Background of the Invention
[0001] This invention relates to the sealing of overlapped rubbery olefinic polymer (i.e.,
homopolymer, copolymer, terpolymer, etc.) sheets to each other, to spliceable sheets,
to a method of making such sheets, and to a transfer tape having particular utility
in the manufacture of the heat-sealable sheets.
[0002] Rubbery olefinic polymer sheet material finds widespread industrial use in applications
where it is necessary to contain or exclude liquids. Compared to vinyl sheet material,
the rubbery olefinic polymer sheet materials have longer life, greater flexibility
and resilience at low temperatures, ability to withstand high temperatures without
stretching or softening unduly, and superior resistance to ultraviolet light. The
most widely used rubbers for. formulating these sheets are polymers of ethylene, propylene,
and diene monomers (commonly known as EPDM), butyl rubber, and blends of the two.
In making rubbery sheet material, the olefinic polymers are commonly blended with
desired fillers, coloring agents, extenders, vulcanizing or crosslinking agents, antioxidants,
etc. to form a "compound", which is then calendered or extruded into sheets (commonly
known as "membranes"), typically on the order of 1.5 millimeters thick and 2 to 6
meters wide. These membranes are then heated to perhaps 150°C. for 2 hours to effect
vulcanization.
[0003] For many of the applications in which rubbery membranes are employed, it is necessary
to overlap and splice the edges of a large number of sheets. Rubbers, which have low
energy surfaces, are unreceptive to many adhesives. Accordingly the splicing procedure
has heretofore typically involved the steps of cleaning the overlapped areas, applying
a primer solution to each face, allowing the solvent to evaporate, applying a contact
adhesive solution to each face, again allowing the solvent to evaporate to leave a
tacky adhesive surface, mating the contact adhesive-coated surfaces, and compacting
the spliced area with a heavy steel roller. Operating in this way, it is possible
to form extremely large spliced membranes which can be used to line water reservoirs,
irrigation canals, sewage lagoons industrial waste pits, and solar energy ponds ;
such products are popularly designated "geomembranes". The splicing process is, however,
extremely labor-intensive and costly.
[0004] Another important application for spliced rubbery membranes is in the installation
of flat roofs for commercial, institutional and industrial buildings. Spliced membranes
are laid over new or existing roofs and typically either fastened down (e.g., at 40-centimeter
intervals) with metal battens or ballasted with round river-washed stones. When employed
on a roof, extremely rigorous demands are placed on the rubbery membranes, particularly
on the splices. Roof temperatures may approach the boiling point of water when exposed
to the summer sun, and they may sink to -30°C. -- or even lower -- during the winter.
[0005] In all of the applications for spliced membranes just described, the splicing has
been a tedious and time-consuming part of fabrication. How to simplify the preparation
of lapped splices has remained an unsolved problem.
Brief Description of the Invention
[0006] The present invention provides an easy, simple, rapid, and effective technique for
splicing rubbery membranes to form larger membranes. The resultant splices are strong,
resistant to temperature extremes, and able to withstand the expansion and contraction
that results from exposure to summer and winter conditions, all the while maintaining
a water-tight seal.
[0007] One aspect of the invention relates to spliceable sheet material having particular
utility in the fabricatic.. of lapped-seam membrane roofing, comprising in combination
a rubbery water-impermeable membrane consisting essentially of thermoset olefinic
polymer having on one side, at least in a border area along one edge, a thin layer
of firmly bonded heat-sealable adhesive of a type that wets the membrane. A presently
preferred material for the rubbery olefin polymer membrane is EPDM, and a presently
preferred adhesive is linear low density polyethylene having a softening point (as
defined in ASTM Test D-16, Procedure 19) of at least 80°C., preferably 100°C., and
most preferably at least 120°C. (It should be recognized that the term "polyethylene"
may include the normally employed stabilizers, filers, extenders, processing aids,
pigments, and the like.) Other suitable adhesives can be formulated from thermoplastic
blends of polyethylene and polypropylene, homopolymers of olefin monomers, polymers
of two or more olefin monomers, etc., provided that-the softening point meets the
stated temperature requirement. To enhance processability, the melt index of the adhesive
is desirably at least 0.5 dl/g, a melt index of about 1 being presently preferred.
