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Патент USA US2411238

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Nov. 19, 1946.
2,411,238
J. ZENDER
PROCESS AND APPARATUS FOR DIALYZING SOLUTIONS
Filed July 8, 1943
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INVENTOR.
BY JUST!
ZENDER - ‘
Patentecl- N... 1c, 1946
2,411,23
v
" . STATES “PATENT time
amass
PROCESS AND‘APPARA'I‘US FOR
DIALYIZING SOLUTIONS
Justin Zender, Fredericksburg, Va.-, assignor to
Sylvania Industrial Corporation, Fredericks
burg, Va., a corporation of Virginia '
Application July 8, 1943, Serial No. 493,918 '
l
7 Claims. (Cl. 210-85)
2
The invention relates in general to dialysis, and,
In the now preferred embodiment the apparatus
in particular, to a process and apparatus for the
separation of a soluble. substance from its solu
comprises a. chamber having headers disposed
transversely adjacent each end to divide the
chamber into three separate compartments,
tion by dialysis, and to correlated improvements
designed to enhance the structure and function
and to extend the uses of such apparatus.
It has been Proposed to dialyze soluble mate
_ tubular dialyzing membranes connected at each
end to the headers and communicating with a
common liquid compartment, and means for pass
ing a ?uid around the tubes in the central com
rials from their aqueous solutions through hydro
philic membranes, such, for example, as sheets of
regenerated cellulose, parchment paper, and the
‘ partment.
?rmly sealed to avoid loss of liquid during dialysis.
-_In the following speci?cations and in the ap
pended claims, the term “dialyzate” will be used
to designate the solution being dialyzed in accord
ance with recent usage in the art; the term “dif
fusate” will designate the solution of the material
which diffuses through the membrane during
To clean the apparatus or to replace a broken
sheet, it is generally necessary to completely dis- -
dialysis, ‘and the term “dialysis” will be used to
designate the diffusion of soluble substances
‘ like.
However, dialyzers employing membranes
in the form of ?at sheets have certain inherent
disadvantages. For example, the edges of the
.sheets must be maintained under pressure or
mantle the dialyzer. Further, to decrease break
through a semi-permeable membrane from one .
age, the membranes must be supported over their
liquid into another. '
‘
surfaces. Finally, such prior apparatus did not '20 4 The invention accordingly comprises the
provide any 'means for retarding the dilution of
features of construction, combinations of ele
the solution being dialyzed. Thus, sheet dialyzers
ments, and arrangement of parts which will‘be
of prior design have generally been complicated
exempli?ed in the construction hereinafter set
in construction, dif?cult to repair or- to clean and
forth and the scope of the invention will be in
capable of handling only small volumes of liquid. -25 dicated in the claims.
Accordingly, it is a general object of the present
For a more complete understanding of the;
invention to provide a dialyzer which will be
nature and objects of the invention, reference
capable of handling large volumes of liquid and
should be had to the accompanying drawings in
which will operate rapidly.
which
It is a further general object to provide a 30
dialyzing apparatus which is easy to construct
and to'clean and in which broken ‘membranes
may be replaced without completely dismantling
Fig. 1 represents a side elevation, partly in’ sec- -
tion, of one embodiment of the apparatus of the
invention;
Fig. 2 represents a cross-sectional view of the
dialysis chamber of the apparatus of Fig. 1
It is another object of the invention to provide .35 taken along the line 2-2 thereof;
a process for the separation of water-soluble
Fig. 3 is a side elevation, partly in section, of
substances from their aqueous solutions in a rapid
one of the dialyzing tubes used in a second em
and ef?cient manner, and in particular for the
bodiment of the apparatus;
separation of products of fermentation from the
Fig. 4 is a side elevation, partly. in section, of ‘
fermented liquor.
_
40 the dialyzer of the invention utilizing a, double
A speci?c object is to provide an-apparatus
tube;
having means for retarding the dilution of the
Fig. 5 is a top plan view, in section, of the-ap
solution being dialyzed._
‘
_
,
paratus of Fig. 4 taken along the line 5—5 there..
Other objects of the invention will in part be
of ; and
_
.
obvious and will in part appear hereinafter.
Figure 6 is a top plan view in section of-the
45
the dialyzer.
According to the present invention, there is
provided an apparatus for the dialysis of solutions
comprising, in combination, a chamber, a .mul
tiplicity of tubular dialyzing membranes disposed
apparatus .of Figure 4 taken along the line 6-6
' thereof.
