U.S. patent application number 12/521006 was filed with the patent office on 2010-02-11 for article comprising an adhesion promoter coating.
Invention is credited to Mark T. Anderson, Bai Feng, Rachael A. T. Gould.
Application Number | 20100035044 12/521006 |
Document ID | / |
Family ID | 39588964 |
Filed Date | 2010-02-11 |
United States Patent
Application |
20100035044 |
Kind Code |
A1 |
Feng; Bai ; et al. |
February 11, 2010 |
ARTICLE COMPRISING AN ADHESION PROMOTER COATING
Abstract
It is desired to find a new class of adhesion promoters to
adhere the granules to the asphalt. Generally, the application is
directed to an article comprising a substrate and a coating on the
substrate, wherein the coating comprises a polyolefin. The
substrate may be a roofing granule. In certain embodiments, the
polyolefin is a chemically modified polyolefin. In some
embodiments, the coating comprises a photocatalytic material.
Inventors: |
Feng; Bai; (Woodbury,
MN) ; Gould; Rachael A. T.; (Forest Lake, MN)
; Anderson; Mark T.; (Woodbury, MN) |
Correspondence
Address: |
3M INNOVATIVE PROPERTIES COMPANY
PO BOX 33427
ST. PAUL
MN
55133-3427
US
|
Family ID: |
39588964 |
Appl. No.: |
12/521006 |
Filed: |
December 17, 2007 |
PCT Filed: |
December 17, 2007 |
PCT NO: |
PCT/US07/87753 |
371 Date: |
October 13, 2009 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
|
|
60878023 |
Dec 29, 2006 |
|
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|
Current U.S.
Class: |
428/323 ;
428/407; 428/413; 428/423.1; 428/480; 428/523 |
Current CPC
Class: |
Y10T 428/31786 20150401;
C08L 2666/04 20130101; C04B 41/52 20130101; C09J 151/06 20130101;
C08F 255/00 20130101; C08L 51/06 20130101; Y10T 428/2998 20150115;
E04D 1/26 20130101; E04D 2001/005 20130101; Y10T 428/31938
20150401; Y10T 428/31551 20150401; Y10T 428/25 20150115; C08L
2666/02 20130101; C09D 151/06 20130101; C08F 255/02 20130101; Y10T
428/31511 20150401; C08L 51/06 20130101; C08L 2666/04 20130101;
C08L 51/06 20130101; C08L 2666/02 20130101; C09D 151/06 20130101;
C08L 2666/04 20130101; C09D 151/06 20130101; C08L 2666/02 20130101;
C09J 151/06 20130101; C08L 2666/04 20130101; C09J 151/06 20130101;
C08L 2666/02 20130101 |
Class at
Publication: |
428/323 ;
428/523; 428/407; 428/413; 428/423.1; 428/480 |
International
Class: |
B32B 5/16 20060101
B32B005/16; B32B 27/32 20060101 B32B027/32; B32B 27/38 20060101
B32B027/38; B32B 27/40 20060101 B32B027/40; B32B 27/06 20060101
B32B027/06 |
Claims
1. An article comprising a substrate; and an adhesion promoter
coating on the substrate, wherein the coating comprises a
polyolefin.
2. The article of claim 1 wherein the substrate is a roofing
granule.
3. The article of claim 1 wherein the polyolefin is a chemically
modified polyolefin.
4. The article of claim 3 wherein the polyolefin is modified with a
chemically reactive group comprising amines, epoxides, anhydrides,
hydroxyls, thiols, isocyanates, acids, halides, or esters.
5. The article of claim 1 wherein the coating comprises a mixture
of polyolefins.
6. The article of claim 5 wherein the mixture of polyolefins
comprise at least one chemically modified polyolefin.
7. The article of claim 6 wherein the chemically reactive group
comprising amines, epoxides, anhydrides, hydroxyls, thiols,
isocyanates, acids, halides, or esters.
8. The article of claim 4 wherein the chemically modified
polyolefin is modified with maleic anhydride.
9. The article of claim 1 wherein the polyolefin is
polypropylene.
10. The article of claim 2 wherein the roofing granule comprises a
photocatalytic material.
