5» 1946-
T. B. COUNSELMAN
2,410,633
TREATING RUBBER SUSPENSIONS
Filed Nov. 4, 1943
2 Sheets-Sheet 1
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‘THEODORE acouusemm,
BY
_
,
_
WW
ATTORNEY
Patented Nov. 5, 1946
2,410,633
UNITED STATES PATENT’ OFFICE
2,410,633
TREATING RUBBER SUSPENSIONS
Theodore B. Counselman, Evanston, Ill., assignor
to The Dorr Company, New York, N. Y., a cor
poration of Delaware
Application November 4, 1943, Serial No. 508,920
11 Claims. (Cl. 260-865)
1
2
In the manufacture of synthetic or arti?cial
rubber there is produced, for example from buta
diene and styrene as basic materials, that which
is known as synthetic or arti?cial latex and which
is therefore often referred to as latex because of
this having a milky appearance resembling nat
ural latex. In the process of producing synthetic
words, while by known methods one may assem
ble and separate from the coagulum the coarser ’
of the synthetic rubber particles; nevertheless dif
iiculty is experienced when one attempts to re
cover the synthetic ?nes of that character where- ~
by they tend to continue in suspension in the
serum and resist removal therefrom.
For effecting a method of removing said co
rubber such synthetic latex is co-polymerized
whereby thereis produced a liquid-solids mix
polymer ?nes, some of which may approach col
ture or suspension, herein referred to as-coagulum 10 loidal conditions or which because of the physical
and which comprises serum or brine as a major
form or condition thereof refuse to respond by
liquid component thereof and synthetic rubber
known process to effective separation from the
solids, crumbs or curds, of varying sizes and here
liquid bearing the same, special treatments are
in collectively referred to as synthetic or arti?cial
required or are preferably resorted to. In order
rubber crumbs or which are more de?nitely re 15 to overcome this di?lculty or apathy respecting
ferred to herein as butadiene styrene co-poly
these ?nes and to assure the effective separation
mers or crumbs. This coagulum therefore com
thereof from the liquid bearing the same, this
prises that which may be viewed as a liquid frac
invention includes the employment of a process
tion of mother liquor on the one hand and a mass
wherein there is realized a ?otation of the ?nes
of such suspended synthetic rubber crumbs on the 20 by exposing the surface of a liquid-solids mixture
other which have occasioned and developed in
bearing the same, as for example the coagulum,
the mother liquor during a suitable reaction
to an overlying gaseous medium maintained at
treatment carried out for realizing the sought for
pressures substantially lower than that of the out
synthetic latex. Some of these crumbs are rela
side atmosphere. Under the in?uence or effect
tively large but there is a certain quantity thereof 25 of the vacuum or sub-atmospheric pressure con
which is extremely small or ?ne ranging down to
ditions of the overlying gaseous medium the ?nes
quasi-colloidal or colloidal size particles.
will rise to the surface of the liquid in a manner
The larger sizes of the crumbs resemble curds
favorable to their ready removal from the surface
of cottage cheese and are of a size up to one-half
of the liquid bearing the same, to wit, as ?oated
inch in diameter. When the coagulum in which 30 material or scum.
‘
said crumbs exist is exposed to normal atmos
In the mother liquor or briny serum, there is
pheric pressure and is relatively quiescent, the ‘
larger co-polymer crumbs rise to the upper por
tions of the serum or mother liquor in which they
were developed, this because the speci?c gravity ‘
thereof is less than that of the brine or serum
often contained soap or fatty matter of a char
acter,that tends to adhere to and continue~w~ith
the yielded solids, as for example, upon the
crumbs even after they have been separated from
the mother liquor. Another aspect of this inven
of the mother liquor in which they are thus
tion is the devising of an effective and efficient
found, but under the indicated state of facts the
manner for separating the synthetic rubber from
smaller size particles or synthetic rubber ?nes or
the liquid fraction or serum of the coagulum and
co-polymers do not readily and quickly rise with 40 it is particularly concerned with the effective
in the serum or mother liquor, neither do they
separation of synthetic rubber crumbs from a
readily and quickly settle within the mother
liquid fraction in which they are yielded or in
liquor in which they are yielded. In fact, much
which they are found.
of said ?nes rather than tending to either rise
A main feature and aspect of the invention re
or settle within the serum tend to remain as rel
volves about a process and system for effecting‘
atively dormant suspensions in the liquid after
an efficient and ready separation of the synthet
the manner of colloidal particles suspended in
ically produced rubber solids and particularly of
the liquid and which continue to remain in sus
such co-polymer crumbs from their mother
pension therein.
liquor.
In fact, the ?ner synthetic rubber particles or
?ner co-polymer grains have a decided tendency
The invention has in view the obtaining of such
synthetically produced solids and particularly
to continue in suspension, to wit, in a manner
according to which they may be referred to as.
such solids as are in the form of crumbs in washed
condition, as for example, in condition in which
they have been freed (a) of substance such as
In other 55 soap Q1: fatty acids and which tend to adhere
solids more or less in colloidal suspension, or as
solids in quasi-colloidal suspension.
'
2,410,838
3
4
thereto or remain therewith, or (b) of some of
the process liquor or brine which would otherwise
remain in the interstices of or on the surface of
objectionable mass it the wash water were other
the crumbs.
wise passed directly to the waste. They would
also constitute a substantial loss in quantity of
synthetic rubber if not recovered and an impor
tant aspect of this invention revolves about the
obtaining, recovering or collecting of the lines
‘
‘The invention hereof is illustrated and de
scribed in connection with the subjecting to a
1 passing with the eiiiuent leaving the separated
solids-removal treatment of a liquid having sus
out larger rubber crumbs.
Another aspect of the invention revolves about
the passing of the rubber ?nes recovered from the
e?luent liquid either back to a preceding portion
pended therein synthetic rubber solids or crumbs,
which suspension or mixture‘containing said syn
thetic rubber crumbs has been realized in a proc
ess according to which such crumbs are produced
from co-polyinerization of certain starting ma
of the process or even to a subsequent portion of
terial that comprehends butadiene and styrene
the process wherein they are made available for
increasing the e?iciency of the rubber yield of
as basic products therefor.
It will be pointed out that the invention hereof 15 the plant.
