Note: Descriptions are shown in the official language in which they were submitted.
Sa~3~
TREATED GLASS FIBERS AND AQUEOUS DISPERSION AND NONWOVEN MAT OF THE GLASS
FIBERS
The preæent invention is directed to treated glass fibers
having good processibility into chopped glass fibers that are readily
dispersible in aqueous solution, and can be produced into glass
fiber-containing paper having good strength properties.
The production of glass fibers from molten glass involves
attenuating fibers from small orifices in a bushing in a glass melting
furnace. The glass fibers usually are attenuated by a mechanical means
and are usually gathered into one or more strands and are either
collected as continuous strands on a winder or are chopped and collected
as wet chopped glass fiber strands. During the attenuation and before
the numerous glass flbers are gathered into one or more strands, a
treating composition, which is known aæ a sizing composition, ls applied
to each of the glass fibers. The aqueous sizing composition is necessary
to provide protection to the glass fibers from interfilament abrasion,
especially when the flbers are gathered together as strands. Also the
sizing composition can be used to promote compatibility between the glass
fibers and any matrix in which the glass fibers are to be used for
reinforcement purposes. The collected continuous strands, or chopped
strands can be dried, or wet chopped strands can be packaged in their wet
condition. The dried continuous glass fiber strands can be chopped or
combined with other glass flber strands to form rovings, or produced into
continuous strand mats or woven. Such steps depend upon the ultimate use
for the glass fibers.
5434
Glass fibers have been used by themselves and in combination
with other types of fibers in the productlon of paper-like sheet
materlals. Glass fibers have been used as such a supplemental fiber in
specialty, synthetic, fiberboard, pulp and composite papers. Also, the
glass flbers are finding a use in glass fiber paper which is a substitute
for papers made of asbestos fiber. Also, in recent years, a nonwoven,
sheet-like mat of chopped glass fibers and/or strands has been utilized
increasingly as a replacement for organic felts such as cellulose mats in
roofing shingles and built-up roofing systems (8UR systems). This usage
and further expanded usage of the glass fiber mats in the roofing
industry is based on sever21 atvantages of the glass fiber mat. These
advantages lnclude: the reductlon ln the amount of asphalt necessary for
the roofing products, the reduction ln welght of the rooflng products,
increa~ed production rates for producing the roofing products, superior
rot resistance, longer product life, and improved fire ratings. These
types of papers and nonwoven, sheet-like mat are usually produced in a
process where chopped fibers, or chopped fiber strands are dispersed in
an aqueous solutlon and formed into a mat of chopped glass fibers and/or
strands. A nonwoven, sheet-like mat product is produced by contacting
the mat of glass fibers with a polymeric binder. An example of a process
to produce such a mat is the "wet-laid" process.
The wet-laid process involves formlng an aqueous tispersion of
chopped fibers or chopped strands usually with agitation in a mixing
tank. The aqueous disperslon, usually referred to as slush, ls processed
into the wet-laid, sheet-like mat by such machines as cylinder or
fourdrinier machines or re technologically advanced machinery, such as
the Stevens Former, Roto Former, Inver Former and the VertiFormer
~285434
machines. The slush is deposited from a head box onto a moving wire
screen or onto the surface of a moving wire-covered cylinder. The slurry
on the screen or cylinder is processed into the nonwoven, sheet-like mat
by the removal of water, usually by a suction and/or vacuum device, and
by the application of a polymeric binder. Water and excess binder are
removed by suction and/or vacuum devices. The binder impregnated
nonwoven, sheet-like glass fiber mat is dried and cured in one or more
ovens.
The strength of the nonwoven, sheet-like mat of glass fibers
must be sufficient to withstand the processing steps and speeds to
produce the nonwoven, sheet-like mat for application in various end
uses. In addition, the finish on the glass fibers and the strength of
the sheet-like mat must be sufficient to permit the mat to be stored in
any desirable form, possibly for an extended period of time without loss
of its cohesive properties. Also, the finish on the glass fibers in the
sheet-like mat should enable the stored mat to be processed into end use
applications without cracking or without the production of large amounts
of static being generated during use. The efficient processability of
the nonwoven, sheet-like mat into various end use applications depends on
the strength properties of the sheet-like mat and also the structure and
ho geneity or uniformity of the arrangement of the glass fibers in the
mat itself.
