U.S. patent application number 13/045710 was filed with the patent office on 2011-07-07 for adhesive strips for assembly, especially formed with three layers and based on thermally cross-linked, viscoelastic acrylate hot-melt adhesives.
This patent application is currently assigned to tesa SE. Invention is credited to Kay Brandes, Sven Hansen, Jorg Speer, Stephan ZOLLNER.
Application Number | 20110165402 13/045710 |
Document ID | / |
Family ID | 35170040 |
Filed Date | 2011-07-07 |
United States Patent
Application |
20110165402 |
Kind Code |
A1 |
ZOLLNER; Stephan ; et
al. |
July 7, 2011 |
Adhesive Strips For Assembly, Especially Formed with Three Layers
and Based on Thermally Cross-Linked, Viscoelastic Acrylate Hot-Melt
Adhesives
Abstract
The invention describes a double-sided pressure-sensitive
adhesive tape of the kind which can be used in particular for
achieving very durable bonds at high temperatures. These adhesive
tapes, especially adhesive assembly tapes for the permanent fixing
of articles to substrates, are preferably of multilayer
construction. The inventive double-sided pressure-sensitive
adhesive tapes are characterized in that the viscoelastic carrier
layer is composed of a photoinitiator-free, thermally homogeneously
crosslinked acrylate hotmelt. They are further characterized in
that these homogeneously thermally crosslinked acrylate hotmelts
have crosslinking sites by way of urethane units. This viscoelastic
carrier layer is covered on both sides in each case by adhesive
layers, preferably pressure-sensitive adhesive layers. These layers
are connected by chemical reaction to the viscoelastic carrier
layer. The operation for producing the adhesive tapes constitutes
the corona pretreatment of the adhesive layers following their
coating onto release material, the two-dimensional application and
shaping of the acrylate hotmelt for thermal crosslinking, a thermal
crosslinker having been added to the hotmelt prior to coating, the
lamination of the layers together, and the afterreaction on the
product in bale form, preferably without introduction of additional
heat for crosslinking. This method ensures particularly effective
anchoring even of different materials, which is particularly
positive for the technical adhesive properties of the adhesive
assembly tape.
Inventors: |
ZOLLNER; Stephan; (Humburg,
DE) ; Hansen; Sven; (Hamburg, DE) ; Brandes;
Kay; (Kaltenkirchen-Moorkaten, DE) ; Speer; Jorg;
(Wrist, DE) |
Assignee: |
tesa SE
Hamburg
DE
|
Family ID: |
35170040 |
Appl. No.: |
13/045710 |
Filed: |
March 11, 2011 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
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11572959 |
Oct 3, 2007 |
7935383 |
|
|
PCT/EP2005/054508 |
Sep 9, 2005 |
|
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13045710 |
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Current U.S.
Class: |
428/220 |
Current CPC
Class: |
B29B 7/90 20130101; C08L
2666/26 20130101; Y10T 428/31855 20150401; C08K 5/29 20130101; C08K
5/0025 20130101; Y10T 428/265 20150115; C08L 33/02 20130101; Y10T
428/1352 20150115; C08F 220/06 20130101; C09J 2433/00 20130101;
C08G 18/6254 20130101; Y10T 428/2848 20150115; Y10T 428/31935
20150401; C09J 7/385 20180101; C08K 5/3492 20130101; C09J 175/04
20130101; B29B 7/487 20130101; Y10T 428/28 20150115; C09J 2301/408
20200801; C09J 133/08 20130101; Y10T 428/1452 20150115; C09J 133/04
20130101; C08F 220/18 20130101; C08L 2666/04 20130101; C08G 18/792
20130101; Y10T 428/31573 20150401; C08G 2170/20 20130101; C08F
220/26 20130101; C08G 18/0895 20130101; C09J 133/04 20130101; C08L
2666/04 20130101; C09J 175/04 20130101; C08L 2666/26 20130101 |
Class at
Publication: |
428/220 |
International
Class: |
B32B 7/12 20060101
B32B007/12 |
Foreign Application Data
Date |
Code |
Application Number |
Sep 9, 2004 |
DE |
10 2004 044 086.7 |
Claims
1-13. (canceled)
14. An adhesive tape having at least one carrier layer and two
outer adhesive layers, wherein the carrier layer is composed of a
photoinitiator-free homogeneously crosslinked polymer of acrylate
and/or methacrylate, and wherein the thickness of the adhesive tape
is between 300 and 10000 .mu.m.
15. The adhesive tape of claim 1, wherein at least one of the
adhesive layers are formed of pressure-sensitive self-adhesive
compositions.
16. The adhesive tape of claim 2, wherein both adhesive layers are
formed of pressure-sensitive self-adhesive compositions.
Description
[0001] This application is a division of application Ser. No.
11/572,959, filed Oct. 3, 2007, now pending, which is a 371 of
PCT/EP2005/054508 filed 9 Sep. 2005 (international filing date)
claiming priority of German Application DE 10 2004 044 086.7, filed
Sep. 9, 2004.
[0002] The invention describes a double-sided pressure-sensitive
adhesive (PSA) tape, in particular a PSA tape of three-layer
construction, of the kind which can be used in particular for
achieving very durable bonding at high temperatures, and also a
method of producing it.
BACKGROUND OF THE INVENTION
[0003] For industrial PSA tape applications it is very common to
employ double-sided PSA tapes in order to join two materials to one
another. A distinction is made here, depending on type, between
single-layer double-sided self-adhesive tapes and multilayer
double-sided self-adhesive tapes.
[0004] Single-layer double-sided self-adhesive tapes, known as
transfer tapes, are constructed such that the PSA layer contains no
carrier and is lined only with corresponding release materials,
such as siliconized release papers or release films. Transfer tapes
may be lined with release materials on one side or both sides.
Often use is made of release papers or release films with different
degrees of siliconization on either side, so that the transfer tape
can be wound readily into a roll and then also applied readily.
Adhesive transfer tapes are frequently used in order to provide any
of a very wide variety of substrates with pressure-sensitive
adhesion. This is accomplished, for example, by laminating the
transfer tape onto the substrate. In that case the release paper
remains as a liner to the PSA layer in the product.
[0005] Relatively thin transfer tapes are often produced with
self-adhesive compositions from solution, whereas thicker transfer
tapes are produced with self-adhesive compositions from the melt or
by means of what is called UV polymerization. In this procedure a
prepolymerized syrup composed of acrylate monomers is coated
between two UV-transparent, antiadhesively coated release films and
is crosslinked on the web by UV irradiation. Specifications that
may be mentioned by way of example include
[0006] U.S. Pat. No. 4,181,752, EP 084 220 A, EP 202 938 A, EP 277
426 A, and U.S. Pat. No. 4,330,590. A disadvantage of this
technology is the often high residual monomer fraction in the
self-adhesive compositions. This fraction of residual monomer is
unacceptable for many applications. Transfer tapes filled with
non-UV-transparent adjuvants cannot be produced in this way.
[0007] DE 43 03 183 A1 also describes a method of producing thick
PSA layers, especially for producing high-performance self-adhesive
articles. In said process a mixture of starting monomers which is
to be polymerized by means of UV radiation is mixed, and thickened
in the process, with a solvent-free, saturated photopolymerizable
polymer, and then this mixture is applied to a dehesively treated
carrier and exposed to UV radiation. A disadvantage is the use of
copolymerized or added photoinitiators, since the layers may
undergo yellowing and, in the event of UV exposure prior to use, an
often marked change in the technical adhesive properties is found.
In that case it is necessary to go to considerable effort and
expense--by means, for example, of UV-impervious packaging--to
ensure that the customer obtains a uniformly high bonding
performance. Moreover, in the event of bonding on UV-transparent
substrates, such as on window glass or transparent plastic
surfaces, for example, there is a risk that layers containing
photoinitiator will undergo aftercrosslinking. This does result
initially in an increase in bond strength, but further crosslinking
causes the layers to become paintlike and undergo embrittlement.
Sooner or later, this leads to the failure of the bond,
particularly under a shearing load.
[0008] Transfer tapes may be foamed or filled in order to improve
their properties, particularly for example in respect of bonding to
uneven substrates. DE 40 29 896 A1 describes a carrierless,
double-sided self-adhesive tape comprising a pressure-sensitive
adhesive layer more than 200 .mu.m thick which contains solid glass
microballs of more than 1.5 g/cm.sup.3 in density. This tape is
said to exhibit particularly effective adhesion. A disadvantage is
the high density as a result of the glass balls that are used.
[0009] Double-sided adhesive tapes of multilayer construction have
advantages over their single-layer counterparts, since the
variation of the individual layers allows specific properties to be
set. For instance, a three-layer adhesive tape, consisting of a
middle carrier layer and two outer layers, can be constructed
symmetrically or asymmetrically. The two outer layers may each be
PSA layers, or, for example, one layer may be a PSA layer and the
other layer a heat-activatable adhesive. The carrier, i.e., the
middle layer, may for example be a film, a nonwoven, a "non-woven"
material or a foam film carrier. Foam or foam like carriers are
often used when there is a requirement for high bond strength to
uneven surfaces or when distances are to be compensated.
[0010] For instance, for adhesive assembly tapes, use is often made
of closed-celled foam carriers based on PE (polyethylene), PU
(polyurethane) or EVA (ethyl-vinyl acetate), which have a
double-faced coating of synthetic rubber PSA or acrylate PSA.
Applications, listed by way of example, are the bonding of mirrors,
trim strips and emblems in automotive construction, further uses in
automobile construction, and also use in the furniture industry or
in household appliances.
[0011] Assembly tapes for the exterior sector generally possess
PSAs based on polyacrylate. This material is particularly
weathering-resistant and very long-lived, and is virtually inert
toward UV light and toward degradation by oxidation or
ozonolysis.