It has been ascertained that when a body of
is directed to or revolves about the removing of
liquid containing synthetic rubber curds sus
curds, crumbs, or ?nes referred to as co-poly- ,
mers developed or realized in and by a butadiene
pended therein is placed under vacuum there
styrene process from the manufacture of that
is realized a prompt rising of the curds, not only
which is referred to as synthetic rubber and which 20 a prompter rising of the larger size crumbs but
also a prompt rising of the rubber ?nes to the
surface of the liquid whereat they can be col
lected as ?oating material or scum which when
in many respects is available as a substitute for
rubber products produced from the sap or gum
obtained from the rubber plants or trees. The
invention hereof is applicable for employment in
handled in the proper manner can be removed
any such process wherein there is realized a 25 from the liquid along one path while clari?ed
liquid-solids mixture embodying such curds,
crumbs, or ?nes synthetically produced by poly
eiiiuent freed of suspended rubber solids can be
passed along another.
merization and'which are to be separated from
The steps just referred to are best carried out
the liquid fraction of the mixture in which they
(a) by establishing and maintaining a body of
were developed or realized.
/
In order to separate the resulting polymerized
synthetically ‘produced rubber solids from such
liquid-solids mixture, there have been proposed
or employed devices such as vacuum filters or
shaking screening mechanisms. Where a vac
uum ?lter is used the solids are collected as a
layer or sheet on the ?ltering medium. The ?l
tering medium may be a. woven wire mesh or
screen or a ?lter cloth, or the equivalent on the
30 liquid within a- con?ning tank so that the surface
of the liquid is constantly exposed to subatmos
pheric pressure conditions of overlying air or gas;
(1)) by continually feeding to such established
body a liquid-rubber mixture containing syn
35 thetic rubber curds in suspension therein; (0)
by continually collecting and removing as ?oat
material from the surface of said body the rub
ber solids rising to the surface thereof and de
livering the collected solids from the tank or
peripheral portion of a rotating drum.
40 container along one path at the same time avoid
The ?ltrate or eilluent leaving the layer or sheet '
ing entrance of outside air into the tank; (11) by
and passing through such medium or screen con
passing clari?ed liquid from a lower portion of
the body, namely, liquid freed of the rubber solids
tains to some extent ?nes which continue with
and which is delivered along a pathway leading
the ?ltrate or eilluent passing from the left-be
from the tank while at the same time avoiding
hind or separated-out rubber crumbs. This ?l
trate if derived from a coagulum is that liquid
entrance of air into the tank; and (e) by remov
ing, according to operative requirements, air or
fraction which has heretofore been referred to
gaseous medium tending to collect within the
as serum, it may be relatively strong or rich in
tank above the body whereby proper sub-atmos
certain desired chemical content and it will con
pheric conditions at the surface of the body will
tain some rubber ?nes which pass therewith from
be constantly maintained.
left-behind rubber crumbs. This ?ltrate or serum
There are diagrammatically illustrated in the
which may be undiluted or‘ which may be only
a minor dilution may be passed to a preceding
portion of the process whereat the serum with
accompanying drawings systems for removing
or re-treatment in the process.
Where one desires to obtain crumbs which had
synthetic rubber solids from a liquid-solids mix
ture containing the same.
In one of said systems there is employed a
vacuum type of apparatus for separating rubber
been washed it is advisable to pass the already
crumbs of varying sizes from a coagulum or other
separated-out and substantially debrined crumbs
liquid suspension of synthetic-rubber solids.
the ?nes therein are made available for re-use '
In another of said systems, the large rubber
derived from the coaglum for a further or wash 60
solids are ?rst separated from the liquor of the
' ing operation and for a dewatering of the washed
process. which is recovered as non-diluted proc
solids. Filters, screens or other suitable appa
ess liquor or as process liquor only slightly di
ratus may be employed for this purpose and here
luted, to wit, as brine or serum herein identi?ed
again the liquid or e?luent passing from the ?l
ters, screen or other separating medium con 65 as a serum containing effluent of minor dilution.
tains ?nes washed out from the larger rubber
crumbs and which pass with the eilluent leaving
the crumbs. This wash water eiliuent contains
some of the much diluted brine and some washed
out solids and may be identi?ed as an eilluent of
major dilution. The rubber crumbs or ?nes re
moved in this manner may seem in quantity rela
tively small; however, in the aggregate they con
Afterwards these initially separated larger rubber
solids are washed and separated from the wash
water, the latter of ‘which may be identi?ed as a
serum containing eiiluent of major dilution.
The serum containing eiiluent of minor dilution
may be passed along one path leading to a prior
portion of the process, or it maybe conducted
along another path leading to a vacuum type of
stitute a considerable amount—a quantity of such
separation apparatus.
extent that they might ultimately collect as an
minor dilution carries rubber solids therewith as
This - serum e?luent of
5
2,410,688
' suspended matter and the treatment in this vac
uum‘separator is to recover the ?ner solids as
?oated material passable from the apparatus
along the one path while leaving behind a clari?ed
serum or brine which can be passed as e?iuent
from the apparatus along another path as for re
use or employment in the process as may be
deemed advisable.
The washing operation dilutes brine in the in
terstices of and remaining on the surface of the
relatively de-brined mass of solids of the initial
separation process, and the wash water e?luent
from this mass has therein a quantity of brine
6
Fig. 3 diagrammatically illustrates such a unit
inione type of environment.
Reference is now made to the drawings in de
tail. Therefrom in connection with the descrip
tion herein set forth, there will be readily appre
ciated and understood the importance and ad
vantageous employment of certain steps or op
erations realizable in and by the vacuum type of .
apparatus referred to in and for the separation
of synthetic rubber crumbs from a liquid fraction
bearing the same and particularly of the smaller
?nes thereof from a liquid fraction bearing the
same in suspension.
or serum and also as suspensions therein a cer
In these ?gures of the drawings there is illus
tain quantity of ?ner synthetic rubber solids. 15 trated a unit adaptable for employment in a syn
thetic rubber producing plant, namely, a unit
The wash water or serum containing e?luent of
embodying a feed-receiving basin I adapted to
major dilution is conducted to a vacuum type of
separation apparatus which particularly func
hold a body of coagulum and a closed top vacuum
tank 2 with associated parts. This vacuum tank
tions to accomplish a ?oating of the suspended
polymerized synthetic rubber solids that are 001 20 2 has a draft tube or feed pipe~3 with a low intake,
section leading from the receiving basin I and an
lectable and removable from the apparatus along
upper delivery section terminating within the
one path while leaving behind a weak but rela
tank at elevation substantially above that of the
tively clari?ed eilluen't which may be passed along
bottom of the tank but lower than that of the
another path for such use or disposition thereof
as may be deemed advisable.
