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Патент USA US2410315

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Oct. 29, 1946.
E; o. sowERwmE, JR
2,410,315
APPARATUS FOR PREPARING FORMED GELS
‘
Filed May 20, 1945
BY
@MW
A TTURN
2,410,315
Patented Oct. 29, 1946
‘UNITED ‘STATES PATENT OFFICE
‘Elbert '0. Sowerivine, Jr., Woodbury,"_N. J.,
as
Socony-Vacuum Oil-Company, Incor
a corporation of New York
Application May 20, 1943,‘ Serial No. 487,715
(01.252-359)
2
iMy invention contemplates the provision "of
This invention relates to apparatus "for'pre
novel means for inhibiting gelation on or in the
2 Claims.
-1
paring and dividing an aqueous colloidal solution
capable of setting to a gel or similar solid'or' semi
solid condition. More particularly, the inven
tion contemplates the formation and subdivision
means for providing streams of sol supplied to
of an aqueous $01 which sets'to form a hydrogel
bination of mixer and divider. In the'drawing:
comprising inorganic oxides in ‘the solid phase.
In thecopending applica'tion'Serial No. 461.454,
?led October 9, 194%, by Milton M. Marisic, which
a body of liquid immiscible with the'sol.
‘In the accompanying drawing are shown a novel
mixing nozzle, a novel divider and a novel com
Figure l‘is a diagrammatic showing of a typical
apparatus according to my invention;
"Figure'Z is a‘ view in vertical section of a mix
issued as Patent No. 2,385,217, on ‘September 18, 10 ing nozzle according to my invention;
7
1945, a process is described for forming hard,
"Figure 3‘ is ‘a'sectional view of one form of
spheroidal beads of ‘inorganic oxides by iniecting
divider‘ contemplated by the invention; and t
solutions which will ‘gel in a predetermined time
Figure it is a view'in‘ partial section of another
into a liquid immiscible therewith and permitting
form
of divider contemplated by theinvention.
gelation of ‘resultant globules of the solution in 15
Brie?y, the inventionprovides for} inhibiting
the immiscible liquid. The resultant globules of
hydrogel are then removed and processed to form
the desired ?nal product.
'I-noperation of suchprocesses, difficulties arise
due to gelation of small portions of. the solution 20
within the mixing nozzle formingideposits of gel
which gradually build up. ‘In the said Marisic
application, it is proposed» to- avoid this di?iculty
gelation'in the mixing nozzle by'heating the'walls
thereof to a‘temperature above ‘the boiling point
of the sol to thereby ‘cause vaporization along
the walls and provide a ‘protective'vapor layer
which prevents gelation'onthe walls. The divider
is provided with a surface layer of a solid ‘hav
ing a melting point‘below the tem‘peratureofthe
‘sol discharged ‘from the mixing nozzle. ‘The ' sol
by means of a‘rota'ry' cleaning member within the
falling on the divider melts this surface during
nozzle. Deposits can also be avoided by high 25 operation and thus provides a continuously re
velocity ?ow within the nozzle. The ?rst means
newed surface and any gel which forms there
includes a moving member within the nozzle
on is carried away by the flow of the sol.> Ac
which occupies space and requires packing at the
cording to one modi?cation of the invention, the
bearings; while high velocity flow impairs the
divider is provided with heat exchange means
capacity of the device to produce uniformly sized 30 whereby a coating of ice may be built up there
globules.
on by freezing of water in the sol during one phase
A divider for increasing the practicable capac
of the operation and melted during another phase,
ity of a single mixing nozzle is described in appli
thus continuously changing the surface without
cation Serial No. 477,168, ?led February 25, 1943,
replacement of the divider at the termination of
by John W. Payne, Edmund L. Sargent and Henry 35 each melting step.
G. Daley. According to the disclosure of the
Thetime required for gelation of the sol is de
latter application, the stream of aqueous sol
pendent upon the temperature of the sol, gela
issuing from a mixing nozzle is projected onto
tion time decreasing with increase in tempera
a downwardly sloping surface so formed as to
ture. When using the combination shown in Fig
divide the stream into a plurality of smaller 40 ure 1, the sol will be heated as formed in the
streams. A typical and preferred form of divider
mixing nozzle and subsequently cooled on the
is conical in shape and provided with grooves
divider and a balance of these factors must be
down the sides from the apex. Provision is made
made with other variables affecting gelation time,
to discharge the stream of aqueous sol onto the
for example acidity and concentration‘ of the sol.
apex of the cone whereby it is divided into a plu 45 It may be noted that gelation time is decreased
rality of smaller streams, each of which is of
by increasing either pH or concentration.
a size to give the desired subdivision of the sol.
