U.S. patent number 3,887,738 [Application Number 05/360,616] was granted by the patent office on 1975-06-03 for carpet backsized with hot melt adhesive and method.
This patent grant is currently assigned to Ashland Oil, Inc.. Invention is credited to Terry H. Shepler, David D. Taft.
United States Patent |
3,887,738 |
Taft , et al. |
* June 3, 1975 |
Carpet backsized with hot melt adhesive and method
Abstract
Hot melt compositions containing copolymer of ethylene and vinyl
acetate and/or alkyl acrylate wherein the alkyl group contains 1-18
carbon atoms; ester of rosin and polyhydric alcohol; and ester of
polyhydric alcohol and dimer and/or trimer of fatty acid are
particularly useful as carpet backing adhesives.
Inventors: |
Taft; David D. (Minneapolis,
MN), Shepler; Terry H. (St. Paul, MN) |
Assignee: |
Ashland Oil, Inc. (Ashland,
KY)
|
[*] Notice: |
The portion of the term of this patent
subsequent to September 11, 1990 has been disclaimed. |
Family
ID: |
27382577 |
Appl.
No.: |
05/360,616 |
Filed: |
May 15, 1973 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
Issue Date |
|
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149843 |
Jun 3, 1971 |
3758431 |
|
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|
121150 |
Mar 4, 1971 |
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Current U.S.
Class: |
428/95;
427/398.3; 428/516; 524/318; 524/562; 524/563; 524/914; 525/166;
525/222; 525/227; 525/240 |
Current CPC
Class: |
C09J
131/04 (20130101); C09D 123/08 (20130101); C09D
123/08 (20130101); C08L 2666/34 (20130101); C09J
131/04 (20130101); C08L 2666/34 (20130101); C08L
2666/34 (20130101); Y10S 524/914 (20130101); Y10T
428/31913 (20150401); Y10T 428/23979 (20150401); C09J
2301/304 (20200801) |
Current International
Class: |
C09D
123/08 (20060101); C09J 131/04 (20060101); C09J
131/00 (20060101); C09D 123/00 (20060101); D03d
027/00 (); D04h 011/00 () |
Field of
Search: |
;161/67,62-66,234,247,245,231 ;156/72,334
;117/161UZ,161UH,76T,90,138.8A ;260/28.5AV,887 |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: McCamish; Marion E.
Parent Case Text
RELATED CASES
This application is a division of copending application Ser. No.
149,843, filed June 3, 1971, now U.S. Pat. No. 3,758,431, which is
a continuation-in-part of copending application Ser. No. 121,150,
filed Mar. 4, 1971, now abandoned.
Claims
What is claimed is:
1. A process for backsizing a tufted carpet having a primary
textile backing and non-woven tufts of synthetic fibers protruding
therefrom which comprises:
a. heating to about 160.degree. F. to about 375.degree. F. a hot
melt coating composition consisting essentially of:
1. copolymer of ethylene and unsaturated ester monomer selected
from the group consisting of vinyl acetate, alkyl arcylate wherein
the alkyl group contains 1 - 18 carbon atoms, and mixtures thereof,
containing from 40 - 85% by weight of ethylene and from 15 - 60% by
weight of said unstaturated ester monomer;
2. ester of rosin and polyhydric alcohol wherein the ester has an
acid value between about 5 and about 40, and melting point range
between 75.degree. and 140.degree. C.; and
3. ester of polyhydric alcohol and dimer and/or trimer or mixture
thereof, of ethylenically unsaturated monocarboxylic fatty acid
having 16 - 22 carbon atoms, wherein said ester has an acid value
of 6 to 40;
b. applying a uniform coating in an amount from about 6 to 40
ounces per square yard of said composition in a molten state to the
back side of said carpet at a coating station while moving said
carpet past said coating station at a speed of from about 15to 80
feet per minute; and
c. thereafter solidifying said coating by cooling it below its
melting point.
2. A tufted carpet comprising:
a. a primary textile backing;
b. tufts of textile fibers protruding from said primary textile
backing and forming the surface of the carpet;
c. a secondary textile backing adjacent to the backside of said
primary textile backing; and
d. the hot melt coating composition of claim 1 being interposed
between said primary and secondary backings.
3. The carpet of claim 2 wherein at least one of the backings or
fibers is a polyolefin.
4. The carpet of claim 3 wherein said polyolefin is
polypropylene.
5. The carpet of claim 2 wherein said secondary backing is a
polyolefin.
6. The carpet of claim 5 wherein said polyolefin is polypropylene.
Description
BACKGROUND OF THE INVENTION
The present invention is concerned with hot melt compositions which
are especially useful as adhesives for the backsizing of tufted
carpets. More particularly the present invention is concerned with
hot melt compositions which are substantially free of wax.
Tufted carpets are composite structures in which the yarn forming
the pile, i.e., the surface of the carpet, is needled through a
base fabric whereby the base of each tuft extends through the base
fabric and is visible on the bottom surface. Tufted carpets are
generally of two types, the first being the type commonly known as
a "nap" carpet where the yarn loops are formed by needling or
punching a continuous yarn just through the base fabric, thus
forming the base of the carpet, while the tops of the loops are
generally 1/4 inch to 3/4 inches long, thus forming the wearing
surface of the carpet. The second tyep of tufted carpet, commonly
known as a "shag" carpet, has the same base as the nap carpet but
the tops of the loops have been split or the tips of the loops have
been cut off. The surface of the shag carpet is thus formed by the
open ends of the numerous U-shaped pieces of yarn - the base of the
U being embedded in the base fabric.
