United States Patent (19) 11) 4,389,363

Molthop 45) Jun. 21, 1983

54 METHOD OF POTTING MICROPOROUS Assistant Examiner-V. K. Rising
HOLLOW FBER BUNDLES Attorney, Agent, or Firm-Paul C. Flattery; Thomas R.
75 Inventor: Susan C. Molthop, Mundelein, Ill. Schuman; Garrettson Ellis
73) Assignee: Baxter Travenol Laboratories, Inc., 57 ABSTRACT
Deerfield, Ill. The ends of bundles of microporous tubing may be
(21 Appl. No.: 203,304 potted in otherwise conventional manner for assembly
as a diffusion device for oxygenation of blood, blood
(22 Filed: Nov. 3, 1980 plasmapheresis, or the like. In accordance with this
51) Int. Cl. ............................................ B22D 11/126 invention, prior to impregnating the bundle ends in
52 U.S. C. ................................. 264/135; 210/321.3; sealant, the micropores of the capillary tubing are filled
29/527.3; 264/136; 264/138; 264/263; 264/267; with a liquid capable of entering the micropores, with
264/279 the result that air in the bores of the tubing cannot mi
58 Field of Search ............... 264/279, 261, 263, 138, grate outwardly through the micropores as the sealant
264/267, 134, 135, 136, 157, 271.1; 29/527.3, impregnates the bundle ends. This, in turn, prevents the
527.1, 527.2; 210/321.3 sealant from advancing into the bores of the tubing to
56 References Cited the level occupied by the sealant outside of the bores of
the tubing, so that the ends of the potted bundle may be
U.S. PATENT DOCUMENTS transversely cut within the block of cured sealant to
3,697,635 10/1972 Dietzsch et al. ................... 29/527.1 expose open bores of the tubing.
4,049,765 9/1977 Yamazaki ............................ 264/261
Primary Examiner-Francis S. Husar 20 Claims, 3 Drawing Figures
U.S. Patent Jun. 21, 1983 4,389,363

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 4,389,363
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During conventional potting operations of capillary
METHOD OF POTTING MICROPOROUS fiber diffusion devices, the bundle of fibers is inserted
HOLLOW FIBER BUNDLES into its housing, and then the liquid potting compound
impregnates the ends of the bundle, while the housing is
BACKGROUND OF THE INVENTION 5 spun about a central axis to hold the potting compound
This application relates to a method for potting bun at the ends of the bundle. Conventionally, the amount of
dles of microporous tubing which may be utilized in penetration of potting compound into the bores of capil
diffusion operations such as the oxygenation of blood, lary tubing at both ends thereof is substantially less than
membrane plasmapheresis, and the like. the level of potting compound permeating the bundle
10 outside of the bores, because the air inside of the bores
Bundles of capillary tubing are currently in extensive
commercial use in dialyzers for blood, with the capil is compressed as the potting compound advances into
lary tubing being typically made of a cellulose-deriva the bores from both ends, causing a counterpressure
tive material. These bundles are commercially assem which inhibits the advance of potting compound into
bled, and then centrifugally potted in known manner, 15 the bores.
for example by the technique of U.S. Pat. No. 4,227,295, As the result of this, when the potting compound is
Method of Potting the Ends of a Bundle of Hollow Fibers cured, one can cut transversely through the middle of
Positioned in a Casing, to Bodnar, et al., to enclose the the potting compound at the ends of each bundle to
bundle into a tubular housing, with the ends of the expose open bores, which is necessary in order to obtain
bundle of capillary fibers being each sealed in a typi- 20 an operating diffusion device by this potting method.