Also, the strength of the sheet-like mat is important for the
strength that the mat gives to any end use product incorporating the
mat. For example, when the sheet-like mat of chopped glass fibers andlor
strands is to be utillzed in producing roofing products, such as
shlngles, and the mat for BUR systems, the sheet-like mat must have
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suffic~ent strength propertles to enable the processing of the sheet-like
mat into these products. The roofing industry ls seeking hlgher
strengths for these products, and this is especially true for dry tensile
and tear strengths of the sheet-like mat.
The uniformity of the arrangement of chopped glass fibers
and/or strands in the nonwoven, sheet-like mat of chopped glass fibers
and/or strands contributes to the strength of the mat and to the ultimate
end product. One problem that exists in preparing a unifor~ mst of
chopped glass fibers and/or strands from an aqueous dispersion is that
glass fibers are not easily dispersed in aqueous media. This difficulty
ln dlspersing the glass fibers occurs initially upon adding the glass
fibers to water. The dispersibility is further complicated by the
tendency of the glass fibers that are scattered somewhat in the aqueous
medium, to reagglomerate to some degree. The reagglomerated glass fibers
are very difficult to redisperse. The lack of a good dispersion of the
glass fibers in the aqueous medium hampers the formation of a uniform
mat, and adversely affects the strengths of the resultant sheet-like mat
or end product incorporating the mst.
Recent glass flber products marketed by PPG Industries, Inc.,
for producing mats of chopped glass fibers from a slush or slurry have
had excellent dlsperslblllty and they have performed well in the previous
glass paper manufacturing processes. Our research has continued in this
fleld to develop even better glass fiber products. The glass
paper-making industry strives for processes with faster line speeds which
necessitate higher drying temperstures for lower weights of the chopped
glass fiber mats, snd for higher tensile strengths in the paper product.
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It is an ob~ect of the present invention to provide chemically
treated glass fibers that are adequately protected from interfilament
abrasion, where the fibers are in the form of choppable bundles of
fibers, and at the same time, provide chemically treated glass fibers
that have good dispersibility and that have good retention of the
chemical treating composition in the aqueous medium, and that are useful
in forming aqueous dispersions of chopped glass fibers and/or strands
that can be produced into non-woven, sheet-like mat having good strength
properties.
It is a further object of the present invention to have
nonwoven, sheet-like mats having one or more polymeric binders having
goot strength properties, such as good wet-strength properties,
dry-strength properties, andtor tear-strength properties to allow for
good processability of the mats themselves, and of the mats into
resulting products, such as base materials for roofing products like BUR
systems, shingles, and flooring.
SUMMARY OF THE INVENTION
Accordingly, the foregoing ob~ects and other objects gleaned
from the following disclosure are accomplished by the present invention.
The treated glass fibers of the present invention have been
treated with an aqueous treating composition applied to the glass fibers
in any manner and comprised of: one or more water soluble, dispersible,
and/or emulsifiable cationic lubricants; one or more water soluble,
~; polyoxyethylene polymers having an effective film forming lecular
weight; water soluble, emulsifiable or dispersible aldehyde-condensate-
:
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reactable, polymeric agent; one or more aldehyde-cond~ ~ te-reactable
coupling agents and a carrier. The lubricantJhas one or more primary,
secondary, and/or tertiary amines. The aldehyde-condensate-reactable
polymeric agent can be polymers such as polyacrylamlde and polyamide
polymers and mixtures thereof in effective white water compatible
amounts. The one or more aldehyde-condensate-reactable coupling agents
have an organic and an inorganic polar functional moiety, and they can be
coupling agents like alkoxylated amino organosilanes,
polyaminorganosilanes, mercapto-organo silanes and ureido organo
silanes. Both the polymeric agent and the coupling agent that are
reactable with the aldehyde-condensate are capable of reacting with each
other and the aldehyde-condensate in the presence of the aldehyde-
condensate. The carrier, e.g. water, is present in sufficient amounts to
enable the treating composition to contact and coat the glass fibers.
The treated glass fibers can have an amount of the treating
composition in the range of about O.Ol to about 1.5 or more weight
- percent on a loss on ignition (LOI) basis, where the treated fibers are
in the form of bundles and/or strands. The treated glass fibers can be
in any form such as continuous glass fiber strands or chopped glass fiber
strands, which are produced as wet chopped or dry chopped glass fiber
strands. When the chopped treated glass fiber strands are dispersed in
aqueous media, the addition to the aqueous media of a dispersion system
containing one or more dispersing agents is not needed. However, if
desired, these agents can be used since the treated glass fibers do not
interfere with the function of the dispersing agents.