The loops of yarn are needled through and embedded in the base
fabric (the combination of which is the raw tufted carpet) thus
forming the tufted base, which must be secured to the base fabric
to prevent the loops from being pulled out of the base fabric. The
tufted bases are generally secured by applying an adhesive to the
back of the raw tufted carpet to bond the tufted yarns to the base
fabric. A secondary backing material is usually also applied to the
back of the raw tufted carpet and bonded thereto with the same
adhesive that bonds the yarn to the base fabric. The application of
the secondary backing material further secures the loops of yarn
since the loops of yarn are then bonded by the adhesive to the
backing material as well as the base fabric.
The yarn used in forming the pile of a tufted carpet can be made of
any type of fiber known in the art to be useful for tufted carpets,
e.g., nylon, acrylics, wool, cotton, rayon and the like.
The base fabric or primary backing may be of any type known in the
art and may be woven, for example, woven jute, woven slit
polypropylene film, burlap, and the like, or may be non-woven
fabric, e.g., needle punched, non-woven polypropylene web.
Likewise, the secondary backing material may be of any type known
in the art, e.g., woven jute, woven slit polypropylene film,
burlap, foam material such as polyurethane foams or blown vinyl
film and non-woven fabrics such as needle punched, non-woven
polypropylene web, and blends of polyesters and polypropylene.
In preparing such tufted carpets, the adhesives are usually applied
to the primary backing which holds the tufted matrix in the form of
a latex. A secondary backing is then usually applied to the carpet.
The carpet is then heated to cure the latex to ensure a bond
between the latex and the tufted carpet, and the latex and the
primary and secondary backings. This curing or drying of the latex
is quite time consuming, expensive, and often leads to rejects
because of insufficient curing during the process. In addition,
overheating of the carpet may occur during the curing which in turn
may affect the shade of the carpet.
In addition to the use of latex as an adhesive carpet backing,
recently there has been some activity in the use of hot melt
adhesives as carpetbackings or sizing adhesives. For example, such
hot melt adhesives have been based upon compositions containing
copolymers of ethylene and vinyl acetate admixed with a wax such as
paraffin wax or microcrystalline wax. For example, U.S. Pat.
3,390,035 discloses a hot melt adhesive consisting essentially of
from 90 to 10% by weight of an ethylene/vinyl acetate copolymer and
from 90 to 10% by weight of a wax. Such hot melt adhesives however
exhibit incompatibility and sometimes separation upon cooling of
the hot melt. In addition, such compositions have not demonstrated
the degree of flexibility and adhesive strength desired by the
carpet industry.
BRIEF DESCRIPTION OF INVENTION
The hot melt composition of the present invention consists
essentially of:
A. about 10 to 50% by weight of copolymer of ethylene and vinyl
acetate and/or alkyl acrylate wherein the alkyl group contains 1-18
carbon atoms, containing from 40 to 85% by weight of ethylene and
from 15 to 60% by weight of vinyl acetate or the C.sub.1 -C.sub.18
alkyl acrylate;
B. about 25 to 65% by weight of ester of rosin and polyhydric
alcohol having an acid value between about 5 and 40, and a melting
point between about 75 and 140.degree.C; and
C. about 10 to 50% by weight of ester of polyhydric alcohol and
dimer and/or trimer of fatty acid and having an acid value of 6 to
40.
The above quantities of copolymer and esters are based upon the
combined weight of the copolymer and ester present in the
composition and not necessarily upon the total composition which
may contain other ingredients.
DESCRIPTION OF PREFERRED EMBODIMENTS
The hot melt composition contains from about 10 to 50% by weight,
and preferably from about 15-35% by weight of copolymer of ethylene
and an unsaturated ester which is vinyl acetate or alkyl acrylate
wherein the alkyl group contains 1-18 carbon atoms. The most
preferred quantity of the copolymer of ethylene and unsaturated
ester is about 20-30% by weight.
The copolymers to be employed in the present invention contain from
40 to 85% by weight of ethylene and from 15 to 60% by weight of
vinyl acetate or C.sub.1 -C.sub.18 alkyl acrylate. Preferably the
copolymer contains about 65 to 82% by weight of ethylene and about
35 to 18% by weight of vinyl acetate or C.sub.1 -C.sub.18 alkyl
acrylate. Generally the copolymer has a melt index of 5-350. Some
examples of suitable alkyl acrylates include methyl acrylate, ethyl
acrylate, propyl acrylate, butyl acrylate, hexyl acrylate,
2-ethylhexyl acrylate, dodecyl acrylate, lauryl acrylate and
stearyl acrylate. Preferably the alkyl group of the acrylate
contains 1-8 carbon atoms.
The most preferred alkyl acrylates are ethyl acrylate and butyl
acrylate. Copolymers of ethylene and vinyl acetate and/or C.sub.1
-C.sub.18 alkyl acrylate are commercially available and their
methods of preparation are adequately described in the literature
including numerous U.S. patents. For example, the procedures
described in U.S. Pat. No. 2,200,429 are useful for preparing the
copolymers of ethylene used in the present invention. The ethylene
copolymers can also contain about 0.001 to 15% by weight of a
comonomer such as acrylic acid, methacrylic acid, itaconic acid,
acrylamide, beta dimethyl aminoethyl methacrylate, beta
hydroxyethyl acrylate, diallyl maleate, diallyl phthalate, diallyl
ether, ethylene glycol dimethacrylate, hydroxypropyl acrylate, or
hydroxypropyl methacrylate.