cally polyurethane potting compound, with the bores of However, in the case of microporous capillary tubing
the capillary fibers communicating through the sealant bundles, during the spinning step, as the potting com
at each end. pound advances into the bores of the microporous capil
A manifold is placed on each end so that the blood is lary tubing, there can be no increase of air pressure in
directed through a flow path which passes through the 25 the bores, because the air easily leaks out of the micro
bores of the fibers. Side manifolds are provided for pores of the capillary tubing. Thus, the level of the
dialysis solution in which the flow path percolates potting compound in the bores becomes essentially
through the bundle of fibers along exterior surfaces equal to the level of the potting compound outside of
thereof, so that the two flow paths are separated by the bores in the bundle, with the result that it is difficult
membrane surfaces defined by the capillary fibers, so or impossible to form a potted bundle in which open
bores pass through a cut section of potting compound to
that diffusion exchange can take place. Dialyzers of this
type are sold by the Artificial Organs Division of Trav be open to the ends of the bundle.
enol Laboratories, Inc. under the trademark CF (R). In accordance with this invention, a method for effec
It is also known that microporous membrane mate tively potting microporous tubing is provided, to permit
rial, in which the pores may be in the micron size range, is such microporous tubing to be utilized in diffusion de
are very desirable for use in the oxygenation of blood vices having, for example, the effective design of the
and also in membrane plasmapheresis. For example, the current capillary fiber dialyzers, with the known manu
TMO (E) blood oxygenator sold by the Artificial Organs facturing and functional advantages which are provided
Division of Travenol Laboratories, Inc. utilizes a micro by that popular and effective design.
porous polypropylene membrane. Also, other micropo- 40 The invention of this application may also be used
rous hydrophobic membranes such as microporous elsewhere, wherever it is desired to pot the ends of
polytetrafluoroethylene may be used for the oxygena microporous tubing.
tion of blood. Likewise, certain known microporous BRIEF DESCRIPTION OF THE DRAWINGS
membranes may be utilized for membrane plasmaphere
sis. Microporous membranes may be used for other 45 For a more complete understanding of this invention,
diffusion operations, as well. reference should now be had to the embodiment illus
By the term "microporous' it is intended to mean trated in greater detail in the accompanying drawings.
that pores exist which permit air and other gases to In the drawings:
rapidly pass through the walls of the tubing, while the FIG. 1 is a perspective view of a conventional tubular
membraneous walls of the tubing retain a semiperme- 50 housing for enclosing a bundle of capillary fibers.
able characteristic, i.e., restricting the flow either of a FIG. 2 is a perspective view of the open end of the
liquid passing through them as in blood oxygenators, or tubular housing of FIG. 1, partially cut-away, to show
restricting a component of the liquid passing through the unpotted capillary fiber bundle contained therein.
them, such as blood cells in membrane plasmapheresis FIG. 3 is a perspective view of the closed end of the
devices. 55 tubular housing of FIG. 1 showing the potted capillary
The designs of diffusion devices utilized by the com fiber bundle.
mercial capillary tubing dialyzers would desirably be DESCRIPTION OF THE INVENTION
utilized with other types of diffusion devices. Particu
larly, it would be desirably used in conjunction with In accordance with this invention, a method is pro
bundles of microporous capillary tubing for the oxyge- 60 vided for potting the ends of a bundle of microporous
nation of blood, membrane plasmapheresis, or other tubing, for example capillary tubing for diffusion de
diffusion operations in which microporous membranes V1CeS.
are utilized. However, a significant manufacturing dis The overall potting technique, which may be gener
advantage has existed, rendering it very difficult to ally conventional, comprises impregnating the ends of
assemble bundles of microporous tubing into diffusion 65 the bundle with a curable fluid sealant, typically with
devices, where the ends of the capillary tubing are pot centrifugation in known manner, curing the sealant, and
ted in a manner similar to the manufacturing techniques thereafter transversely cutting through the sealant
for capillary fiber dialyzers. impregnated ends of the bundle to expose open bores of
 4,389,363
3. 4.
the tubing surrounded on their exteriors by cured seal tubular housing 12 with curable fluid potting compound
ant. or sealant 26.