A second aspect of the present invention is a method of
producing an aqueous dispersion of chopped treated glass fibers and/or
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strands. A third aspect is a nonwoven, sheet-llke, glass
fiber-containing mat produced from such a dispersion by the removal of
some water from the aqueous dispersion that is present on a wlre screen
or cylinder. The glass fiber-containing mat is contacted with the one or
more aldehyde-condensate polymeric binders to produce the nonwoven,
sheet-like mat having good strength properties such as wet and dry
tensile strength and tear strength to be useful as a base or supporting
layer in roofing products and flooring products and other products, where
a good strength mat is requlred along with a Class A fire rating and good
rot reslstance.
DETAILED DESCRIPTION OF THE INVENTION
The treating composition of the present invention provides good
protective propertles for the glass fibers, when they are gathered into
strands for continuous glass fiber strands, or when they are in the form
of chopped glass fibers and/or strands. Hereinafter, in the
speciflcation and claims. both fibers and strands will be referred to
collectively as fibers. The chopped treated glass flbers of the present
invention can be dispersed in aqueous media or white water systems to
result in good dispersibility even in the absence of a dispersing agent.
In making and using a nonwoven, sheet-like mat of the glass fibers, good
strength properties are required for the processability of the mat into
end use products such as shingles and other roofing products or flooring
products. Certain properties for these ultimate products are necessary.
These properties include one or more of the following: good tear
strength, good flexibility and good wet, dry and hot-wet tensile
strengths.
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It has been discovered that a majority, if not all, of these
properties can have good values with the use of the treated glass fibers,
aqueous dispersion and glass fiber-containing, nonwoven, shçet-like mat
of the present invention. The achievement of obtaining good properties
in these areas is effected by the synergistic influence of the chemical
components making up the treating composition on the glass fibers, the
interrelationship between the chemical treating composition and the
surface of the glass fibers, and the interrelationship between the
treatment on the glass fiber surface and the-polymeric binder used to
make the nonwoven sheet-like mat.
In the specification and in the claims, the below defined terms
have the following meanings. The effective film forming molecular weight
of the polyoxyethylene polymer is that molecular weight that enables the
polyoxyethylene by itself to form a solid or liquid, coalesced and
integrated film, that maintains the form as an integral and at least near
continuous film on curved surfaces such as fibers.
The "white water system" is an aqueous solution in which the
glass fibers are dispersed and which can contain numerous dispersants,
thickeners, softening or hardening chemicals. Examples of various white
water systems include aqueous solutions having polyacrylamide polymers
such as the Separan polymer available from Dow Chemical Company, alone or
with hydroxyethyl cellulose and the like suspending aids to provide a
highly viscous aqueous solution at high material concentrations. Also,
white water systems include those having any of the numerous amine oxide
surfactants as shown in U.S. Patent 4,179,331. An example of the
polyacrylamides are those shown in U.S. Patent 4,395,306. In addition to
such chemicals as polyacrylamides or amine oxides being present in the
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~85434
white water system, there can also be present small amounts of
surfactants such as polyethoxylated derivatives of amide condensation
products of fatty acids and polyethylene polyamines as is shown in U.S.
Patent 4,265,704. Also numerous other chemical agents can be added to a
white water system as is known by those skilled in the art.
The "effective white water compatible amount" is that amount
which results in an amount of an aldehyde-condensate-reactable polymeric
agent on the glass fibers, which when combined with the amount of an
aldehyde-contensate-reactable, polymeric agent in the white water system,
glves a total amount of one particular aldehyde-condensate-reactable
agent 80 that the amount toes not detrimentally affect the tensile
strength of the final glass flber paper product.