Some commercially available copolymers of ethylene suitable for the
purposes of the present invention are Ultrathene 636X, which is a
copolymer of 72% ethylene and 28% vinyl acetate with a melt index
of 24, Ultrathene 638 which is a copolymer of 69% ethylene and 31%
vinyl acetate with a melt index of 24; Ultrathene 639 which is a
copolymer of 70% ethylene and 30% vinyl acetate with a melt index
of 120; Ultrathene 664 which is a copolymer of 50% ethylene and 50%
vinyl acetate with a melt index of 50; Ultrathene 662 which is a
copolymer of 45% ethylene and 55% vinyl acetate with a melt index
of 100; Ultrathene 633 which is a copolymer of 81% ethylene and 19%
vinyl acetate with a melt index of 20; CoMer EVA 501 which is a
copolymer of 72% ethylene and 28% vinyl acetate with a melt index
of 350; CoMer EVA 505 which is a copolymer of 72% ethylene and 28%
vinyl acetate with a melt index of 20; CoMer EVA 605 which is a
copolymer of 67% ethylene and 33% vinyl acetate with a melt index
of 20; Elvax 150 which is a copolymer of 67% ethylene and 33% vinyl
acetate with a melt index of 25; Elvax 240 which is a copolymer of
72% ethylene and 28% vinyl acetate with a melt index of 22-28;
Elvax 250 which is a copolymer of 72% ethylene and 28% vinyl
acetate with a melt index of 12-18; Elvax 350 which is a copolymer
of 75% ethylene and 25% vinyl acetate with a melt index of 16-22,
Elvax 40 which is a copolymer of 60% ethylene and 40% vinyl acetate
with a melt index of 45 to 70; CoMer DPDA-9169 which is a copolymer
of 82% ethylene and 18% ethyl acrylate with a melt index of 20; and
the Zetafax resins which are copolymers of ethylene and butyl
acrylate. The Ultrathene polymers are available from USI, the CoMer
polymers from Union Carbide, the Elvax polymers from Dupont and the
Zetafax polymers from Dow Chemical.
The composition also contains from about 25 to 65% by weight and
preferably about 35-55% by weight and most preferably about 40-50%
by weight of ester of rosin and polyhydric alcohol. The ester has
an acid value between about 5 and 40 and most preferably between
about 10 and 20, and a melting point range between about 75.degree.
and 140.degree.C, and preferably between about 90.degree. and
115.degree.C.
The most preferred melting point is between about 90.degree. and
100.degree.C. The polyhydric alcohol used in forming this ester
generally contains from 2 to 6 alcohol groups and is a saturated
aliphatic compound.
Some suitable dihydric alcohols include among others the lower
glycols such as ethylene glycol, 1,2-propanediol, 1,3-propanediol,
diethylene glycol, triethylene glycol, tetraethylene glycol,
hexamethylene glycol, 1,3-butanediol, 1,4-butanediol, and
2,3-butanediol. Some suitable alcohols which contain from 3 to 6
alcohol groups include glycerol, trimethylol propane,
trimethylolethane, pentacrythritol, and hexitols, such as mannitol
and sorbitol
Of course, mixtures of alcohols may be employed in preparing this
ester. One such mixture is Sutro 250 which is available from Atlas
Chemical Industries, Inc., and is a mixture of essentially
straight-chain polyhydric alcohols of 3 to 6 carbon atoms. Sutro
250 and other Sutro polyhydric alcohols are described in Industrial
Polyol Bulletin LG-93 Rev. 4M-11/66, Sutro Polyols, Atlas Chemical
Industries, Inc., Chemicals Division, Wilmington, Del., 19899,
which is incorporated herein by reference.
The preferred polyhydric alcohol is pentaerythritol. The rosin
employed is generally a wood or tall oil rosin.
The ester may be prepared, for instance, by reacting 100 parts of
the rosin and about 6 to 15 parts by weight of the alcohol such as
pentaerythritol in the presence of a metallic catalyst at elevated
temperature of 200.degree.-250.degree.C until the desired acid
value is reached.
The hot melt composition also contains from about 10 to 50%,
preferably about 20-45%, and more preferably about 25-35% by weight
of ester of polyhydric alcohol and dimer and/or trimer of aliphatic
ethylenically unsaturated monocarboxylic fatty acid having 16-22
carbon atoms. Correspondingly, the dimer contains 32-44 carbon
atoms and the trimer contains 48-66 carbon atoms. The preferred
dimers and trimers are the dimers and trimers of oleic acid and/or
linoleic acid. The most preferred dimers and trimers are the dimers
and trimers of tall oil fatty acids.
Also the dimer and/or trimer may be employed as a mixture with such
other materials as monomeric aliphatic ethylenically unsaturated
monocarboxylic fatty acids having 16-22 carbon atoms, polymeric
forms of the monomeric aliphatic ethylenically unsaturated
monocarboxylic fatty acids higher than trimer, rosin acids, and
dimerized rosin. Preferably the dimer and/or trimer is employed as
a mixture with rosin acids and dimerized rosin. When employing a
mixture it should contain at least 20% by weight of the dimer
and/or trimer and/or higher polymers of the acids. Such mixtures
are commercially available. Of particular importance is Emtall 664
available from Emery Industries, Inc., Cincinnati, Ohio. This
mixture according to Emery contains about 25-30% by weight of dimer
and/or higher polymers of tall oil fatty acids and about 40-55% by
weight of rosin acids. The rosin acids include both monomeric and
polymeric forms of the acid. The remainder is fatty acids having an
average chain length of about 18 carbon atoms or higher, and
unsaponafiables. Another commercially available material is Fatty
Acid 7002 available from Arizona Chemical. This mixture contains
about 45% by weight of dimerized tall oil fatty acids, 25% by
weight of trimerized and higher polymers of tall oil fatty acids,
6% of C.sub.20 fatty acids, 13% of rosin acids, 2% of
unsaponafiables, and 7% of C.sub.18 fatty acids. In addition,
conventionally supplied pure dimer or trimer acids or mixtures
thereof may be employed in the preparation of this ester. The
polyhydric alcohol used in forming this ester generally contains
from 2 to 6 alcohol groups.