11. The article of claim 10 wherein the photocatalytic material
comprises TiO.sub.2, ZnO, WO.sub.3, SnO.sub.2, CaTiO.sub.3,
Fe.sub.2O.sub.3, MoO.sub.3, Nb.sub.2O.sub.5,
Ti.sub.xZr(.sub.1-x)O.sub.2, SiC, SrTiO.sub.3, CdS, GaP, InP, GaAs,
BaTiO.sub.3, KNbO.sub.3, Ta.sub.2O.sub.5, Bi.sub.2O.sub.3, NiO,
Cu.sub.2O, SiO.sub.2, MoS.sub.2, InPb, RuO.sub.2, CeO.sub.2,
Ti(OH).sub.4, or combinations thereof.
12. The article of claim 11 wherein the photocatalytic material
comprises crystalline anatase TiO.sub.2, crystalline rutile
TiO.sub.2, crystalline ZnO or combinations thereof.
13. The article of claim 10 wherein the photocatalytic material is
doped with a dopant.
14. The article of claim 13 wherein the dopant is C, N, S, F, Pt,
Pd, Au, Ag, Os, Rh, RuO.sub.2, Nb, Cu, Sn, Ni, Fe, or combinations
thereof.
15. The article of claim 1 wherein the article has a reflectivity
of at least about 20% at substantially all points in the wavelength
range between 770 and 2500 nm.
16. An article comprising a first coated substrate, comprising
first substrate and an adhesion promoter coating comprising a
polyolefin on the first substrate; a second substrate, wherein the
first coated substrate and the second substrate are attached and
the coating on the first substrate is between the first substrate
and the second substrate.
17. The article of claim 16 wherein the first coated substrate is a
roofing granule.
18. The article of claim 16 wherein the second substrate comprises
an asphalt layer.
19. The article of claim 16 wherein the polyolefin is a chemically
modified polyolefin.
20. The article of claim 19 wherein the polyolefin is modified with
a chemically reactive group comprising amines, epoxides,
anhydrides, hydroxyls, thiols, isocyanates, acids, halides, or
esters.
21. The article of claim 16 wherein the coating comprises a mixture
of polyolefins.
22. The article of claim 21 wherein the mixture of polyolefins
comprise at least one chemically modified polyolefin.
23. The article of claim 22 wherein the chemically reactive group
comprising amines, epoxides, anhydrides, hydroxyls, thiols,
isocyanates, acids, halides, or esters.
24. The article of claim 19 wherein the chemically modified
polyolefin as modified with maleic anhydride.
25. The article of claim 16 wherein the polyolefin is
polypropylene.
26. The article of claim 17 wherein the roofing granule comprises a
photocatalytic material.
27. The article of claim 26 wherein the photocatalytic material
comprises TiO.sub.2, ZnO, WO.sub.3, SnO.sub.2, CaTiO.sub.3,
Fe.sub.2O.sub.3, MoO.sub.3, Nb.sub.2O.sub.5,
Ti.sub.xZr(.sub.1-x)O.sub.2, SiC, SrTiO.sub.3, CdS, GaP, InP, GaAs,
BaTiO.sub.3, KNbO.sub.3, Ta.sub.2O.sub.5, Bi.sub.2O.sub.3, NiO,
Cu.sub.2O, SiO.sub.2, MoS.sub.2, InPb, RuO.sub.2, CeO.sub.2,
Ti(OH).sub.4, or combinations thereof.
28. The article of claim 27 wherein the photocatalytic material
comprises crystalline anatase TiO.sub.2, crystalline rutile
TiO.sub.2, crystalline ZnO or combinations thereof.
29. The article of claim 26 wherein the photocatalytic material is
doped with a dopant.
30. The article of claim 29 wherein the dopant is C, N, S, F, Pt,
Pd, Au, Ag, Os, Rh, RuO.sub.2, Nb, Cu, Sn, Ni, Fe, or combinations
thereof.
31. The article of claim 16 wherein the article has a reflectivity
of at least about 20% at substantially all points in the wavelength
range between 770 and 2500 nm.
Description
CROSS REFERENCE TO RELATED APPLICATION
[0001] This application claims the benefit of U.S. Provisional
Patent Application No. 60/878023, filed Dec. 29, 2006, the
disclosure of which is incorporated by reference herein in its
entirety.
FIELD
[0002] The present application is directed to coatings, especially
coatings used as adhesion promoters.
BACKGROUND
[0003] Asphalt-based roofing systems and products are well known.