[0012] Also known are adhesive assembly tapes with middle layers of
rubber, styrene block copolymers, and polyurethane. All of these
materials fail to possess the same good aging and thermal stability
properties of polyacrylate. Systems based on acrylate block
copolymers are resistant to aging but are not sufficiently
heat-resistant for high-performance requirements, since these
systems are crosslinked only physically by way of styrene or methyl
methacrylate domains. When the softening temperature of the domains
is reached (as in the case of styrene block copolymers), the PSAs
soften. Consequently, the bond fails.
[0013] Another disadvantage of typical foam adhesive tapes is that
they can easily split. If, for example, PE foam is used, this
material softens on heating to about 100.degree. C., and the bond
fails. Double-sided assembly tapes of this kind are unsuitable for
high-grade applications. Foams based on PU are indeed more
temperature-stable, but have a tendency to yellow under UV and
sunlight exposure. They too are often unsuitable for
high-performance applications.
[0014] For a number of years there have been double-sided adhesive
tapes available which are of three-layer construction with an
acrylate core. This viscoelastic acrylate core is foamlike. Its
foamlike structure is achieved through the admixture of hollow
glass or polymer balls to the acrylate composition, or else the
acrylate composition is foamed by means of expandable polymeric
"microballoons". Provided adjacent to this viscoelastic layer are
in each case PSAs, based in the majority of cases likewise on
acrylate, rarely on synthetic rubber, or else in special cases on
heat-activatable adhesive layers. The advantages of the
viscoelastic acrylate core arise on the one hand from the physical
properties of the polyacrylate (which, as already mentioned, are a
particular weathering stability and long life, and substantially
inert behavior toward UV light and toward degradation by oxidation
or ozonolysis). As a result of the design of the acrylate core
layer, determined for example by the comonomer composition, nature
and proportion of certain fillers, and the degree of crosslinking,
these products are especially suitable for bonding articles to
substrates having uneven surfaces. Depending on the choice of PSA,
a broad spectrum of properties and bond strengths can be
covered.
[0015] Nevertheless, as a result of their preparation, the
aforementioned systems have critical disadvantages. The
viscoelastic acrylate core layer is prepared by a process of
two-stage UV polymerization. In the first step of that process a
mixture based on acrylate monomers, 10% by weight acrylic acid and
90% by weight isooctyl acrylate for example, is prepolymerized to a
conversion of approximately 10%-20% by UV irradiation in a reactor
in the presence of a photoinitiator. Alternatively, this "acrylic
syrup" can also be obtained by thermally initiated free radical
polymerization. In the second step this acrylic syrup, often after
further photoinitiator, fillers, hollow glass balls, and
crosslinker have been added, is coated between antiadhesively
coated UV-transparent films, and is polymerized to a higher degree
of conversion on the web, by means of repeated UV irradiation, and
in the course of this polymerization it is crosslinked. The
completed three-layer product is obtained, for example, after the
PSA layers have been laminated on.
[0016] The production of "relatively thick" viscoelastic layers in
particular must in many cases be carried out in the absence of
oxygen. In that case the composition is protected by a lining of
film material, and UV initiation takes place through the films. PE
and PP films which are sometimes used for this purpose deform under
the conditions of crosslinking reaction (in the case of
UV-initiated polymerization, heat of reaction is liberated, and can
cause deformation of non-temperature-resistant film) and are
therefore poorly suited. UV-transparent films such as PET are more
thermally stable; in this case, however, it is necessary to add to
the composition a photoinitiator which reacts to longwave
radiation, in order for the reaction to take place. As a
consequence of this, these layers have a tendency to undergo
aftercrosslinking under UV light or sunlight. This process negates
the advantage specific to the polyacrylate as a material. A further
disadvantage is that fillers not transparent to UV cannot be used.
Moreover, as a result of the process, there remains a high residual
monomer fraction in these products. Possible reduction of residual
monomer through a reduction in coating speed or through intensive
subsequent drying is not very economic. The maximum achievable
layer thickness is very heavily dependent on the wavelength of the
photoinitiator used. Layers can be produced of up to about 1 mm,
albeit with the disadvantages specified above. Layers any thicker
than this are virtually impossible to obtain.
[0017] A particular disadvantage in the case of acrylate layers
produced by two-stage UV polymerization, UV crosslinking or
electron beam treatment is a more or less strongly pronounced
profile of crosslinking through the layer. Toward the irradiation
source, the UV-crosslinked layer is always more strongly
crosslinked than on the side opposite the UV radiation source. The
degree of the crosslinking profile is dependent for example on the
layer thickness, on the wavelength of the photoinitiator that is
used, and also on the wavelength of the radiation emitted by the UV
radiation source.
[0018] Specifications DE 198 46 902 A1 and DE 101 63 545 A1 propose
using EBC (electron beam) irradiation or UV irradiation from both
sides in order to lower the resulting crosslinking profile and to
provide virtually homogeneous crosslinking of thick
UV-crosslinkable acrylate PSA layers in particular. However, the
layers produced in this way still have a crosslinking profile, and,
moreover, the process is very costly and inconvenient. Moreover, it
would be virtually impossible to use in order to produce
viscoelastic acrylate carriers; instead, the preparation of PSA
layers in particular is described.
[0019] A disadvantage of viscoelastic acrylate carriers which
exhibit a profile of crosslinking through the layer is their
inadequate capacity for distributing stresses in a uniform way. One
side is always either overcrosslinked or undercrosslinked. An exact
balance can never be struck between adhesive and cohesive
properties for the entire layer, but instead only for a small
section.
[0020] EBC-crosslinked layers as well always exhibit a profile of
crosslinking in accordance with the layer thickness and the
material. With EBC-crosslinked layers as well it is impossible to
set the crosslinking exactly. Nevertheless, EBC crosslinking
proceeds without added photoinitiators, thereby removing some,
although not all, of the disadvantages associated with the
UV-irradiated layers. Depending on the accelerator voltage and on
the thickness of the material to be irradiated, it is possible to
vary the thickness of the irradiated layer. Layers above about 500
.mu.m in thickness, particularly if filled with inorganic fillers
such as glass balls, for example, can no longer be economically
irradiated. Here, therefore, there is an upper limit on the layer
thicknesses that are achievable.
SUMMARY OF THE INVENTION
[0021] It is an object of the invention, accordingly, to provide an
adhesive tape which comprises an acrylate-based viscoelastic
carrier layer which no longer has the abovementioned disadvantages
and which instead is notable for good technical adhesive properties
and very good anchoring of the layers to one another and which can
be utilized in particular as an adhesive assembly tape. The
adhesive tape ought to possess consistent properties through the
carrier layer; in other words, in particular, it ought not to
exhibit any profile of crosslinking.
DETAILED DESCRIPTION
[0022] In accordance with the invention this object is achieved by
means of a double-sided adhesive tape having at least one carrier
layer and two adhesive layers, the carrier layer being composed of
a photoinitiator-free, homogeneously crosslinked polyacrylate,
which thus exhibits no profile of crosslinking through the
layer.
BRIEF DISCUSSION OF THE DRAWINGS
[0023] FIG. 1 is a diagrammatic representation of the process for
producing the adhesive tape of the invention.
[0024] FIG. 2 illustrates the construction of the three-layer
adhesive-polyacrylate carrier-adhesive system of the invention in a
two-roll unit.
[0025] FIG. 3. illustrates a test of the holding power of the
adhesive tape of the invention.
[0026] The crosslinked, polyacrylate-based carrier layer is in
particular a carrier layer which is viscoelastic, i.e., which shows
flow behavior on a substrate, and at the same time possesses at
least partly elastic properties.
[0027] One preferred embodiment of the invention is given by a
three-layer adhesive tape which comprises as its viscoelastic
carrier a photoinitiator-free, homogeneously thermally crosslinked
acrylate hotmelt which at least on one side, in particular on both
sides, is covered with a pretreated, preferably corona-pretreated
adhesive. With particular preference the carrier layer is joined to
the adhesive layers by means of chemical reaction.
[0028] Between the carrier layer and one or both adhesive layers
there may in each case be a barrier layer, particularly in order to
prevent any migration of additives or chemical compounds.
[0029] With different advantageous embodiments of the adhesive tape
it is also possible for the features of the individual embodiments
of the invention to be combined with one another.
[0030] The adhesive tape of the invention, i.e., in particular, the
three-layer adhesive assembly tape with a homogeneously crosslinked
viscoelastic polyacrylate carrier, is advantageously obtained by
the method described in the following text: At least one thermal
crosslinker is added in the melt, preferably under precise
temperature and time control, to a polyacrylate copolymer (referred
to simply below as "polyacrylate") based on acrylic esters and/or
methacrylic esters. The polyacrylate together with the crosslinker
is conveyed to a coating unit, more preferably with an extruder,
more preferably still with a compounding extruder in which the
crosslinker has already been added and in which, where appropriate,
the concentration of the polyacrylate has already taken place; in
this regard, compare the diagrammatic representation in FIG. 1,
where the numbers and symbols have the following definitions: 1.1
polyacrylate feed, 1.2: addition of crosslinker, 1.3: extruder, RW:
doctor roll; BW: coating roll. In or after this coating unit the
material is introduced between two adhesive layers each of which
has been pretreated, preferably corona-pretreated, and has been
coated two-dimensionally onto a carrier material (also referred to
as a liner; particularly siliconized release film or release
paper). Preference is given to coating and lamination by means of
double-roll, multiroll or nozzle coating, very preferably with the
coating unit illustrated later on below.
[0031] The crosslinking of the polyacrylate introduced in this way
takes place in the layer, and in particular the thermal
crosslinkers which have been added to the polyacrylate react with
the pretreated boundary layer. In this case there is a chemical
attachment of the adhesives to the resultant viscoelastic carrier
layer. This provides for effective anchoring of carrier material
(polyacrylate) and adhesive layers.