In accordance with this invention, to make the above Both ends of the sealant-impregnated bundle are
potting technique operative with microporous tubing, transversely cut to expose the open bores of the capil
prior to impregnating the bundle ends in sealant one fills. 5 lary tubing. Prior to placement of end manifold 18 over
the micropores of the tubing with a liquid capable of open end 24 of tubular housing 12, but after potting
entering the micropores, with the result that air in the compound 26 has cured and after the ends of the bundle
bores of the tubing cannot migrate outwardly through have been cut to expose the open bores of the capillary
the micropores as the sealant impregnates the bundle tubes, the liquid remaining in the micropores of the tube
ends, if kept below a certain critical pressure, called the O walls is washed from bundle 22 with a volatile solvent.
bubble pressure as defined below. Accordingly, the FIG. 3 shows sealant-impregnated end 30. The capil
level of sealant within the pores of the capillary tubings lary tubes in end 30 are surrounded on their exteriors by
may be held radially outwardly by air pressure within cured potting compound 26 which also defines the sepa
the bores, relative to the level of sealant permeating 15 rate flow paths through the diffusion device. End mani
through the bundle in the areas exterior to the bores of fold 18 having inlet port 28, covers end 24 of tubular
the tubing. housing 12 on the completed device.
The micropores may typically be filled by dipping the For example, the capillary tubes may consist essen
bundle in the particular liquid used, and then draining tially of a polyolefin, and the liquid which is placed in
the liquid from the bores of the tubing in the bundle so the micropores may be a fatty ester containing at least
that the liquid is retained in the micropores and the bore 10 carbon atoms per molecule, for example isopropyl
is substantially emptied of liquid. myristate or other fatty esters such as amyl caproate,
It is generally preferable for the liquid to be capable butyl caproate, diethyl suberate, isoamyl caprylate,
of wetting the material of the capillary tubing. The dimethyl sebacate, or methyl caproate.
liquid may be preferably selected to provide a bubble There is no inherent limitation of the material or size
pressure of at least 2 cm. of mercury over atmospheric. 25 of the microporous tubing which may be processed in
The term “bubble pressure' defines the pressure neces accordance with this invention. It is only necessary to
sary to force air through the liquid-filled micropores, find an appropriate liquid capable of occupying the
resulting in the reinstitution of the air-permeable char micropores of the tubing and capable of providing an
acteristic of the microporous tubing. The particular adequate bubble pressure to temporarily block gas flow
through the micropores. For example, the capillary
bubble pressure provided is a function of the material of tubing may consist essentially of poly(ethylene vinyl
the microporous tubing and the size of the micropores, acetate) or other polyolefin derivatives, or any other
as well as the particular liquid used. hydrophilic or hydrophobic material. Also single mi
The bubble pressure is selected by proper selection of croporous tubes may be processed, or bundles of any
liquid and the like, so that the bubble pressure exceeds 35 number of tubes.
the maximum air pressure produced in the bores of the The above fatty ester materials may be used with
capillary tubing by the potting process. hydrophobic microporous tubing materials such as
After the sealant has cured, the liquid in the micro polypropylene, and the particular liquid utilized to fill
pores may be washed from the bundle with a volatile the micropores in accordance with this invention is also
solvent, for example, a volatile fluorocarbon liquid such 40 not limited, so that any appropriate liquid may be used,
as a Freon-type liquid, or any other type of liquid which preferably liquids having a boiling point of 50° C. or
is miscible with the liquid in the micropores. more, although such a limitation is not absolute. Gener
Turning now to the drawings, FIG. 1 illustrates diffu ally, hydrophobic liquids are used with hydrophobic
sion device 10 which may be made in accordance with tubing materials.
this invention. Diffusion device 10 is comprised of tubu 45 When hydrophilic materials are used, such as micro
lar housing 12 having side manifolds 14, 16 and end porous polysulfone materials for membrane plasmaphe
manifolds 18, 20. resis, it may be desirable to use a hydrophilic liquid
FIG. 2 illustrates unpotted bundle 22, comprised of rather than a hydrophobic liquid to fill the micropores.