The polyoxyethylene polymer present on the glass fibers is a
water soluble, tispersible or emu'lsifiable polyoxyethylene polymer with
an effective film forming molecular weight of at lea6t lO0,000 Nv
measured by the viscosity of an aqueous solution by any method known in
the Ft. The upper limit of the molecular weight for the polyoxyethylene
polymer is a practlcal limltation regardlng the solubility,
dispersibllity or emulsifiability of the polyoxyethylene polymer in
aqueous solutions. Preferably, the lecular weight ranges from around
600,000 to 4,000,000 Mw ant most preferably around 900,000 Mw. The upper
limit of the molecular weight has a practical limitation due to the
increase in viscosity of the aqueous chemical treating composltlon
resultlng from the use of higher molecular weight polyoxyethylene
polymers. In treating glass fibers during thelr formation wlth the
aqueous chemical treating compositlon, the aqueous chemlcal treating
composition should not have a viscoslty of much greater than 40 to 50
g_
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centipoise at room temperature. When the chemical treating compositioo
is a gel rather than a solution, the treating composition can have a
higher viscosity and a higher molecular weight polyoxyethylene polymer
can be used. The glass transition temperature of the polyoxyethylene
polymer should be less than about -20C and preferably is around -50 to
-70C for molecular weights exceeding 100,000. When the molecular we$ght
of the polyoxyethylene polymer is less than around 100,000 Mv and it is
used ln an aqueous chemical treating composition, additional components
should be added to the aqueous chemical treating composition. These
components would produce a coalesced and integral film from the aqueous
chemical treating composition upon moisture reduction and would reduce
any plasticizing effect of the other components in the composition. Any
additional component known to those skilled in the art for accomplishing
these purposes can be used.
A suitable polyoxyethylene polymer which can be used is
available from Union Carbide under the trade designation POLYOX resins
designated as WSR-1105 having a molecular weight of 900,000 or WSR-205
having a molecular weight of 600,000 or the WSRN-3,000 having a molecular
weight of 400,000. The solution viscosity can be determined at 25C with
a No. 1 spindle at 50 rpm. The POLYOX material is a water soluble resin
which is nonionic and thermoplastic and it has a common structure of:
(-0-CH2CH2)-n where the degree of polymerization, , varies from
about 2,000 to about 100,000. With the repesting unit having a molecular
weight of 44, the polymer has a corresponding molecular weight in the
range of about 100,000 to about 5,000,000 Mn. These materials are solids
at room temperature, and they can have either a broad or narrow
distribution of molecular weights. Their appearance is a white powder
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with a particle size as percent by weight through a No. 20 USBS sieve of
98 minimum, and they have: a melting point (crystal x-ray) of 65C; a
volatiles content, as supplied by percent by weight of less than 1; an
alkaline earth metals percent by weight of calcium oxide of 0.5; a powder
bulk density of 24 pounds per cubic feet (117.2 kg/m2); and a solution pH
of 7-10. The amount of the polyoxyethylene polymer present in the
aqueous chemical treating composition for treating the glass fibers of
the present lnvention is an amount greater than around 30 weight percent
solids of the aqueous chemical treating composition and preferably in an
amount which is the predominant amount of the solids. The upper limit of
the amount in the aqueous chemical treating composition i8 that amount
which does not increase the viscosity above around 40-50 centipoise at
25C. In addition, the polyoxyethylene polymer can be a polyoxyethylene
homopolymer or can have very minor amounts of polyoxypropylene repeating
units. The polyoxyethylene polymer can be dispersed in water by any
method known to those skilled in the art.
Also poly(vinyl alcohol) can be present in the aqueous chemical
treating composition with the polyoxyethylene of any of the
aforementioned molecular weights. The amount of the poly(vinyl alcohol)
present is an effective film forming amount with or without consideration
of the amount of polyoxyethylene that is present.
In addition, the aqueous chemical treating composition has
present one or more aldehyde-condensate-reactable polymer agents. These
polymeric agents are those that are capable of interaction bonding with
the aldehyde-condensate-reactable coupling agent and the
aldehyde-condensate resinous material used as the paper binder. Typical
paper binders are urea fo D ldehyde, melamine formaldehyde, phenol
8S434
formaldehyde, epichlorohydrin and amino resins and anionic or cationic
modified versions thereof and mixtures of the various resins. These
resinous materials have some unreacted formaldehyde or aldehyde donor or
methylene donor like paraformaldehyde hexamethylene tetramine and the
like and methylol groups like N-methylol groups in urea formaldehyde.
The aldehyde-condensate-reactable polymeric agent is capable of reacting
with the excess aldehyde or methylene donor or formaldehyde and the
methylol groups. These reactions are those such as formation of
methylene linkages or methylene and ether linkages through bimolecular
reactions and/or methyleneurea formation and polymerization reactions.
