Document jmQ1MRQOn4xKVEyy7Xoq75b1N
FILE NAME Adhesives ADH DATE 1977 Apr 19
DOC ADHOOO
DOCUMENT DESCRIPTION 1977 Apr 19 US Patent - Lakshaman - Adhesive Composition
Lakshmanan
54 ADHESIVE COMPOSITION
75
Inventor
Pallavoer R. Lakshmanan Allison
Park Pa
73 Assignee Gulf Research & Development
Company Pittsburgh Pa
Filed
22 Filed
Jan. 2 1976
21 Appl No 646,061
52
51 58
260/27 R 29.6 RB
Int Cl
29.6 RW
Field
of
Search 260
Search
COSL
93/00
.._ 29.6 RB 27 29.6 RW
II 4,018,732
45 Apr. 19 1977
56
References Cited
UNITED STATES PATENTS
22,,997766,,220033
2/1944 3/1961
Smith
PrimaryExaminer 1. Marquis
Assistant Examiner E. Parker
29.6
57
ABSTRACT ABABSTSRACT TRACT
of an disper- of An adhesive mastic
composition consisting essentially sion coa nrotsian iesnteir nangd polymer latex a water
a filler or fillers
5 Claims No Drawings
1
ADHESIVE COMPOSITION
BACKGROUND OF THE INVENTION
1 Field of the Inuntian
4,018,732
2
vlaulsuoef hreirgiediutsyedis i3s0t0he temperature temperature at which the modu-
kilograms of An essential ingredient
per square centimeter
the copolymer is that it be of
molecular
of
2,0 0,0 0 weight preferably range about 50,000 to $ about 2,000,0002,000,000 preferablypreferably about 80,000 to
1.400.000
about
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United States Patent
Lakshmanan
Adhesive composition
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4,018,732 April 19 1977
Abstract
An adhesive mastic composition consisting essentially of an
dispersion of a rosin ester and a filler or fillers
containing polymer latex a water
Inventors Lakshmanan Pallavoor R. Allison Park PA Assignee Gulf Research & Development Company Pittsburgh PA
Family ID 24591583
Appl No 646,061
Filed
January 2 1976
Current U.S. Class Current CPC Class
Current International Class
Field of Search
524/270 524/272
93/04
C09J 133/08 20130101 C09J 193/04 20130101 C08L
20130101 C08L 33/08 20130101 C08L 33/08 20130101 20130101 C08L
93/00 20130101 C09J 193/04 20130101 C09J 133/08
C08L 93/04 20130101 20130101 C08L 2666/04
20130101
20130101 C08L
2666/26 20130101 C08L 2666/04 20130101 C08L
2666/26 20130101
C09J 193/04 20060101 C09J 133/06
193/00 20060101 C09J 133/08
20060101 C09J
20060101 C08L 93/00 20060101
C08L 93/04 20060101 C08L 093/00 )
27,29.6RW
2343091 2976203
References Cited Referenced By
U.S. Patent Documents
February 1944
March 1961
Smith
Young
Primary Examiner Marquis Melvyn I. Assistant Examiner Parker William E.
Claims
I claim
1. An improved adhesive composition consisting essentially of 1 an
substance selected from the
aqueous dispersion of a polymeric
about two to about four
group consisting of a insoluble linear copolymer and salts thereof of
weight percent of an acid selected from the
acid and the dimer of methacrylic acid about five to about 25
group consisting of itaconic acid fumaric
weight weight percent of a member selected from the
2,000,000 the salt being selected from the group consisting of those of ammonium alkali metals
formed with a soluble amine the dispersion containing about 30 to about 55
and those
and at least about 30 weight percent by weight of copolymer 2 a rosin
weight percent of water
fillers said components being present in the following amounts
ester dispersion and 3 a filler or
2. The composition of claim 1 wherein the components of the composition are within the
following ranges 38.0,T0h0e0 ctoomapboosuitti1o,n50o0f,c0l0a0im 1 wherein the molecular weight of the copolymer is within the range of about
4. The composition of claim 1 wherein the rosin ester is a dispersion based on an ester of
polyfunctional alcohol having from two to four carbon
rosin with
atoms
5. The composition of claim 1 wherein the filler is calcium carbonate
6. The composition of claim 1 wherein the filler is clay
Description
BACKGROUND OF THE INVENTION INVENTION
1. Field of the Invention
This invention relates to an adhesive mastic composition consisting essentially of an
polymer latex a water dispersion of a rosin ester and filler or fillers
containing
a a provides
having a long open time which also tensile shear strength of at least about 250 pounds per square inch gauge 17.5 kilograms per
square centimeter in wood to wood bonding application
2. Description of the Prior Art
In U.S. Pat No. 2,976,203 to Young et al there is disclosed an adhesive
of a polyfunctional acid and the dimer of
composition containing a copolymer
methacrylic acid methyl methacrylate or acrylonitrile and an ester
of acrylic acid with an alcohol and optionally a filler
of such adhesives it is desired to improve the
and a thickening agent In the commercial utilization
shear strength By open time mean the
open time thereof while
maintaining extremely high tensile
of two substrates and the
time interval between the application of the adhesive
mating of the two substrates to each other
to one or both
SUMMARY OF THE INVENTION
I have found that the addition of a
an improved adhesive
water dispersion of a rosin ester to the composition defined above
composition having an open time of at least about ten
results in
about 30 minutes which also provides a tensile shear
minutes preferably about 15 to
gauge 17.5 kilograms per square centimeter
strength of at least about 250 pounds per square inch
square inch gauge about 17.5 to about 35
generally in the range of about 250 to about 500 pounds
kilograms per square centimeter in wood to wood
per
application
bonding
Those components common to the
with
the
exception
of
the
Young
molecular
et
al
adhesive
and
to
the
adhesive
defined
and
claimed
herein
there is present herein
weight of the copolymer substantially identical in
are
an aqueous dispersion of a insoluble
composition Thus