microporous capillary tubes, extending from open end Specifically, water may be used in such an instance to
24 of tubular housing 12. At this stage in the manufac SO fill the micropores during the potting process, or alter
ture of the diffusion device, individual microporous, natively methanol, or dimethylether, acetone, ethylene
capillary tubes of bundle 22 have been filled by dipping glycol, and the like. Water, or methanol, for example,
the entire bundle 22 in a liquid capable of entering the may then be air-blown out of the micropores to dry the
micropores. After entire bundle 22 has been dipped into tubing after the potting operation.
and removed from the liquid capable of entering the 55 The potting compound must naturally be compatible
micropores, liquid in the bundle 22 is drained. Liquid with the particular microporous tubing used, and it is
drains from the bores of the individual capillary tubes so generally preferred for the liquid used herein to fill the
that the bores are substantially emptied of liquid. A micropores to be substantially compatible and miscible
portion of the liquid, however, is retained in the micro with the uncured potting compound, so as not to exhibit
pores in the walls of the capillary tubes. This results in 60 anti-adhesive effects.
a bundle comprised of individual capillary tubes with A partial and incomplete list of other liquids which
bores open for their entire length, but with the micro may be used in appropriate circumstances to fill the
pores in the wall of the capillary tubes being liquid micropores of tubing include dodecane, mineral oil,
filled. Consequently, the micropores in the walls of the naphtha, toluene, dioctyl ether, butyl acetate, decyliso
capillary tubes no longer permit gases to pass rapidly 65 propylketone, or any other liquid which is preferably
through the walls of the tubes. non-reactive to the capillary tubing and sufficiently
In FIG. 3, bundle 22 is shown after it has been potted, compatible with the material of the tubing to fill the
by conventional centrifugal potting, at both ends of micropores.
 4,389,363.
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It is generally preferred for the average pore size of with a liquid capable of entering said micropores,
the micropores to range from 0.02 to 20 microns, which whereby air in the bore of said tubing cannot mi
includes the present operative pore sizes of microporous grate outwardly through said micropores in the
membranes for the oxygenation of blood or membrane walls as the sealant impregnates the tubing ends.
plasmapheresis. 5 2. The method of claim 1 in which, after curing said
The disclosure herein and the example below is for sealant, said liquid is washed from the tubing with a
illustrative purposes only, and is not intended to limit volatile solvent, and the tubing is air-dried.
the invention of this application, which is as defined in 3. The method of claim 1 in which said micropores
the claims. are filled by dipping said tubing in said liquid, and then
EXAMPLE I
10 draining said liquid from the bores of the tubing.
4. The method of claim 1 in which said potted tubing
Polypropylene capillary tubing having a bore diame is placed in a housing to define separate flow paths
ter of about 200 microns, an outer diameter of about 250 along the tubing bore and exterior.
to 320 microns, and micropore sizes of about 0.1 micron 5. The method of claim 1 in which said microporous
(available from the Celanese Company), was wound on 15 tubing consists essentially of a polyolefin, and said liq
a reel to form a loop of several thousand strands, and uid is a fatty ester containing at least 10 carbon atoms
then cut into bundles. The bundles were inserted into per molecule.
tubular housings of a design similar to conventional 6. The method of claim 5 in which said polyolefin is
housings for the CF (R) capillary dialyzer sold by Trave essentially polypropylene.
nol Laboratories, Inc. and described above. The basic 20 7. The method of claim 6 in which said fatty ester
design of the housing and the specific centrifugal pot liquid is isopropyl myristate.
ting technique utilized is that described in U.S. Pat. No. 8. The method of claim 1 in which said liquid is
4,227,295, Method of Potting the Ends of a Bundle of washed from the tubing with a volatile fluorocarbon
Hollow Fibers Positioned in a Casing, to Bodnar, et al. the liquid.
disclosure of which is incorporated by reference herein. 25 9. The method of claim 1 in which the average pore
In accordance with this invention, prior to placement size of said micropores is from 0.02 to 20 microns.
