USOO6974.

554B2

(12) United States Patent (10) Patent No.: US 6,974,554 B2

Cox et al. (45) Date of Patent: Dec. 13, 2005

(54) POTTING METHOD FOREIGN PATENT DOCUMENTS

(75) Inventors: David John Cox, Penreth (AU); Georg B; 2. : B1 ''.
Schnieder, Bad Kreuznach (DE); EP O 763 758 A1 10/1996
Fufang Zha, Westmead (AU); Joachim EP 920 904 A2 6/1999
Muller, Thornleigh (AU); Cinzia Lea,
Winston Hills (AU) (Continued)
(73) Assignees: U.S. Filter Wastewater Group, Inc., OTHER PUBLICATIONS
Warrendale, PA (US); Pall Seitzschenk U.S. Appl. No. 10/298,471, Nov. 15, 2002, Gallagher et al.
Filtersystems GmbH, Bad Kreuznach U.S. Appl. No. 10/369,813, Feb. 18, 2003, Zha et al.
(DE) U.S. Appl. No. 10/406,807, Apr. 2, 2003, Johnson et al.
(*) Notice: Subject
patent istoextended
any disclaimer, the termunder
or adjusted of this
35 YSS. Appl.
E. N. 8.i. SE
No. 10/428,601, May 2.St.
1, , Zha et al.1
U.S.C. 154(b) by 25 days. U.S. Appl. No. 10/437,202, May 12, 2003, Muller.
U.S. Appl. No. 29/119,130, Feb. 24, 2000, Johnson et al.
Almulla et al., Desalination 153 (2002) 237–243.
(21) Appl. No.: 10/676,458 Rosenberger et al., Desalination 151 (2002) 195-200.
(22) Filed: Sep. 30, 2003 Derwent Abstract Accession No. 2001–142268/15, JO1 JP,
O O A1, 200034932 (Mitsubishi Rayon Co. Ltd.), Dec. 12, 2000.
(65) Prior Publication Data International Search Report in Corresponding PCT Appli
US 2005/0087898 A1 Apr. 28, 2005 cation No. PCT/AUO2/OO436.
Related U.S. Application Data (Continued)
(63) Continuation of application No. PCT/AU02/00436, filed on Primary Examiner gela Ortiz
Apr. 4, 2002. (57) ABSTRACT
7
(51) Int. Cl." .......................... B29C 4514; B2. 706 A method of forming a pot for an array of hollow fiber
(52) U.S. Cl. ...................... 264/40.6; 264/255; 264/263; membranes (7) is provided, including the steps of placing
264/277 the ends (6) of the fiber membranes (7) in a mould (5);
(58) Field of Search ................................ 264/40.6, 255, forming a first layer (20) of curable resin material in a
264/261, 263, 271.1, 277, 310, 311; 425/121, non-cured State around the fiber membrane ends (6), apply
123, 127,425, 382.2; 156/296; 96/8, 10; ing a second layer (21) of a polyurethane resin material to
210/500.23 the first layer (20) prior to full curing of the first layer, the
polyurethane resin material layer being chemically reactive
(56) References Cited with the first layer material to form an adhesive bond
U.S. PATENT DOCUMENTS therebetween; at least partially curing both layers and
a removing the pot formed from the mould (5), wherein the
3,228.876 A 1/1966 Mahon second layer material is of higher flexibility than the first
3,693.406 A 9/1972 Tobin layer material when each layer is fully cured. Apparatus for
3.
2- -- 12
A 3. 2. st st al
Ippey et al.
performing the method is also disclosed.
(Continued) 14 Claims, 2 Drawing Sheets
 US 6,974,554 B2
Page 2