For convenience in use, the softening point of the heat-sealable adhesive should not
exceed 250°C., and preferably is significantly lower, to minimize the possibility
of degrading the rubbery membrane.
[0008] A presently preferred spliceable sheet material of the type described in the preceding
paragraph is one in which linear low density polyethylene is adhered to the border
area on one side of the rubbery sheet material adjacent a lateral edge and also on
the border area on the other side adjacent the opposite lateral edge, this arrangement
lending itself to a natural shingling type of overlapping.
[0009] A simple but unique transfer tape having particular utility in making the spliceable
border areas of the sheet material just described comprises a release liner having
strippably adhered to one face a thin layer of heat-sealable adhesive. A preferred
transfer tape construction comprises a polyester film release liner, e.g., biaxially
oriented polyethylene terephthalate, carrying a heat-sealable thermoplastic polyolefin
layer, e.g., linear low density polyethylene. Spliceable rubbery sheet material may
then conveniently be fabricated by placing the adhesive surface of the transfer tape
in contact with the appropriate area or areas of the rubbery membrane and applying
sufficient heat and pressure to melt the adhesive and bond it to the membrane. A particularly
preferred method is to place the transfer tape in contact with the unvulcanized sheet
material, apply sufficient pressure to maintain intimate contact between the tape
material and heat the assembly to a temperature high enough to vulcanize (i.e., crosslink,
or thermoset) the olefin polymer and, at the same time, soften the adhesive, thereby
permitting it to wet and upon cooling, bond firmly to the olefinic polymer sheet.
The release liner may then remain in place to protect the adhesive from contamination
and be removed at the time a splice is to be made.
[0010] Because it is difficult, expensive, and time-consuming to conduct field evaluations
of products made in accordance with the invention, a number of tests have been developed
to provide information that relates directly to some aspect of roofing end use requirements.
These tests, which incorporate built-in safety factors, are briefly described below.
[0011] 1. T-Peel Test. In this test, two 2.54-cm wide x 15-cm long x 1.14-mm thick strips
of commercially available EPDM-based membrane, each provided with a 38-micrometer
layer of heat-activatable adhesive, are superposed in coextensive adhesive-to-adhesive
contact and approximately 5 cm at one end laminated for one minute in a press at 160°
C. and 20 k
Pa. Conventional T-peel tests are then performed in tensile testing equipment in which
the jaws are separated at a rate of 30.5 cm/minute. For roofing applications, initial
values should be at least 8.8 N/cm when tested at room temperature. After being subjected
to any one of the conditions described below and then re-tested, T-peel values should
be at least 17.5 N/cm.
a. Temperature Cycling. T-peel samples are exposed to room temperature for one week,
-18°C. for one week, room temperature for another week, -18°C. for one week, and then
tested.
b. Hot Water Immersion. Two hours after being prepared, T-peel samples are immersed
for 24 hours in 70°C. water, removed, dried, and tested at room temperature.
c. Delayed Hot Water Immersion. 24 hours after being prepared, the T-peel samples
are immersed in 70°C. water for 24 hours, removed, and tested as in sub-paragraph
"b".
d. High Humidity. T-peel samples are exposed to 38°C. and 100% relative humidity for
one week, removed, dried, and tested at room temperature.
e. Heat Aging. Samples are placed in a 70°C. oven for one week, removed, and tested
at room temperature.
f. Heat Resistance. T-peel samples are heated as in sub-paragraph "e" but tested at
70°C.
g. Weather Resistance. Samples are exposed to the artificial weathering conditions
provided by a "Weatherometer" machine in accordance with ASTM Test D-750. Tests are
performed after 250 and 500 hours.
h. Freeze-Thaw Resistance. T-peel samples are immersed in room temperature water for
one week and then placed in a -18°C. freezer for one week. They are removed and tested
at room temperature.
2. Softening Point. Strips of the heat-sealable roofing membrane 2.54 cm wide are
overlapped 2.54 cm adjacent one end of each and bonded for one minute, adhesive-to-adhesive,
in a 160°C. press at a pressure of 20 kPa. The spliced strip is then removed and tested
in accordance with a modified form of ASTM-D816 Procedure 19. In this test, the end
of one strip is gripped between the jaws of a holder, the remainder of the spliced
strip extending vertically, with a 2.27-kg weight attached to the free end. The assembly
is then placed in a 65°C. oven and the temperature raised 0.5°C./minute until failure
occurs; the acceptable threshold temperature is 1200C.
