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Патент USA US2057598

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Oct. 13, 1936.
Filed Oct. 23, 1934 w
5 Sheets-Sheet l
0a.‘ 13, 1936.
Filed Oct. 23, 1934
3 Sheets~Sheet 2
Oct. 13, 1936.
Filed Oct. 25, 1934
3 Sheets-Sheet 3
Patented Oct. 13, 1936
rnocess orisrmm'rm‘c A mourn m'ro
Paul 'Schuftan, Hollriegelskreuth, near Munich,
Ernst Karwat, Grosshesselohe, near Munich,
and Albrecht Steinbach, Wiesbaden, Germany '
Application October 23, 1934, Serial No. ‘149,668 '
. In Germany November 1,1933
12 Claims. _(CL 62-124)
This invention relates to a process for resolv-_
ing solutions and liquid mixtures into their con
stituents by crysallizing and separating individ
ual constituents thereof.
It is known to'separate and recover constitu
ents of solutions by converting either the solute
or the solvent into the solid condition and then
separating the solid and liquid phases. In.this
manner salts can be deposited from solutions,
10 and concentrates can be produced from liquids
(such as 'milk) by freezing out the contained
water. For the latter- purpose’ in particular, it
has been proposed either to. transform the liquid
into a more or less compact "pulp of ice crystals
by cooling accompanied by agitation, or to freeze
the liquid into blocks and then crush the blocks
and then separate the ice from the mother liquor,
for example by centrifuging.
' Denying drawings which illustrate -= -
: |
ically and by way of example‘ various embodi
ments of apparatus suitable for carrying the
present invention into practical effect, and in_ 5
Figs. 1 and 2 are respectively a transverse sec-'
tion and a' top plan view of a refrigeration cell;
Fig. 3 is a longitudinal section through a re
frigerating apparatus embodying a plurality of
refrigeration cells on the line 3-3 of Fig. 4;
'- Fig. 4 is a top plan view of Fig; 3; Fig. 5 is a section through a second embodi
ment of refrigerating apparatus; and
Fig. 6 is a front elevation withparts broken
away showing the interior in section, of a cen 15
vtrifugal apparatus for the treatment of the ice
masses produced in the-refrigeration cells.
In carrying out the invention, the milk after
having been freed from gas-if desired by evac
uation—is cooled in a circular annular vessel 5, m
The present invention contemplates a process
.20 -for resolving solutions into their constituents
which is substantially simpler in operation than the internal diameter and height of which corre
the processes hithertosuggested. To this end, spond to the dimensions of the basket 24 of the
according to the invention, the liquid to be re -centrifuge 23 (Fig. '6). It has been ascertained
solved is cooled in,a. vessel of a shape adapted to that,- under these conditions, the ice is deposited
25 that of the apparatus employed for separating in the form of acicular,. or'lamelliform crystals, 25
the solid and liquid phases, the cooling being which are practically all orientated in the direc
tion of the steepest temperature gradients,
' carried to suchan extent. that a structurally
stable body that is to\say,-'a solid body which namely in the radial direction of the annular
vessel I, the concentrate accumulating, at ‘the
retains its shape, is-obtained which can be di
30 rectly inserted into the separator and further ‘same time, in the radially disposed interstices and 30
channels between the ice crystals. The. cooling
treated therein.
The temperature gradient during the cooling. process is continued until the desired amount of
process should be greatest in the direction in _ice.has been precipitated, or at least to such an
extent that the ice skeleton formed in the re
which the forces act during the subsequent sep
frigeration vessel l is su?iciently strong to allow 35
35 aration of the crystals, and concentrate. Ex
' periments have shown that, in such case, the
the mixture of ice and concentrate to be trans
orientation of the crystals formed coincides with
‘the direction of the action of force during the
ferred to the centrifuge 23 without collapsing.
separation, so that a particularly easy and ef-.
annular block of ice is taken out of the refrig
eration vessel I, if necessary after warming the 40,
walls of the latter, and inserted, without loss or!
shape, in‘the cage 24 of the centrifuge 23.