Some suitable dihydric alcohols include among others the lower
glycols such as ethylene glycol, 1,2-propanediol, 1,3-propanediol,
diethylene glycol, triethylene glycol, tetraethylene glycol,
hexamethylene glycol, 1,3-butanediol, 1,4-butanediol, and
2,3-butanediol. Some suitable alcohols which contain from 3 to 6
alcohol groups include glycerol, trimethylolpropane,
trimethylolethane, pentaerythritol, dipentaerythritol, and
hexitols, such as mannitol and sorbitol. Of course, mixtures of
alcohols of the above as well as Sutro 250 may be employed in
preparing this ester.
The preferred polyhydric alcohols contain from 3-6 alcohol groups.
The most preferred polyhydric alcohols are glycerine and
pentaerythritol. This ester should have an acid value between about
8 and 40, and preferably between 10 and 25 and a viscosity of
between about 1.0 to 40.0 stokes, preferably 2.0-20.0 stokes, as
measured in mineral spirits at a 70% non-volatile
concentration.
This ester can be prepared by reacting the dimer and/or trimer or
mixture containing the dimer and/or trimer with the polyhydric
alcohol under esterification conditions, e.g.,
200.degree.-250.degree.C, until the desired acid value is obtained.
For instance, the desired ester can be prepared by reacting about
100 parts by weight of the dimer and/or trimer and about 5 to 35
parts by weight of polyhydric alcohol, such as pentaerythritol, in
the presence of a calcium acetate catalyst. The reaction mixture is
heated to 400.degree.F and held at that temperature for 1 hour.
After this the temperature is raised to between about 480.degree.
and about 500.degree.F and is held there until the reaction is
complete as evidenced by a product having an acid value and
viscosity within the desired ranges. The mixture is usually held at
the 480.degree. to 500.degree.F temperature range for about 10-15
hours. If desired, the reaction time can be reduced by carrying the
reaction out under a partial vacuum of about 15 to 20 inches of Hg.
Similarly this dimer and/or trimer ester can be prepared together
with the ester of rosin and polyhydric alcohol by adding the dimer
and/or trimer, the rosin and polyhydric alcohol together and
esterifying.
The various quantities set forth above for the ethylene copolymer,
the rosin ester and the dimer and/or trimer ester are based upon
the combined weight of these components and not necessarily upon
the total composition which may include other ingredients.
The melting point of the ingredients in this invention is a
softening point which is determined by a modified mercury drop
method.
The hot melt composition of the present invention contains up to
about 70% by weight of a solid filler material based upon the total
composition. Preferably the composition contains between about 40
and 60% by weight of the solid filler material based upon the total
composition. Some suitable solid fillers are calcium carbonate,
clay, and talc. Calcium carbonate is the preferred filler. One
feature of the present invention is the ability to incorporate such
large quantities of solid filler material into the composition
without detracting from the coating properties of the composition
to such an extent as to render the composition unsuitable for its
intended purpose. Flame retardant fillers may also be employed to
improve the flame retardant properties of the carpet. Such fillers
are sold under the trade designation of Phosgard obtainable from
Monsanto and Firmaster obtainable from Michigan Chemical.
The composition of the present invention may also contain up to
about 2% by weight and preferably from about 0.1 to 1% by weight of
an antioxidant based upon the total composition. Some suitable
antioxidants include 2,2.sup.1 -methylene bis
(-4-methyl-6-tert.butylphenol), 2,4,6-tri-tert.butylphenol,
2,6-di-tert.butyl-4-methylphenol, 4,4.sup.1 -thio-bis
(-6-tert.butyl-m-cresol), butylated hydroxy anisole, and butylated
hydroxy toluene. The preferred antioxidant is 2,2.sup.1 -methylene
bis (-4-methyl-6-tert.butylphenol).
The hot melt compositions of the present invention provide
excellent adhesion between the pile loops and the primary backing
and between the secondary backing and the carpet. This excellent
adhesion can be observed from the force in pounds required to pull
one of the pile loops loose from the primary backing and from the
amount of force in pounds required to separate the secondary
backing from the carpet.
In addition the compositions exhibit surprisingly high flexibility,
elongation and tensile properties. Also the hot melts of the
present invention are surprisingly soft as compared to
ethylene/vinyl acetate copolymer compositions containing wax, thus
facilitating the coating procedure. Moreover the compositions of
the present invention are less likely to support combustion than
are various wax containing hot melt compositions. Therefore, they
are much safer to use.
Unlike the wax containing hot melt compositions, the present
compositions are quite compatible and are not opaque at elevated
temperatures. This high compatibility between the components of the
present invention greatly diminishes the problem of possible
separation of the components of the composition after they have
been applied to the substrate and are allowed to age. In addition,
the excellent properties of the present compositions are readily
reproducible from batch to batch. In the wax containing hot melt
compositions however it is quite difficult to reproduce a uniform
product in that small changes in the melting point of the wax
drastically vary the coating characteristics of the
composition.
Surprisingly, the compositions of the present invention demonstrate
their excellent adhesion properties when applied to polyolefin
substrates such as polyethylene and polypropylene. Polyolefin
fibers and/or secondary backings have not been commercially
employed to the extent desired because of the difficulty in finding
adhesive compositions suitable for adhering polyhydric substrates
to other substrates or to each other. The present compositions
however surprisingly are excellent adhesives for these polyolefin
substrates.