They include, for example, asphalt shingles and asphalt roll
roofing. Many conventional materials are utilized as raw materials
in the manufacture of asphalt roofing systems and products.
[0004] Asphalt roofing systems and products generally comprise a
fiberglass or organic matting, which is filled and/or coated with
various asphalt materials. Generally, the matting is filled with a
"saturant" asphalt. A saturant asphalt is oil-rich and relatively
non-viscous, to provide maximum waterproofing and saturation of the
matting. The saturant asphalt serves as a preservative, a
waterproofing agent and an adhesive agent.
[0005] The saturated substrate is sealed by application of a
harder, more viscous "coating" asphalt to one or both sides of the
substrate. Coating asphalts generally contain finely divided
minerals therein as stabilizers or fillers. Such compounds as
igneous rock mineral fines, silica, slate dust, talc, micaceous
materials, limestone and dolomite have been utilized as fillers to
render the coating asphalt more shatter-proof and shock-proof in
cold weather.
[0006] The exterior, outer, or exposed surface of asphalt roofing
systems and products is generally provided with a covering of
granular material or roofing granules embedded in the coating
asphalt. The granular material generally protects the underlying
asphalt coating from damage due to exposure to light, in particular
ultraviolet (UV) light. That is, the granules reflect light and
protect the asphalt from deterioration by photodegradation. In
addition, such granular material improves fire resistance and
weathering characteristics. Further, colors or mixtures of colors
of granular material may be selected for aesthetics.
[0007] In general, the mineral materials, particles or granules are
embedded into the coating asphalt under pressure and are retained
therein by adherence to the asphalt. With respect to each granule,
the asphalt may be viewed as a "hot sticky mud" into which the
granules are pressed. When the asphalt cools, pockets having the
granules retained therein are formed.
[0008] Good adherence of the roofing granules to the roofing
product is beneficial. Loss of granules reduces the life of the
roof, since it is associated with acceleration of photodegradation
of the asphalt. In addition, the aesthetics of the roofing system
may be compromised if granules are lost. Further, reduction of
granule loss during installation improves safety conditions on the
roof.
[0009] The granule may be coated with a variety of materials, to
render unique and desirable properties. For example, granules are
generally treated with an adhesion promoter. Typically, the
adhesion promoter has been silicone.
SUMMARY
[0010] It is desired to find a new class of adhesion promoters to
adhere the granules to the asphalt. Generally, the application is
directed to an article comprising a substrate and a coating on the
substrate, wherein the coating comprises a polyolefin. The
substrate may be a roofing granule. In certain embodiments, the
polyolefin is a chemically modified polyolefin. In some
embodiments, the roofing granule comprises a photocatalytic
material.
[0011] The application is also directed to an article comprising a
first coated substrate, comprising a first substrate and a coating
comprising a polyolefin, and a second substrate, wherein the first
coated substrate and the second substrate are attached and the
coating on the first substrate is between the first substrate and
the second substrate.
DETAILED DESCRIPTION
[0012] The present application is directed generally to adhesion
promoter coatings for bonding a first substrate and a second
substrate together. The adhesion promoter coating is generally
between the two substrates. This adhesion promoter coating is
especially useful in the manufacture of roofing materials, such as
roofing shingles and roll roofing. For example, asphalt roofing
materials may comprise at least a matting, asphalt, and granules.
The granules comprise a first substrate, and the asphalt and
matting comprise a second substrate.
[0013] A variety of materials may be utilized as the matting for
the roofing materials. In general, the matting may comprise a
non-woven matting of either fiberglass or cellulose fibers.
Fiberglass matting may be used in the asphalt roofing products
industry and is a typical matting for use with methods and in
products according to the present application. Cellulose matting,
sometimes referred to as organic matting or rag felt may also be
utilized.
[0014] Fiberglass matting is commercially available from
Owens-Corning Fiberglass Corporation, Toledo, Ohio and Manville
Roofing Systems, Denver, Colo. These, and other
commercially-available mattings, are utilized in embodiments of the
present invention. It is recognized that any fiberglass mat with
similar physical properties could be incorporated into the present
application with satisfactory results. Generally, the fiberglass
matting is manufactured from a silicate glass fiber blown in a
non-woven pattern in streams of about 30-200 micrometers in
diameter with the resultant mat approximately 1-5 millimeters in
thickness.