'
25 upper interior portion of the tank.
In this tank there is held and maintained a‘
The ?nes recovered both from the serum con
continuously changing body of liquid undergoing
taining e?iuent of minor dilution and from the
treatment, the surface level of which is normally
serum containing eiliuent of major dilution can
maintained up to an elevation substantially_a_bove
be passed either to a preceding portion of the
process or to a subsequent portion of the rubber 30 that in the bottom of the tank but somewhat
lower than that of the upper interior portion of
producing process as may be deemed advisable
the tank and there is also maintained within the
having in view the particular requirements of the
upper interior portion of the tank, air or other
particular synthetic rubber producing process em
gaseous medium directly overlying said ever
ployed.
' The fundamental features of the apparatus for 35 changing body of liquid and to which the surface
of the ever changing body of liquid is constantly
performing the separation of the synthetic rub
exposed. The tank has means as will hereinafter
ber solids-either largeuor ?ne solids—-from the
appear for sucking the air or gaseous medium
liquid in which they are suspended are diagram
maticaliy illustrated in each of the systems re 40 from the interior of the tank whereby the air
or gaseous medium in the tank will be main
ferred to and constitute an important instrumen
tained under vacuum as it is sometimes referred
tality thereof. For convenience said apparatus ‘ to,
or as otherwise expressed, whereby the air or
may be referred to as a vacuum type of crumb
gaseous medium will be maintained at pressures
separating apparatus.
substantially below that of the air outside of the
The vacuum'type of crumb separation appara
tank. The sub-atmospheric pressure of this gas
tus has been adopted for the separating from a
eous medium is such as will be indicated by not
liquid-solids mixture bearing the same of syn
less than substantially 9 inches of mercury.
thetic rubber ?nes because the latter are not
I have ascertained that a vacuum or sub-atmos
readily settleable from the liquid because the
pheric pressure type of ?otation operation can
colloidal characteristics thereof tend to cause said
‘be advantageously employed to effect quick rising
?nes to continue as colloidal or quasi-colloidal
and ready removal of the synthetic rubber ?nes
suspensions.
The same process and apparatus which is well
adapted for removing of the dif?cultly settleable
?nes from a liquid is e?’ective for removing the
larger size of rubber crumbs and therefore it
becomes logical to employ this apparatus not only
for removing the ?nes, but also at the same time
for removing the coarser solids, and in this man
ner avoid the necessity of employing separate and
quite dissimilar types of machines for the separat
ing-out operation.
In said drawings which constitute a part of
from a coagulum or liquid fraction bearing the
same and I have adopted as a practical form of
apparatus for accomplishing this quick and ready
removal of the small ?nes a type of apparatus
possessing the fundamental features of operation
embodied in and by the vacuum type of apparatus
illustrated in and by Figs. 1 and 2.
In the unit or apparatus of Figs. 1 and 2 gas
bearing mother liquid having polymerized syn
thetic rubber crumbs which were yielded therein
is fed as a liquid suspension of polymerized syn
thetic rubber solids which is delivered to the basin
I through a supply tube or conduit 4. The basin
Figure 1 diagrammatically illustrates a vacuum 65 has an over?ow partition 5 rising from the bot
type of separation unit functionable in a synthetic
tom thereof whereby the interior of the basin is
rubber plant for separating synthetic rubber
divided into a relatively large receiving and stor
crumbs from a process liquid fraction, or brine
ing section 6 and a small section ‘I for receiving
and according to which unit the separated-out
overflowed liquid and solids at the ?ow delivery
synthetic rubber crumbs are deliverable along
side of the partition.
I
one path ‘while the liquid fraction is deliverable
This partition is made up of removable and re
along another path.
placeable boards 8 and collectively constitutes a
Fig. 2 is a horizontal sectional view taken on
structure providing an adjustable height dam
the plane indicated by the broken line 2—2 of
the upper edge 9 of which constitutes an over?ow
Fig. 1 and looking in the direction of the arrows. 75 weir at the top of the partition. The adjustment
this specification:
2,410,638
7
8
of the height of this dam is according to the quan
tity of the liquid-solids mixture to be retained in
In the construction shown there is an auxiliary
con?ning structure 23 which may be viewed as
part of the launder and which embodies a wall
the large section of the basin but it can be em
ployed to release into the smaller section a con
member or‘ portion 24, a cap member or top por
tion 25 and a lower member or bottom portion 28
for providing therein a control chamber 21. In
treated. The unit is designed so that there is
this chamber there is disposed an adjustable suc
constantly contained in the smaller section ‘I suf
tion nozzle means 28 constituting an intake end
?cient of the over?owed liquid-solids mixture to
of a pumping means 29 provided for withdrawing
insure the maintaining of the intake end ill of the
10 gas or air from the upper interior portion of the
.__draft tube 3 in submergence.
trolled out?ow of liquid-solids mixture to be
The crumb separating tank as shown, embodies
an upright marginal wall H, cylindrical in plan,
the’ upper horizontally-extending edge l2 of
tank.
ignated as I3. The tank has a bottom member or
28 and an upper horizontal tubular section 32
This pumping means 28 embodies an air suc
tion pump P having a suction pipe line 30 leading
thereto from the interior portion of the height
which provides that which may be called a. clari
?ed-liquid over?ow weir edge that determines the 15 control chamber 21. This suction pipe line 38
includes the adjustable nozzle means 28 at and
normal operative level of the ever changing body
of liquid which is normally maintained within the
for the intake end thereof, a rising tubular sec
tion 3| leading upwardly from the nozzle means
tank. This ever changing body of liquid is des
?oor portion l4 sloping downwardly and vinwardly 20 leading from the rising section 3| and connected
to the pump P at the suction side thereof.
from the lower edge portion of the marginal wall.
The tank also has a launder structure providing an
The nozzle means 28 is pivotally mounted so
that it can be adjusted whereby the intake tip
portion 33 thereof can be positioned as to the
embodies a lower annular member l5 extending 25 height or elevation. This adjustment is attained
through the medium of a shaft 34 connected to
outwardly from the marginal wall, to wit, from an
and extending laterally from the nozzle means
elevation thereof slightly lower than that of the
and providing a horizontally extending support
upper or over?ow weir edge 12. The launder
ing axis therefor and a handle 35 which is dis
structure also embodies a rising outer wall portion
l5 extending upwardly from the outer edge of the 30 posed outside of the structure providing the
enclosed launder for receiving liquid overflowed
from the upper edge l2. The launder structure
member l5 and an upper annular member or
height control chamber.