The hot melt compositions of the present invention can be prepared
by any of the conventional means by which two or more ingredients
are brought into intimate contact with each other. For example, the
ester of the polyhydric alcohol and rosin; the ester of the
polyhydric alcohol and the dimer and/or trimer; and the
antioxidant, if used, are added to a mixing vessel which is
blanketed in a nitrogen atmosphere. The mixture is then heated to
about 350.degree.F. The copolymer of ethylene and vinyl acetate
and/or C.sub.1 -C.sub.18 alkyl acrylate is then slowly added with
stirring to the heated mixture. The stirring is continued at this
temperature until a clear melt forms. The filler, if used, can then
be added to the mixture slowly with stirring until thoroughly
dispersed therein. The molten mixture can then be pumped directly
to a carpet coating apparatus or can be cooled for storage and used
at some later time.
The composition of the present invention can be applied to the
particular substrate by any of the well known methods of applying
coatings of molten adhesives. For example, the hot melt coating can
be applied by extrusion, a heated doctor blade, or by passing the
bottom surface of the tufted material in contact with the top
surface of a rotating roller partially submerged in a tank of the
molten adhesive. It is convenient to employ a doctor blade in order
to control the thickness of the adhesive on the roller.
The carpets prepared according to the present invention are useful
wherever carpets are used, for example, on floors and on stairways
in homes, restaurants, hotels, office buildings, and in passenger
sections of ships, trains, airplanes, and automobiles.
The composition is applied to the carpet in amounts ranging from
about 6 to about 40 ounces per square yard of carpet and preferably
from about 12-28 ounces per square yard and at a temperature of
about 160.degree.F and 375.degree.F. It is, of course, understood
that the temperature must be maintained so that melting or
decomposition of the textile backings and fibers do not occur, and
must be substantially above the melting point of the coating
composition. From about 15 to 80 feet of carpet per minute can be
coated with the composition of the present invention.
In order to better understand the present invention, the following
examples are given in which all quantities are by weight unless the
contrary is set forth:
EXAMPLE A
Preparation of Ester of Rosin and Pentaerythritol
910 parts of tall oil rosin, 90 parts of pentaerythritol, and 0.5
parts of oxalic acid are charged to a reactor and heated to
250.degree.C. The reactor is fitted for esterification. The
reaction is continued until an acid value of 35 is reached. Vacuum
is then applied until the acid value is less than 20. The material
is cooled to 200.degree.C and filtered into a cooling pan. The
ester has an acid value of 7.5, a viscosity of 1.2 stokes in
toluene at 70% non-volatiles, and a Gardner color of 12+.
EXAMPLE B
Preparation of Ester of Emtall 664 and Sutro 250
325 parts of Emtall 664 and 47 parts of Sutro 250 are charged to a
reactor fitted for esterification and heated to 400.degree.F. The
reaction is continued for 3 hours until an acid value of 12.4 is
reached. The material is cooled to room temperature for use in the
hot melt compositions.
EXAMPLE C
Preparation of Ester of Pentaerythritol and Mixture Containing
Dimerized Tall Oil Fatty Acids
936 parts of Emtall 664, 114 parts of pentaerythritol, and 0.17
parts of a calcium acetate catalyst are charged to a reactor which
is blanketed in a nitrogen atomsphere. The reaction mixture is then
heated to 200.degree.C and held at that temperature for 1 hour. The
temperature is then raised to between about 250.degree.C and about
271.degree.C and is held there for about 15 hours, at which time
the reaction is complete. The ester has an acid value of 12-18, a
viscosity of 2.5-4.0 stokes in mineral spirits at 70%
non-volatiles, and a Gardner color of 9-12.
EXAMPLE D
Preparation of Ester of Pentaerythritol, Ethylene Glycol, and
Mixture Containing Dimerized and Trimerized Tall Oil Fatty
Acids
1500 parts of Fatty Acids 7002, 90 parts of pentaerythritol, and 47
parts of ethylene glycol are charged to a reaction vessel fitted
for esterification. The reaction mixture is heated to 365.degree.F
where water begins to distill and then to 465.degree.-485.degree.F
over a period of 4-5 hours. The reaction mixture is cooled slowly
to room temperature. The ester has an acid value of 24 and a
viscosity of 19.0 stokes in mineral spirits at 70%
non-volatiles.
EXAMPLE E
Preparation of Ester of Glycerine and Mixture Containing Dimerized
and Trimerized Tall Oil Fatty Acids
1500 parts of Fatty Acids 7002 and 132.8 parts glycerine are
charged to a reaction vessel which is blanketed in a nitrogen
atmosphere. The reaction mixture is then heated to
440.degree.-460.degree.F and held at that temperature for 3-4
hours. The reaction product has an acid value of 17.2, a viscosity
of 9.0 stokes in mineral spirits at 70% non-volatiles, a color of
13+.
EXAMPLE 1
The raw tufted carpet is a shag carpet composed of a jute base
fabric weighing about 10 ounces/yard.sup.2 and tufted with about 14
ounces/yard.sup. 2 of bulked continuous filament nylon carpet yarn
which is needled into the base fabric at 6 needles per inch across
the width of the base fabric and about 6 stitches per running inch
of base fabric. The tuft loops extend 1/4inch above the base fabric
and the tufted bases extent 1/16 inch below the base fabric. The
secondary backing material is woven polypropylene weighing about
3.5 ounces/yard.sup.2.