[0015] Cellulose felt (dry felt) is typically made from various
combinations of rag, wood and other cellulose fibers or
cellulose-containing fibers blended in appropriate proportions to
provide the desirable strength, absorption capacity and
flexibility.
[0016] Roofing asphalt, sometimes termed "asphalt flux", is a
petroleum based fluid comprising a mixture of bituminous materials.
In the manufacture of roofing materials, it is generally desirable
to soak the absorbent felt or fiberglass matting until it is
impregnated or saturated to the greatest possible extent with a
"saturant" asphalt, thus the asphalt should be appropriate for this
purpose. Saturant asphalt is high in oily constituents which
provide waterproofing and other preservatives. Matting saturated
with saturant asphalt are generally sealed on both sides by
application of a hard or more viscous "coating asphalt" which
itself is protected by the covering of mineral granules. In the
case of fiberglass mat based asphalt roofing products, it is well
understood that the coating asphalt can be applied directly to the
unsaturated fiberglass mat.
[0017] The asphalts used for saturant asphalt and the coating
asphalt are generally prepared by processing the asphalt flux in
such a way as to modify the temperature at which it will soften. In
general, the softening point of saturant asphalt may vary from
about 37.degree. C. to about 72.degree. C., whereas the softening
point of desirable coating asphalt may run as high as about
127.degree. C. The softening temperature varies among the roofing
industry and may be modified for application to roof systems in
varying climates.
[0018] In general, conventional, commercially available, asphalt
systems may be utilized in applications of the present
invention.
[0019] Roofing granules are generally applied to the surface of the
asphalt on, for example, a roofing shingle. In general, they
comprise colored slate or rock granules either in natural form or
artificially colored by a ceramic coating.
[0020] In general, any mineral material which is opaque, dense, and
properly graded by screening for maximum coverage can be used
conventionally and in roofing products of the present invention.
Generally, these materials are crushed and graded to a desired
size. Any size granule or distribution of sizes may be useful in
the roofing material industry may be used in the present
application. Methods to color such granules are generally known in
the art. See, for example, Beyard et al. in U.S. Pat. No. 3,752,696
which is incorporated herein by reference.
[0021] Suitable base granules can be selected from a wide class of
relatively porous or non-porous and weather-resistant rock or
mineral materials. Suitable minerals may include igneous rock, trap
rocks, slates, argillite, greystone, greenstone, quartz, quartzite,
certain granites or certain synthetic granules made from clay or
other ceramics.
[0022] The granule may be coated with a variety of materials, to
render unique and desirable properties. These coatings may be
continuous or discontinuous. For example, it is desirable to have a
coating which reduces dust and assists in the water repellency of
the granule. Multiple coatings may be applied either sequentially
or simultaneously.
[0023] In the present application the granules arc generally coated
with an adhesion promoter. In specific embodiments, the adhesion
promoter comprises a polyolefin. For the purpose of the present
application, a polyolefin is a polymer with an olefin backbone.
Polymers include oligomers of low molecular weight. The polyolefins
of the present application include a wide range of number average
molecular weights, including, for example, as low as 300 to as high
as 1,000,000. Olefins include ethylene, propylene, butene, and the
like. These olefins can be aliphatic, aromatic, cyclic or other
olefins. The polyolefin may be a homopolymer or a copolymer of
olefins. In addition to one or more olefins, the polyolefin can
optionally comprise one or more other monomer units, such as
styrenes, acrylics, urethanes, and others known in the art. Such
copolymers include random and block copolymers.
[0024] In certain embodiments, the polyolefin is chemically
modified. For the purpose of the present application, a chemically
modified polyolefin comprises a polyolefin which has been
functionalized with a chemically reactive group. The chemically
reactive group may be, for example, amines, epoxides, anhydrides,
hydroxyls, thiols, isocyanates, acids (e.g. carboxylic and
sulfonic), halides, esters, and the like.
[0025] In some embodiments, the chemically reactive group is a
maleic anhydride. In specific embodiments, the chemically modified
polyolefin is a maleic anhydride modified polypropylene. Examples
of such chemically modified polyolefins include those sold under
the tradename EPOLENE polymers, available from Eastman Chemical,
Inc.; FUSABOND materials, available from E.I. Du Pont de Nemours
Company; and OREVAC resins, available from Akema, Inc.