,
The pumping means 29 is also preferably
equipped with a vacuum controlling means 36
over?ow weir edge I2 and extending inwardly
that is connected to the suction pipe line 30 by a
from the rising outer wall portion 18.
The upper portion of the tank is completed by 35 pipe connection 31. The vacuum controlled
means 36 is provided with an outwardly spring
a top member or cap portion l8 rising from the
pressed relief valve 38 which yields to allow an
inner edge portion of the upper annular member
out?ow of outside air into the suction line only
IT. This top or cap member I8 is relied upon to
after liquid hasbeei sucked into and upwardly
complete with the launder structure a relatively
gas-tight upper portion for the tank. Within the 40 within the rising section and for a substantial
portion thereof but which valve opens before the
interior of the tank there is provided a cylindrical
liquid within the rising pipe section 3| reaches
baiile member l9 that is circular in plan and which
the upper horizontal section 32. In this way
extends upwardly from a lower interior portion of
there is assured continuation of conditions
the tank, namely, from an elevation lower than
that of the over?ow weir edge l2 to an elevation 45 whereby the pump P will never have to receive
and deliver water and whereby the pump can
higher than that of the over?ow weir edge l2.
continue to operate to receive and deliver only
This baf?e member [9 is carried from the cylin
air or other gaseous medium supplied thereto
drical marginal wall H through the medium of
through the horizontal top section 32 of the suc
spacing and supporting brackets 20. The cylin
drical ba?ie l9 and the marginal wall II function 50 tion line 38.
When the reduced pressure conditions within
to provide between them an up?ow conduit 2|
the top portion of the tank change whereby the
leading from a lower interior‘ portion of the tank
liquid within the rising section can drop or fall
towards the over?ow weir edge l2.
from the rising section 3| and from the nozzle
This up?ow conduit 2| is annular in plan and
section l1 at elevation higher than that of the
affords means whereby there can be realized a 55 means 28 thereof, the pumping means can then
function to withdraw some of the gaseous me
dium from within the upper interior portion of
the tank whereby to continue and maintain the
and over the weir edge l2. The region within
relatively uniform up?ow of clari?ed liquid from
the lower interior portion of the tank towards
required sub-atmospheric pressure conditions
this baiiie member l9 occupies a relatively large
portion of the horizontal cross-sectional area of 60 therein for satisfactory operation of the appara
tus or unit.
the tank and also a substantial portion of the
depth of the liquid-holding portion of the tank.
As previously indicated the normal operative
surface level of the liquid undergoing treatment
There is provided therein that which may be
in the tank 2 is determined by the elevation of
referred to as a zone wherein incoming liquid syn
thetic rubber-solids mixture is received for treat 65 the over?ow weir i2 and above this body of liquid
there is constantly maintained in zone 46 the
ment and wherein the ever changing liquid body
heretofore mentioned overlying body of air or
I3 is held during the vacuum treatment thereof
other gaseous medium which is continued at
within the tank.
pressures substantially sub-atmospheric because
. The enclosed launder provided by the upper
portion of the marginal wall H, the lower an 70 of the operation of ‘the pumping means 29. The
general structure of the tank and associated parts
nular ring IS, the rising outer wall portion l6 and
are such that during the normal operation and
the upper annular ring I‘! is designated as 22 and
functioning thereof there is avoided any short
is referred to as a clari?ed liquid-receiving laun
circuiting entrance of air into the tank from the
der because of its receiving the liquid over?ow~
ing thereinto from the weir edge I2.
75 exterior thereof either through the feeding
9
2,410,688
means leading to the tank or through the means
by which clarified liquid is released and passed
from the tank, or through the means by which
?oated and collected rubber crumbs are passed
from the tank as scum.
.
From that which has preceded and also from
an inspection of Figs. 1 and 2 it will be manifest
that the gaseous medium which is within the
upper portion of the tank occupies the entire re
, gion therein which is at elevation higher than
that of the over?ow weir edge I2. It will also be
noted that this sub-atmospheric pressure gaseous
medium extends across not only the full upper
portion of the tank within the area de?ned by
._
receiving trough "there is provided ?oat-sweep
ing means comprising a vertical shaft 10 extend
ing from the exterior of the tank through a
sealing packing ‘II at the top of the tank. This
' shaft is supported from suitable bearing means
‘I2 provided at the top of the tank. A motor
actuated means ‘I3 is also provided for turning the
shaft. The shaft carries outwardly extending
arms 14 having resilient sweeping members 13
extending downwardly therefrom and dipping
into the liquid body within the con?nes of the
cylindrical ba?ie I9. As this shaft turns about
its vertically extending axis the arms with
resilient sweeping members depending therefrom
the over?ow weir edge I2 but also so as to overlie 15 serve to engage and impel the ?oating rubber
all of the liquid within the over?owed liquid
receiving launder, including the liquid within the
crumbs up the ramp past the overpass transfer
edge into the receiving hopper or trough 50 from
control chamber 23 of the latter. In other words
which they pass from the downwardly extending
passage area for the gaseous medium is provided
tubular member 53.
at 33 and 39 between the uppermost interior por 20 In connection with the foregoing, it will be
tion of the top or cap portion of the tank on the
noted that the depending or tubular members
one hand and the upper interior portions of the
40 and 53 in effect constitute depending baro
launder structure, including the upper portion of
metric legs the lower ends of which constantly
the control chamber 26 thereof on the other
dip into sealing liquid and by which the par
hand.