In that embodiment of they apparatus shown
in Figs. 1 and 2, the dialyzing chamber proper
therein, means to pass the solution to be dialyzed 50 comprises a vertical outer chamber 10, which is
into contact with one surface of the tube, means
shown as a cylindrical chamber, but which may
to pass another liquid into contact with the
be of any cross-sectional shape. The chamber is
other surface of the tube, and preferably means
to continuously concentrate the solution. being
dialyzed so as to increase the rate of dialysis.
closed at the top by a removable plate II, and is
closed’ at the bottom by a conical base [2, which
55 is provided with a drain I3 having a valve l4.
' 2,411,288
,
Situated, adjacent the. ends inside the chamber
"I8. ‘there are positioned headers I8 and 16, each
-.4
‘
the invention can be arranged without transcend
ing the scope of the invention so as to provide
provided with a plurality of holes. Short sections
thatthe dialyzate and the di?'usate both ?ow up
of pipe H are threaded into theupper header I5
ward or downward in the same direction instead
and similar sections of pipe 22 are threaded into 5 of ?owing countercurrent to each other as shown
in Fig.1.
_
the lower header I6, These pipes serve to anchor
the dialysis tubes I8 to the headers.
C
,
Further, the apparatus of the type shown in
The chamber-1H] is provided with a removable
1 may be so readily modi?ed by anyone
side portion 38 which makes the interior accessi
‘skilled in the art, without transcending the‘ scope
ble from the outside. When it is desired to 10 of the present invention so that the chamber I8
change or replace a tube, the apparatus is ‘
and the tubes I8 are ‘disposed’ in a horizontal
plane. Inasmuch as the tubes I8 during oper
ation are‘ not only completely ?lled with liquid
drained, the bolts 39 removed, and the side por
tion 38 of the chamber and the plate I I taken
out. The‘ upper end of the tube is then pulled
but- also are completely surrounded by liquid,
through the section of pipe l'L/and the end turned 15 the tubes willrequire little or no horizontal sup;
down over the upper end of the pipe H to form
port. ‘If the tubes I8 are ?lled with .dialyzate,
I the cuff 23. The band 24, which may be formed
which has a higher speci?c‘gravity than the dif- .
‘ of rubber, as shown, or of metal or the like, is
fusate, the ‘tubes will tend to ?oat so that they -
then slipped over the cut? 23, anchoring it se
can be kept in position merely by suitable guide
curely to the pipe IT. A band‘24' similar to the, 20
pins. i
‘
'
band 24 is then slipped over the free lower end
There is also shown in Figs. '3, 4, 5v and 6 an
of the tube‘ I8, and the end of the tube inserted‘ , other embodiment of the apparatus of the invenover the upper end of the lower pipe 22'. The
tion in which the dialyzing tubes are double or
band 24' vis'then slipped down“ over the end of
multiwalled.v Referring to Fig. 3, this-embodi
_ ‘the tube I8, anchoring it securely to the pipe 22. 25 ment comprises. an inner dialyzing tube I811.
The coupling shown in Fig. 1 has the advantage
surrounded by a dialyzing tube I8b of vlarger di- >
‘of maintaining the maximum diameter of the
tube I8 at the joint, and thus does not interfere
ameter, and, if necessary, supported externally. >
by means of a textile ‘tube I8c made of an open
mesh fabric whether of woven, knitted, or braided
with the flow of the liquid through the tube I8. ’
The dialysis tubes I8 may be disposed and 'ar- 30 construction. The surrounding outer dialyzing
ranged within the chamber I0 in any desired
tube IN: is particularly advantageous when-it is
manner, in rows, for example, or in concentric
desired to concentrate the dialyzate while it is
circles as shown in Fig. 2.
' being subjected simultaneously to dialysis. Thus
The space between >
the tubes can be varied as desired, ‘but in general
a distance of the order of 1/2 to 1 inch is sum- 35
cient. It is to be understood‘ that a space exists
around all of the vtubes illustrated in Fig. 2, and
that none of these tubes are in direct‘contact
with each other along their longitudinal surfaces.
It is to be understood that the apparatus shown 40
in Fig.‘ 1 may be constructed and arranged so
that the dialyzate may be caused to pass inside
’ the tubes. or outside the tubes, but for the pur
pose of illustration only, the apparatus of Fig, 1
is constructed and arranged so that the 'dialyzate 45
a plurality of the tubes‘ illustrated in Fig, 3 may
be supported between the headers as shown' in
the apparatus of Fig. 4,‘ leaving an air space'35
can be introduced into the lower section 25 of a
‘Illa requires the‘ use of double headers at'the.