[0026] In some embodiments, the granules may be made
photocatalytic. Photocatalysts are further described in U.S. Pat.
Nos. 6,569,520; 6,881,701 and US patent application US2005/0142329
(10/746,829), assigned to 3M Innovative Properties Company and
incorporated by reference herein.
[0027] Upon activation or exposure to sunlight, photocatalysts are
thought to establish both oxidation and reduction sites. These
sites are thought to produce highly reactive species such as
hydroxyl radicals that are capable of preventing or inhibiting the
growth of algae or other biota on the coated article, especially in
the presence of water. Many photocatalysts conventionally
recognized by those skilled in the art are suitable for use with
the present invention. Specific examples of photocatalysts include
transition metal photocatalysts. Examples of suitable transition
metal photocatalysts include TiO.sub.2, ZnO, WO.sub.3, SnO.sub.2,
CaTiO.sub.3, Fe.sub.2O.sub.3, MoO.sub.3, Nb.sub.2O.sub.5,
Ti.sub.xZr(.sub.1-X)O.sub.2, SiC, SrTiO.sub.3, CdS, GaP, InP, GaAs,
BaTiO.sub.3, KNbO.sub.3, Ta.sub.2O.sub.5, Bi.sub.2O.sub.3, NiO,
CU.sub.2O, SiO.sub.2, MoS.sub.2, InPb, RuO.sub.2, CeO.sub.2,
Ti(OH).sub.4, and combinations thereof. Particularly preferred
photocatalysts include crystalline anatase TiO.sub.2, crystalline
rutile TiO.sub.2, crystalline ZnO and combinations thereof.
[0028] To improve spectral efficiency, photocatalysts may be doped
with a nonmetallic element, such as C, N, S, F, or with a metal or
metal oxide, such as Pt, Pd, Au, Ag, Os, Rh, RuO.sub.2, Nb, Cu, Sn,
Ni, Fe, or combinations thereof.
[0029] In some embodiments, the granules may be made
anti-microbial. Examples of such functionalized roofing granules
can be found, for example in WO 02/10244, incorporated herein by
reference. In some embodiments, the granule is made anti-microbial
with the addition of Cuprous Oxide. See, e.g., U.S. Pat. No.
3,528,842, incorporated by reference herein.
[0030] In some embodiments, the roofing granules exhibit reflection
of infared light. Examples of such functionalized roofing granules
can be found, for example, at United States Patent Application
Publication Number 2005/0142329, incorporated herein by reference.
Generally, such granules provide a non-white construction surface
having a reflectivity of at least about 20% at substantially all
points in the wavelength range between 770 and 2500 nm.
[0031] A variety of additives, such as stabilizers and fillers, may
be utilized in asphalt-based roofing systems. For example,
additives may be added to the adhesion promoting coating on the
granule, for example stabilizers, antioxidants, surfactants, and
the like. In addition, igneous rock mineral fines, silica, slate
dust, talc, micaceous materials, dolomite, limestone and trap rock
may be utilized as stabilizers or fillers in the coating asphalt.
These compounds are utilized in conventional systems and they may
be used in improved systems (for example rubber modified asphalt)
according to the present application in the same manner. Such
materials render the asphalt base improved with respect to shatter
resistance, shock resistance, and tensile strength. In addition,
they provide fire protection. Also, they provide raw material cost
savings and improved weathering characteristics. Additives may also
include reflective particles, for example additives that reflect
infrared light. Examples include those described in U.S. Patent
Application Number 2007/021825, assigned to 3M Innovative
Properties Company and incorporated by reference herein.
EXAMPLES
[0032] These examples are merely for illustrative purposes only and
are not meant to be limiting on the scope of the appended claims.
All parts, percentages, ratios, etc. in the examples and the rest
of the specification are by weight, unless noted otherwise.
Materials Used in the Examples
[0033] Kiln fired, untreated roofing granules WA7100-Grey,
available from 3M Company, Saint Paul, Minn. Maleic anhydride
modified polypropylene Epolene E43 (Mn=3900 g/mol, Mw=9100 g/mol,
Acid Number: 45), available from Eastman Chemical Company,
Kingsport, Tenn. L-500 oil, available from Cross Oil Refining &
Marketing, Inc., Smackover, Ark. Sodium Silicate PD (37.0 wt % with
2.75 wt % ratio of SiO.sub.2/Na.sub.2O), available from PQ Corp.,
Valley Forge, Pa. Tetraethyl ortho silicate, available from Aldrich
(TEOS, 98%) TiO2 aqueous dispersion W2730X, available from Degussa
AG as experimental material, Frankfurt, Germany.