25 ticular clari?ed liquid is conveyed or the collected
Referring now to the clari?ed liquid release
rubber crumbs are conveyed and delivered to
means. This includes the structure providing
the exterior of the vacuum tank and in a manner
the annular up?ow conduit 2I leading from a
whereby there is minimized or avoided entrance
lower interior portion of the vacuum tank, the
of outside air into the interior of the tank in
over?ow weir I2, the structure providing the en 30 cident to such transfer.
closed over?ow receiving launder 22 and the con
As to the draft tube, in the construction shown
trol chamber 26 thereof, a clari?ed-liquid re
the draft tube 3 is provided at the upper terminal
ceiving and release box 42, a pipe or tubular
portion thereof with a ?aring portion 83 the upper
member 40 extending downwardly from the lower
edge 34 of which is disposed at elevation proxi
portion of the control chamber 26 into a body of
mate but somewhat lower than that of the over
sealing liquid 4I maintained within the receiv
?ow weir edge I2. There also extends outwardly
ing box 42 up to an elevation 43 determined by
from the upper edge 84 an annular plate 35, spaced
an over?ow weir or darn 44 within the box 42.
radial brackets 83 carried by and extending in
This box 42 is also sometimes referred to as a
wardly from the cylindrical baiile member aiford~
clari?ed-liquid release box. The clari?ed liquid
ing support for the annular plate 85 and through
which is released from the tank passes down
the medium of the latter for the ?aring portion
wardly from the over?ow launder 22 through this
at the rising terminal of the draft tube 3.
pipe 40 into the body of liquid 4I whereby the
A sump 90 is provided in the bottom of the
sealing liquid is continued and from which any
tank for receiving any sedimented material that
excess accumulations of clari?ed-liquid over?ow
may pass or be passed thereto. A valve controlled
the upper edge of the dam 44 and are passed
pipe 9| leads from this sump and terminates in
from the release box 42 as through the pipe 45.
a box 92 when a body of sealing liquid 93 can be
As to the means for receiving collected ?oating
maintained. This valve controlled pipe can be
rubber crumbs and for passing the scum of col
employed to discharge sediment or liquid from the
lected rubber crumbs from the interior to the ex 50 bottom of the tank while at the same time the
terior' of the vacuum tank this comprises an open
sealing liquid 93 can be relied upon to minimize
top trough or ?oat-receiving hopper 50 provided
or avoid entrance or back?ow of outside air into
within the tank, a receiving box 55 and a pipe or
the tank.
tubular section 53 extending downwardly from
The system of Fig. 3 has in view the‘ receiving
the trough thence outwardly through the tank 55 and treating of coagulum, that is, a serum with
structure and into a body of sealing liquid 54
rubber crumbs mixture suspended therein, such
maintained within the receiving box 55 up to an
as has been obtained from a co-polymerization of
elevation determined by an over?ow weir or dam
synthetic latex derived in the performing of a
56 within the box 55. Any ?oating material pass
synthetic rubber producing process.
ing downwardly from the trough through the leg 60
According to this system, the coagulum which is
53 is received in this liquid-holding section of
sometimes described as a liquid-solids mixture,
the box 55. As it accumulates it over?ows the
of which the liquid fraction is brine while the
weir 55 and can be released from the box 55
solids are rubber crumbs of varying sizes in the
through the valve-controlled pipe 58. As to the
brine solution or serum, is supplied along a path
open top trough or ?oat-receiving hopper 50 this
way It" into a de-brining tank or initial liquid
has an overpass edge 5| with ramp 52 leading
solids separating instrumentality I02 having a
upwardly thereto. This overpass edge 5| is at
screening or ?ltering medium I03 on which the
elevation preferably slightly higher than that of
rubber crumbs lodge as a layer or mass I04
the over?ow weir edge I2 and the trough is dis
and from which the brine leaves as a serum
posed so as to receive ?oating material passed or 70 containing eiiiuent of minor dilution collecting
passing thereto as it rises to and collects at the
within the lower portion I 05 of the tank I02.
upper surface of the body of liquid within the
This eiiluent brine carries therewith a certain
tank.
amount of the ?ner rubber crumbs, herein re
In order to insure a positive transfer of the
ferred to as ?nes which continue as solids sus
' ?oating rubber crumbs to and into the ?oat 75 pension therein. The eiliuent bearing the ?nes
2,41o,ess
12
therein passes from the tank I02 into and along
a pathway or valve controlled pipe line I06.
The rubber crumbs of the initially separated
layer or mass I 04 are sometimes referred to as de
bearing the same according to the disclosure re
specting the apparatus or unit of Figs. 1 and 2.
As to the wash water e?luent from pipe line I26,
this can be passed by a valve-controlled connec~
brined crumbs but it will be noted that a certain in tion I2'I to the pipe line II8 leading to the re
quantity of brine continues in the layer or mass
ceiving basin 30I.
I04. The crumbs constituting this mass are con
For convenience the vacuum type of crumb
ducted or conveyed as along chute or conduit
separation apparatus or unit that embodies the
I I I into an initial washing tank or instrumentality
brine receiving basin 20l has been herein identi
I I2 having a screening or ?ltering medium I I3 on
?ed as brine crumb separation unit BCU, while
which the rubber crumbs lodge-and are supported
the apparatus or unit embodying the basin 30I
as a mass or layer II4 while being supplied and
has been herein identi?ed as the' wash water
washed with water delivered thereto along the
crumb separating unit WWU.
pathway or valve-controlled water supply line
In Fig. 3 the parts of the brine crumb separa
H0. The wash water thus applied washes out
tion unit BCU which correspond to like parts in
the remaining brine and also carries therewith
unit of Fig. 1 bear reference characters which
certain of the ?ner grains from the layer H4
are 200 greater than that of the corresponding
and the water leaving the layer collects as wash
reference characters of Fig. 1. Likewise with
water eiliuent in the lower portion I I5 of the tank
respect to the parts of the wash water crumb
I I 2. This wash water eiliuent bearing some brine 20 separation unit WWU they bear reference char
and also quantities of the washed out synthetic
acters which are 300 greater than of the refer
rubber ?nes suspended therein, which is some
ence characters of unit of Fig. 1. As the units
times referred to as a serum bearing e?iuent of
ECU and WWU and the functioning parts there
major dilution, is pased from the washing tank
of correspond to and function according to the
I I2 into and along a pathway or valve-controlled
disclosure respecting the corresponding parts of
pipe line II 6. ,
'
the apparatus or unit of Fig. 1 extended com
ments in regard to the construction and operation
washed mass II4 are conducted or conveyed as
of the apparatus or units ECU and WWU are un
along a chute or conduit I 2I into a second or
necessary at this time.
subsequent washing tank or instrumentality I22 30 In connection with the operation of the brine
having a screen ?ltering medium I23 on which
crumb separation unit BCU, it will be noted that
the thus transferred crumbs lodge or are sup
the brine eiliuent bearing ?nes supplied to the
ported as a mass or layer I24 while being sup
feed-receiving basin 20I passes from the latter
From the washing tank H2 the crumbs of the
plied and washed with water delivered thereto
from a valve-controlled line I20.
through the draft tube 203., and is delivered from
The eiliuent 35 the ?aring top 283 of the latter into the ever
of this subsequent washing operation also carries
changing body of liquid 2I3 within the closed
a certain quantity of further washed out ?nes
which continue with it. The secondary wash
water e?luent is passed from the lower portion
top vacuum tank 202.