The raw tufted carpet is passed under and adjacent to an extruder
where the bottom (non-pile) surface is coated with about 24
ounces/yard.sup.2 of a molten coating composition at a temperature
of 350.degree.F and having the following formula:
Parts ______________________________________ Copolymer of 67%
ethylene and 12.0 33% vinyl acetate, having an inherent viscosity
of 0.74 (0.25%) in toluene at 86.degree. F), a melt in- dex of 20
(ASTM-D-1238-577), and a softening point of 220.degree.F(ring and
ball) (CoMer 605) Ester from Example A 24.0 Ester from Example C
13.8 2,2'-methylene bis (-4-methyl-6- 0.2 tert.butylphenol)
CaCO.sub.3 (No. 1 White) 50.0
______________________________________
The molten composition which is kept at 350.degree. F is forced
through the extruder head onto the back of the raw tufted carpet as
it passes by the extruder head. The carpet then passes underneath a
heated doctor blade which evenly distributes any excess adhesive
that may be present. The carpet then passes between two rollers at
which point the secondary backing material from the upper roll is
applied to the back side of the carpet. The carpet is then passed
into a forced-air cooling section 10 feet in length to set the
coating composition. The primary backing of jute and the secondary
backing material are firmly bonded to each other, and the base of
each loop in the pile is firmly bonded to the primary backing. A
pull of 26 pounds is required to pull one of the pile loops loose
from the primary backing. The carpet has a T "peel" of about 25-27
pounds. In addition the carpet demonstrated excellent resistance to
delamination when subjected to repeated bending and
straightening.
In addition the percent elongation of a 40 mil film of the
composition is greater than 600 percent as measured on an Instron
Tensile Tester.
EXAMPLE 2
Example 1 is repeated except that the coating composition has the
following formula:
Parts ______________________________________ Copolymer of 72%
ethylene and 2.0 28% vinyl acetate, having an inherent viscosity of
.54 (0.25% in toluene at 36.degree. F), a melt in- dex of 350
(ASTM-D-1238-577) and a softening point of 180.degree.F(ring and
ball) (CoMer EVA 50l) Copolymer of 67% ethylene and 1.0 33% vinyl
acetate, having an inherent viscosity of .74 (0.25% in toluene at
86.degree. F), a melt in- dex of 20 (ASTM-D-1238-577) and a
softening point of 220.degree.F(ring and ball) (CoMer EVA 605)
Copolymer of 82% ethylene and 9.0 18% ethyl acrylate having an in-
herent viscosity of .81 (0.25% in toluene at 36.degree. F), a melt
in- dex of 51 (ASTM-D-1238-577) and a softening point of
307.degree.F(ring and ball) (CoMer DPD 9169) Ester from Example A
24.0 Ester from Example C 13.8 2,2'-methylene bis (-4-methyl-6- 0.2
tert. butylphenol) CaCO.sub.3 [No. 1 White] 50.5
______________________________________
The primary backing of jute and the secondary backing of
polypropylene are firmly bonded to each other, and the base of each
loop in the pile is firmly bonded to the primary backing. A pull of
32 pounds is required to pull one of the pile loops loose from the
primary backing. The carpet has a T "peel" of about 20-23 pounds.
In addition the carpet demonstrates excellent resistance to
delamination when subjected to repeated bending and
straightening.
In addition the percent elongation of a 40 mil film of the coating
composition is greater than 600 % as measured on an Instron Tensile
Tester.
EXAMPLE 3
Example 1 is repeated except that the coating composition has the
following formula:
Parts ______________________________________ Copolymer of 67%
ethylene and 12.0 33% vinyl acetate, having an in- herent viscosity
of .78 (0.25% in toluene at 86.degree. F), a melt in- dex of 250
(ASTM-D-1238-577), and a softening point of 240.degree.F(ring and
ball) (Elvax 150) Ester from Example A 22.0 Ester from Example C
13.4 2,2'-methylene bis (-4-methyl-6- 0.4 tert.butylphenol)
CaCO.sub.3 (No. 1 White) 52.2
______________________________________
The primary backing of jute and the secondary backing of
polypropylene are firmly bonded to each other, and the base of each
loop in the pile is firmly bonded to the primary backing. A pull of
20-25 pounds is required to pull one of the pile loops loose from
the primary backing. The carpet has a T "peel" of about 25 pounds.
In addition the carpet demonstrated excellent resistance to
delamination when subjected to repeated bending and
straightening.
EXAMPLE 4
Example 1 is repeated except that the coating composition has the
following formula:
Parts ______________________________________ Copolymer of 72%
ethylene and 24.9 28% vinyl acetate, having an inherent viscosity
of .86 (0.25% in toluene at 86.degree. F), a melt in- dex of 24
(ASTM-D-1238-577), and a softening point of 242.degree.F(ring and
ball) (Ultrathene 636) Ester from Example A 46.3 Ester from Example
C 28.1 2,2'-methylene is (-4-methyl-6- 0.7 tert.butylphenol)
CaCO.sub.3 (No. 1 White) 100.0
______________________________________
The primary and secondary backing of jute materials are firmly
bonded to each other, and the base of each loop in the pile is
firmly bonded to the primary backing. A pull of 20-25 pounds is
required to pull one of the pile loops loose from the primary
backing. The carpet as a T "peel" of about 20 pounds. In addition
the carpet demonstrated excellent resistance of delamination when
subjected to repeated bending and straightening.
EXAMPLE 5
Example 1 is repeated except that the coating composition has the
following formula:
Parts ______________________________________ Copolymer of 72%
ethylene and 25.0 28% vinyl acetate, having an inherent viscosity
of 0.86 (0.25% in toluene at 86.degree. F), a melt in- dex of 24
(ASTM-D-1238-577), and a softening point of 212.degree.F(ring and
ball) (Ultrathene 636X) Ester from Example A 56.0 Ester from
Example E 19.0 2,2'-methylene bis (-4-methyl-6- 0.75
tert.butylphenol) CaCO.sub.3 (No. 1 White) 100.0
______________________________________
The primary backing of jute and the secondary backing of
polypropylene are firmly bonded to each other, and the base of each
loop in the pile is firmly bonded to the primary backing. A pull of
25 pounds is required to pull one of the pile loops loose from the
primary backing. The carpet has a T "peel" of about 20 pounds. In
addition the carpet demonstrated excellent resistance to
delamination when subjected to repeated bending and
straightening.