weight percent of a polyfunctional acid such as itaconic
copolymer of about two to about four
acid about five to about 25 weight percent of
acid fumaric acid and the dimer of methacrylic
thereof and the remainder one
methyl methacrylate or acrylonitrile including mixtures
atoms
such
as
methyl
or more
acrylate
esters
of acrylic
acid
with
an
alcohol
having from
one
to
18
carbon
ethyl acrylate butyl acrylate cyclohexyl acrylate
ethylhexyl acrylate t-
octyl acrylate dodecyl acrylate octadecyl acrylate etc. and
can have a pH of about 2.5
water insoluble salts thereof The
about 6.6 Proportions of thetosaebveoruatl7c.o0mpoorneevnetnshoifghteher but preferably the pH is between aboucto4m.p0osaintdion
copolymers are such so as to provide a T.sub.1
a The salt of the copolymer can be obtained by the use of
potassium or a soluble
ammonia an alkali metal such as sodium or
and
trimethylamine
are
amine such representative
as
a
lower
aliphatic
amine
of
which
triethylamine
diethylamine
ammonia or
volatile
amine
is
morpholine employed the
monoethanolamine
or
triethanolamine
Preferably
as
cation of the salt of the acid copolymer
Methyl methacrylate acrylonitrile or mixtures thereof is
minimum of about five weight weight percent of these
an essential ingredient of the composition A
adhesive
to
hold
the
adhesive
coating
in
place
monomers in the
is
essential
to
obtain
sufficient
rigidity
in
the
component depends upon the content of
final adhered structure The upper limit of the
about two weight percent of acid about 2t5heweaigchtiwdeigahtnpdertcheenptaortfitchuilsar acrylate employed At the lower limit of
acid content is increased to about four
component can be employed but as the
weight percent the maximum content of this
component that is
about 15 weight percent whereas with the
methyl methacrylate or acrylonitrile
higher alcohol acrylates such as butyl acrylate the amount of
can be as high high as about 25 weight percent
The acid component is needed to provide specific adhesion to a wide variety of substrates and
those of hydrophylic or metallic character
especially to
As noted particular ester of acrylic acid that is employed can be chosen from a wide
of
includes
methyl
acrylate
ethyl
acrylate
butyl
acrylate
cyclohexyl
acrylate
group esters
ethylhexyl acrylate
that
acrylate dodecyl acrylate octadecyl acrylate etc. Preferably the copolymers are made from
octyl
ethyl acrylate or butyl acrylate because of the availability and inexpensiveness of these monommeetr hysl acrylate
The aqueous dispersion containing the copolymer defined above can contain about 30 to about 60 weight
percent water and at least about 30 weight weight percent of the copolymer or the salt thereof
weight
the composition comprises about 50 to about 60 weight
Preferably however
the copolymer or the salt thereof
weight percent and about 40 to about 50 weight weight percent of
These dispersions can be prepared for example by following the procedure of the Young et al patent referred
to above
The second necessary component of the adhesive composition defined and claimed herein is a rosin ester Rosins and their esters are old and well known and are described for example on pages 139 to 141 and 141 to 143 respectively of the Encyclopedia of Polymer Science and Technology Volume 12 Interscience Publishers Division of John Wiley and Sons Inc. 1970. In particular the rosin esters used herein are those wherein the carboxyl group on the resin component of the rosin has been esterified with
alcohol having from two to four carbon atoms such as glycol glycerol pentaerythritol eatcp.olTyhfousnectdieofnianled on
page 143 of said encyclopedia are particularly useful herein
Rosin ester dispersion is obtained for example by dispersing a prepared solution of rosin ester in some suitable solvent in water containing a surfactant under high high speed agitation The solvent employed for the rosin ester solution can be selected amongst such solvents as toluene xylene ethyl acetate methyl ethyl ketone mineral spirits glycol ethers such as ethylene glycol mono ethyl ether acetate and chlorinated solvents such as trichloroethylene However butyl acetate is a preferred solvent Similarly the surfactant
used for obtaining a dispersion can be other than sodium oleate e.g. a ionic surfactant such as alkylaryl
polyether alcohols or anionic surfactants such as sodium alkylaryl polyether sulfonate
Examples of rosin and its esters that can be employed are glycerol esters of rosin pentaerythritol esters of rosin and the corresponding rosin or its esters obtained from dehydrogenated disproportionated polymerized and hydrogenated rosins Modified rosins such as modified rosin and rosin derivitives can also be employed
a The third necessary component herein is filler the purpose of which is to increase the tensile strength of the
adhesive and to reduce the cold flow or creep thereof Examples of fillers that can be used herein include
CaCO.sub.3 clay silicates ZnO etc. In general the fillers will be of a particle size that will range from
about 0.05 to about 75 microns preferably in the range of about 0.5 to about 10 microns
range
Optionally other materials normally added to adhesives of the type defined and claimed herein for a particular purpose can also be included in the final composition For example the composition can contain
from about 0.5 to about 20 weight percent of each of a thixotropic or thickening agent such as asbestos
treated clays fumed silicas etc a surfactant wetting agent or emulsifier such as Triton 405 Rohm and Haas Philadelphia Pa which is an octyl phenoxy polyethoxy ethanol a dispersant such as Tamol 850 Rohm and Haas Philadelphia Pa which is an aqueous solution of sodium polyacrylate etc.