The ?nes rise and are
collected by the resilient member 218 at the
outer ends of the horizontal tuming arms 214
I25 of the secondary washing tank I22 along the 40 whereby they are swept towards and beyond the
pathway or pipe line I26.
over-pass edge 25I of the receiving hopper 250.
The de-brined and the twice washed and de
From this hopper the fines are delivered through
watered rubber crumbs constituting the coarser or
the tubular section or barometric leg 253 into the
sealing liquid 254 within the receiving box 255
from which the accumulated portion thereof 'is
released as over?ow through the pipe 256. The
processing as may be desired and in order.
clari?ed liquid, to wit, the serum freed of ?nes,
It is feasible to pass the brine effluent of the
leaves from a lower portion of the tank 202', to
?rst tank I02 from the brine e?luent line I06
wit, through the up?ow conduit 22I which is an
leading therefrom by pumping the brine through 50 nular in plan, over?ows the weir edge 2I2 and
the valve-controlled pipe line I01 to a preceding
enters the enclosed launder 222 and flows there
portion of the‘ process or by passing the brine
from downwardly into and through the baro
from the line I06 into a valve-controlled branch
metric leg by the tubular member 240 which
line I08 connected to a feed or pipe line I09
constantly dips into sealing liquid 24I in the
leading to and delivering into a brine receiving , receiving box 242 and from which the accumu-v
basin 20I constituting a feed-receiving basin for
lating brine or serum is released as over?ow
a vacuum type of crumb separation apparatus
through the pipe 245. Suitable vacuum condi
identi?ed as BCU, namely a vacuum type of
tions are maintained in this unit through the
crumb separation apparatus embodying the
medium of the pumping mechanism collectively
features of construction and functioning to sepa 60 indicated as 229.v
rate synthetic rubber ?nes from the brine or liquid
In like manner the wash water effluent bear
fraction bearing the same according to construc
ing ?nes which has been delivered through pipe
tion and method of operation already described in
line H6 into the feed-receiving basin 30I is
connection with the synthetic crumb separation ‘ ‘passed from the latter through the draft tube
apparatus or unitof Figs. 1 and 2.
65 303' into the ever changing body of liquid main
As to the wash water e?luent from pipe line
tained in the closed top vacuum tank 302 where
II6, this can be optionally passed at will by a
in a liquid-solids separation takes place whereby
valve-controlled branch II'I“ to the feed line or
the ?nes ?oat. These ?oating ?nes are passed
pipe I03 leading to the aforementioned receiving
into the open top trough or hopper 350 from
basin 20l or by a valve-controlled branch I I'Ib to 70 which they pass downwardly and into the baro
a feed line or pipe I I6 leading to a receiving basin
metric leg 353 into the ?nes-receiving tank or
30I of a second crumb separating unit identi?ed
box 355 from which they pass as over?owed dis
as WWU and which like BCU embodies the fea
charge through the pipe 358 while the clari?ed
tures of construction and function to separate
liquid or wash water freed of ?nes passes up
synthetic rubber ?nes from a liquid fraction 75 wardly from a lower portion of the tank through
larger synthetic rubber crumbs derived from the
coagulum are conveyed from the last washing
tank I22 along the pathway I31 for such further
2,410,888 »
13
.
the annular up?ow conduit portion 32i past the
14
um liberated from, directly overlying and engag
ing the surface portion of such ever-changing
body; maintaining such medium at pressures
vsubstantially sub-atmospheric by applying sue
tion thereto; continually feeding such suspension
from a locality outside of said ever-changing body
and delivering the same to the body proximate
the surface thereof and whereat the thus-deliv
over?ow edge 3l2 into the enclosed launder and
whereby clari?ed wash water eilluent ultimately
passes into and downwardly through the baro
metric leg 340 into the receiving basin or release
box 3“ from which there is a release of clari
?ed liquid to discharge along the line 345.
If the synthetic rubber ?nes thus recovered
from the crumb separation units are to be in
ered suspension comes under the direct influence
corporated with the already washed out larger 10 of the overlying gaseous medium thereby further
crumbs in the pathway I31, this can be accom
ing a liberating of certain quantities of said gases
plished by passing the recovered ?nes alonga
and furthering the ?oating of ?ne polymer sus
pathway or pipe line that comprises the pipe
pended particles to said exposed surface portion
line sections 60, 6| and 62 leading to I31. If a
of said body; continually collecting ?oating poly
valve 59 is closed, then it is feasible to pass the 15 mer particles and removing them from said body
?nes from the wash water crumb separating unit
from the region whereat they are exposed to said
WWU to the pathway I31 while the crumbs from
overlying gaseous medium to a locality outside of
the brine crumb separation unit BCU can be
said region; and continually removing liquid frac
passed as along the pathway or pipe line 63, as
suming the valve at 64 is open to a preceding 20 tion from a lower portion of said ever-changing
body to a locality outside of said body.
portion of the process.
}
.
2. In a butadiene styrene co-polymer process
Respecting the serum or brine which is sepa
for the manufacture of arti?cial rubber wherein
rated out by the brine crumb separation unit
there is involved the obtaining of co-polymer
BCU this can be taken care of ?rst as by passing
the brine from box 242 through pipe 245 into a 25 crumbs from gas-bearing and gas-releasing briny
suspensions provided by a coagulum comprising
box or basin 65 from which the brine can be
such crumbs as a solids fraction thereof and
passed as by pump 66 and pipe line 61 to any
serum as a liquid fraction thereof and bearing
preceding portion of the process where the brine
therein gases liberatable from the suspension
can be used.