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 US 6,974,554 B2
Page 3

FOREIGN PATENT DOCUMENTS JP 06-114240 4/1994

JP O7-OOO77O 1/1995
EP O 920 904 A2 6/1999 JP O7-275665 10/1995
EP 1 052 012 A1 11/2000 JP O8-O10585 1/1996
FR 2 674 448 A1 2/1992 JP O9-141063 6/1997
FR 2 699 424 A1 6/1994 JP 10-156149 6/1998
GB 2 2S3572 A 9/1992 WO WO 90/00434 1/1990
JP 58-O88OO7 5/1983 WO WO 96/41676 12/1996
JP 61-097006 5/1986
JP 61-107.905 5/1986 OTHER PUBLICATIONS
JP 61-2572O3 11/1986
JP 61-263605 11/1986 Patent Abstracts of Japan, vol. 010, No. 373, Dec. 12, 1986,
JP 62-0044.08 1/1987 and JP 61 167406 A (Sumitomo Bakelite Co Ltd.), Jul. 29,
JP 62-114609 5/1987 1986.
JP 62-140607 6/1987 Patent Abstracts of Japan, vol. 017, No. 102, Mar. 1993, and
JP 62-17954O 8/1987 JP 04 293527 A (Daicel Chem Ind Ltd), Oct. 19, 1992.
JP 63-O97634 4/1988 Patent Abstracts of Japan, vol. 014, No. 314, Jul. 5, 1990,
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JP O2-284.035 11/1990 Patent Abstracts of Japan, vol. 011, No. 371, Dec. 3, 1987,
JP O3-018373 1/1991 and JP 62. 1447708 A(Daicel Chem Ind Ltd), Jun. 27, 1987.
JP O3-028797 2/1991 Patent Abstracts of Japan, vol. 005, No. 195, Dec. 11, 1981,
JP 31-0 10445 5/1991 and JP 56 118701 A (Kuraray Co Ltd.), Sep. 17, 1981.
JP 04-310223 11/1992 European Search Report in European Appl. No. 02712648,
JP O5-023557 2/1993 Completed Jan. 26, 2005.
JP O5-157654 6/1993
JP 06-071120 3/1994 * cited by examiner
U.S. Patent Dec. 13, 2005 Sheet 1 of 2 US 6,974,554 B2
U.S. Patent Dec. 13, 2005 Sheet 2 of 2 US 6,974,554 B2

2.