In order to facilitate the withdrawal of the
fective separation of the liquid and solid phases
results. The lowest temperature attained in cool
ing must be above the eutectic temperature‘ of
the constituents to be separated, since otherwise,
complete separation of the constituents is funda
45 mentally impossible. Nevertheless, in certain
circumstances, ‘for example when a high rate
of cooling is desired, a partial descent below the
eutectic temperature is permissible, if s the '
moulded‘ body be correspondingly warmed prior
On the termination of the cooling process, the
_ '
moulded body from the refrigeration ‘vessel I, ~
the latter is preferably of downwardly tapering 45
design. The upper edges 4 of the vessel are
curled over outwards, so that the block of ice_
can be easily removedyby
the vessel,
without the milk becoming contaminated with‘
the freezing brine. A slightly different method 50
to the separation of the two phases.
The process. of the present invention will here ‘ of. extracting the frozenblock consists in allow
inafter be more fully described as applied to the ing hooks or carriers 2 (Figs; 1, 2 and 6) to
production of a milk concentrate by freezing out freeze into the ice, and employing such devices
the water and then separating the concentrate for‘ withdrawing the moulded body and trans
55 from the ice, and with reference to the'accom-. ferring it. to the centrifuge.
In the subsequent centrifuging process, the. moved from the centrifuge conjointly ‘with the
centrifugal forces generated act in exactly the
same direction as that in which the interstices
interchangeable sieve or carrier 2, and‘ is melted
by direct or indirect heat exchange with the
between the crystals'which-are occupied by the‘
concentrate, are disposed. Consequently, in the
herein-described process, the concentrate is read
In order to shorten the Yfreezingperiod and
also to ensure the most complete separation of
ily and extensibly separated from the ice, where- the concentrate. 'from the ice in centrifuging,
as hitherto,-the concentrate (and therefore dry the width of the annular refrigeration vessel
substance) always remained so closely im-. should not exc‘eeda few centimeters. In order
‘10 prisoned between theindividual. crystals, rela
further to increase thetransmission of heat be 10
tively orientated in diiferent directions, that tween the .refrigerating'medium, and the milk,
even the most intensive centrifuging enabled the refrigeration vessel is moved in relation to
only ‘a relatively incomplete separation to be the refrigerating medium-for example by ro
obtained. In general, the steepesttemperature
tation on its axis--on the one hand, and on the
gradient can be sodirected- that the direction’ . other hand a moderate movement towards the 15
in which the separation of the solid phase from
refrigerating walls is imparted to the milk. In
‘particular, a movement havinga powerful verti
plane as that in which the crystalline lamellae .‘ cal component, is imparted to the refrigerating
the liquid phase takes place, lies in the same
‘ liquid, so that, in the main, it ?ows in a vertical
Should. wrongly orientated crystals tend‘to direction along the walls of the refrigeration 20
v grow at the edges. andrims of the annular ice ' vessel.
block, from which the concentrate is di?icult .to . _ .The cooling of the annular refrigeration cells .
expel, the, transition of heat, and thus the rate will hereinafter be more ‘_ fully ‘explained, with
of growth of such crystals, can be reduced, by_ reference to Figs. 3 to 5;
.the provision of heat-insulators ,3, (Figs. ‘1 and
In Fig. 3, ll represents the refrigerating tank 25
2) > at these places, so as to preventthe occur
for the cells, said tank being cooled, for example
by the evaporation of a refrigerating liquid, such
'- rence of this source of trouble.
By operating in the herein described manner,‘
as ammonia, in the pipes H2. The wall 5 has an .
relatively compact ice is obtained, in thin strata opening forthe' propeller l3 and other openings
30 exhibiting narrow intermediate channels. The ' from which the pipes 15 project upwardly. The 30
ice has a temperature, below 0? 0., corresponding annular freezing vessel I is positioned so that it
to ‘a state of equilibrium with the concentrate. , surrounds one of the pipes I5 and lies' between
When moisture ‘now penetrates into‘the narrow ' other of the pipes. In operation the cooling liq- _
-channels--for example as the result of the in- uid flows down through the‘propeller [3, over
terior surface of the‘ ice block becoming par
tially melted by' th'ewarm air agitated by the
the pipe l2, up through pipes.l-5 .and out of the 35
open endsthereof, down over both the inner and
I ' centrifuge-the water freezes in the channels of
outer' walls of the freezing‘ vessel l, and back
v» the still colder interior‘of' the iceblock, thereby
along the upper- face ‘of the partition wall 5 vto
the propeller I3. The pipes l5 can be replaced
choking said channels and rendering impossible
40 further separation of ice and-concentrate.
this account, in carrying out the invention, any
warming of the inner surfaces of the'ice block
in the centrifuge is‘ prevented, for example by
' employing an'annular cage--si_milar_to there
45 frigeration. vessel-the inner wall. 25 of the cage
being ‘solid and thus’ keeping the ice .ring out
.of ‘contact with
air. .