in the dialyzer housing, cut bundles of polypropylene 10. The method of claim 1 in which said tubing con
microporous fibers are immersed in isopropyl myristate sists essentially of poly(ethylene-vinyl acetate).
liquid. The bundle is then removed from the liquid and 11. The method of claim 1 in which said liquid capa
turned vertically so that the liquid runs out of the bores 30 ble of entering said micropores is capable of wetting the
of the fibers, but is retained in a thin film on the outer material of said capillary tubing.
wall of the bore of the fibers and in the micropores 12. The method of claim 1 in which said liquid in said
thereof. Thereafter, the bundle of fibers is potted with a micropores is selected to provide a bubble pressure of at
urethane potting compound by the technique described least 2 cm. of mercury over atmospheric.
in the patent application cited immediately above. The 35 13. The method of potting the ends of a bundle of
potting compound is restricted in its entry into the bores capillary tubing having microporous walls, which com
at the ends of the capillary fibers because of compres prises centrifugally impregnating the ends of said bun
sion of air in the bores, with the air being prevented dles with a curable, fluid sealant, curing said sealant,
from leaving the bores by the presence of the isopropyl and thereafter transversely cutting through the sealant
myristate liquid in the micropores. As the result, the impregnated ends of said bundle to expose the open
potting characteristics of the bundle processed herein bores of said tubing surrounded on their exterior by
approximates the potting characteristics of fibers which cured sealant, the improvement comprising, in combi
are not microporous. nation:
After the urethane potting compound has cured into prior to impregnating said bundle ends in sealant,
a resilient, elastomeric mass in the housing, it may be 45 filling the micropores in the walls of said tubing
transversely cut at the ends in conventional manner to with a liquid capable of wetting the material of said
expose the open bores of the microporous fibers. tubing, whereby air in the bores of said tubing
Following this, the potted bundle of fibers in the cannot migrate outwardly through said micropores
tubular housing can be washed with liquid Freon mate in the walls as the sealant impregnates the bundle
rial to remove the residual isopropyl myristate from the 50 ends, said micropores being filled by dipping the
system, followed by air-drying to remove all Freon bundle in said liquid and then draining said liquid
material. Thereafter, end caps of conventional design, from the bores of the tubing in the bundle while
for example those shown in U.S. Pat. No. 4,283,284, retaining liquid in the micropores in the walls of
Hollow Fiber Dialyzer End Seal System, to Schnell may the tubing, and including the step, after curing said .
be added to the ends of the housing to complete the 55 sealant, of washing said liquid from the micropores
assembly of a diffusion device of microporous fibers in the walls of the tubing in the bundle with a vola
made in accordance with this invention. tile solvent, and air-drying the bundle.
That which is claimed is: 14. The method of claim 13 in which said potted
1. The method of potting the ends of capillary tubing bundle is placed in a housing to define separate flow
having microporous walls, which comprises impregnat paths along the tubing bores and exteriors.
ing the ends of said tubing with a curable, fluid sealant, 15. The method of claim 14 in which said capillary
curing said sealant, and thereafter transversely cutting tubing consists essentially of a polyolefin, and said liq
through the sealant-impregnated ends of said tubing to uid is a fatty ester containing at least 10 carbon atoms
expose an open bore of said tubing surrounded on its per molecule.
exterior by cured sealant, the improvement comprising, 65 16. The method of claim 15 in which said polyolefin
in combination: is essentially polypropylene.
prior to impregnating said tubing ends in sealant, 17. The method of claim 15 in which said fatty ester
filling the micropores in the walls of said tubing liquid is isopropyl myristate.
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18. The method of claim 15 in which said liquid is said micropores is selected to provide a bubble pressure
*. . . of at least 2 cm. of mercury over atmospheric.
w from the bundle with a volatile fluorocarbon 20. The method of claim 15 in which the average pore
1quid. size of said micropores is from 0.02 to 20 microns.
19. The method of claim 15 in which said liquid in. 5 sk x x k is

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