[0032] The time after the crosslinking system has been metered in
the compounding assembly up until the polyacrylate composition that
forms the carrier is shaped between the adhesives, particularly
between the adhesives coated on liners, is referred to as the
processing time. Within this time, the viscoelastic carrier layer,
which is now undergoing crosslinking, can be coated gel-free with
an optically good coating pattern. Crosslinking then takes place
primarily after coating on the web under mild conditions, which are
harmful neither to carrier nor to liner; in other words, with
particular advantage, without the influence of actinic radiation
such as additional UV irradiation or electron beams. This produces
a homogeneously crosslinked layer, in other words one which does
not exhibit a profile of crosslinking through the layer.
[0033] The base composition used for the carrier layer, in
particular for the viscoelastic carrier layer, comprises
polyacrylates, which are polymers based at least partly on acrylic
esters and/or methacrylic esters.
[0034] With preference in accordance with the invention a portion
of the acrylic esters and/or methacrylic esters contains primary
hydroxyl groups. In a preferred procedure the fraction of the
acrylic and/or methacrylic esters containing primary hydroxyl
groups is up to 25% by weight, based on the polyacrylate.
[0035] It may also be of advantage if the polyacrylate includes
some copolymerized acrylic acid.
[0036] For the method of the invention for producing the adhesive
tape, as a basis for the viscoelastic carrier, it is preferred to
use a polyacrylate which can be traced back to the following
reactant mixture: [0037] a) acrylic esters and/or methacrylic
esters of the following formula
[0037] CH.sub.2.dbd.CH(R.sup.I)(COOR.sup.II) where R.sup.1.dbd.H or
CH.sub.3 and R.sup.II is an alkyl chain having 1 to 20 C atoms,
with a fraction of 65%-99% by weight, [0038] a2) acrylates and/or
methacrylates whose alcohol component contains at least one primary
hydroxyl group, and/or vinyl compounds which are copolymerizable
with acrylates and contain at least one primary hydroxyl group,
with a fraction of 1% to 20% by weight, [0039] a3) and, if the
fractions of a1) and a2) do not add up to 100% by weight,
olefinically unsaturated monomers containing functional groups,
with a fraction of 0% to 15% by weight.
[0040] The monomers are preferably chosen such that the resulting
polymers have a glass transition temperature of -40.degree. C. to
+80.degree. C., understood to be a dynamic glass transition
temperature for amorphous systems and to be the melting temperature
for semicrystalline systems, and being determinable by means of
dynamechanical analysis (DMA) at low frequencies.
[0041] In order to obtain a correspondingly preferred polymer glass
transition temperature, T.sub.g, of -40 to +80.degree. C., and in
accordance with the above remarks, the monomers are very preferably
selected, and the quantitative composition of the monomer mixture
advantageously chosen, in such a way as to result in the desired
T.sub.g value for the polymer in accordance with an equation (E1)
in an analogy to the Fox equation (cf. T. G. Fox, Bull. Am. Phys.
Soc. 1 (1956) 123).
1 T g = n w n T g , n ( G1 ) ##EQU00001##
[0042] In this equation, n represents the serial number of the
monomers used, w.sub.n the mass fraction of the respective monomer
n (% by weight), and T.sub.g,n the respective glass transition
temperature of the homopolymer of the respective monomer n, in
K.
[0043] With great preference use is made for a1) of acrylic or
methacrylic monomers which are composed of acrylic and methacrylic
esters having alkyl groups of 1 to 20 C atoms, preferably 4 to 9 C
atoms. Specific examples, without wishing to be restricted by this
recitation, are methacrylate, methyl methacrylate, ethyl acrylate,
n-butyl acrylate, n-butyl methacrylate, n-pentyl acrylate, n-hexyl
acrylate, n-heptyl acrylate, n-octyl acrylate, n-octyl
methacrylate, n-nonyl acrylate, lauryl acrylate, stearyl acrylate,
behenyl acrylate, and their branched isomers, such as isobutyl
acrylate, 2-ethylhexyl acrylate, 2-ethylhexyl methacrylate,
isooctyl acrylate, and isooctyl methacrylate, for example. Further
classes of compound to be used for a1) are monofunctional acrylates
and/or methacrylates of bridged cycloalkyl alcohols, composed of at
least 6 C atoms. The cycloalkyl alcohols may also be substituted,
as for example by C-1-6 alkyl groups, halogen atoms or cyano
groups. Specific examples are cyclohexyl methacrylates, isobornyl
acrylate, isobornyl methacrylates and 3,5-dimethyladamantyl
acrylate.
[0044] Great preference is given to using, for a2), monomers which
contain hydroxyl groups, very preferably primary hydroxyl groups.
Examples of a2) are hydroxyethyl acrylate, hydroxyethyl
methacrylate, hydroxypropyl acrylate, hydroxypropyl methacrylate,
6-hydroxyhexyl methacrylate, 4-hydroxystyrene, and ally alcohol,
this recitation not being conclusive.
[0045] Monomers for a3) are, for example, olefinically unsaturated
monomers having functional groups such as carboxylic acid groups,
acid anhydride groups, phosphonic acid groups, amide or imide or
amino groups, isocyanate groups, epoxy groups or thiol groups.
Examples of a3) are acrylic acid or methacrylic acid, maleic
anhydride, itaconic anhydride, itaconic acid, glyceridyl
methacrylate, glyceryl methacrylate, vinyl acetic acid,
.beta.-acryloyloxypropionic acid, trichloroacrylic acid, fumaric
acid, crotonic acid, aconitic acid, acrylonitrile dimethylacrylic
acid, N,N-dialkyl-substituted amides, such as
N,N-dimethylacrylamide, N,N-dimethylmethacrylamide,
N-tert-butylacrylamide, N-vinylpyrrolidone, N-vinyllactam,
dimethylaminoethyl methacrylate, dimethylaminoethyl acrylate,
diethylaminoethyl methacrylate, diethylaminoethyl acrylate,
N-methylol-methacrylamide, N-(buthoxymethyl)methacrylamide,
N-methylolacrylamide, N-(ethoxy-methyl)acrylamide, and
N-isopropylacrylamide, this recitation not being conclusive.
[0046] As further hardening comonomers it is possible for
macromonomers to have been copolymerized into the polyacrylate.
Particularly suitable macromonomers are those as described in EP 1
361 260 A1, such as 2-polystyreneethyl methacrylate having a
molecular weight Mw of 13 000 g/mol. The macromonomer-modified,
thermally crosslinked acrylate hotmelts which result on
crosslinking have a greater shear strength, owing to the fact that
they are physically and thermally crosslinked.
[0047] The polyacrylates are particularly suitable for inventive
further processing as carrier material if they are prepared by
bulk, solution or emulsion polymerization and if desired are
subsequently concentrated, particularly if they contain volatile
constituents. Concentration may be carried out advantageously in a
devolatizing extruder, particularly in the same way as DE 102 21
402 A1, page 3, lines 22-68.
[0048] In one preferred procedure the polyacrylates have a
weight-average molecular weight M.sub.w of at least 300 000 g/mol
up to a maximum of 1 500 000 g/mol. The average molecular weight is
determined by size exclusion chromatography (GPC) or
matrix-assisted laser desorption/ionization coupled with mass
spectrometry (MALDI-MS). It can be advantageous to carry out the
polymerization in the presence of regulators such as thiols,
halogen compounds, and, in particular, alcohols (isopropanol), in
order to set the desired weight-average molecular weight M. The
polymerization time, depending on conversion and temperature, is
between 2 and 72 hours.
[0049] Also particularly suitable for the inventive further
processing are polyacrylates which have a narrow molecular weight
distribution (polydispersity <4). These compositions have a
particularly high shear strength after crosslinking for a
relatively low molecular weight. Given that, in comparison to a
normally distributed polyacrylate, a narrow-distribution
polyacrylate needs a lower molecular weight for the same level of
cohesion, there are reductions in viscosity and in operating
temperatures. Hence a narrow-distribution polyacrylate allows a
particularly long processing time.
[0050] Narrow-distribution polyacrylates can be prepared by anionic
polymerization or by controlled free-radical polymerization
methods, the latter being especially suitable. Examples are
described in U.S. Pat. No. 6,765,078 B2 and DE 10036901 A1 or US
2004/0092685 A1. Atom transfer radical polymerization (ATRP) as
well can be used with advantage to synthesize narrow-distribution
polyacrylates, the initiator used preferably comprising
monofunctional or difunctional secondary or tertiary halides and
the halide or halides being abstracted using complexes of Cu, Ni,
Fe, Pd, Pt, Ru, Os, Rh, Co, Ir, Ag or Au (EP 0 824 111 A1; EP 826
698 A1; EP 824 110 A1; EP 841 346 A1; EP 850 957 A1). The various
possibilities of ATRP are further described in specifications U.S.
Pat. No. 5,945,491 A, U.S. Pat. No. 5,854,364 A, and U.S. Pat. No.
5,789,487 A.
[0051] Optionally it is also possible to add plasticizers, resins
and fillers to the viscoelastic acrylate layer. Suitable fillers
are hydrophilic or hydrophobic silica gels such as Aerosils or
Ultrasils, inorganic fillers such as chalk, titanium dioxide,
calcium sulfate and barium sulfate, and organic fillers such as
polymer beads or fibers based on cellulose, polyethylene,
polypropylene, polyamide, polyacrylonitrile, polyester,
polymethacrylate and/or polyacrylate.