In addition the percent elongation of a 40 mil film of the coating
composition is greater than 630 percent as measured on an Instron
Tensile Tester.
EXAMPLE 6
Example 1 is repeated except that the secondary backing material is
jute weighing about 10 ounces/yard.sup.2.
The primary and secondary backing materials are firmly bonded to
each other, and the base of each loop in the pile is firmly bonded
to the primary backing. The carpet has a T peel of more than 50
pounds. In addition the carpet demonstrated excellent resistance to
lamination when subjected to repeated bending and
straightening.
EXAMPLE 7
Example 2 is repeated except that the secondary backing material is
jute weighing about 10 ounces/yard.sup.2.
The primary and secondary backing materials are firmly bonded to
each other, and the base of each loop in the pile is firmly bonded
to the primary backing. The carpet has a T peel of about 50 pounds.
In addition the carpet demonstrated excellent resistance to
delamination when subjected to repeated bending and
straightening.
EXAMPLE 8
Example 1 is repeated except that the secondary backing material is
non-woven polyester/polypropylene weighing about 4.2
ounces/yard.sup.2.
The primary and secondary backing materials are firmly bonded to
each other, and the base of each loop in the pile is firmly bonded
to the primary backing. The carpet has a T peel of about 25-30
pounds. In addition the carpet demonstrated excellent resistance to
delamination when subjected to repeated bending and
straightening.
EXAMPLE 9
Example 2 is repeated except that the secondary backing is
non-woven polyester-polypropylene weighing about 4.2
ounces/yard.sup.2.
The primary and secondary backing materials are firmly bonded to
each other, and the base of each loop in the pile is firmly bonded
to the primary backing. The carpet has a T peel of about 18-20
pounds. In addition the carpet demonstrated excellent resistance to
delamination when subjected to repeated bending and
straightening.
EXAMPLE 10
Example 3 is repeated except that the secondary backing material is
jute weighing about 10 ounces/yard.sup.2.
The primary and secondary backing materials are firmly bonded to
each other, and the base of each loop in the pile is firmly bonded
to the primary backing. The carpet has a T peel of about 25-30
pounds. In addition the carpet demonstrated excellent resistance to
delamination when subjected to repeated bending and
straightening.
EXAMPLE 11
Example 3 is repeated except that the secondary backing material is
non-woven polyester/polypropylene weighing about 4.2
ounces/yard.sup.2.
The primary and secondary backing materials are firmly bonded to
each other, and the base of each loop in the pile is firmly bonded
to the primary backing. The carpet has a T peel of about 30 pounds.
In addition the carpet demonstrated excellent resistance to
delamination when subjected to repeated bending and
straightening.
EXAMPLE 12
Example 4 is repeated except that the secondary backing is
non-woven polyester/polypropylene weighing about 4.2
ounces/yard.sup.2.
The primary and secondary backing materials are firmly bonded to
each other, and the base of each loop in the pile is firmly bonded
to the primary backing. The carpet has a T peel of about 45 pounds.
In addition the carpet demonstrated excellent resistance to
delamination when subjected to repeated bending and
straightening.
EXAMPLE 13
Example 4 is repeated except that the secondary backing material is
jute weighing about 10 ounces/yard.sup.2.
The primary and secondary backing materials are firmly bonded to
each other, and the base of each loop in the pile is firmly bonded
to the primary backing. The carpet has a T peel of about 25-35
pounds. In addition the carpet demonstrated excellent resistance to
delamination when subjected to repeated bending and
straightening.
EXAMPLE 14
Example 5 is repeated except that the secondary backing material is
non-woven polyester/polypropylene weighing about 4.2
ounces/yard.sup.2.
The primary and secondary backing materials are firmly bonded to
each other, and the base of each loop in the pile is firmly bonded
to the primary backing. The carpet has a T peel of greater than 30
pounds. In addition the carpet demonstrated excellent resistance to
delamination when subjected to repeated bending and
straightening.
EXAMPLE 15
Example 5 is repeated except that the secondary backing material is
jute weighing about 10 ounces/yard.sup.2.
The primary and secondary backing materials are firmly bonded to
each other, and the base of each loop in the pile is firmly bonded
to the primary backing. The carpet has a T peel of more than 30
pounds. In addition the carpet demonstrated excellent resistance to
delamination when subjected to repeated bending and
straightening.
COMPARISON EXAMPLE 16
Example 1 is repeated except that the coating composition has the
following formula:
Parts ______________________________________ Copolymer of 67%
ethylene and 14.0 33% vinyl acetate having an inherent viscosity of
.78 (0.25% in toluene at 86.degree. F), a melt in- dex of 25
(ASTM-D-1238-577) and a softening point of 240.degree.F(ring and
ball) (ELVAX 150) Rosin WW (Available from Tenneco) 30.6 Polypale
(Available from Picco) 8.2 2,2'-methylene bis (-4-methyl-6- 0.2
tert.butylphenol CaCO.sub.3 (No. 1 White) 30.0 Wax --Paraflint RG
Fisher- 17.0 Tropsch wax having a melting point of 215.degree. F
______________________________________
A pull of 18 pounds is required to pull one of the pile loops loose
from the primary backing. The carpet has a T peel of about 1.5
pounds. The carpet demonstrated considerable delamination when
subjected to repeated bending and straightening. The percent
elongation of a 40 mil film of the coating composition is only
30.