Evaluation of Embedded Granule Adhesion to Asphalt Substrate
[0034] The dry rub test is a standard test method for the
determination of granular adhesion to mineral-surfaced roofing
under conditions of abrasion. The procedure is described in ASTM
standard D4977 "Test Method for Granule Adhesion to Mineral
Surfaced Roofing by Abrasion", incorporated herein by reference.
Dry rub tests conducted to evaluate granular adhesion in products
according to the present application, were conducted in compliance
with this standard.
[0035] In general, a brush with 22 holes, each containing bristles
made of 0.012 inch diameter tempered steel wire (40 wires per hole,
set with epoxy) was used to abrade the granular surface of a
specimen of mineral-surfaced roofing. The adhesion is assessed by
weighing the amounts of granules that are displaced and become
loose as a result of the abrasion test. The testing apparatus is a
machine designed to cycle a test brush back and forth
(horizontally) across a specimen at a rate of 50 cycles in a period
of about 60-70 seconds while the brush assembly rests on the
specimen with a downward mass of 5 pounds .+-.1/4 ounce with a
stroke length of 6.+-.1/4 inch. The testing machine used is
available commercially, as the 3M Granule Embedding Test Machine
and Abrasion Test Brushes, 3M Company, St. Paul, Minn.
[0036] A minimum of two 2-inch by 9-inch specimens were utilized
for each test, and any loose granules were removed from the
specimen with gentle tapping. Each specimen was then weighed and
the mass was recorded. The specimen was then clamped to the test
machine and the brush was placed in contact with the specimen (with
activation of the machine so that the specimen was abraded 50
complete cycles, the brush traveling parallel to the long axis of
the specimen). The specimen was then removed and weighed; the loss
in mass then being calculated.
[0037] In a typical test, nine scrub specimens were used for each
rub condition to be tested. For example, nine for testing the
specimen as received, and nine for a 7-day test in which the sample
was soaked for seven days in deionized water prior to conducting
the rub test.
[0038] The sample to be wet rub tested was placed in a soak tank
with deionized water at a temperature of 70.degree. F..+-.2.degree.
F. (21.degree. C..+-.2.degree. C.) for the specified period of
time. When the soak period has ended, a sample to be tested is
removed from the soak tank and gently blotted followed by weighing
and recording the initial weight. The rub test is then conducted as
outlined above, followed by recording the final weight. The initial
weighing and rub test followed by final weighing was conducted in a
timely manner to avoid water evaporation error.
Water Repellency Test
[0039] Water repellency test was performed by placing approximately
25.0 g of treated granules into a 20 ml test tube, which was then
inverted onto a flat surface, thereby forming a loose cone-shaped
granule aggregate pile. A 15 mm diameter indent was then created by
pressing the bottom of the test tube onto the tip of cone-shaped
granule aggregate pile. About 3 to 5 drops of Di water was placed
into the indent, and time was recorded until the water
disappeared.
Dust Measurement
[0040] Dust measurement of the treated granules was evaluated using
a MetOne Particle Counter (Model 237B, available from Pacific
Scientific Instruments, Wauconda, Ill.). The instrument was
operated according to the manufacturers instructions. To perform
the test, an ambient reading (dust reading of empty chamber) was
first recorded. Then 50.0 g of full grade granules were poured into
the funnel which was connected to the reading unit, and the
recorder was simultaneously turned on. The test stopped after 35
seconds and the Total Count Reading at 0.3 microns was recorded
(referred to as the dust reading). The actual sample dust reading
was obtained by subtracting the ambient reading from the machine
recorded dust reading. An average of three replicates was reported
as net sample dust reading in the units of particles/ft.sup.3.
Experimental
Preparation of Post-Treatment E43/Oil Solution
[0041] A 3.50% E43 oil solution was prepared by adding 100 g of
L-500 oil and 3.50 g of Epolene E43 polymer to a 4 oz glass jar
containing a magnetic stirring bar. The jar was then sealed and
stirred in a 120.degree. C. oil bath overnight, dissolving the E43
polymer to make the solution, and which can be applied when it is
either cool or hot. A 5.00% E43 oil solution was prepared
similarly, using 5.0 g of Epolene E43 in 100 g of L-500 oil.