Nonexclusive examples of these polymeric agents include:
polyacrylamide and/or polyamide where the former is capable of covalently
reacting with the urea formaldehyde while the latter is capable of
hydrogen bond reactions with the urea formaldehyde. Which of the
aldehyde-condensate-reactable agents is used depends not only on the
interaction bonding capability with the aldehyde-condensate resinous
material of the paper binder but also depends on the composition of the
white water system in which the glass fibers are to be dispersed. If the
white water system has an incompatible amount of polyacrylamide, then the
polyamide is used as the aldehyde-condensate, or more particularly, the
urea formaldehyde, reactable polymeric agent. If the white water system
is devoid of any polyacrylamide, then the polyacrylamide and/or polyamide
can be is used in the aqueous chemical treating composition as the
reactable polymeric agent. If the white water system has polyamide
present, then the polyacrylamide and/or polyamides can be used in the
aqueous chemical treating composition. The polyacrylamide is a stronger
reacting polymeric agent for aldehyde condensates like urea formaldehyde
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than is the polyamide. Hence, higher quantities of the polyamide are
tolerated by the white water system compared to quantities of the
polyacrylamide. The total amount of polyacrylamide in a white water
system combining the amount present on the glass fibers and the amount
used as a suspending agent in the white water should not exceed around 20
weight percent of the solids of the aqueous chemical treating
composition.
Nonexclusive examples of the polyacrylamide that can be used in
the aqueous chemical treating composition are those poLyacrylamides
having the structure (-CH2CHCONH2). The polyacrylamides can range
from anionic to cationic. The polyacrylamide should be water soluble,
dlspersible or emulsifiable and ordinarily, polyacrylamide is rapidly
wetted by water and can be dissolved in all proportions. Higher solution
concentrations of the polyacrylamides can increase the viscosity of the
aqueous chemical treating composition to too high a level. A
nonexclusive example of the polyacrylamide is that available from Dow
Chemical Company under the trade designation Strength Resin 87D which $s
slightly anionic and has a molecular weight of 500,000. A nonexclusive
example of a polyamide resin which can be used in the aqueous chemical
treating composition is that available from Georgia Pacific Company,
Resin Division, Atlanta, Georgia under the trade designation GP2925.
This polyamide is an amber colored liquid having a percent solids of 20
to 20.5, a viscosity in centistokes of 140 to 200, a specific gravity of
1.04 to 1.05, a weight per gallon in pounds of 8.7, a pH at 25C of 6.9
to 7.3, a boiling point of 100C, a flash point of none to boiling and a
storage life at 25C of six months. In addition, the polyamide resin may
contain a trace of free epichlorohydrin.
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The amount of the polyacrylamide is preferably around 2 to
about 10 and most preferably about 4 to about 8 weight percent of the
solids of the aqueous chemical treating composition for white water
systems containing little or no polyacrylamide resins. For white water
systems already containing the higher amounts of polyacrylamide resin,
the reactable polymeric agent is the polyamide in amounts in the aqueous
chemical treating composition that range from about 1 to about 50 weight
percent of the solids of the aqueous chemical treating compasition.
Higher amounts of the polysmides appear to have a detrimentsl effect on
tensile strengths of the glass fiber paper product. Any method known to
those skilled in the art for placing, dispersing or emulsifying the
polyamide resin or polyacrylamide resin in aqueous solutions can be used.
The aqueous chemical treating composition also has present an
aldehyde-condensate-reactable organo silane coupling agent such as
alkoxylated gamma aminoalkyltrialkoxy silane, polyamino organo silanes,
mercapto functional organo silanes and ureido-functional organo silanes.
These organo silane coupling agents can be in unhydrolyzed or hydrolyzed
form, silanol form or in the siloxane polymeric form. The organo moiety
of these organo functional silane coupling agents is a difunctional
organic radical selected from the lower alkyl or aliphatic hydrocarbons
having less than 8 carbon atoms. The organic group bonded with the
oxygen in the organo functional silane coupling agent can be the same or
different organic moieties selected from lower alkyl or aliphatic
hydrocarbons having less than 8 and preferably less than 5 carbon atoms.