COMPARISON EXAMPLE 17
Example 1 is repeated except that the coating composition has the
following formula:
Parts ______________________________________ Copolymer of 67%
ethylene and 14.0 33% vinyl acetate having an inherent viscosity of
.78 (0.25% in toluene at 86.degree. F), a melt in- dex of 25
(ASTM-D-1238-577) and a softening point of 240.degree.F(ring and
ball) (ELVAX 150) Rosin WW (Available from Tenneco) 38.3
2,2'-methylene bis (-4-methyl-6- 0.3 tert.butylphenol Barium
sulfate 30.0 Wax -- Paraflint RG Fisher- 17.4 Tropsch wax having a
melting point of 215.degree. F
______________________________________
A pull of 23 pounds is required to pull one of the pile loops loose
from the primary backing. The carpet has a T peel of about 3.5
pounds. The carpet demonstrated considerable delamination when
subjected to repeated bending and straightening. The percent
elongation of a 40 mil film of the coating composition is only
200.
COMPARISON EXAMPLE 18
Example 1 is repeated except that the coating composition has the
following formula:
Parts ______________________________________ Copolymer of 72%
ethylene and 17.5 28% vinyl acetate having an inherent viscosity of
.85 (0.25% in toluene at 86.degree. F), a melt in- dex of 15
(ASTM-D-1238-577) and a softening point of 280.degree.F(ring and
ball) (ELVAX 250) Rosin WW (Available from Tenneco) 40.8
2,2'-methylene bis (-4-methyl-6- 0.2 tert.butylphenol) CaCO.sub.3
No. 1 White) 30.0 Wax -- Paraflint RG Fisher- 11.5 Tropsch wax
having a melting point of 215.degree. F
______________________________________
A pull of 25 pounds is required to pull one of the pile loops loose
from the primary backing. The carpet has a T peel of about 3.5
pounds. The carpet demonstrated considerable delamination when
subjected to repeated bending and straightening. The percent
elongation of a 40 mil film of the coating composition is 365.
COMPARISON EXAMPLE 19
Example 1 is repeated except that the coating composition has the
following formula:
Parts ______________________________________ Copolymer of 67%
ethylene and 10.0 33% vinyl acetate having an inherent viscosity of
.78 (0.25% in toluene at 86.degree. F), a melt in- dex of 22-28
(ASTM-D-1238-577) and a softening point of 240.degree.F(ring and
ball) (ELVAX 150) Rosin WW (Available from Tenneco) 21.8 Polypale
(Available from Picco) 5.9 2,2'-methylene bis (-4-methyl-6- 0.2
tert.butylphenol) CaCO.sub.3 (No. 1 White) 50.0 Wax -- Paraflint RC
Fisher- 12.1 Tropsch wax having a melting point of 215.degree. F
______________________________________
A pull of 25 pounds is required to pull one of the pile loops loose
from the primary backing. The carpet has a T peel of about 2
pounds. The carpet demonstrated considerable delamination when
subjected to repeated bending and straightening. The percent
elongation of a 40 mil film of the coating composition is 40.
COMPARISON EXAMPLE 20
Example 16 is repeated except that the secondary backing is jute
weighing about 10 ounces/yard.sup.2.
The carpet has a T peel of about 30 pounds. The carpet demonstrated
considerable delamination when subjected to repeated bending and
straightening.
COMPARISON EXAMPLE 21
Example 17 is repeated except that the secondary backing is jute
weighing about 10 ounces/yard.sup.2.
The carpet has a T peel of about 8 pounds. In addition the carpet
demonstrated considerable delamination when subjected to repeated
bending and straightening.
COMPARISON EXAMPLE 22
Example 18 is repeated except that the secondary backing is jute
weighing about 10 ounces/yard.sup.2.
The carpet has a T peel of about 35 pounds. In addition the carpet
demonstrated considerable delamination when subjected to repeated
bending and straightening.
COMPARISON EXAMPLE 23
Example 19 is repeated except that the secondary backing is jute
weighing about 10 ounces/yard.sup.2.
The carpet has a T peel of about 23 pounds. In addition the carpet
demonstrated considerable delamination when subjected to repeated
bending and straightening.
COMPARISON EXAMPLE 24
Example 16 is repeated except that the secondary backing is
non-woven polyester/polypropylene weighing about 4.2
ounces/yard.sup.2.
The carpet has a T peel of about 6.5 pounds. In addition the carpet
demonstrated considerable delamination when subjected to repeated
bending and straightening.
COMPARISON EXAMPLE 25
Example 17 is repeated except that the secondary backing is
non-woven polyester-polypropylene weighing about 4.2
ounces/yard.sup.2.
The carpet has a T peel of about 7 pounds. In addition the carpet
demonstrates considerable delamination when subjected to repeated
bending and straightening.
COMPARISON EXAMPLE 26
Example 18 is repeated except that the secondary backing is
non-woven polyester-polypropylene weighing about 4.2
ounces/yard.sup.2.
The carpet has a T peel of about 10 pounds. In addition the carpet
demonstrated considerable delamination when subjected to repeated
bending and straightening.
COMPARISON EXAMPLE 27
Example 19 is repeated except that the secondary backing is
non-woven polyester-polypropylene weighing about 4.2
ounces/yard.sup.2.
The carpet has a T peel of about 4 pounds. In addition the carpet
demonstrated considerable delamination when subjected to repeated
bending and straightening.
The pull required to pull one of the pile loops loose from the
primary backing is determined by attaching a sample of the carpet
to a Chatillon tension tester. The pile is pulled at 12 inches/min.
until it pulls out and the value in pounds is recorded from the
tester. The above procedure is repeated five more times and the
average of the six tests is used as the value.
The T-Peel is determined by attaching a sample of the carpet having
about 4 inches of laminated surface in an Instron Tensile Tester
and pulling at 12 inches/min. the sample apart at an angle of
180.degree..
A comparison of Examples 1-15 with 16-27 clearly establishes that
the compositions of the present invention possess unexpectedly
excellent adhesive properties, particularly when applied to a
polyolefin containing substrate.
* * * * *