‘top andbottom of the chamber. Accordingly. the
between the tubes. The side walls of the cham
ber 35.are solid as shown in the ?gure. However,.
there are no front and back walls to the cham
ber 35, as‘ is fully brought out in Figure 5. Thus ‘
it is possible to blow air through the chamber 35
across the outer surface of the tube I8c, thus
causing an evaporation of liquid through the wall
of the tube I8b, as shown in Figure 5.
Positioning ‘the double tubes in the chamber
the chamber I8 by means of the pipe 28, the di
alyzate ?lling the lower section of the pipe up
outer tubes I 8b and I80 are a?lxed to the inner
ward through the interior of the tubes I8-and
headers I5a and Ilia, while the inner tube I8a 7'
?lling the upper section 21 until ‘it over?ows‘ 50' is a?ixed to the lowermost header I5 and the
‘through the outlet 28. The di?usate will be 111-.
troducedinto the intermediate chamber 29 at
a the top through the pipe 38 and will be removed '
‘ uppermost header It. In this embodiment, it'is
preferable to have the dialyzate occupy the space ,
between the tubes 18a and I'8b, and to have the
at the bottom through the pipe 3|. It is to be \ diifusate occupy the space in the interior of the
understood that the circulation of the dialyzate 55 tube I8a. Accordingly. referring to Fig. '4, the
and/or of the diffusate may be continuous or
dialyzate is introduced into the lower section 25a
intermittent. ‘When it is desired to clean the
through the inlet ‘tube 26a so that it ?lls the‘ '
apparatus, the dialyzate may be drained off
lower section and rises through the space be
through the exhaust ‘pipe I3 which is positioned
tween the tubes I So and I8!) and ?lls the upper
at the lowermost point of the bottom section 25. 60 section 21a and ?ows out through the exit tube
It should be noted that the present apparatus
28a. The diifusate can be introduced at the top
is so constructed that the dialylzing tubes I8 are
of the chamber into the section 86 through the
completely submerged in liquid so that no por~
pipe 30a, whereupon it ?lls this section and ?ows - '
tion isin contact withthe air. This is a desir
down through the interior of the tube I 8a and
able feature since it has been found that cer- 85' ?lls the lower section 81 from which it passes
tain- membranes, particularly those formed of
throughythe exit tube 3| a.
non-?brous cellulosic materials, are attacked by i ' Since the front and back walls of the chamber
certain bacteria or organisms found in fermented , v35 are open, ltlis a simple matter to a?ix the“
sugar solutions and molasses ‘resulting in the
tubes I81) and rI8c to'the header IIa. In order/
rapid deterioration -,of .the‘membrane.» This ac- 70 to provide access to the inner ‘tubes I841 in the
tion is avoided or substantially retarded when
chamber 25a-and to the upper parts of the outer
the'm'embranes are completely submerged in the
tubes I8b_ and I8c in the chamber 2'Ia'and the
liquid, and precautions are taken to avoid in
upper part of the innertubes I8a, and. the chem; '
troducing bubbles of air in either of ,the liquids.
ber 36, removable front portions are provided in
' It'is also to be understood that the apparatus of 75, the walls of the chambers.‘ A typical construc
5
2,411,238 '
tion oi’vthe walls of each of these chambers is
the wet gel state, i, e., while they are swollen
shown in Figure 6 which represents ‘a cross—sec
with water.
tional view of the chamber 25a taken along the
line 6-6 of Figure 4. The removable front wall
portion 45 is ailixed to the apparatus wall‘ Illa
by means of the bolts 41. Similar removable wall
portions are provided in chambe'rs'Z‘la and 36.
,_
.