23

20
24

Figure 2
 US 6,974,554 B2
1 2
POTTING METHOD temperature changes within Said first layer to determine the
State of the curing process.
This application is a continuation, under 35 U.S.C. S 120, It is important that the Second layer be applied to the first
of International Patent Application No. PCT/AU02/00436, layer prior to curing of the first layer being completed So that
filed on Apr. 4, 2002 under the Patent Cooperation Treaty there are Sufficient active sites available for the chemical
(PCT), which was published by the International Bureau in reaction required to adhere one layer to the other can take
English on Oct. 17, 2002, which designates the United States place. Proper adhesion of the two layerS is required to
and claims the benefit of Australian Provisional Patent prevent ingress of feed between the layers and growth of
Application No. PR 4215, filed Apr. 4, 2001. bacteria etc. between the layerS leading to damage and
FIELD OF THE INVENTION
breakage of fibres and consequential contamination of the
filtrate. The use of this proceSS also eliminates the need for
The present invention relates to potting methods for Special adhesives and primers to produce adhesion between
porous hollow fibre membranes typically used in filtration the layers.
Systems. 15
A necessary condition for the adhesion of the two layers
is the chemical reaction between Some of the components of
BACKGROUND OF THE INVENTION the two different layers. For epoxy/polyurethane layers, it is
The potting materials used to Support and hold arrays of desirable that one of the epoxy components is reactive with
porous hollow fibre membranes are usually a compromise the isocyanate groups of the polyurethane (preferably
between materials which have sufficient rigidity to provide amines or amides).
adequate Support but Sufficient Softness and flexibility to According to a Second aspect, the present invention
avoid breakage of the fibres where they enter the pot. Too provides an apparatus for potting hollow fibre membranes
rigid a material produces rapid breakage of fibres adjacent including:
the pot while too soft a material does not have sufficient a mould for receiving the ends of said hollow fibre
mechanical Strength to adequately Support the fibres. The 25 membranes,
materials are also chosen to resist breakdown as a result of means for forming a first layer of curable resin material in
exposure to various types of feed as well as cleaning fluids a non-cured State around Said fibre membrane ends in Said
used to maintain the fibres. mould,
Known Systems employ Single layers of epoxy, polyure means for applying a Second layer of polyurethane resin
thane or Silicon materials, however, each Suffer from the material to Said first layer prior to full curing of Said first
disadvantages outlined above. layer, Said Second layer polyurethane resin material being
The present invention seeks to overcome or at least chemically reactive with said first layer material to form an
ameliorate one or more of the disadvantages of the prior art adhesive bond therebetween and Said Second layer polyure
outlined above or at least provide a useful alternative. thane resin material being of higher flexibility than said first
35 layer material when each layer is fully cured.
SUMMARY OF THE INVENTION
Preferably, the mould includes Separate means for flowing
According to one aspect, the present invention provides a Said first and Second layer materials into the mould. For
method of forming a pot for an array of hollow fibre preference, Said materials are fed into a centrifuge before
membranes including the Steps of placing the ends of Said 40
being flowed along a conduit or tube into the mould.
fibre membranes in a mould; forming a first layer of curable Preferably, a Single centrifuge may be used having Separate
resin material in a non-cured State around Said fibre mem Sections to receive the respective first and Second layer
brane ends, applying a Second layer of polyurethane resin materials.
material to Said first layer prior to full curing of Said first Although, a centrifuge is the preferred tool used in the
layer, Said Second layer of polyurethane resin material being 45 method, it will be appreciated that other techniqueS Such as
chemically reactive with Said first layer material to form an Static potting are equally applicable to the inventive method.
adhesive bond therebetween; at least partially curing both
layerS and removing the pot formed from Said mould, BRIEF DESCRIPTION OF THE DRAWINGS
wherein Said Second layer material is of higher flexibility
than Said first layer material when each layer is filly cured. A preferred embodiment of the invention will now be
It will be appreciated that any known method of Sealing
50 described, by way of example only, with reference to the
the open fibres may be used prior to the potting proceSS accompanying drawings in which:
described above. FIG. 1 shows a simplified schematic diagram of the
Preferably, the curable resin material is an epoxy resin. potting apparatus used to perform the potting method in
The use of an epoxy resin has been found to be advantageous 55
accordance with one embodiment of the present invention;
and
when potting fibre membranes which typically contain
hydroscopic liquids which may produce Sealing problems FIG. 2 shows a cross-sectional view of one potted end of
between the fibres and the pot when polyurethane resin is the fibres illustrating one embodiment of the invention.
used.
DETAILED DESCRIPTION OF THE
In one preferred form the layer of higher flexibility is 60
PREFERRED EMBODIMENT
produced by adding one or more flexibilising agents to the
components of the material forming the first layer of lower Referring to FIG. 1, the potting apparatus comprises a
flexibility. mould 5 for receiving the ends 6 of the fibres membranes 7.
Preferably, the method includes the step of the monitoring The mould 5 includes a cylindrical cavity 8 for receiving the
the curing process of the first layer to determine the optimal 65 fibre membranes 7. The cavity 8 has an enlarged-diameter
time in which to apply the Second layer thereto. For base portion 9 for holding the prepot 10 which serves to
preference, the Step of monitoring includes monitoring the Support the fibres during the potting process. A tube or hose
 US 6,974,554 B2
3 4
11 connects one bowl 12 of a centrifuge 13 to the base 14 of What is claimed is:
the mould cavity 8. A second tube 15 connects a second bowl 1. A method of forming a pot for an array of hollow fibre
16 of the centrifuge 13 to the upper portion 17 of the mould membranes, each fibre membrane comprising an end, the
cavity 8. method comprising:
placing the ends of the fibre membranes in a mould;
In use, the material for forming the first relatively hard forming a first layer of a curable resin material in a
layer of the pot is dispensed into bowl 12 of the centrifuge non-cured State around the ends, wherein the Step of
13 and flowed along tube or hose 11 into the lower portion forming a first layer of a curable resin material further
14 of the mould cavity 8 to form a first layer around the fibre comprises monitoring a curing process of the first layer
ends 6. Prior to full curing of this material, a Second material to determine an optimal time at which to apply a Second
for forming the second softer layer is dispensed into bowl 16 layer to the first layer;
and flowed along tube or hose 15 into the mould cavity 8 to applying a Second layer of a polyurethane resin material
apply the Second layer of material to the first layer. The to the first layer prior to full curing of the first layer,
layerS chemically react to form an adhesive bond between wherein the polyurethane resin material is chemically