Preparation of Treated Roofing Granules
[0042] Working example A: 1000 g of untreated, kiln fired WA7100
granules were heated in an oven at 360.degree. F. (182.degree. C.)
for 1 hour and then poured into a gallon size stainless steel
beaker affixed to a paint shaker. 2.587 g of the 3.5% E43 oil
solution was added dropwise during shaking (equivalent to a loading
of 0.17 lb E43/Ton of granules and 5.0 lb oil/on of granules). The
components were shaken for another 3 min after the completion of
the addition of E43/oil solution. The treated granules were then
placed in an oven at 176.degree. F. (80.degree. C.) for one hour,
removed and allowed to cool.
[0043] Working example B: This example was prepared the same as
working example A, but used 2.625 g of 5.0% E43 oil solution to
treat 1000 g of untreated, kiln fired WA7100 granules (equivalent
to a loading of 0.26 lb E43/Ton of granules and 5.0 lb oil/Ton of
granules)
[0044] Roofing shingles were manufactured from each of the Working
examples using the process similar to that outlined in U.S. Pat.
No. 4,352,837, and these shingles were then cut as described above
for testing. The results of this testing were tabulated in Table
1.
TABLE-US-00001 TABLE 1 Adhesion evaluation on asphalt roofing
strips 7 day water Water Net Dust Dry rub soak repellency Reading
testing loss Wet rub Samples Post-treatment (min) (particles/0.06
ft.sup.3) (g) testing loss (g) Comparative None 0 514023 0.39 2.38
Example 1 Working E43 oil 35 5612 0.61 2.16 Example A (0.17 lb/ton)
Working E43 oil 5 1808 0.13 1.01 Example B (0.26 lb/ton)
*Comparative Example 1 was prepared on a different day than Working
Examples A and B.
Preparation of TiO2 Coated Roofing Granules WA7100
[0045] A 250 mL blender cup was charged with: TiO2 aqueous
dispersion W2730X (1.67 g), deionized water (50.00 g), Sodium
Silicate PD (0.60 g), and a freshly prepared mixture of tetraethyl
ortho silicate (TEOS, 98% from Aldrich) in ethanol/water (10.00 g,
mixture molar ratio: TEOS:EtOH:H.sub.2O=1:40.7:53.6). The mixture
was well mixed by swirling, and then slowly poured onto 1000 g of
mechanically stirred, untreated, kiln fired WA 7100 granules, which
had been heated in an oven at 200.degree. F. (93.degree. C.) for
one hour prior to coating. After the completion of pouring, the
granules were stirred for about 2 minutes while manually scraping
the sides of the container with a metal spatula to ensure an even
coating. The granules were then heated with a heat gun for about 4
minutes (granules appeared to be dry and loose) and then fired at
575.degree. F. (302.degree. C.), removed from the oven, and allowed
to cool.
[0046] Working example C: this example was prepared exactly same
way as working example A, but used 2.587 g of 3.5% E43 of oil
solution to treat 1000 g of TiO2 coated WA7100 granules.
[0047] Working example D: this example was prepared exactly same
way as working example A, but used 2.625 g of 5.0% E43 of oil
solution to treat 1000 g of TiO2 coated WA7100 granules.
[0048] Roofing shingles were manufactured from each of the Working
examples using the process similar to that outlined in U.S. Pat.
No. 4,352,837, and these shingles were then cut as described above
for testing. The results of this testing were tabulated in Table
2.
TABLE-US-00002 TABLE 2 Adhesion evaluations on actual asphalt
roofing strips made from TiO2 coated WA7100 7 day water Water Net
Dust soak repellency Reading Dry rub testing wet rub testing
Samples Post-treatment (min) particles/0.06 ft.sup.3) loss (g) loss
(g) Comparative None 0 577856 0.60 6.15 Example 2 Working E43 oil
45 20666 0.16 1.58 Example C (0.17 lb/ton) Working E43 oil 120
11000 0.15 1.18 Example D (0.26 lb/ton) * Comparative Example 2 was
prepared on a different day than Working Examples A and B.
[0049] Various modifications and alterations of the present
invention will become apparent to those skilled in the art without
departing from the spirit and scope of the invention.
* * * * *