Nonexclusive examples of the urea formaldehyde-reactable organo silane
coupling agent include: the gamma aminopropyltriethoxy silane,
ethoxylated gamma aminopropyltriethoxy silane such as that available
~.~85434
commercially from Union Carbide Corporation under the trade designation
A-1108, the polyamino organo functional silane coupling agent such as
N-beta(aminoethyl) gamma aminopropyltrimethoxy silane (A-1120), the
material available from Union Carbide (A-1130), which is a polyamino
organo silane coupling agent and the ureido silane having the structure
H2NCONHC3H6Si(OC2H5)3, 50 percent in methanol, available
under the trade designation A-1160. The presence of other types of
organo silane coupling agents is not needed, since one or more of the
aldehyde-condensate-reactable organo functional silane coupling agents
give adequate performance. The addition of further different types of
organo silane coupling agents provide little extra benefit. The amount
of the aldehyde-condendate-reactable organo silane coupling agent present
in the aqueous chemical treating composition depends upon the type of
aldehyde-condensate-reactable, polymeric agent. When the reactable
polymeric agent is polyacrylamide, the aqueous chemical treating
composition can have lower amounts of the aldehyde-condensate-reactable
organo silane coupling agent. ~n the other hand, when the reactable,
polymeric reacting agent is polyamide, the aqueous chemical treating
composition has a higher amount of the aldehyde-condensate-reactable
organo silane coupling agent. Also, mixtures of the aldehyde-
condensate-reactable silane coupling agents can be used. With the
polyacrylamide present in the aqueous chemical treatin8 composition, the
amount of the organo silane coupling agent can be up to around 25 weight
percent of the solids of the aqueous chemical treating composition. When
the polyamide is present in the aqueous chemical treating composition,
the organo silane coupling agent can be present in an amount up to around
50 weight percent of the solids of the aqueous chemical treating
composition.
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The treating composition of the present inventlon has one or
more water soluble, dispersible or emulsifiable cationic lubricant
surfactants having one or more primary, secondary and/or tertiary amine
moieties. Nonexclusive examples of the cationic lubricating surfactants
lnclude: aliphatlc mono, dl, ant polyamlnes like N-alkyl trimethyl-
enediamine, 2-alkyl-2-imidazoline or 1-(2-aminoethyl)-2-alkyl-2-
imidazoline, where, respectively, the alkyl groups can be those such as
soya alkyl, tallow alkyl, coco alkyl or 9-octa-decyl or mixtures of
alkyls, heptadecenyl, undecyl or heptadecyl,-nonyl or mixtures of alkyls,
where these compounds are water soluble, dispersible or emulsifiable.
Also compounts can be used that are like: amlne oxldes, polyoxyalkylene
alkylamines, 1-(2-hytroxyalkyl)-2-alkyl-2-imidazolines, 2-hydroxylalkyl-
2-lmitazollne, or N,N,N',-tetrakis-substituted alkylene diamine
terlvatives or rosin terived amlnes, where the alkyl groups can be llke
cetyl, lauryl, myristyl, stearyl, coco, hydrogenated tallow, hexadecyl,
tallow octadecyl, alkyl groups for polyoxyalkylene, aliphatic and resin
monoamlnes, where the alkylene ls ethylene or an e~uivalent alkyl groups
wlth from about 8 to about 22 carbon atoms, soybean oil and soya. Other
useful catlonic surfactants lnclude polyoxyethylene alkyl and alicyclic
amlnes, where any of the aforelisted alkyl groups and any of the known
allcyclic groups can be used. These cationic materials are more fully
tescrlbed ln the "Encyclopedia of Chemical Technology", Kirk and Othmer,
Vol. 19, pages 554-563, The Interscience Encyclopedia, Inc., N.Y. These
;~ cationic materials include those like polyoxyethylene linear alkyl
amlnes, and polyoxyethylene dihydroabietyl amines. Also useful are the
condensation reaction products of carboxylic acids, fatty acids with di
or polyamines or dialkylene or polyalkylene amines and polyalkoxylated
derivatlves thereof.
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35434
A particularly useful class of catlonic surfactants are the
lubricant cationic surfactants that are alkyl lmidazoline derivatives,
which lncludes compounds of the class, n-alkyl-N-amido-alkyl
imidazolines, which may be formed by causing fatty acids or carboxylic
acids to react with polyalkylene polyamines under conditions which
produce ring closure. The reaction of tetraethylene pentamine with
stearic acid is exemplary of such a reaction. These imidazolines are
described more fully in U.S. Patent No. 2,200,815 and other imidazolines
are described in U.S. Patent Nos. 2,267,965;-2,268,273; and 2,353,837.
The most useful cationic lubricating surfactant is that available under
the brandname Catlon-X softener from Lyndal Chemical Co., Lyndhurst, NJ.
The amount of the cationic surfactant in the treating
composition is ln the range of about 5 to about 30 weight percent of the
sollds of the aqueous treatlng composition. The amount of the cstionic
surfactant will vary in this range depending on the number and type of
cationic groups present in the cationic surfactant. Preferably the
amount of cationic lubricating surfactant is in the range of about 10 to
about 20 weight percent of the solids of the composition.