[0052] In addition it is possible for fillers of low flammability,
such as ammonium polyphosphate, for example, and also electrically
conductive fillers, such as conductive carbon black, carbon fibers
and/or silver-coated beads, for example, and also ferromagnetic
additives, such as iron(III) oxides, for example, and also
additives for producing foamed layers, such as expandants, for
example, solid glass balls, hollow glass balls, expandable
microballoons, aging inhibitors, light stabilizers and/or ozone
protectants to be added or incorporated by compounding into the
polyacrylate before or after the latter has been concentrated.
[0053] Optionally it is possible to add the typical plasticizers in
concentrations up to 3% by weight. Examples of plasticizers which
can be metered in include low molecular mass polyacrylates,
phthalates, water-soluble plasticizers, plasticizer resins,
phosphates or polyphosphates.
[0054] The additives can be added before or after the polyacrylate
has been concentrated.
[0055] To produce thick carrier layers it is possible for these
layers to be additionally filled and/or foamed. For these purposes
the polyacrylate is admixed with solid glass balls, hollow glass
balls or expanding microballoons, preferably before the thermal
crosslinker is added.
[0056] In accordance with the invention a thermal crosslinker is
added to the polyacrylate. In one very advantageous embodiment the
added thermal crosslinker is an isocyanate, preferably a trimerized
isocyanate. With particular preference the trimerized isocyanates
are aliphatic or amine-deactivated isocyanates.
[0057] Suitable isocyanates are, in particular, trimerized
derivatives of MDI [4,4-methylenedi(phenyl isocyanate)], HDI
[hexamethylene diisocyanates, 1,6-hexylene diisocyanate] and/or
IPDI [isophorone diisocyanates,
5-isocyanato-1-isocyanatomethyl-1,3,3-trimethylcyclohexane],
examples being the products Desmodur.RTM. N3600 and XP2410 (each
from BAYER AG: aliphatic polyisocyanates, low-viscosity HDI
trimers). Also highly suitable is the surface-deactivated
dispersion of micronized trimerized IPDI that is BUEJ 339.RTM., now
HF9.RTM. (BAYER AG).
[0058] Also suitable in principle for crosslinking, however, are
other isocyanates, such as Desmodur VL 50 (MDI-based
polyisocyanate, Bayer AG), Basonat F200WD (aliphatic
polyisocyanate, BASF AG), Basonat HW100 (water-emulsifiable
polyfunctional isocyanate based on HDI, BASF AG), Basonat HA 300
(allophanate-modified polyisocyanate on isocyanurate. HDI basis,
BASF) or Bayhydur VPLS2150/1 (hydrophilically modified IPDI, Bayer
AG), this recitation not being conclusive.
[0059] The addition of the thermal crosslinker to the polyacrylate
takes place in the melt, preferably under precise temperature and
time control.
[0060] The addition and incorporation of the thermally reactive
crosslinking system into the polyacrylate matrix takes place
preferably in continuous compounding assemblies. In accordance with
the invention these assemblies are designed so that, with thorough
commixing and simultaneously low introduction of shearing energy, a
short residence time is ensured for the composition after the
crosslinking system has been metered. The compounding assemblies
are preferably extruders, especially twin-screw extruders and/or
planetary roller extruders. It is particularly advantageous if the
spindles of the extruder are heatable and/or coolable.
[0061] With advantage, and in order to optimize the time window of
the reaction, the addition may be made in the extruder in which the
polyacrylate composition has already been concentrated.
[0062] The crosslinkers are added at one or more locations in the
assemblies, preferably in unpressurized zones. It is also favorable
if the thermally reactive crosslinker substances are added in
finely divided form to the polyacrylate, such as in the form of
aerosol, in fine droplets, or in dilution in a suitable diluent
such as a polymer-compatible plasticizer.
[0063] With advantage the residual monomer content of the
polyacrylate for the carrier layer when the thermal crosslinker is
added is not more than 1% by weight, in particular not more than
0.3% by weight, based on the polyacrylate.
[0064] With advantage the residual solvent content of the
polyacrylate for the carrier layer after concentration when the
thermal crosslinker is added is not more than 1% by weight, in
particular not more than 0.3% by weight, based on the
polyacrylate.
[0065] A preferred procedure is to use the thermal crosslinker, in
particular the trimerized isocyanate, at 0.1% to 5% by weight, in
particular at 0.2% to 1% by weight, based on the polyacrylate.
[0066] In one advantageous development of the method of the
invention the temperature of the polyacrylate for the carrier layer
when the thermal crosslinker is added is between 60.degree. C. and
120.degree. C., more preferably between 70.degree. C. and
100.degree. C.
[0067] The polyacrylate melt with the crosslinker added is
transported to a coating unit, preferably directly through the
extruder in which the addition of the crosslinker and, where
appropriate, the concentration of the composition have already
taken place. There, pretreated, especially corona-pretreated,
pressure-sensitive adhesive layers are laminated onto both sides of
the partly crosslinked--that is, not yet fully
crosslinked--viscoelastic carrier layer. Reactive isocyanate groups
in the carrier layer may react at this stage with the hydroxyl
functionalities of the PSA layers laminated on. This has a
beneficial effect on crosslinking. Even compositions which are
otherwise very difficult to anchor can be attached in this way to
the viscoelastic carrier layer.
[0068] Suitable adhesive layers of the adhesive tape of the
invention comprise in principle all kinds of adhesives that can be
anchored on the carrier.
[0069] With great preference in a sense of the invention use is
made of pressure-sensitive adhesives (PSAs). In one preferred
procedure a pretreated, especially corona-pretreated, polyacrylate
layer is laminated on to both sides. It is also possible to use
adhesive layers, particularly acrylate-based adhesive layers, that
have been pretreated by other methods, provided that in these
adhesives there are already functional groups, and/or their
functional groups formed as a result of the pretreatment, that
enter into chemical bonds with isocyanate groups.
[0070] Particularly preferred PSAs are all-acrylate compositions or
those which contain no migratable components such as resins or
plasticizers in any notable concentration.
[0071] Great preference is given in the sense of the invention to
all-acrylate PSAs which have been coated beforehand onto
siliconized polyester liners.
[0072] As well as PSAs, suitability is also possessed by hotmelt
adhesive layers or heat-activatable layers, which are laminated
preferably onto one side of the viscoelastic layer. This gives
products having a asymmetric construction.
[0073] Examples of suitable base polymers for adhesives (both PSAs
and other adhesives) are natural rubber, synthetic rubbers,
acrylate block copolymers, styrene block copolymers, EVA, many
polyolefins, polyurethanes, polyvinyl ethers, and silicones.
[0074] Preference is given to adhesives with no notable fractions
of migratable constituents, and which are so highly compatible with
the polyacrylate of the carrier layer that they could migrate into
it in a significant amount.
[0075] Examples of PSA layers very suitable in accordance with the
invention are described in EP 1 308 492 A (page 27, line 23 to page
12, line 56).
[0076] The adhesives, preferably PSAs, coated onto release material
can be pretreated by all known physical or chemical methods which
form reactive groups that are able to react with isocyanates. It is
also possible to use all known techniques for priming, it being
possible for the primer layers to be applied both from solutions or
from dispersions onto the adhesive layers. Application may also
take place in an extrusion or coextrusion process. Preferred
physical methods are flame pretreatment, corona pretreatment,
atmospheric plasma pretreatment or vacuum plasma treatment. Great
preference attaches to corona pretreatment directly before the
lamination of the still-reactive viscoelastic carrier layer.
[0077] In certain cases, particularly when using PSAs with
migratable constituents such as styrene block copolymers or rubber,
it may be sensible to use a barrier layer, made of polyamide, for
example. Other materials too, however, which fulfill this purpose
are allowable. Then, advantageously, in order to produce a
double-sided adhesive assembly tape, either the barrier layer is
applied to an adhesive which has been coated beforehand onto a
release material, after which pretreatment takes place by the
techniques described above on the barrier layer side, and
lamination takes place to the still-reactive viscoelastic carrier
layer. Alternatively the barrier layer can be applied to the
viscoelastic carrier layer and then coated with the adhesive.
[0078] Directly after the operation of coating by means of roll
application or extrusion die, the viscoelastic carrier layer is
partially crosslinked, but not yet sufficiently crosslinked.
Coating in this context means the shaping of the very substantially
solvent-free carrier composition, blended with crosslinker, into
corresponding layers, and application between the pretreated
adhesive layers applied onto material in web form. The degree of
crosslinking at this point in time, therefore, may not have
advanced past a point where the processability of the PSA, in
particular in respect of a good coating pattern, is no longer
ensured.
[0079] The processing time is 3-30 minutes, preferably 5-20
minutes, more preferably 5-10 minutes.
[0080] The construction of the three-layer adhesive-polyacrylate
carrier-adhesive system takes place preferably via a two-roll unit
(cf. FIG. 2). By means of a distributor nozzle (1) or other
suitable unit, the viscoelastic composition (3) that forms the
eventual carrier material, and which is already compounded with the
crosslinker and, where appropriate, with fillers, is supplied to
the roll nip where it is introduced between the two adhesive layers
(6a, 6b), which have been subjected beforehand to a pretreatment,
in particular a corona treatment (8) (corona conduction preferably
set: 10 to 200 W min/m.sup.2), preferably 30-160 W min/m.sup.2,
very preferably 80-120 W min/m.sup.2. The adhesives, coated in
particular onto antiadhesive auxiliary carriers (7a, 7b), are
introduced into the apparatus via the rolls W1 and W2, in such a
way that the adhesive sides are facing one another.
[0081] The shaping of the viscoelastic composition into a
viscoelastic film takes place between the calender rolls W1 and W2
in the roll nip, and at the same time there is coating with the two
supplied adhesives (6a, 6b). The purpose of pretreating the
adhesives, in particular within a corona station (8), is to improve
the anchoring of the adhesives on the shaped, viscoelastic carrier
layer. This treatment produces active OH groups on the surface of
the adhesives, which after the three-layer assembly has been
produced lead to improved chemical attachment to the viscoelastic
carrier layer.
