Jan. 5, l1937. ' \ -H. B.

' CALDWELL ‘ 2,057,043

i >VACUUM CRYSTALLIZER AND> METHOD OF CRY-STALLIZING
Filed OCT'. 25, 1935

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 l' Patented Jan. 5, ` I
2,061,043

UNITED STATES:anni:PATENT oF’Fic/B .

VACUUM CBYSTAILIZEB AND METHOD‘OF
"CBYSTALLIZIN .

umm n. oneven. 'New' rm. N. r., mami :o

Swenson >Evapin'atoi' Company, Harvey» Ill.,a
corporation of Illinois
appnc'emn october g5, 193s, anni No. 695.095
' nomini. l(criss-_45) ' -

This invention relates to vacuum crystallizers ` an opening Il which communicates with a suita
and method oi crystallizing. The invention has ble device Il for creating a vacuum within the
particular relation to the method of and appa shell lil _and compressing the vapors removed .
ratus for. crystailizingy disclosed in my priori-‘at from the shell. This evacuating means may be
5 ent- 1,865,614 issued July 5, 1933, according'to any oi the pumps or electors known in' this art. 5
which crystallization is eiieoted by subjecting' the In the speciiic embodiment illustrated the ,evacug
solution to a vacuum whereby thesolution is ating means l1 is a booster elector which is sup- ’
cooled to the temperature at which crystals de i plied with high pressure steam through a pipe i8.
posit. The. vacuum is produced by a suitable y 'I'his steamis supplied to a steam chest I9 from
10 compressing device and the vapors are condensed which it passes through a chamber 20 through 10
by a suitable cooling fluid, which may be at a tem- ` nozzles 2|. The chamber 20 communicates with
perature substantially higher than the tempera the opening ii. The nozzles 2| terminate in the
ture of the solution from which the crystals are converging portion ot a' venturi 22, which venturi
_ being deposited. ` v . ,l delivers into a condenser 23.` Thecondenser 23
lo - One ot the principal objects oi the invention is is shown by way of example as comprising a 15
to provide. an improved method of andapparatus `chamber through which passes a Icoil 24, through -
for crystallization. \ which suiti'ible> cooling fluid >is' passed. Said
» A further object of the invention isto provide chamber communicates- with the barometric leg
an improved method of and apparatus for crystal 25 sealed by a trough 2G. The chamber is also
go lization, which ,is substantially continuous and Aconnected to a vacuum pump 2l which exhausts
' can be continued for prolonged periods o! time air introduced into the system with the liquid
without ceasing operations. . ~ - supplied or introduced by- leakage. . .
Other obiectsr‘advantages and capabilities of With an eilicient evacuating means ~Il of the
\ the invention will appear from the following de ‘type shown and 'an'e'ilicient condenser 2,3 'the
m scriptlon oi’ a preferred embodiment' thereof, apparatus thus far described is a very eiïective 25
I te. .n in commotion with .the accompanying means for cooling liquid introduced into the shell
u.: in whicha ‘ ' Il_l. For example, it is quite feasible to freeze
‘ i» '1 e 1 is a diagrammatic view ot a crystallizer water in the shell i0, notwithstanding thel fact
embodying my invention, and ' that the cooling water available for use inthe coil
' a0 Pig. 2 is a sectional view taken on the line 2--2 23 is at ordinary summer temperatures. 3@
o! Fis. 1. . « . ~lin crystallizing salts from solutions containing
Referring to the drawing, the reference nu them the solution is introduced by the pipe I5 and
meral I0 designates- an evaporating shell. the the booster ejector il is put into operation, like
upper part >of which is substantially cylindrical in wise the vacuum pp 21. 'As a result of the
35 form.' the lower part being hopper shaped and high vacuum> produced in the shell I0, for ex- 35
communicating .with aÍ barometric leg Il which ample a vacuum of 29 inches of mercury when
, may be provided with a valve I2. The barometric the atmospheric pressure stands at 30 inches, a
leg I'I» extends downwardly and terminates in a certain amount of ebullition occurs within the
trough I3 which is adapted to make a liquid seal shell l0 and the resulting evaporation cools the
4o at the bottom of .the leg Il. It will be under liquid to a point where crystals deposit to ade- 4@
stood that the leg I i is oi sumcient height so that sired extent.- - " » .