' .
by plates, or the like devices for guiding the 40
A somewhat different method of cooling is r‘ep
resented in Fig.5. In this case, the annular re
Irigeration cell I is not completely immersed in
the brine tank, but the brine flows from a high
level cooling tank, through the pipes I 6 and I], _,
Ito the distributing pipes 18‘ and I9, by‘ which it
_ A- sinteringeffect; however, may beexerted, ' is sprayed against the upper edge of the refrigy
for. the ‘same reasons, on theice block by the oration cell I, then ‘runs down the latter, is colWashing liquid. This di?iculty is. overcome by ‘lected in the vessel 21 and then, returned to the 50
using instead .of pure water, in the first washing,
.a solutionthe concentration of which is ‘adapted
brine cooler by the pump 22. The advantage of‘
this method is that the amount of brine-to be
kept in ‘circulation is substantially less than in
to the temperature of theice-for the timev being,
‘_ so that the stripping liquid in the channels can-. the case of the usual cell tanks, and it is there-‘ I
fore possible toadapt the brine temperature ‘to
55‘ not freeze. To this end, use. is made, for ex
.ample, of- progressively more dilute solutions, the momentary freezing temperature in the cells,
during the stages of the process. Moreover, the
" I sprayedon to'the ice through an atomizer noz
zle' 21-. When the ice has reached 0°C., it may expensive cell. tanks otherwise required can be
be ~_washed with ~pure water, if desired. This replaced by a simple wooden enclosure.
A' somewhat different method: consists inset 60
60 method of stripping ‘the ice can be combined in
a simple. manner, with the‘. protection against _ ting the" cells inrotation and providing spiral
sinter'i'ng, by allowing a ,pre-cooled gas, more stages or. strips' on the interior _-wall and-if. de
particularly'air, to ?owover the inner wall‘ of the sired also on the ,outer wall of‘ the cells,'which
r‘ ice ring. The'temperature of the gas'during devices impart a su?icient vertical movement to
the centrifuging of the ‘concentrate, is approxi the refrigerating 'liquid‘ dining the rotation, of
mately'the same as the vmelting ‘temperature of
'The' advantages of the herein described ‘new
the ice-for the time being. For the purpose of
- '70
.65 '
the stripping operation, its ‘temperature is grad
process are ‘that the operation is simpli?ed and ~
ually raised in the desired degree, so that small
the apparatus substantially. cheapened.‘ ~ In con
trast to the processes- operating by imparting
quantities of ice water are~ formed, which, at
the{ outset,‘ form with the dry‘ substances ad
, movement to-the material. to be cooled, the me- .
her'ing to the ice a concentrated solution which . chanical stressing of the walls is absent, so that
‘becomes progressivelymore dilute, as the result weaker wall material, such as ‘enamel, can' be
~ of the stripping, during the process.
The centrifuged ice block is preferably re
employed in place of rustless steel. Moreover, _ '
the ,effectthat may be‘ produced‘ by material 75 j
g 1_
_ scraped oil! from the walls or. stirrer-s, .on the‘
- ,?avour of sensitive substances, such as milk and
phase by subjecting the mass to centrifugal force.
5. A process for the separation of the .con
‘fruit juices, is prevented. By- comparison with
stituerits of liquids as de?ned in claim 1 in.
. ‘the processes in which'the solution to'be concen-
which the mass has two substantially parallel
5 trated is frozen to a'block. the latter being then? faces and the liquid phase thereof is separated, 6
' '
v‘crushed-land further treated vin a centrifuge, the _ by forcinga ‘fluid through the mass in the direc
newprocess offers the advantage that the freez- tion perpendicular to said faces.
in'g period is sulwtantially reduced, one working
6. Process for the separation of the constitu
stage "is saved,- the purity of the product‘ being cuts of liquids as de?ned in claim 1 in which
10 thereby improved and the loss of cold and sub-, in‘ cooling the body of liquid a temperature '10
‘stance lessened. Furthermore, as the result of gradientis' maintainedin a predetermined di
‘the orientation‘of the crystals, theseparation of rection through said body whereby an orienta
the two phases can be carried out with the same tion -'of the resulting solid phase of the mass
expenditure of labour and with an improved in said direction is produced and in which, in
15 yield. ~
the separation of the solid and liquid phases,
' The invention is obviously not restricted to the
the force for displacing the liquid phase is-applied
foregoing example of concentrating milk, but can
in said direction.