In addltion to the foregoing chemical compounds, the treating
composition of the present invention may have any of the chemical
compounds, which are known to be useful in aqueous treating compositions
for treating glass fibers to be dispersed in aqueous media. Nonexclusive
examples include additional film forming polymers, lubricants,
:: :
ant1oxidants, bactericides and the like. Preferably, starches and
nonpolymeric amide compounds that are water soluble or dispersible such
as urea or monoamides, diamides, amine-containlng amides, carbamide and
derivatives, where the amide and amine groups are primary or secondary or
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128S434
mixtures thereof are not used in the present invention. The addition of
these compounds to the composition does not serve any addltional function
or contribute any additional benefit for the composition.
Also present in the treating composition of the present
invention is a liquid carrier, which is preferably water to make the
treating composition an aqueous treating composition. The amount of
water present in the aqueous treating composition is that amount
necessary to give the treating composltion a total solids content within
a level, whereby the viscoslty of the aqueous treating composition is
effective for application to glass filaments, that is, a composition with
a vl8cosity of around 0.6 to about 50 centipolse at 60C or less.
Particularly, the aunt of water present in the aqueous treating
compositlon 18 sufflcient to give a total solids (nonaqueous) content of
the aqueous treating composltion in the range of about 1 to about 25
percent by weight and preferably about 2 to about lO percent by weight of
the aqueous treating composltion.
The treating composition of the present invention can be
prepared by any method and with any equipment known to those skilled in
the art for preparing aqueous treating compositions to be applled to
glass flbers. For instance, the chemical compounds can be added
sequentially or simultaneously to water or in any order whatsoever.
The aqueous treating composition can be applied to any of the
glass fibers by any method known to those skilled in the art. For
instance, the glass fibers can be prepared by mechanical attenuation or
the like from batch compositions known as "E" glass or "621" glass or any
more environmentally acceptable derivatlves thereof, and other types of
glasses such as "A" glass, "C" glass, or "S" glass via direct or indirect
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melting operations. In preparing the glass fiber strand, the filament
diameter of the glass fibers maklng up the strands can vary from around 3
microns to around 20 microns or higher and preferably around 9 to around
18 microns. The aqueous treating composition can be applied to the glass
fibers after they are formed and during their attenuation by any type of
applicator such as belt applicators, roll applicators or any applicator
which enables the liquid to contact the glass fibers. The amount of the
aqueous treating composition applied to the glass fibers should be
sufficient to glve at least a partial or intermittent coating of the
treating composition on the treated glass fiber strand or around 0.01 to
about 5 weight percent of the treated glass fiber strand. The treated
glass fibers can be chopped directly as fibers or gathered into one or
more glass fiber strands and chopped, where the fibers or strands are
chopped during the process of forming the glass fibers after the treating
composition has been applied to them. The chopped lengths vary from
about 1/16 (1.59 mm( of sn inch to about 3 inches (76.2 mm) and more
particularly about 1/2 inch (12.7 mm) to about 1 inches (25.4 mm). Such
a process is commonly referred to in the art as the wet chop process.
The amount of the moisture on the wet-chopped glass fiber is usually in
the range of up to about 20 weight percent of the treated fibers and
preferably up to about 15 weight percent and most preferably between
about 9 and about 15 weight percent. Also the glass fibers can be
treated and gathered lnto strands much like the wet chop process, but the
flbers are collected as contlnuous glass flber strands lnto a forming
; package and subsequently chopped ln a remote wet chop process or after
drying in a dry chop process into lengths slmllar to those of the direct
wet chop process.
.
:: -- 19 --
~285434
The aqueous dispersion of the treated glass fibers is achieved
merely by placing the wet or dry chopped glass fibers of the desired
length into a batch of water with or without dispersing aids usually with
agitation and/or turbulence to form a dispersion of glass fibers for use
in the wet-laid process or other paper making processes. The amount of
the chopped treated glass fibers in the aqueous dispersion can range from
about O.OOl to about 5 but preferably about 0.01 to about 3 weight
percent of the aqueous dispersion. Although the treated glass fibers of
the present invention can be used without dispersion aids, any of the
conventional dispersion aids can be used with the chopped, treated glass
fibers of the present invention. Nonexclusive examples of such
dlspersion aids that can be used include the polyoxyethylated tallow
amlne dispersing agent available from GAF Corporation under the trade
designatlon "Katapol" agents like VP 532 used alone or in conjunction
with thickeners like hydroxy and/or carboxy alkyl cellulose, especially
the hydroxy ethyl and hydroxy methyl celluloses and soluble or
dispersible salts thereof such as that avallable from Hercules, Inc.