[0082] The width of the roll nip and the pressure of the rolls
determine the layer thickness of the carrier.
[0083] The process outlined above is particularly suitable for
producing viscoelastic three-layer constructions with layer
thicknesses between 100 .mu.m and 10 000 .mu.m, preferably between
300 .mu.m and 5000 .mu.m, at production speeds of between 0.5 m/min
and 100 m/min.
[0084] Depending on the viscoelastic compositions and antiadhesive
carrier materials used, the surface temperatures of the rolls are
set at preferably between 25.degree. C. and 200.degree. C., more
preferably between 60.degree. C. and 150.degree. C., and very
preferably between 80.degree. C. and 120.degree. C. Suitable
surfaces for the two calender rolls used include all of the
materials that are familiar to the skilled worker, such as steel,
chromium-plated steel, stainless steel, plastics, silicones,
ceramics, and combinations of the stated materials.
[0085] Amazingly, and surprisingly for the skilled worker, the bead
of composition rotating within the roll nip does not undergo mixing
with the supplied adhesives. It would have been expected that the
adhesive would be dissolved at least partly by the antiadhesively
furnished carrier, and would undergo mixing with the rotating bead
of composition.
[0086] The crosslinking reaction, especially with isocyanates,
proceeds preferably without catalyses. In the case of
functionalized acrylate copolymers that contain no copolymerized
acrylic acid, the reaction proceeds preferably with aromatic and/or
aliphatic isocyanates at slightly elevated temperatures. In the
case of functionalized acrylate copolymers that contain
copolymerized acrylic acid, the reaction rate is faster. Here an
operationally stable process is accomplished preferably with the
slower-reacting aliphatic isocyanates or surface-deactivated
isocyanate emulsions.
[0087] Even without any heat being supplied, the crosslinking
reaction proceeds to completion under standard conditions (room
temperature). Generally, the crosslinking reaction with the
multifunctionalized isocyanate is very largely at an end after a
storage period of up to 14 days, in particular of four to ten days,
and the ultimate cohesion of the composition has been reached. At
the same time, as a result, the viscoelastic carrier layer attaches
chemically to the outer layers of adhesive that have been laminated
on.
[0088] The crosslinking with isocyanates forms urethane groups
which link the polymer chains. This linkage results in an increase
in the cohesion of the viscoelastic carrier layer and hence in the
shear strength of the product.
[0089] The physical properties of the viscoelastic carrier and of
the end product, particularly the viscosity, flow-on behavior, heat
stability, and shear strength, can be influenced not only by the
comonomers and, where appropriate, fillers selected but also by the
degree of crosslinking, thereby allowing the end product to be
optimized through an appropriate choice of the reaction conditions.
Various factors determine the operational window of this process.
The most important influencing variables, particularly in the case
of unblended systems, are operational temperature and coating
temperature, residence time in the compounding extruder and coating
assembly, type of crosslinker (deactivated, aliphatic, aromatic),
crosslinker concentration, fraction of hydroxyl groups in the
polymer, fraction of copolymerized acid groups in the polymer, and
the average molecular weight of the polyacrylate.
[0090] A number of relations are described below with regard to the
preparation of the polyacrylate of the invention, these relations
optimizing the production method but not being restrictive of the
concept of the invention:
[0091] For a given concentration of crosslinker, an increase in the
operating temperature leads to a reduced viscosity, which enhances
the coatability of the viscoelastic composition but reduces the
processing time. An increase in processing time is obtained by
lowering the crosslinker concentration, lowering the molecular
weight, lowering the concentration of hydroxyl groups in the
polymer, lowering the acid fraction in the polymer, using less
reactive isocyanates, and lowering the operating temperature. An
improvement in the cohesion of the viscoelastic composition can be
obtained in different ways. One way is to raise the crosslinker
concentration, which reduces the processing time. With the
crosslinker concentration constant, it is also possible to raise
the molecular weight of the polyacrylate, which is possibly more
efficient. The abovementioned parameters must be adapted
appropriately in accordance with the desired profile of
requirements of the composition and/or the product.
[0092] Where expanding microballoons are used in the production of
foamed layers, the composition or the shaped layer is
advantageously activatable in an appropriate manner by introduction
of heat. A corona-pretreated polyacrylate layer can then be
laminated on, preferably, to both sides of this foamed layer.
Advantageously the foamed layer is smoothed by the lamination of
the corona-pretreated PSA layers, or separately, by means of rolls,
for example.
[0093] As a result of the combination of the carrier formulas and
adhesive formulas, the adhesive tape of the invention exhibits
outstanding properties, of a kind which could not have been
foreseen by the skilled worker, and, consequently, the use of the
tape is possible in particular as an adhesive assembly tape for
high-performance applications. This is also true in particular for
its implementation as a self-adhesive tape. The inventive
advantages are significant in particular at application
temperatures of between 100 and 130.degree. C. Furthermore, on
account of the very good anchoring and homogeneous crosslinking,
the plasticizer resistance is outstanding. The bond strength on
plasticizer-containing substrates remains high even after storage,
and the anchoring of the layers to one another remains very good.
Delamination of the layers is not observed even following storage
against plasticizer-containing substrates.
[0094] On account of the high flexibility of the carrier, the
adhesive tape conforms very well to uneven substrates. A durable
bond is produced between adhesive tape and substrate, and does not
fail even under high shearing forces and bending-moment stresses,
even at high temperatures and even after storage under UV
irradiation and moisture.
[0095] An adhesive tape of this kind can be used, for example, in
the furniture industry, where mirrors, strips or trim are to be
durably bonded. On account of the outstanding properties of the
product, its use as an assembly material is also advantageous in
many areas of industry, when different surfaces, especially
UV-transparent surfaces, such as window glass or transparent
plastics, are to be durably bonded to one another.
[0096] As a result of the homogeneous crosslinking through the
layer, the technical adhesive performance is equally good on each
side. With the same adjacent adhesive layers and the same surface
structures, the technical adhesive properties of the respective
sides are also the same. The viscoelastic carriers do not exhibit
any profile of crosslinking through the layer.
[0097] With the method of the invention it is possible,
furthermore, to offer very thick adhesive tapes. The viscoelastic
carrier layer can be particularly thick, since in principle this
process is not subject to any limit on layer thickness, in contrast
to crosslinking via UV or EBC irradiation. In particular it is also
possible to produce filled and foamed viscoelastic layers. In
addition, prior to the addition of the thermal crosslinker, it is
sensible to add solid glass beads, hollow glass beads or expanding
microballoons to the polyacrylate. Where expanding microballoons
are used, the composition or the shaped layer is preferably
activated in an appropriate way by means of introduction of heat. A
corona-pretreated polyacrylate layer can then be laminated on,
preferably, on both sides to this foamed layer. Advantageously the
foamed layer is smoothed by the lamination of the corona-pretreated
adhesive layers or separately, between two rollers, for
example.
[0098] It is possible to obtain layers colored and filled in any
desired way. Moreover, the residual monomer content of the
viscoelastic layers, as of the three-layer product as a whole, is
very low. A particularly advantageous possibility is that of being
able to produce the homogeneously crosslinked viscoelastic acrylate
carrier of the three-layer, double-sidedly adhesive-furnished
adhesive tape at coating speeds of above 50, preferably 100
m/min.
[0099] For certain applications the adhesive tape of the invention,
in this case in the form of an intermediate product, can be
improved or further adapted to requirements by means of additional
irradiation with actinic radiation (UV light or electron beams, for
example).
EXAMPLES
[0100] The exemplary embodiments which follow are intended to
illustrate the invention, without the choice of the examples given
being intended to restrict the invention unnecessarily.
[0101] Test Methods:
[0102] Solids Content:
[0103] The solids content is a measure of the fraction of
nonvolatiles in a polymer solution. It is determined
gravimetrically by weighing the solution, then evaporating the
volatile fractions in a drying cabinet at 120.degree. C. for 2
hours, and weighing the residue again.
[0104] K Value (According to FIKENTSCHER):
[0105] The K value is a measure of the average size of molecules of
high-polymer compounds. It is measured by preparing one percent (1
g to 100 ml) toluene solutions of polymer and determining their
kinematic viscosities using a VOGEL-OSSAG viscometer. Standardizing
to the viscosity of the toluene gives the relative viscosity, from
which the K value can be calculated by the method of FIKENTSCHER
(Polymer 8/1967, 381 ff.).
[0106] Gel Permeation Chromatography GPC
[0107] The average molecular weight M.sub.w and the polydispersity
PD were determined by the company Polymer Standards Service at
Mainz. The eluent used was THF containing 0.1% by volume
trifluoroacetic acid. Measurement was made at 25.degree. C. The
precolumn used was of type PSS-SDV, 5.mu., 10.sup.3 .ANG., ID 8.00
mm.times.50 mm. Separation was carried out using the columns of
type PSS-SDV, 5.mu., 10.sup.3 and also 10.sup.5 and 10.sup.6 each
of ID 8.0 mm.times.300 mm. The sample concentration was 4 g/l and
the flow rate 1.0 ml per minute. Measurement was made against PMMA
standards.
[0108] 90.degree. Bond Strength to Steel (Open and Lined Sides)
[0109] The bond strength to steel is determined under test
conditions of 23.degree.+/-1.degree. C. room temperature and
50%+/-5% relative atmospheric humidity. The specimens were cut to a
width of 20 mm and adhered to a steel plate. Prior to the
measurement, the steel plate must be cleaned and conditioned. For
that purpose the plate is first wiped with acetone and then left in
the air for 5 minutes to allow the solvent to evaporate. The side
of the transfer tape facing away from the test substrate was then
lined with a 50 .mu.m aluminum foil, to prevent the specimen
stretching in the course of measurement. After that, the test
specimen was rolled onto the steel substrate. For that purpose the
tape was run over back and forth with a 2 kg roller 5 times, at a
rolling speed of 10 m/min. Immediately after this rolling, the
steel plate was inserted into a special mount which allows the
specimen to be peeled vertically upward at an angle of 90.degree..