From that which has preceded, it will be mani 30 when the surface of the suspension is exposed to
overlying gaseous medium whose pressure is less
fest that the crumb separation apparatus which
than that which the suspension was previously
is described in connection with the unit or ap
subjected to, the method comprising establish
paratus of Figs. 1 and 2 can be employed to
ing an ever-changing body of said suspension
separate out the rubber crumbs of varying sizes
from the liquid fraction in which they are found 35 and maintaining the surface thereof directly
exposed to a gaseous medium liberated from and
while according to the system of Fig. 3 one can
remove the larger crumbs as by screening or
?ltering and can remove ?ner crumbs from brine
bearing the same and can also remove ?ner
overlying the ever-changing body, continually
supplying suction to the gaseous medium over
lying said ever-changing body to maintain pres
crumbs from wash water e?luent bearing the .40 sure thereof substantially below that to which
the suspension was previously exposed and all
same.
of this while the following operations are carried
Whereas the foregoing describes the treatment out, namely, while continually supplying quan
of synthetic rubber suspensions to recover the
titles
of said coagulum and delivering it as feed
rubber particles, this invention is equally ap
and towards the surface level of the
plicable to reclaim natural rubber solids that 45 proximate
body, while removing co-polymer crumbs ?oating
are in suspension phase as a result of practicing
at the surface of said body and delivering the
processes for the recovery or reclaiming of such
removed
crumbs to a region outside of said body,
rubber. This is especially true where rubber
and while passing liquid relatively free of said
?nes are dif?cult to separate from suspension
crumbs from a lower region of said body to a
and would otherwise be lost by passing into the 50 locality
outside of the same.
'
sewage with the waste water-—where such rubber
3.
In
a
butadiene
styrene
process
for
the
pro
?nes are detrimental to subsequent sewage treat
duction of basic crude products usable in or for
ment processs.
the production of synthetic rubber and in which
It will be manifest that according to the dis
process there is the obtaining of co-polymer
closure hereof one can readily adopt the method 55
crumbs from a briny serum-crumb mixture real
hereof to any part of a synthetic rubber produc
ized in the process, wherein the co-polymer
ing process wherein it is desired to remove ,rub
crumbs are of varying sizes ranging from coarse
ber crumbs from a liquid wherein the same was
particles to and including small particles sus
yielded or exists. The invention can be particu
pended in the liquid fraction provided by serum
larly employed where one desires to eliminate or
and wherein there are in the serum gases which
collect from the liquid bearing the same syn
are liberatable when the serum-crumb mixture
thetic rubber ?nes which may be in colloidal ‘or
is subsequently exposed to an overlying gaseous
quasi-colloidal condition.
medium of pressure less than that to which the
I claim:
.
i
serum mixture is exposed; a continuous method
1. In a butadiene styrene co-polymer process 65 including establishing and maintaining an ever
for the manufacture of arti?cial rubber and the
changing body of liquid provided by such serum
recovering of ?ne co-polymer particles from the
crumb mixture, constantly exposing the surface
briny suspensions thereof wherein there are gases
of said ever-changing body to an overlying con
liberatable from such suspensions when the lat
?ning body of gaseous medium liberated from
ter are exposed to subsequent sub-atmospheric 70 said serum-crumb mixture, applying suction to
pressure conditions; the method comprising es
said con?ned gaseous medium to maintain pres
tablishing an ever-changing body provided by
sures thereupon substantially less than that of
such suspension and maintaining the surface level
the serum-crumb mixture supplied thereto, con
thereof up to an operative elevation; exposing a
stantly supplying serum-crumb mixture from a
surface portion of such body to a gaseous medi 76 region outside of the ever-changing body and
i
-15
2,410,033
l6
delivering the serum-crumb mixture thus sup- .5 suspensions therein thereby obtaining asecondary
plied into said ever-changing body within the
brine-bearing ei‘iluent of major dilution and in
reach of the suction in?uence of said overlying
suring the existence in said secondary eilluent of
gaseous medium, removing ?oating crumbs from
gases when the secondary eiiluent is subsequently
the surface of said ever-changing body and de
exposed to pressures less than that at which the
livering the removed crumbs outside of said ever
washing operation was carried out, establishing
changing body and also outside of said gaseous
and maintaining an ever-changing liquid body,
medium while at the same time substantially
exposing an upper portion of said liquid body di
avoiding entrance of air into said overlying gasrectly to the suction effect of a gaseous medium .
eous medium, and passing clari?ed serum from 10 overlying the same, sucking gases from said over-'
a lower portion of said ever-changing body to a
lying gaseous medium for maintaining the pres
region outside of the same while at the same
sure thereof lower than that existing when said
time substantially avoiding entrance of outside
secondary eiliuent was obtained, passing quanti
air into said overlying gaseous medium.
ties of said secondary e?luent as feed material into
4. In the production and obtaining of buta
said body and delivering the same at elevation
diene styrene co-polymer crumbs from a briny
proximate that of the surface of said body, col
coagulum containing such crumbs as a sus
lecting ?ne solids which assemble as ?oating ma
pended solid fraction thereof and process liquid
terial on the surface of said liquid body and
as a liquid fraction thereof, the method compris
within the region overlain by said gaseous med
ing establishing and con?ning the ever-changing 20 ium, transferring collected ?oated material as
body of said process liquor and maintaining the
recovered ?ne solids to a locality outside of said
surface thereof up to an operative level, expos
region, which transfer of ?ne solids is in a man
ing the upper surface portion of said body to an
ner for avoiding any substantial leakage of air
overlying gaseous medium derived from said
into said overlying gaseous medium. passing
briny coagulurn and applying suction thereto 25 clarified liquid from a lower portion of said body
whereby to maintain the same at pressures sub
whereat the suction e?ect of the overlying gas
stantially sub-atmospheric, passing said agitated
eous medium is substantially less than that at
suspension into and delivering it within said
the overlain surface of said body, delivering the
con?ned body at elevation proximate that of the
- thus passed clari?ed liquid to a locality outside
operative surface level of the body whereby the
of said body and in a manner for avoiding any
coagulum thus delivered within said ever-chang
substantial leakage of air into said body, and
ing body is under the direct in?uence of said
passing the recovered ?ne solids to a portion of
overlying sub-atmospheric pressure gaseous me
the synthetic rubber producing process.