‘ . when the shell is evacuated to a substantial degree,-
for example.- about 29 inches of mercury, the
surface oi' the liquid in the shell I Il isat a rela
tivelyl low point on the'cylindrical portion thereof,
so that ample vapor space is provided above the
.surl'ace‘ior the ebullition which takes place.
Suitable stirring means are provided for agitat
lng the ,liquid wlthin‘the shell l0. These'mcans
60 may?` suitably consist o! propellersv M_ mounted on
shaits i! which -are driven by suitable means (not
shown) 'so as to agltate the liquid thoroughly.
The solution from which salts are to be crystal
\ lined is suppliedby a valved pipe Il.
i», The mercado! the shell II isprovldedwlth
'I‘he vapors from the'ahell I0 together with the
,steam introduced bypipe I8 are commingled in.
the venturi 22 and are i‘lnally condensed in the
condenser 23. In practicing crystallization in 45
this manner I have found that` a considerable
_ amount oi salt is deposited on the_ walls of the
shell’ Il above the liquid level, this deposit result
ing from the splashing of the chilled solution
upon these walls.~V Here the iilm- oi liquid is sub- oo I
lected to the full effect of the vacuum and the
water evaporates therefrom rapidly so that the
deposit grows as the crystallization is continued.
» ` I have also found that the overhead carries with
it a certain amount oientrainment which builds 66
 »,ooaoss
up on the nozzles 2|, which “nomles are at high Having thus described my invention I declare
temperature owing to the passage of steam there that what I claim is: v
through. The entrainment hitting these nonies l, A vacuum crystallizer comprising a chamber.
is immediately deprived of its water content so adapted to contain solution and provide a vapor
that the salts build up thereon. _ „ space thereabove, means for withdrawing vapors
In order to render the operation continuous I to_ create a vacuum in the chamber and com
provide within the shell I0, preferably at a posi press the withdrawn vapors, cooling means for
tion as high as possible therein, a spray Pipe 2s condensing said compressed vapors, and means
which is preferably annular in form and provided for injecting liquid upon surfaces within the va
with spray openings adapted to distribute liquid por space oi' said chamber in order to prevent
around the whole surface of the cylindrical wall accumulation of solute thereon.
of the shell. This liquid is adapted to iiow down 2. A vacuum crystallizer comprising a chamber
wardly over this surface and remove any salts adapted to contain solution and provide a va
deposited thereon or prevent the deposition of por space thereabove, means for withdrawing va
any salts thereon. 'I'he pipe 2. communicates pors to create a vacuum in the chamber and com 15
with .one or more valved pipes 2l so that a con press the withdrawn vapors, cooling means for
trolling supply of liquid can be supplied to pipe condensing said compressed vapors, and means
28 continuously or at intervals. The nature of for injecting liquid upon the internal surfaces of
the liquid supplied to the pipe 2l will depend , the vapor withdrawing means in order to prevent
upon the nature of the precipitate on the walls. accumulation of solute thereon. 20
or the salt or substance which isbeing crystal Y 3. A. vacuum crystallizer comprising a shell
lized. The solvent in the solution being evapo adapted to contain solution and provide a va
rated is always suitable. In many cases where por space thereabove, means for withdrawing
the solution being evaporated is relatively dilute, vapors tocreate a vacuum in the chamber, and
‘a certain portion of the feed supplied to the means for injecting liquid upon the internal sur 25
shell lil may be introduced by the pipe 2l. In faces of the vapor withdrawing means in order
order to remove the, deposit of salts or the like to prevent accumulation of solute thereon.
upon the nozzles 2| I provide a valved pipe 3l 4. 'I‘he method of crystallizing solute Lfrom
adapted to deliver water or other suitable liquid solutions which consists in supplying said _solu
upon these homes. In the embodiment of the in tion to a closed chamber, maintaining a vapor
vention illustrated I have shown the pipe 3l de space above said solution in said chamber, with
livering into the top wall of the chamber 2l. drawing vapors from said space and maintaining
' In addition to the supply of liquid by means of the a substantial vacuum therein thereby causing a
pipe 30, I prefer to provide in opposite walls of fall of temperature below that necessary for the
the chamber 2li, openings 3l for the supply of precipitation oi' crystals, injecting ~liquid upon
further quantities of liquid. ’.'ll‘heL openings ll surfaces within said vapor space to prevent ac
are preferably located near the level of the low cumulation of solute thereon and- withdrawing
est nozzles 2| so that the. overhead can'ies the said crystals from said chamber. _
spray with it over the outer surfaces of the noa 5. 'I‘he method of crystallizing _ solute from
40 zles whereby the deposit of solute is effectively solutions which consists in supplyinß said solu
prevented or removed. The openings _ 3i are' tion to a closed chamber provided with an ejector
supplied with said liquid by means oi’ valved pipes communicating with the .upper portion of said
32. It is to be understood that it is not intended chamber, withdrawing vaporsfrom said space by