The bond strength was measured using a Zwick tensile testing
machine. In the case of application of the lined side to the steel
plate, the open side of the transfer tape is first laminated
against the 50 .mu.m aluminum foil, the release material is removed
and the tape is adhered to the steel plate, rolled on in the same
way and subjected to measurement.
[0110] The results measured for both sides, open and lined, are
reported in N/cm and have been averaged from three
measurements.
[0111] Holding Power (Open and Lined Sides)
[0112] Sample preparation took place under test conditions of
23.degree. C.+/-1.degree. C. room temperature and 50%+/-5% relative
atmospheric humidity. The test specimen was cut to 13 mm and
adhered to a steel plate. The bond area is 20 mm.times.13 mm
(length.times.width). Prior to the measurement, the steel plate was
cleaned and conditioned. For that purpose the plate is first wiped
with acetone and then left in the air for 5 minutes to allow the
solvent to evaporate. After bonding, the open side was reinforced
with a 50 .mu.m aluminum foil and rolled over twice back and forth
with a 2 kg roller. Then a belt loop was attached to the protruding
end of the transfer tape. The whole assembly was then suspended
from a suitable apparatus and loaded with 10 N. The suspension
apparatus is such that the weight loads the sample at an angle of
179.degree.+/-1.degree.. This ensures that the transfer tape cannot
peel from the bottom edge of the plate. The measured shear
withstand time, the time between suspension of the specimen and its
falling off, is reported as holding power in minutes and
corresponds to the average value from three measurements. For the
measurement of the lined side, the open side is first reinforced
with the 50 .mu.m aluminum foil, the release material is removed,
and the tape is adhered to the test plate in the same way as
described. The measurement is made under standard conditions
(23.degree. C., 55% atmospheric humidity).
[0113] Rolling Ball Tack (Open and Lined Sides)
[0114] The rolling ball test was used to measure the tack of the
specimens with a very short contact time. Measurement took place
under test conditions of 23.degree. C.+/-1.degree. C. room
temperature and 50%+/-5% relative atmospheric humidity. The
transfer tape was fixed, with the side under test facing upward,
under gentle tension, on the working plate, which was oriented
exactly horizontally. Subsequently a ramp 65 mm high was placed on
the specimen strip and a clean ball, cleaned with acetone and
weighing 5.6 g, was rolled down the ramp. The distance between the
leading edge of the ramp and the center point of the rolled ball
which has come to rest was measured. The value reported is the
average from 5 measurements per side.
[0115] SAFT--Shear Adhesive Failure Temperature (Open and Lined
Sides)
[0116] The SAFT test is an accelerated test of the short-term
temperature resistance of the transfer tapes. The specimens were
reinforced with a 50 .mu.m aluminum foil and the remaining adhesive
side was adhered to a ground steel test plate which had been
cleaned with acetone, and then overrolled six times using a 2 kg
steel roller at a speed of 10 m/min. The bond area of the sample,
height.times.width, was 13 mm.times.10 mm. The top part of the
specimen, which protrudes beyond the test plate by 2 mm, was
reinforced with a shear adhesive strip. At this point, after the
sample had been suspended vertically, the travel sensor was
applied.
[0117] The sample under measurement was loaded at the bottom end
with a weight of 50 g. The steel test plate with the bonded sample
was then heated, starting at 25.degree. C. and at a rate of
9.degree. C. per minute, to the final temperature of 200.degree. C.
Using the travel sensor, the slip travel of the sample was measured
as a function of temperature and time. The measurement was ended
when the envisaged final temperature was reached or when a slip
travel of >1000 .mu.m was attained.
[0118] The SAFT test is able to provide two test features: SAFT
shear travel or SAFT short-term temperature resistance. The SAFT
shear travel is the slip travel in .mu.m when the final temperature
is reached. The SAFT short-term temperature resistance is the
temperature at which a slip travel of 1000 .mu.m is attained. Both
sides are measured: the open side and the lined side. The value
reported is in each case the average of a duplicate
determination.
[0119] Wall Hook Test
[0120] FIG. 3 shows the testing of the pressure-sensitive
polyacrylate layers (layer A and/or C). A test specimen (3.1) fixed
between two polished steel plates (3.2) and measuring 30
mm.times.30 mm is pressed for 1 minute at 0.9 kN (force P). After
that, a lever arm (3.3) 9 cm long is screwed into the top steel
plate, which is subsequently loaded with a 1000 g weight (3.4).
Care is taken to ensure that the time between pressing and loading
is not more than 2 minutes (t.ltoreq.2 min).
[0121] A measurement is made of the holding power, i.e., the time
between the suspension of the specimen and its falling off. The
result reported is the holding power in minutes, as the average
value from a triplicate determination. The test conditions are
23.degree. C.+/-1.degree. C. and 50% rh+/-5% rh (rh=relative
humidity).
[0122] Measurements were carried out in each case on the open side
and the lined side.
[0123] Pressure-Sensitive Polyacrylate Adhesive 1 (PA1):
[0124] A 100 l glass reactor conventional for free-radical
polymerizations was charged with 2.8 kg of acrylic acid, 8.0 kg of
methyl acrylate, 29.2 kg of 2-ethylhexyl acrylate and 20.0 kg of
acetone/isopropanol (95:5). After nitrogen gas had been passed
through the reactor for 45 minutes with stirring, the reactor was
heated to 58.degree. C. and 20 g of azoisobutyronitrile (AIBN, Vazo
64.RTM., DuPont) were added. Subsequently the external heating bath
was heated to 75.degree. C. and the reaction was carried out
constantly at this external temperature. After a reaction time of 1
h a further 20 g of AIBN were added. After 4 h and 8 h the reaction
mixture was diluted with 10.0 kg each time of acetone/isopropanol
(95:5) mixture. For reduction of the residual initiators, after
both 8 h and 10 h, 60 g portions of bis(4-tert-butylcyclohexanyl)
peroxydicarbonate (Perkadox 16.RTM., Akzo Nobel) were added. The
reaction was discontinued after a reaction time of 24 h and the
reaction mixture was cooled to room temperature. Subsequently the
polyacrylate was blended with 0.4% by weight of aluminum(III)
acetylacetonate (3% strength solution, isopropanol), the blend was
diluted with isopropanol to a solid contents of 30%, and then
coating took place from solution onto a siliconized release film
(50 .mu.m polyester). (Coating speed 2.5 m/min, drying tunnel 15 m,
temperatures: zone 1: 40.degree. C., zone 2: 70.degree. C., zone 3:
95.degree. C., zone 4: 105.degree. C.). The coat weight was 50
g/m.sup.2.
[0125] Pressure-Sensitive Polyacrylate Adhesive 2 (PA2):
[0126] A 100 l steel reactor conventional for free-radical
polymerizations was charged with 4.0 kg of acrylic acid, 36.0 kg of
2-ethylhexyl acrylate and 13.3 kg of acetone/isopropanol (96:4).
After nitrogen gas had been passed through the reactor for 45
minutes with stirring, the reactor was heated to 58.degree. C. and
20 g of azoisobutyronitrile (AIBN, Vazo 64.RTM., DuPont) were
added. Subsequently the external heating bath was heated to
75.degree. C. and the reaction was carried out constantly at this
external temperature. After a reaction time of 1 h a further 20 g
of AIBN were added. After 4 h and 8 h the reaction mixture was
diluted with 10.0 kg each time of acetone/isopropanol (96:4)
mixture. For reduction of the residual initiators, after both 8 h
and 10 h, 60 g portions of
bis(4-tert-butylcyclohexanyl)peroxydicarbonate (Perkadox 16.RTM.,
Akzo Nobel) were added. The reaction was discontinued after a
reaction time of 24 h and the reaction mixture was cooled to room
temperature. Subsequently the polyacrylate was blended with 0.4% by
weight of aluminum(III) acetylacetonate (3% strength solution,
isopropanol), the blend was diluted with isopropanol to a solids
content of 30%, and then coating took place from solution onto a
siliconized release film (50 .mu.m polyester). After drying
(coating speed 2.5 m/min, drying tunnel 15 m, temperatures: zone 1:
40.degree. C., zone 2: 70.degree. C., zone 3: 95.degree. C., zone
4: 105.degree. C.) the coat weight was 50 g/m.sup.2.
[0127] B. Production of the Viscoelastic Carriers
[0128] Preparation of the Starting Polymers for the Viscoelastic
Carriers of Examples VT 1 to 6
[0129] The preparation of the starting polymers is described below.
The polymers investigated were prepared conventionally via
free-radical polymerization in solution.
[0130] HEMA=hydroxyethyl methacrylate
[0131] AIBN=2,2'-azobis(2-methylbutyronitrile)
[0132] Perkadox 16=bis(4-tert-butylcyclohexyl)peroxydicarbonate
[0133] Base Polymer 1 (B1)
[0134] A reactor conventional for free-radical polymerizations was
charged with 27 kg of 2-ethylhexyl acrylate, 27 kg of n-butyl
acrylate, 4.8 kg of methyl acrylate, 0.6 kg of acrylic acid, 0.6 kg
of HEMA and 40 kg of acetone/isopropanol (93:7). After nitrogen gas
had been passed through the reactor for 45 minutes with stirring,
the reactor was heated to 58.degree. C. and 30 g of AIBN were
added. Subsequently the external heating bath was heated to
75.degree. C. and the reaction was carried out constantly at this
external temperature. After 1 h a further 30 g of AIBN were added
and after 4 h the batch was diluted with 10 kg of
acetone/isopropanol mixture.