Referring speci?cally to Figure 1, a vessel 10
By this means a single nozzle may be used to pro
encloses a column of liquid immiscible with the
vide many streams, thus greatly reducing the
sol, for example, mineral oil. Below the column of
number of nozzles required, each of which must 50 oil is a relatively shallow layer of water which
be ?tted with at least two metering pumps, or
is caused to flow by admitting fresh water at H
other suitable controls. In the said application,
and withdrawing water containing spheroidal gel
the conical divider is described as having a sur
globules by pipe i2. Two solutions which will re
face not wetted by the aqueous sol, thus prevent
act to form the desired sol are admitted to a
55
ing adherence and gelling of the sol on the divider.
2,410,315
mixing nozzle l3 by pipes I4 and [5 from meter
A metallic base 26, which may include heat ex
ing pumps l6 and I1.
change tubes as shown in Figure 3, is covered by
The mixing nozzle I3 is constructed in such
a layer 21 of a meltable substance such as ice. A
manner that heat may be applied to the inner
plurality of grooves 28 in the top surface pro
walls thereof, as by a heat exchange medium or
vide paths for the small streams desired. The
direct heating means. In the embodiment of Fig
grooves are not essential but do give considerably
ure 2, heat is supplied by an electric heating coil
smoother operation in dividing the sol. If heat
l8 embedded in an outer layer l9 of insulating
exchange
means are included, circulation of a
material. Current is supplied to the coil l8 by
leads 2B. The heating coil is adjacent to but in 10 ?uid therethrough can be used to control melt
ing away of the surface. In operations using the
sulated from a liner 2| which may advanta
embodiment of Figure 3, which is also prefer
geously be metallic. It will be apparent that so
ably grooved, a refrigerant may be circulated
lutions admitted by inlet pipes l4 and I5 will be
through tubes 25 until a substantial layer of ice
rapidly and completely mixed inside the nozzle
is built up by freezing out water from the sol,
while the hot liner will cause a minor amount of
whereupon the refrigerant ?ow is discontinued or
vapor to be generated which forms a protective
a ?uid of different temperature is circulated, per
blanket between the liner and the contents of the
mitting melting of the ice.
nozzle. Due to the short period of residence of
The surface coating of divider 22 should, in
the aqueous ?uid in the nozzle, the amount of
general,
have a melting point below about 100° F.
vaporization relative to the total ?uid is slight 20 I claim:
and the rise in temperature of the liquid is- only
1. In a device for dividing a stream of a gel
a few degrees.
able sol into a plurality of smaller streams, a
Upon discharge from the nozzle, the sol falls on
divider of generally conical shape, means to
the apex of a divider 22 which is adapted to split
maintain said divider in position with the apex
the stream of sol into a plurality of smaller
streams. Any type of sloping surface may be used , thereof directed upwardly, the outer surface of
said divider having a plurality of grooves extend
for this purpose, but best results are to be ob
ing down the surface thereof from about the
tained by using a conical divider having a plu
apex, said grooves being coated with a layer of
rality of grooves down its surface from the apex.
ice, and means to discharge a stream of gelable sol
The divider is supported from the wall of vessel
onto the apex of said divider.
H] as shown. In the embodiment illustrated, the
2. In a device for dividing a stream of a gel
support includes pipes 23 and 24 for circulation
able sol into a plurality of smaller streams, a
of a heat exchange medium to and from divider
divider of generally conical shape, means to main
22.
'
tain said divider in position with the apex there
-A divider provided with means for conducting
a heat exchange medium in heat exchange rela 35 of directed upwardly, the outer surface of said
divider having a plurality of grooves extending
tionship with the surface of the divider is shown
down
the surface thereof from about the apex,
in Figure 3. Tubes 25 from the heat exchange
said grooves being coated with a layer of ice,
medium are formed in the divider itself whereby
means to conduct a heat transfer ?uid in indirect
the surface of the divider may be cooled or heated.
‘In Figure 4 is shown a divider having a sur 40 heat exchange relationship with said surface, and
means to discharge a stream of gelable sol onto
face formed of a substance which melts at a tem
the apex of said divider.
perature below that of the sol supplied thereto.
ELBERT O. SOWERWINE, JR.
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