The composition can be prepared in any suitable or convenient manner For example the individual
substantially . components are brought together in any suitable
1/2 to about 3 hours until each of the
or desired order and merely mixed for example for about
dispersed in the final adhesive
components of the mixture are
composition
uniformly spatially
The components of the adhesive
composition can be present in the following amounts
Containing Parts by weight Broad RangeRange Preferred Range
100 100 Rosin Ester Dispersion 40 Per Cent Solids 20-150 25-75 FPilolleyrm2e5r-4D0i0sp5e0r-s1io5n0 57 Per Cent Solids
DESCRIPTION OF PREFERRED EMBODIMENTS The process can further be illustrated by the following Preparation of Rosin Ester Dispersion
to 0.06 cm The assembly was then maintained at 73.degree 73.degree F. 23.degree C. and 50
humidity for selected periods of time The aged specimens were then tested for their percent relative
using an Instron Tensile Testor at
tensile lap shear strength
the
a jaw speed of 0.5 inch or 1.25 cm per minute The maximum strength of
lap joint at break was recorded and the average of five was reported
For the test demonstrating the effect lapsed time or open time after application of the adhesive on the rate
of the bond strength development samples were prepared as outlined above except that in certain instances
the second set of samples positioned on the surface carrying the adhesive was removed and left
various periods of time namely 10 20 and 30 minutes after which
exposed for
seven days at 73.degree F. 23.degree C. at 50 percent relative humitdhietyywaefrteerrwehaiscsehmtbhleeydwaenrdettheesnteadgiend tfhoer
manner described above
The results obtained are tabulated below in Table I.
TABLE I
Grams Composition Control Claimed Adhesive
Rhoplex 495 57 Per Cent 100 100 Zonester 85
Dispersion 40 Per Cent None 42 CaCO.sub.3 90 90 Clay 10 10 Asbestos Fiber 3 3 Bentone LT 2 Per Cent
Solution 47 47 Triton 405 2.2 2.2 Tamol 850 0.3 0.3 Composition T 2.5 2.5 Water 20.0 5.0
Tensile Shear Strength psig cm.sup.2
Minutes
30.3 10 14.55 20.3 20 165 11.6 20.2 30 7.87 19.0
0 228
In the above table Rhoplex 495 is an acrylic emulsion of about 57 percent solids having a viscosity of
about 2000 cps at 25.degree C. made by Rohm and Haas Philadelphia Pa Zonester 85 is a
of tall oil rosin made by Arizona Chemicals Company Wayne N.J Bentone LT is form
glycerol ester
made and sold by NL Industries Inc. Hightstown Hightstown N.J. and serves as a thixotropic aagent Torifttornea4te0d 5 claiys an
octyl phenoxy polyethoxy ethanol wetting agent and emulsifier made by Rohm and Haas Tamol 850 is a
foam dispersant aqueous solution of sodium polyacrylate made by Rohm and Haas and Composition T
Nis.Ja.n anionic sodium polymetaphosphate primary pigment dispersant made by Merck and Co. Rahway
The superiority of the adhesive defined and claimed herein is apparent from the data in Table I. Note that
when the control adhesive was employed in the tests and the substrates were bonded together with no
time the tensile shear strength was 228 pounds per square inch gauge below the minimum desired open
shear strength of 250 pounds per square inch gauge and was reduced to 112
tensile
after 30 minutes open time This is in contrast with the claimed
pounds per square inch gauge
composition wherein the initial tensile shear
strength was 431 pounds per square inch gauge and even after an open time of 30 minutes the tensile shear
strength had stabilized at 271 pounds per square inch gauge well within the minimum desired tensile shear
strength of 250 pounds per square inch gauge
Obviously many modifications and variations of the invention as hereinabove set forth can be made without departing from the spirit and scope thereof and therefore only such limitations should be imposed as are
indicated in the appended claims
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