to limit the invention to this disposition of the said ejector and maintaining a substantial vacu
45 means for supplying liquid to the ejector, since um therein- thereby causing a fall of temperature
such means may be located in any position below that necessary for the precipitation of
whereby they are effectively adapted to remove crystals, injecting liquid into said ejector to pre
or prevent deposit of the solute on the nonies 2i. vent accumulation of solute therein. and with
_ While the liquid supplied to the ejector may drawing said crystals' from said chamber.
50 suitably be a solvent for the solute, this is not 8. A vacuum crystalliser comprising a chamber
necessary since the removal of the deposit is at adapted to contain solution and provide a vapor
least partially mechanical due to great changes space thereabove, means for withdrawing vapors
of temperature fracturing the deposit. I nnd to create avacuum in the chamber and compress
that after running for one hour, that by turn -the withdrawn vapors, said means including
ing on the liquid supply for _three minutes and ejector tubes adapted to convey steam at high
then turning on the steam the deposit is sub temperature, cooling means for condensing said
stantially fractured and falls from the noßles. compressed vapors and steam, and means for in
In the preferred manner of operating, I prefer jecting liquid upon the outer surfaces of said
to supply a small amount 'of liquid continuously ejector -tubes for the purpose oi' removing accu
by the pipes 2l, that is, an amount of liquid mulated solute therefrom.
which will keep any entrainment striking the 7. A vacuum crystallizer comprising a shell
walls from depositing crystals thereon or which _adapted to contain solution and provide a vapor
will cause crystals on the walls to.remain slushy space thereabove, means for withdrawing vapors
and become washed down by the stream of liquid. to create a vacuum in the chamber, said means
As stated above, it is preferred to supply liquid comprising ejector tubes adapted to convey steam
by pipes 3l and I2 for short periods at compara at hightemperature, and means for injecting
tiveLv long intervals, for example, periods oi' liquid upon the exterior vsurfaces of said ejector
about three minutes at intervals of about one tubes, for the purpose of removing accumulated
hour. ’ l solute therefrom.
Although- the invention has been -described in 8. The continuous method of crystallizing so 70
connection with the specific details of_a_prei'erred lute from solutions which consists in supplying
embodiment thereof, it is not intended that such said solution continuously to a closed chamber
details should be considered limitative of the in so as to pass over unsubmersed portions of the
vention except so far as set forth in the accom wall thereof so as to prevent deposition of solute
panying claims. thereon, maintaining _a “Por space above said
 2,067,043 3
solution in said chamber, continuously withdraw taining a substantial vacuum therein, thereby
ing vapors from said space and maintaining a causing a fall of temperature below that neces
substantial vacuum therein, thereby causing a sary for the precipitation of crystals, intermit
fall of temperature below that necessary for the tently injecting liquid upon said ejector tubes to
precipitation of crystals, and continuously with remove solute deposited thereon, and continuous
drawing said crystals from said chamber. ly withdrawing said crystals from said chamber.
9. The continuous method of crystallizing so-y 11. A continuous method of crystallizing solute
lute from solutions which consists in supplying from- solutions which consists in continuously
'said solution to a closed chamber, maintaining supplying said solution to a closed chamber pro
10 a vapor space above said solution in said cham vided with an ejector communicating with the
ber, continuously withdrawing vapors from said upper portion of said chamber, said ejector com
space and maintaining a substantial vacuum prising an ejector tube adapted to convey steam
therein, thereby causing a fall of temperature ` at high temperature, continuously withdrawing
below that necessary for the 'precipitation of . vapors from said space by said ejector and main
15 crystals, continuously injecting liquid upon sur taining a substantial vacuum therein, thereby 15
faces within said vapor space to prevent accu causing a fall of temperature below that neces
mulation of solute thereon, and continuously sary for the precipitation of crystals, injecting
withdrawing said crystals from said chamber. liquid into said chamber so as to cause the in
10. The continuous method of crystallizing so jected liquid to flow down the unsubmerged walls
20 lute from solutions which consists in continuously thereof and prevent accumulation. of solute there 20
supplying said solution to a closed chamber pro on, intermittently injecting liquid upon the ex
vided With an ejector communicating with the terior of the ejector tubes for the purpose of
upper portion of said chamber, said ejector com removing solute deposited thereon, and contin
vprising an ejector tube conveying steam at uously removing said crystals from said chamber.
high temperature, continuously withdrawing va 25
pors from said space by said ejector and main HAROLD B. CALDWELL.