'‘ -
" be similarly applied to the concentration of other
'7. Process for‘ the separation of the constitu
liquids, especially such as are sensitive to ?avour- .ents of liquids as de?ned in claim 1 in which an
. 20 ing in?uences. It can also be ‘applied to- the
puri?cation of dissolved substances, suchvas an-, hydrous acetic acid, or salts.- ‘
_' <
annular-body of liquid is converted into an an- 20
nular' structurally stable mass by maintaining
a temperature gradient radially of said-body and’
It is moreover‘ immaterial for the purposes ‘of
the present invention whether the separation of
25 the solid and liquid phasesbe performed in a' centrifuge. The only essential feature is to pro-
in which the force serving to separate the liquid
phase from the solid phase of the mass is applied
radially thereof. 7
‘ 8. Procas for the separation of the constitu
duce, ‘by refrigeration, amoulded body- that can ents of liquids as de?ned in claim 1 in which an ,
be directly transferred into the separating de- _ annular body of liquid is transformed'into an
. vice, and that the cooling is performed in such annular structuralLv stable mass and the liquid
' . 30 a manner. that theorlentation of the crystals phase of said mass is separated from the solid 30
the direction of the forces e?ect-
ing the-separation: of the two phases.
Thus, for
phase by centrifugal‘ force acting radially of
example when ?lters are employed for separating
" “thetwophases, the moulded body issshaped as a
.4 9. Process for the separation or the constitu
ents of liquids as de?ned in claim 1 inwhich a
corresponding to the-?lter, said disc being body of liquid having'at least two substantially 35
cooledfrom the end surfaces'in such a manner
parallel faces is transformed into a structurally
, a» -~ .thatsthe crysigls and the channels containing - stable mass by‘ cooling while maintaining a
the mother liquor are orientated at right; angles temperature gradient between said facesrperpen=—~~—~~'
‘ ‘to said'surfaces and therefore in the direction of dicular theretmand in which the, liquid phase is, '40 the suction e?ort of the ?lter.
1; ,sepmatedfrom the ‘solid phase by force applied 40'
we claim:\—->\'m\
perpendicular to said parallel faces.
1..A process for the‘éeparation of the con-
10. Process for the separation of the constitu=
stituents- of liquids whichcomprises transform- ' cuts of 'liquidsasde?ned’in'claimd inwhicha
,ing a body of a liquid by cooling into a strucfturalwlbndy-ofrliquid having at least two substantially
" ' 45 _ly stable massofthejsame‘shapeas'said body of
liquidsaid mass comprising ‘a solid and a liquid
parallel faces is transformed into‘ a structurally 45,
. stable mass by cooling while maintaining a tem-
H ~ " a
phase, and applying force to said mass without‘! peijaturegradient between said faces perpendicw
‘ ~dislntegration'thereof' for the separation of' said
solid and liquid phases.
lar thereto, and in which the liquid phase is
, separated from the‘ solid phase by forcing a
.2. A process for the separation ‘of the con-- ?uid through the mass in a directionperpen- 50
stituents of liquids as ‘de?ned in claim 1 in ‘ dicular to said faces.
which. the-solid and liquid'phases‘of said mass
11. A process for the. separation of‘the-con
- are separated by subjecting the massto centrif- ' stituents of liquids as de?ned inv ‘claim 1 in which
' -
'the mass‘ is washed with a liquid which will not
3. A process for the separation of the con- . solidifyat the‘temperatura of the mass.
~ stituents of liquids as de?ned-in claim 1 in‘ ; 12. A process for the separation of the con
, 'whichithe solid ‘and’ liquid phases of said mas ‘ 'stit‘uents' of liquids as de?ned in claim 1 in which
aTreseparated by forcing a ?uid
a stream of- gasrat a slightly higher temperature
1 than‘ the mass is contacted therewith.
60' 4.-A process for the separation of the con-.
stituents of liquids as de?ned in
1- in
which the mas is annular in shape and in which
.the liquid phase is separated from the- solid._ -
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