[0135] After 5 h and after 7 h, reinitiation was carried out with
90 g of Perkadox 16 each time. After a reaction time of 22 h the
polymerization was discontinued and the product was cooled to room
temperature. The polyacrylate has a K value of 69, a solids content
of 54.6%, an average molecular weight of Mw=819 000 g/mol, and a
polydispersity (Mw/Mn)=7.6.
[0136] Base Polymer 2 (B2)
[0137] In the same way as for example 1, 36.0 kg of 2-ethylhexyl
acrylate, 21.0 kg of tert-butyl acrylate, 2.4 kg of acrylic acid
and 0.6 kg of HEMA were polymerized in 40 kg of acetone/isopropanol
(93:7). Initiation was carried out twice with 30 g of AIBN each
time, twice with 90 g of Perkadox 16 each time, and dilution was
carried out with 10 kg of acetone/isopropanol mixture (93:7). After
a reaction time of 22 h the polymerization was discontinued and the
product was cooled to room temperature.
[0138] The polyacrylate has a K value of 60.0, a solids content of
53.5%, an average molecular weight of Mw=602 000 g/mol, and a
polydispersity (Mw/Mn)=7.1.
[0139] Base Polymer 3 (B3)
[0140] The same procedure was used as for example 1. For the
polymerization, 36 kg of 2-ethylhexyl acrylate, 20.4 kg of methyl
acrylate, 2.4 kg of acrylic acid and 1.2 kg of HEMA were
polymerized in 40 kg of acetone/isopropanol (90:10). Initiation was
carried out twice with 30 g of AIBN each time, twice with 90 g of
Perkadox 16 each time, and dilution was carried out with 10 kg of
acetone/isopropanol mixture (90:10). After a reaction time of 22 h
the polymerization was discontinued and the product was cooled to
room temperature.
[0141] The polyacrylate has a K value of 57, a solids content of
53.8%, an average molecular weight of Mw=526 000 g/mol, and a
polydispersity (Mw/Mn)=6.8.
[0142] Base Polymer 4 (B4)
[0143] A reactor conventional for free-radical polymerizations was
charged with 36 kg of 2-ethylhexyl acrylate, 21 kg of tert-butyl
acrylate, 2.4 kg of acrylic acid, 0.6 kg of HEMA, 40 g of benzyl
dithiobenzoate and 40 kg of acetone. After nitrogen gas had been
passed through the reactor for 45 minutes with stirring, the
reactor was heated to 58.degree. C. and 30 g of AIBN were added.
Subsequently the external heating bath was heated to 75.degree. C.
and the reaction was carried out constantly at this external
temperature. After 1 h a further 30 kg of AIBN were added and after
4 h the batch was diluted with 5 kg of acetone. After 5 h and after
7 h, 90 g portions of Perkadox 16.TM. (Akzo) were added. After a
reaction time of 22 h the polymerization was discontinued and the
product was cooled to room temperature. The polyacrylate has a K
value of 53.6, a solids content of 54.9%, an average molecular
weight of Mw=479 000 g/mol, and a polydispersity (Mw/Mn)=2.4.
[0144] Method 1: Concentration of the Base Polymers for the
Viscoelastic Carriers:
[0145] The acrylate copolymers (base polymer 1-4) functionalized
with hydroxyl groups are freed very largely from the solvent by
means of a BERSTORFF single-screw extruder (concentrating
extruder). The parameters given by way of example here are those
for the concentration of base polymer 1. The speed of the screw was
160 rpm, the motor current 16 A, and a throughput of 61.5 kg
liquid/h was realized. For concentration, a vacuum was applied at 3
different domes. The reduced pressures were, respectively, 440
mbar, 50 mbar and 5 mbar, the lowest vacuum being applied in the
first dome. The exit temperature of the concentrated hotmelt was
104.degree. C. The solids content after this concentration step was
99.8%.
[0146] Method 2: Production of the Filler-Modified Viscoelastic
Carriers, Blending with the Thermal Crosslinker
[0147] The acrylate polymers concentrated by method 1 were melted
in a feeder extruder (single-screw conveying extruder from
TROESTER) and using this extruder were conveyed as a polymer melt
into a twin-screw extruder (LEISTRITZ, Germany, ref. LSM 30/34).
The assembly is heated electrically from the outside and is air
cooled by a number of fans. The geometry of the mixing screws was
chosen such that effective distribution of the fillers and of the
crosslinking system in the polymer matrix is accompanied by the
assurance of a short residence time of the acrylate composition in
the extruder. For these purposes the mixing screws of the
twin-screw extruder were arranged so that conveying elements are in
alternation with mixing elements. The addition of the fillers and
of the respective crosslinking system takes place with appropriate
metering equipment, at two or more sites where appropriate, into
the unpressurized conveying zones of the twin-screw extruder.
Metering aids are used where appropriate to meter the crosslinking
system. It is possible if desired to connect a vacuum pump to the
twin-screw extruder in order to free the compounded self-adhesive
composition from gas inclusions. The ready-compounded acrylate
composition is then supplied, by means of a melt pump downstream of
the mixing extruder, to a distributor nozzle, which conveys the
viscoelastic carrier into the first roll nip of the coating
calender. Coating of the self-adhesive compositions of the
invention takes place by means of a two-roll calender in accordance
with one of the methods described below.
[0148] Method 3: Production of the Three-Layer Constructions by
Means of Two-Roll Calender
[0149] The method was carried out as described in FIG. 1. Using
distributor nozzle (1) the viscoelastic composition (3), already
compounded with the crosslinking system and, where appropriate,
fillers, is supplied to the roll nip. The shaping of the
viscoelastic composition to a viscoelastic film takes place between
the calender rolls (W1) and (W2) in the roll nip between two
self-adhesive compositions (7a, 7b), which in turn are supplied
coated onto antiadhesively furnished carrier materials (5a, 5b). In
this case there is, simultaneously, shaping of the viscoelastic
composition to the set layer thickness, and coating with the two
self-adhesive compositions supplied. In order to improve the
anchoring of the self-adhesive compositions (7a, 7b) on the shaped
viscoelastic carrier layer (4), the self-adhesive compositions,
before being fed into the roll nip, are corona-treated by means of
corona station (8) (corona unit from VITAPHONE, Denmark, 100 W
min/m.sup.2). This treatment produces active OH groups on the
surface of the self-adhesive compositions, which after the
three-layer assembly has been produced lead to improved chemical
attachment to the viscoelastic carrier layer.
[0150] The web speed on passing through the coating unit is 40
m/min.
[0151] Downstream of the roll nip, an antiadhesive carrier (5a) is
lined where appropriate, and the finished three-layer product (6)
is wound up with the remaining second antiadhesive carrier
(5b).
[0152] Presented below are specific examples relating to the
production of the self-adhesive compositions and coating of the
adhesive tapes of the invention, without any intention that the
invention should be unnecessarily restricted by the choice of
specified formulations, configurations, and operational
parameters.
Example MT 1
[0153] The base polymer B1 was concentrated by method 1 (solids
content 99.7%) and then blended by method 2 with 1.6% by weight
(based on acrylate copolymer) of the trimerized aliphatic
diisocyanates Desnnodur XP 2410 (BAYER AG, Germany). To improve its
capacity for being metered, the trimerized diisocyanate was diluted
1:3 with the liquid phosphate ester REOFOS 65 (GREAT LAKES, USA).
The operational parameters are summarized in table 1. Coating
between the composition layers PA 1, which have been coated
beforehand onto siliconized polyester films, takes place on the
two-roll applicator mechanism at roll temperatures of 100.degree.
C. by method 3. The layer thickness of the viscoelastic carrier VT
1 was 82 .mu.m. The corona power was 100 W min/m.sup.2.
[0154] After 7 days' room-temperature storage, the technical
adhesive data were measured for both the open and the lined sides.
The data of example 1 are summarized in table 2.
Example MT 2
[0155] The base polymer B1 was concentrated by method 1 (solids
content 99.7%) and then blended in the same way as in example 1
with 0.8% by weight (based on acrylate copolymer) of the trimerized
aliphatic diisocyanates Desmodur XP 2410 (BAYER AG, Germany).
Subsequently, in the same way as in example 1, coating between
composition layers PA 1, which have each been coated beforehand
onto siliconized polyester films, takes place on the two-roll
applicator mechanism by method 3. The layer thickness of the
viscoelastic carrier VT 2 was 800 .mu.m. The corona power was 100 W
min/m.sup.2.
[0156] After 7 days' room-temperature storage, the technical
adhesive data were measured for both the open and the lined sides.
The data of example MT 2 are summarized in table 2.
Example MT 3
[0157] The base polymer B1 was concentrated by method 1 (solids
content 99.7%) and then blended by method 2 with 6.5% by weight of
hollow glass beads Q-CEL 5028 (Potters Industries) and 2.13% by
weight (based on acrylate copolymer) of the hydrophilic aliphatic
polyisocyanates Bayhydur VP LS 2150/1 (BAYER AG, Germany). The
operational parameters are summarized in table 1. Coating between
the composition layers PA 1, which have been coated beforehand onto
siliconized polyester films, takes place on the two-roll applicator
mechanism at roll temperatures of 100.degree. C. by method 3. The
layer thickness of the viscoelastic carrier VT 3 was 865 .mu.m. The
corona power was 100 W min/m.sup.2.
[0158] After 7 days' room-temperature storage, the technical
adhesive data were measured for both the open and the lined sides.
The data of example MT 3 are summarized in table 2.