3. Dynamic Shear. Samples, prepared as in the softening point test, are mounted in
a tensile testing machine, the jaws of which are separated at the rate of 1.3 mm/minute
until failure occurs. A force of 275 kPa or more is considered acceptable.
4. Static Shear. Lap-spliced samples are prepared as in the preceding two tests. One
end of the spliced sample is gripped in the jaws of a holder, with the remainder of
the sample extending vertically. To the free end is then attached a 2.27-kg weight
and the assembly placed in an 82°C. oven. Failure should not occur in less than 24
hours.
5. Low Temperature Flexibility. Two 2.54 cm x 12.5 cm strips of heat-sealable roofing
membrane are superposed in adhesive to adhesive contact and bonded in a 160°C. press
under a pressure of 20 kPa for one minute. The resulting laminate is conditioned in
a freezer maintained at -34°C. for 24 hours. An operator, wearing gloves to avoid
heating the samples, then bends the sample around a 1.27-cm. diameter refrigerated
steel rod, removes it, and bends it in the opposite direction around the rod, repeating
the cycle five times. No evidence of delamination should occur.
Detailed Description
[0012] The invention will now be described with the aid of illustrative but non-limiting
examples, in which all parts and percentages are by weight unless otherwise indicated.
Example 1
[0013] A linear, low density polyethylene (Union Carbide "
G-Resin 7047 Natural 7"), having a melt index of 1.0, was extruded through a slot die
having an opening of 0.56 mm at a die head temperature of 250°C. Immediately after
emerging from the die, the extruded polyethylene film was contacted by a 38-micrometer
polyester film; the resulting laminate was pulled between a rubber roll and metal
roll, located approximately 75 mm from the die opening. The rolls were driven at a
considerably faster surface speed than the rate at which the polyethylene was extruded,
so that the polyethylene thickness was reduced to approximately 90 micrometers. Samples
approximately 75 mm x 100 mm were then cut from the laminate and used for further
testing. The polyethylene was tack-free at room temperature.
[0014] A sample of the laminate was positioned with the polyethylene layer against a smooth
sheet of 1.5-mm cured EPDM rubber, and placed for 30 seconds in a press heated to
218°C. under a pressure of approximately 35 kPa. The sample was then removed from
the press and allowed to cool to room temperature, after which the polyester release
liner was stripped away, exposing the heat-sealable polyethylene surface. The stripping
force required was about 0.03 N/cm width. Values of at least about 0.02 N/cm are desirable
for ease in processing, values somewhat in excess of 0.1 N/cm being satisfactory but
not preferred. Significantly higher stripping values make the product more difficult
for the end user to remove the release liner.
Example 2
[0015] A polyethylene-polypropylene blend (Eastman Chemical Company "Tenite" 5321E polyallomer)
was extruded through a 0.38-mm 240°C. die head and processed as in
Example 1.
[0016] The adhesive-coated EPDM products made in accordance with the preceding examples
were then tested in accordance with the previously described procedures. Results are
tabulated below:

[0017] In factory production operations, it has been found convenient to apply the linered
heat-sealable adhesive directly to the uncured EPDM rubber membrane in 5.0 - 7.5-cm
strips along the border of one side adjacent the edge. The assembly is then subjected
to 375 kPa pressure at 150°C. to cure the EPDM rubber and simultaneously bond the
heat-sealable adhesive firmly thereto. Workers in the field lay out the rubber membrane
in a manner such that the heat-sealable portion of one strip of material overlaps
the edge of an adjacent strip of material, after which they remove the liner. Heat
is then applied, either directly to the adhesive or to the opposite side of the adhesive-bearing
rubber membrane in the splice area, to soften the adhesive and cause it to bond firmly
to the underlying edge of the adjacent strip.