On the other hand, when it is desired to sepa- ,
rate a hydrophilic organic liquid from water or
organic compounds of a di?erent type there may
_ be employed tubes formed of hydrophobic col
loidal materials as a class of which there may
During the operation 'of’the apparatus shown
be given by way of example, tubes formed of
synthetic resins such as polyvinyl resins, methyl
in Figs. 4 and 5, the soluble substances are caused
to di?use from the layer of dialyzate which passes
in the space between the tubes l_8a and “lb into
the diifusate which is ?owing through the in- '1
terior of the tube ma. Simultaneously, water or
methacrylate resins, chloroprene, nylon, chlorin
ated rubber and the like, or from an organic sol
solvent from the diffusate will be ?owing through
the tube l8a into the dialyzate thus diluting the 15
dialyzate. If the procedure of dilution is not re- '
tarded, it will result in the slowing down of the
process of dialysis,vthe rate of which depends
ent-soluble cellulose derivative such, for exam
ple, as a cellulose ester, cellulose ether, mixed
cellulose ester, mixed cellulose ether, a mixed
ether ester of cellulose, as well as tubes formed
of two or more resinsor two or more cellulose
derivatives, also tubes formed from a mixture
of a hydrophobic‘resin with a hydrophobic cellu- upon the difference in concentration of the sol
lose derivative. When hydrophobic tubes are em
uble' material between the dialyzate and the dif
20 ployed they are preferably used in the swollen
fusate. Thus, according to one embodiment of
gel state, i. e., while they are saturated with the
the present invention, air is blown over the out
organic liquid which it is desired toevaporate
side of the multiwalled tube so that water is
through the tube.
continuously evaporated from the diffusate
. ,
_ The present apparatus is adapted forv dialyz
through the wall lab and through the open mesh
fabric iBc. It has been found, for example, that 25 ing both organic and inorganic substances from
organic or aqueous solutions. On the one hand,
when the tube Iilb is formed of regenerated cel
organic substances may be separated from aque
lulose and the diffusate is an aqueous solvent,
ous or non-aqueous. organic; solutions by use of a
the rate of evaporation of water through the re
semi-permeable hydrophobic tubing, while on the
generated cellulose tube I812 is the same as the
rate of evaporation from the same solution con 30 other hand water-soluble substances maybe sep
arated from aqueous solutions by use of a hydro
tained in a bath. In other words, the rate of
philic tubing. Accordingly, the present appara
evaporation appears to be independent of the
tus may be used for separating inorganic or or
membranes. ‘This appears to be due to the fact
that the water diffuses in the wall of the tube 35 ganic crystalloids from their solutions, or for
separating crystalloids from colloids, or for sepa
I81; and evaporates from its external surface.
rating inorganic substances from organic sub
Thus, the present invention provides a process
stances, or for separating organic ‘liquids from
and apparatus by which the dialysis can be car
aqueous
or non-aqueous solutions. In particu
ried' out simultaneously with the concentration
of the dialyzate so that the decrease in the rate 40 lar, the apparatus is applicable for the separa
tion of glycerine, butylene glycol, citric acid, su
of dialysis resulting from dilution of the diilusate
gar and inorganic salts and the like, from their
can be substantially retarded or prevented.
aqueous solutions.
'
_
‘
'
' Preferably, the air which is caused to flow over
the tube |8c is'air heated to an elevated tem
perature of the boiling point of Water, but pref
erably between 50 and 60° F. The heat trans
ferred to the dialyzate is thus advantageous in
.The heating of the dialyzate from 70 to 100° C.
serves a four-fold purpose: (a) to continuously
concentrate the dialyzate since water is evapo
rated in the evaporator; (b) to increase the rate
of dialysis; (c) to eliminate dissolved air and air
bubbles; (d) to sterilize the dialyzate and pre
preventing further fermentation and increasing
‘the rate of dialysis. Any conventional air blower
vent further fermentation.
.
and air heater may be employed.
50
The apparatus has many advantages, namely,
For treating aqueous liquid compositions, the
the dialyzing membranes being in the form of a
tubes I8, I81: and l_8b' may be formed of any hy
drophilic ?lm-forming material, such, forexam
ple, as parchment paper, tubes made from leather
waste as sold under the trade names “Brech
tee ” and “Naturin” and tubes made from any
?lm-forming non-?brous oellulosic materials as
a class. ,For the treatment of aqueous ?uid com
positions where it is desired to cause the diffusion
and separation of water or water-miscible or
ganic compounds from inorganic or organic sub,
stances whether liquid or solids, there is prefer
' ably employed a hydrophilic cellulosic tube such,
tube are more self-supporting than ?-at sheets
and they can-be readily anchored atv each end
without danger of leaks. When a tube breaks,
55 the liquid may be quickly drained from the ap
paratus and a tube replaced without dismantling
' the ‘ entire apparatus.
Since the tubes are not
constricted at the entrance or exit ‘(where they
are joined to the headers, the ?ow of liquid there
60 through is not retarded and there is no. tendency
for sediment to collect inside the tube; further, a
rapid ?ow can be maintained through the tubes.