Example MT 4
[0159] The base polymer B2 was concentrated by method 1 (solids
content 99.7%) and then blended by method 2 with 18% by weight of
Mikrosohl chalk (MS40, Sohlde) and 0.19% by weight (based on
acrylate copolymer) of the hydrophilic aliphatic polyisocyanates
Bayhydur VP LS 2150/1 (BAYER AG, Germany). The operational
parameters are summarized in table 1. Coating between the
composition layers PA 1, which have been coated beforehand onto
siliconized polyester films, takes place on the two-roll applicator
mechanism at roll temperatures of 100.degree. C. by method 3. The
layer thickness of the viscoelastic carrier VT 4 was 790 .mu.m. The
corona power was 100 W min/m.sup.2.
[0160] After 7 days' room-temperature storage, the technical
adhesive data were measured for both the open and the lined sides.
The data of example MT 4 are summarized in table 2.
Example MT 5
[0161] The base polymer B3 was concentrated by method 1 (solids
content 99.8%) and then blended by method 2 with 3% by weight of
nonexpanded hollow microbeads Expancel 092 DU 40 (Akzo Nobel,
Germany) and 1.0% by weight (based on acrylate copolymer) of the
trimerized aliphatic diisocyanates Desmodur XP 2410 (BAYER AG,
Germany). The operational parameters are summarized in table 1.
Heat is introduced to expand the mixture in the extruder, and then
coating between the composition layers PA 1, which have been coated
beforehand onto siliconized polyester films, takes place at roll
temperatures of 130.degree. C. by method 3. The layer thickness of
the expanded viscoelastic carrier VT 5 was 740 .mu.m. The corona
power for pretreating the pressure-sensitive adhesive layers was
100 W min/m.sup.2.
[0162] After 7 days' room-temperature storage, the technical
adhesive data were measured for both the open and the lined sides.
The data of example MT 5 are summarized in table 2.
Example MT 6
[0163] The base polymer B6 was concentrated by method 1 (solids
content 99.8%) and then blended by method 2 with 5% by weight of
hydrophobized silica gel Aerosil R 972 (Degussa, Germany) and 1.0%
by weight (based on acrylate copolymer) of the trimerized aliphatic
diisocyanates Desmodur XP 2410 (BAYER AG, Germany). The operational
parameters are summarized in table 1. Coating between the
composition layers PA 1, which have been coated beforehand onto
siliconized polyester films, subsequently takes place at roll
temperatures of 100.degree. C. by method 3. The layer thickness of
the viscoelastic carrier VT 6 was 750 .mu.m. The corona power for
pretreating the pressure-sensitive adhesive layers was 100 W
min/m.sup.2.
[0164] After 7 days' room-temperature storage, the technical
adhesive data were measured for both the open and the lined sides.
The data of example MT 6 are summarized in table 2.
Example MT 7
[0165] In analogy to the production of MT 3, the base polymer B1
was concentrated by method 1 (solids content 99.7%), blended by
method 2 with 6.5% by weight of hollow glass beads Q-CEL 5028
(Potters Industries) and 2.13% by weight (based on acrylate
copolymer) of the hydrophilic aliphatic polyisocyanates Bayhydur VP
LS 2150/1 (BAYER AG, Germany), and coated by method 3 at roll
temperatures of 100.degree. C. between the composition layers PA 2,
which had been coated beforehand onto siliconized polyester films.
The layer thickness of the viscoelastic carrier VT 3 was 865 .mu.m.
The corona power for pretreating the pressure-sensitive adhesive
layers was 100 W min/m.sup.2.
[0166] After 7 days' room-temperature storage, the technical
adhesive data were measured for both the open and the lined sides.
The data of example MT 7 are summarized in table 2.
[0167] Completely surprising for the skilled worker is the
coatability of the hotmelt composition following the addition and
incorporation by mixing of the isocyanate crosslinking system into
the polyacrylate composition at the temperatures of between
60.degree. C. and 120.degree. C., preferably between 70.degree. C.
and 100.degree. C., prevailing within the compounding assembly. By
coatability is meant in this context the capacity for the shaping
of the crosslinker-blended polyacrylate composition into
viscoelastic carrier layers and for its application between
corona-pretreated pressure-sensitive adhesives which are in the
form of webs and are on release material, this application taking
place by means of coating nozzles or roll coating mechanism.
[0168] What was expected was a crosslinking or gelling of the
viscoelastic carrier composition, so that subsequent application by
coating would no longer have been possible. In actual fact,
however, the viscoelastic carrier compositions described can be
applied by coating within a certain time period after the metered
addition of crosslinker, and compounding.
[0169] The processing time is heavily dependent on molecular weight
and hydroxyl functionalization of the polyacrylate composition, and
also on the type and amount of the crosslinking system used and the
prevailing operational conditions, such as composition temperature
and geometry of the compounding assembly, for example.
[0170] In accordance with the known prior art, the skilled worker
would have expected an immediate reaction of the isocyanates with
the OH groups present in the polyacrylate, thereby making the
partially crosslinked composition undercoatable. To avoid this, he
or she would have had to use blocked isocyanates at extremely high
temperatures, with the disadvantage of the blocking agents
remaining in the adhesive and causing disruption. This would
severely disrupt the adhesive performance of the adjacent
pressure-sensitive adhesive layers.
[0171] Nor would the skilled worker have expected that effective
aftercrosslinking of the viscoelastic carrier compositions would be
possible at room temperature without the controlled influence of
actinic radiation, as shown significantly by SAFT and the 10N steel
holding power.
[0172] As is apparent from the data in the table, the inventively
double-sidedly adhesive assembly tapes have very good technical
adhesive data. A particular positive is the balanced adhesive
profile of the respective sides. With the same layer of adhesive on
both sides of the adhesive tape, their technical adhesive data are
virtually the same. This shows the homogeneous crosslinking through
the layer. This is surprising for the skilled worker. Moreover,
these three-layer adhesive tapes do not exhibit any delamination.
The anchoring of the layers to one another is very good, as a
result of the corona treatment of the pressure-sensitive adhesive
layers and the aftercrosslinking of the adjacent viscoelastic
carrier layer.
TABLE-US-00001 TABLE 1 Viscoelastic carriers Crosslinker
incorporation and coating Fraction of Crosslinker Throughput of
Rotational Setpoint Base polymer adjuvants type and amount
composition speed temperature K [% by [% crosslinker through TSE of
TSE TSE Example Polymer value weight] based on polymer] [kg/h]
[1/min] [.degree. C.] VT 1 B1 69 -- 1.6% 10 100 100 XP 2410 VT 2 B1
69 -- 0.8% 10 100 100 XP 2410 VT 3 B1 69 6.5% 2.13% 11 100 80
Hollow Bayhydur glass VP LS beads 2150/1 Q-CEL 5028 VT 4 B2 60 18%
0.19% 16 150 100 Mikrosohl Bayhydur MS 40 VP LS C160 2150/1 VT 5 B3
57 3% 1.0% 10 100 125 Expancel XP 2410 092 DU 40 VT 6 B4 54 5% 1.0%
10 100 100 Aerosil R XP 2410 972 Crosslinker incorporation and
coating Current Pressure Temperature Coating temperature consump-
at exit of composition doctor roll/ Processing Coat- Layer tion TSE
TSE after TSE coating roll time weight thickness Example [A] [bar]
[.degree. C.] [.degree. C.] [min] [g/m.sup.2] [.mu.m] VT 1 12 15
100 100/100 10 870 825 VT 2 11 15 98 100/100 15 840 800 VT 3 11 15
98 100/100 5 750 865 VT 4 19 38 123 100/100 15 985 790 VT 5 10 28
140 130/130 5 375 740 VT 6 18 25 100 100/100 10 800 750
TABLE-US-00002 TABLE 2 Product construction and technical adhesive
data for the three-layer constructions Bond strength to steel
Holding power 10N Wall test SAFT Three-layer product Total [N/cm]
23.degree. C. [min] [min] [.mu.m] Viscoelastic thickness Open Lined
Open Lined Open Lined Open Lined Example PSA 1 carrier layer PSA 2
[.mu.m] side side side side side side side side MT 1 50 g/m.sup.2
VT 1 50 g/m.sup.2 923 10.6 10.7 7300 7368 5400 5300 750 .mu.m 754
.mu.m PA 1 PA 1 (200.degree. C.) (200.degree. C.) MT 2 50 g/m.sup.2
VT 2 50 g/m.sup.2 900 11.8 11.6 5328 5450 3876 3860 937 .mu.m 915
.mu.m PA 1 PA 1 (200.degree. C.) (200.degree. C.) MT 3 50 g/m.sup.2
VT 3 50 g/m.sup.2 862 8.5 8.7 >20 000 >20 000 9320 9360 340
.mu.m 325 .mu.m PA 1 PA 1 (200.degree. C.) (200.degree. C.) MT 4 50
g/m.sup.2 VT 4 50 g/m.sup.2 885 10.7 10.6 15 460 15 386 7540 7468
545 .mu.m 552 .mu.m PA 1 PA 1 (200.degree. C.) (200.degree. C.) MT
5 50 g/m.sup.2 VT 5 50 g/m.sup.2 838 13.5 13.6 >20 000 >20
000 >10 000 >10 000 795 .mu.m 801 .mu.m PA 1 PA 1
(200.degree. C.) (200.degree. C.) MT 6 50 g/m.sup.2 VT 6 50
g/m.sup.2 850 12.7 12.6 >20 000 >20 000 >10 000 >10 000
250 .mu.m 256 .mu.m PA 1 PA 1 (200.degree. C.) (200.degree. C.) MT
7 50 g/m.sup.2 VT 3 50 g/m.sup.2 964 9.5 9.4 >20 000 >20 000
>10 000 >10 000 322 .mu.m 342 .mu.m PA 2 PA 2 (200.degree.
C.) (200.degree. C.)
* * * * *