[0018] In circumstances where the rubber membrane has an embossed or irregular surface,
adhesion in the splice area will be enhanced if confronting border portions of the
overlapped strips are both provided with a heat-sealable coating. This construction
can be achieved during factory production by making sure that a first heat-sealable
transfer tape is positioned on one side adjacent one edge and a second heat-sealable
transfer tape is positioned on the other side adjacent the second edge.
[0019] In some circumstances, it may be advantageous to coat one entire side of the rubber
membrane with heat-sealable coating. With completely coated membranes of this type,
rolls of the membrane may be slit to any desired width, e.g., to fit narrow portions
of a roof, while still maintaining heat-sealable coating adjacent each edge. Another
advantage achieved by overall coating with heat-sealable adhesive is the ability to
seal directly to the upper surface of batten strips that have been nailed or otherwise
affixed to the roof substrate, thereby permitting completely imperforate roofing membrane
construction. For such purposes, it is advantageous to use batten strips made of polyethylene,
which are not only moisture- and rust-resistant but also inherently possess heat-sealable
properties and are compatible with the thermoplastic olefinic heat-sealable coating
on the roofing membrane. If, of course, the polyethylene batten strips are used only
in the spliced areas, it is adequate to have heat-sealable adhesive only in the border
area of the lower membrane, where it will contact the batten strip.
[0020] It will be appreciated that varying the composition of the rubber membrane may make
it desirable to modify the heat-sealable adhesive composition. Also, as indicated
earlier in the discussion of this invention, the performance requirements for roof
construction are somewhat more strenuous than may be required for such other applications
as pond or swimming pool liners; for such uses, other heat-sealable adhesives should
be able to perform effectively. Those skilled in the art will, however, have no difficulty
in determining suitable adhesives to be employed in appropriate circumstances, considering
the foregoing discussion.
1. A spliceable sheet material having particular utility for use in the fabrication
of lapped-seam membrane roofing, comprising in combination:
a rubbery water-impermeable membrane consisting essentially of thermoset olefin polymer,
said membrane having on one side, at least in a border area along one edge, a thin
layer of firmly bonded heat-sealable adhesive that is capable of wetting the thermoset
olefin polymer and that has a softening point of at least about 80°C..
2. The sheet material of claim 1 wherein the heat-sealable adhesive has a softening
point of at least 100°C.
3. The sheet material of claim 1 wherein the heat-sealable adhesive has a softening
point of at least 120°C. but not more than 250°C.-
4. The sheet material of claim 3 wherein the olefin polymer consists essentially of
polymerized ethylene, propylene, and diene monomers (EPDM).
5. The sheet material of claim 4 wherein the heat-sealable adhesive is linear low
density polyethylene having a melt index of about 1.0.
6. The sheet material of claim 1 wherein the heat-sealable adhesive is protectively
covered by a strippable liner.
7. A transfer tape comprising a release liner having strippably bonded to one face
a thin layer of thermoplastic heat-sealable adhesive.
8. The transfer tape of claim 7 wherein the release liner is a film of biaxially oriented
polyethylene terephthalate and the adhesive is a polyolefin having a softening point
of at least 80°C..
9. A spliced membrane made by overlapping the adjacent borders of the sheet material
of claim 1, so that the heat-sealable adhesive is interposed between the two thermoset
olefin polymer membranes, and applying sufficient heat and pressure to bond the overlapped
borders to each other.
10. The spliced membrane of claim 9 wherein the T-peel values of the spliced borders
are at least equal to 17.5 N/cm, the dynamic shear is at least 70 N/cm, the softening
point is at least 120°C., the static shear is at least 24 hours, and the low temperature
flexibility requirements are satisfactory, all as measured in accordance with the
tests described herein.
11. A method of making the spliceable sheet material of claim 1 comprising the steps
of:
a. obtaining an uncured but curable sheet of polyolefinic compound,
b. placing in contact with a lateral border on one side of said sheet a transfer tape
comprising a thermoplastic olefinic layer carried by a strippable release liner, the
olefinic layer of the tape having a softening point of at least 80°C, and being in
contact with said sheet, to form an assembly,
c. subjecting said assembly to elevated pressure and temperature for a time sufficient
to cure said compound and firmly bond the heat-sealable thermoplastic olefinic layer
to the cured sheet material, said release liner remaining in position until said sheet
material is to be spliced, at which time it is removed.