dium, collecting such crumbs assembling as ?oat
7. In the production of synthetic rubber ac
material at the surface of said body, transferring 35 cording to a butadiene styrene process in which
along one path said collected ?oating material
there is realized a liquid-solids mixture compris
from within the overlying gaseous medium and
ing process liquor that includes brine and co
transferring the same to a locality outside of
polymers as solids of varying sizes, the method
said gaseous medium while avoiding any sub
comprising separating large solids from the pro
stantial leakage of outside air into said atmos 40 cess liquor; passing separated large solids along
pheric pressure gaseous medium incident to said
one path, passing along another path process li
transfer, passing process liquid from along an
quor bearing ?ne solids and from which the large
other path from a lower region of said body while
solids have been separated; washing the sepa
avoiding any substantial leakage of outside air
rated large solids while exposing to atmospheric
into said body incident to said passing of liquid
pressure whereby to further remove entrained
therefrom, and passing the collected transferred
portions of liquor; passing along a third path the
crumbs for further treatment.
wash
water e?luent hearing some of the washed
5. A method according to claim 4, wherein
out process liquor and also carrying as suspen
the overlying gaseous medium is maintained at
sub-atmospheric pressures substantially not 50 sions therein washed out ?ne solids derived from
the separated large solids; insuring the existence
higher than that realized by a suction pull re
in said wash water eiiluent of gases employable in
the performing of the method, which are releasa
whereby the surface level of the column is not
ble and which rise to an overlying gaseous med
less than ‘7 inches above that of the surface level
ium of such gases at sub-atmospheric pressures
of body of mercury exposed to the atmosphere 55 when a body of such wash water eiliuent is di
and from which the elevated column was lifted,
rectly exposed to such sub-atmospheric pressure
agitating such briny coagulum to be treated while
gaseous medium; establishing an ever-changing
exposed to atmospheric pressure air.
liquid body; exposing an upper surface portion of
6. In the production of synthetic rubber ac
said liquid body to a gaseous medium of such
cording to a butadiene styrene process in which 80 gases liberated from liquid supplied for providing
co-polymers in the form of solids of varying sizes
such body and directly overlying such body; feed
are produced and developed under conditions
ing such wash water ei?uent with such gases
wherein they are eidstent in the liquid-solids mix
therein and delivering such fed eiiluent proximate
ture of which the liquid fraction comprises process
the upper surface of said liquid body; sucking
liquor that includes brine and of which the solids
gases from said overlying gaseous medium for
fraction includes said solids, the method com
maintaining pressures thereof substantially sub
quired to lift a con?ned column of mercury
prising initially separating from such mixture
atmospheric whereby~ to e?'ect the liberating of
large solids removable along a solids discharge
quantities of gases in the wash water e?iuent thus
pathway, collecting process liquor from said ini
fed and delivered whereby to further the ?oating
tially separated operation as a primary brine 70 to the surface portion of said liquid body ?ne
bearing e?iuent of minor dilution and conducting
solids suspended in the wash water eiiiuent fed
the same along a liquid ?ow-path leading from
and delivered proximate the surface of the liquid
said initially separated solids, supplying wash
body; collecting ?ne solids ?oating within the
water to the initially separated solids, collecting
region overlain by the sub-atmospheric pressure
the wash water with fine co-polymer solids as 76 gaseous medium; removing the thus collected ?ue
2,41o,ess
l8
solids and delivering the same to a locality‘ \ according to a butadlene styrene process in which
whereat they are discharged outside of the region
whereat they were collected; and passing clari
?ed liquid'from a lower portion of the ever
v there is obtained a liquid-solids mixture compris
ing as a solids fraction butadiene styrene-co
polymers and has a liquid fraction process liquor
changing body and delivering said transferred 5 that includes brine and releasable gases, the
liquid to a locality o'utside of said body.
separating of such solids from said liquid frac
8. In the production of synthetic rubber accord
tion by a method comprising establishing from
ing to claim 7, the aerating of wash water e?iuent
such liquid-solids mixture an ever-changing li
before feeding it to the ever-changing body.
quid body having a surface portion overlain and
9.- In the production of synthetic rubber accord 10 directly exposed to a gaseous medium provided by
ing to claim 7, the passing of the collected and
gases released from such process liquor, sucking
gases from the overlying gaseous medium whereby
removed ?ne solids to a, portion of the butadiene
styrene ‘process for employment therein. »
ll). In the treating of a briny suspension bear
to maintain the same at pressures substantially
, sub-atmospheric, maintaining the surface of
ing, as solids therein, butadiene styrene co 15 said body up to an elevation providing an opera‘
polymers and also bearing gas releasable when
.tive surface level, passing such liquid solids mix
exposed to an overlying gaseous medium derived
ture as feed into said ever-changing body and
from said suspension‘ when at lesser pressures
delivering it at elevation approximately that of
than that at which suspensions were previously
the operative surface level of said body whereby
subjected, the method comprising exposing a body 20 the liquid solids mixture as thus delivered comes
of such suspension to an overlying gaseous med
under the effective in?uence of said overlying
ium obtained as gaseous medium released under .
gaseous medium, collecting at the surface of said
said lesser pressures and maintaining such lesser
body and within the region overlain by said gas
pressures to effect releasing of quantities of gases
eous medium co-polymer solids assembled as
rising within said body and thereby furthering
?oating material within said region, removing
the ?otation of solids of such suspension to the
the thus collected solids from said region and dis
surface of said body andv of which rising gases
charging them to a locality outside of said region
some pass directly into the‘ overlying gaseous
while at the same time substantially avoiding the
medium, collecting from the surface of said body
entrance of air into the overlying gaseous medium
and within the region overlain by said gaseous ' 30 at said region and which might otherwise take
medium solids ?oating upon said body and re
place incident to said removal and discharge, and
moving the thus collected solids from a region '
withdrawing clari?ed liquid derived from a por
where collected to a locality of the region over- ,
tion of the ever-changing body that is at elevation
lain by said gaseous medium while maintaining
lower than that of the‘inwardly passed liquid
the required lesser pressure conditions for said
solids mixture as delivered into the body and
overlying gaseous medium, and passing from a
transferring it for discharge to a locality outside
lower portion of said body of liquid substantially
of said body and away from the in?uence of said
freed of said solids and delivering it as a clari?ed
overlying gaseous medium and during such trans
liquid fraction to a locality outside of said body
ferring of the clari?ed liquid substantially avoid
while at the same time ‘maintaining the required 40 ing entrance of air into said body and thus into
lesser pressure conditions for said gaseous medium _
the region overlain by said gas incident to said
overlying the body.
transferring and discharge of said clari?ed liquid.
11. In the art of producing synthetic rubber
THEODORE B. COUNSELMAN.
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