-Thus, there is provided a means for continuously
concentrating the dialyzate while preventing the
for example, as one formed of regenerated cellu
lose ‘or cellulose hydrate which has been pro 65 rate of dialysis from dropping too rapidly, there
by resulting in an increase in the yield.
duced by regeneration from viscose or' from solu
Since certain changes in carrying out the above
tions of cellulose in inorganic or organic solvents
process and in the constructions set forth, which
or from cuprammonium cellulose or by the de
esteri?cation of cellulose'esters such as, by the
denitrationof cellulose nitrate, also membranes
formed of alkali-soluble, water-insoluble cellu
embody the invention, may be made without de
parting from its scope, it is intended that all
matter contained in the above description or
shown in the accompanying drawings shall be.
lose ethers, gelatine (insolubilized), casein, al
interpreted as illustrative and not in a limiting
ginates, and the like ?lm-forming hydrophilic'
sense.
plastic materials. Such tubes are employed'in 75 Having described my invention, what I claim
2,411,285 '
.
' as new and desire to secure by Letters Patentis:
1. An apparatus for the dialysis of solutions
comprising, in combination, a chamber, a multi
plicity of tubular dialyzing membranes compris
ing outer tubes of relatively large diameter and
_ tubes of relatively small diameter, disposed in
said tubes of large diameter, means spaced within
said chamber supporting said tubular dialyzing
membranes, means to pass the solution to be
dialyzed through the outer tube into contact with
onesurface of the inner tube, means to pass an
otherliquid through the inner tube into contact
with the ‘other surface of the inner tube, and‘
means to continuously concentrate the solution.
being dialyzed so as to increase the rate of di
alysis.
‘
2. An apparatus for the dialysis of solutions
comprising, in combination, a chambena multi
8,
,
i
.
being connected to the inner headers, means
to pass a solution through the- inner tube,
means to pass a diiferent solution through the
.space between the inner and the outer tube, and
insJanS to pass a. ?uid on the outside of the outer
u
e.
-
4. An apparatus according to claim 3 in which '
. there is provided means for passing air over the
surface of, the outer dialyzer tube so as to eva
porate liquid from the surface of said tube.
5. A process‘ for the dialysis of solutions com
prising passing the solution to be dialyzed into
contact ‘with one surface of a dialyzing mem
brane in the form of a tube, passing another liq? "
uid into contact with the other surface of said
tube, and continuously concentrating the solu-‘
tion being dialyzed at a point spaced from the
dilalyzing membrane, and continuously recircu
lating the concentrated solution, whereby the
plicity of tubular dialyzing membranes, compris
concentration gradient between the dialyzate and
20
ing outer tubes ofsrelativeiy large ‘diameter and
the di?usate is maintained at its-highest level
tubes of relatively small diameter disposed in said
throughout the dialysis process.
tubes of large diameter having tubular support
6. A process for dialyzing solutions comprising
for the outer tube comprising an, open mesh fab- ‘
passing the solution to be dialyzed through an
ric, disposed therein, means spaced'within said
outer tubular dialyzer, in contact with an inner
chamber supporting said tubular dialyzing mem 25. tubular dialyzer which is concentric with the ?rst
branes, means to pass the solution toqbe dialyzed
tubular dialyzer, passing another liquid through
through the outer tube into contact with one sur
and in contact with the inner tubular dialyzer,
face of the-inner tube, means to pass another
and passing air over the‘external surface of the
liquid into contact with the other surface of the
outer tubular dialyzer whereby a liquid is caused
30
inner tube, and means to continuously concen
to be evaporated from said dialyzer.
trate the solution being dialyzed so as to increase
7. A process for dialyzing solutions comprising
the rate of dialysis.
passing the solution to be dialyzed through a tu
3. An apparatus for thedialysis of solutions
comprising, in combination, a chamber having
inner and outer headers disposed transversely
adjacent each end and de?ning a space between
bular dialyzer of relatively large diameter in‘
with tubular dialyzer of smaller diam
3.5 contact
eter which is disposed inside said larger tubular
dialyzer, passing another liquid through and in
them, dialyzing membranes in the form of inner
contact with the tubular dialyzer of smaller di
and outer concentric tubes of different diameters
ameter, and passing a third ?uid over the exter
disposed in said space and connected at each 40 nal surface ofithe. larger tubular dialyzer.
end to said headers, the inner tube being con
JUSTIN ZENDER.
nected to the outer headers and the outer tube
' '
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