the first and Second layers. At an appropriate curing Stage the 15 reactive with the curable resin material to form an
potted fibres are removed from the mould 5. adhesive bond between the first layer and the second
In Some applications, it may be possible to use a single layer, and wherein a fully cured polyurethane resin
bowl and tube to flow the materials sequentially into the material is of a higher flexibility than a fully cured
mould to form the two layers. curable resin material;
at least partially curing the first layer and the Second layer,
In order to determine the optimal time during the curing Such that a pot is formed; and
of the first layer for applying the Second layer, the tempera removing the pot from the mould.
ture profile of the first layer material may be monitored, at 2. The method according to claim 1, wherein the curable
least during the initial Set up of the process. The temperature resin material comprises an epoxy resin.
profile indicates the various Stages of the curing proceSS and 25
3. The method according to claim 1, wherein the first layer
when the Second layer may be applied to ensure that comprises at least one flexibilising agent.
Sufficient free sites are available for chemical bonding 4. The method according to claim 1, wherein the Step of
between the two layers. Once the optimal time has been monitoring comprises monitoring a temperature change
determined for a particular material combination further within the first layer to determine a State of the curing
monitoring is unnecessary. proceSS.
A steep rise in temperature indicates that the majority of 5. A method of forming a pot for an array of hollow fibre
the curing reaction is taking place. The optimal time for the membranes, each fibre membrane comprising an end, the
addition of the second layer has been found to be within +5 method comprising:
minutes of the time of this temperature rise and preferably, 35 placing the ends of the fibre membranes in a mold;
t2 minutes. providing a potting sleeve within the mould to receive a
The embodiment shown in FIG. 2 illustrates a method first layer and a Second layer, wherein the potting sleeve
using a potting Sleeve 23 to enhance the interfacial binding comprises adhesion means, wherein the adhesion
means assist in adhesion of at least one of the curable
between the potting layerS 20, 21. The quantity of potting
materials or the width of the potting sleeve 23 is selected to 40 resin material and the polyurethane resin material to the
ensure that the interface 24 of the two layers is within the potting sleeve;
potting sleeve 23. The potting sleeve 23 is formed from forming a first layer of a curable resin material in a
material which ensures good adhesion between its inner non-cured State around the ends,
Surface and the two potting materials. Besides the Selection applying a Second layer of a polyurethane resin material
is of the potting sleeve material, roughening the inner 45 to the first layer prior to full curing of the first layer,
Surface of the Sleeve 23 can also enhance the binding of the wherein the polyurethane resin material is chemically
potting materials with the sleeve 23. Further enhancement reactive with the curable resin material to form an
can be achieved by forming grooves 25 in the potting sleeve adhesive bond between the first layer and the second
23. Due to the adhesive force between the potting materials layer, and wherein a fully cured polyurethane resin
and the potting sleeve 23, it serves to reduces any movement 50 material is of a higher flexibility than a fully cured
or detachment of the two potting layers 20, 21 at the curable resin material;
interface 24, and therefore enhances the binding of the two at least partially curing the first layer and the Second layer,
potting layerS 20, 21. Such that a pot is formed; and
The potting method outlined above provides a number of removing the pot from the mould.
advantages over the prior art including improved Support of 55 6. The method according to claim 5, wherein a surface of
the fibres Serves to reduce breakages at the fibre/pot inter the potting sleeve in contact with at least one of the curable
face. In Some applications it is also possible to dispense with resin material and the polyurethane resin material is rough
ened.
the usual potting sleeve as the pot formed by this method has 7. The method according to claim 5, wherein the potting
Sufficient rigidity to be Self-Supporting. This produces a 60 sleeve comprises at least one protrusion formed on a Surface
manufacturing Saving as in Some cases Shrinkage of the of the potting sleeve in contact with at least one of the
potting materials relative to the potting sleeve produces gaps curable resin material and the polyurethane resin material.
which are again undesirable in terms of leakage and bacte 8. The method according to claim 5, wherein the potting
rial growth. In Such cases the pot must be discarded. sleeve comprises at least one indentation formed on a
It will be appreciated that further embodiments and exem 65 Surface of the potting sleeve in contact with at least one of
plifications of the invention are possible without departing the curable resin material and the polyurethane resin mate
from the Spirit or Scope of the invention described. rial.
 US 6,974,554 B2
S 6
9. A method of forming a pot for an array of hollow fibre comprises monitoring a curing process of the first layer to
membranes, each fibre membrane comprising an end, the determine an optimal time at which to apply a Second layer
method comprising: to the first layer.
placing the ends of the fibre membranes in a mould; 12. The method according to claim 9, further comprising
forming a first layer of a curable resin material in a the Step of providing a potting sleeve within the mould to
non-cured State around the ends, wherein the curable receive a first layer and a Second layer, wherein the potting
resin material comprises epoxy groups; sleeve comprises adhesion means, wherein the adhesion
means assist in adhesion of at least one of the curable resin
applying a Second layer of a polyurethane resin material material and the polyurethane resin material to the potting
comprising amine groups or amide groups to the first sleeve.
layer prior to full curing of the first layer, wherein the 13. The method according to claim 9, further comprising
amine groups or amide groups of the polyurethane resin the Step of providing a potting sleeve within the mould to
material chemically react with the epoxy groups of the receive a first layer and a Second layer, wherein the potting
curable resin material to form an adhesive bond
sleeve comprises at least one protrusion formed on a Surface
between the first layer and the Second layer, and 15 of the potting sleeve in contact with at least one of the
wherein a fully cured polyurethane resin material is of curable resin material and the polyurethane resin material.
a higher flexibility than a fully cured curable resin 14. The method according to claim 9, further comprising
material; the Step of providing a potting sleeve within the mould to
at least partially curing the first layer and the Second layer, receive a first layer and a Second layer, wherein the potting
Such that a pot is formed; and sleeve comprises at least one indentation formed on a
removing the pot from the mould. Surface of the potting sleeve in contact with at least one of
10. The method according to claim 9, wherein the first the curable resin material and the polyurethane resin mate
layer comprises at least one flexibilising agent. rial.
11. The method according to claim 9, wherein the step of
forming a first layer of a curable resin material further