under the trade designatlon "Natrasol" or other thlckeners llke "Separan
AP273" polyamlde from Dow Chemical Company and the like. Another example
of a disperslng agent that can be used with the chopped glass fiber
strands of the present invention is the dispersing agent available from
Diamond-Shamrock Chemical Company under the trade designation
"Nopcosperse" and especially the "Nopcosperse" FFD product. The
Nopcosperse FFD product is a blend of alkyl sulfate quaternary of the
alkyl amino fatty acid amide or amine in a water dlspersible, mineral oil
with an inorganlc silica defoaming agent. Other examples of dispersing
agents that can be used include the quaternary ammonium compounds such as
~ - 20 -
.: . .
.
~2~35434
those available under the trade designation "Arquad 2 HT-75" and the
llke. Also, quaternary ammonlum surfactants can be used such as those
available under Arquad and Aliquat trade designations and mlxtures of
amine oxides with derivatized guar gum and mixture of guar gum and
isostearic amides can be used. Also amine oxide or polyacrylamide
suspending agents can be used.
The nonwoven, sheet-like mat of treated chopped glass fibers
can be made by any method and with any apparatus known to those skilled
in the art. For exampls, a hand mold method-and apparatus can be used or
the Fourdrinier paper machine or cylinder machines can also be used.
Also, the machines known as Stevens former of the Beloit Corporation and
the Rotoformer from the Sandy Hill Corporation and the Inver former from
the Beloit Corporation and the Vertiformer from the Black Clawson Company
can all be used to form the mat of the present invention. In the
wet-laid process, the aqueous dispersion of glass fibers may be diluted
by white water and held in a head box of any of the aforementioned
machines. The white water is water containing similar dispersing agents
as the aqueous dispersion, where the white water is fresh and/or
recirculated from collection points in the process of forming the
nonwoven mat. The aqueous dispersion from the head box is placed on a
screen or cylinder, where some water is removed usually by vacuum or
suction apparatus. After sufficient water has been removed, the mat has
a polymeric binder applied to it, and any excess binder is removed
usually by vacuum or suction means. The binder-containing mat is dried
and cured in one or more ovens to produce the nonwoven, sheet-like mat.
The mat may be collected usually in a large roll weighing from several
hundred pounds to close to 1,000 pounds (454 kg).
- 21 -
~..285434
The polymeric binders that are used to produce the sheet-like
mat are any of the group of so-called "wet strength" resins, which
include reslns such as aldehyde-condensate resins, like urea
formaldehyde, and resins such as cationlc polyamide eplchlorohydrln
commercially available from Hercules, Inc. under the trade name "Kymene
557 H", and cationic urea-formaldehyde reslns available from Hercules,
Inc. under the trade deslgnations "Kymene 882" and "Kymene 917". Also,
melamine-formaldehyde type resins and phenol formaldehyde type resins and
resorclnol formaldehyde type reslns and polymerlzable polyfunctlonal
N-methylol compounds, notably N-methylol ureas such as dimethylol urea
and N-methylol melamine type resins and other amino resins known to those
skllled in the art can be used. Other types of resins that can be used
are polyvinyl alcohol, polyvinyl acetate, and acrylic polymers and
copolymers. Also, mixtures of resins can be used such as the urea
formaldehyde or melamine formaldehyde resins mixed with styrene butadiene
copolymer latices and other latices and/or acrylic polymers or copolymers
like acrylamide. The amount of binder used ln the nonwoven, sheet-llke
mat product is in the range of about 3 to about 45 percent, preferably
about 10 to about 30 percent based on the welght of the unfinlshed mat.
If the amount of binder is too great, the porosity of the mat could be
adversely affected, and, lf the amount ls too low,
the lntegrity of the mat could be adversely affected. After the binder
is applled, the binder-contalning glass fiber mat is dried to set or cure
the binder. This can be accomplished with can driers or any one or more
drylng devlces used in the art.
The nonwoven, sheet-like glass flber mat of the present
inventlon is suitable for use as a replacement for felt in shlngles and
; '
- 22 -
~!~2~3S43~
also for use in built-up roofing (BUR) systems and for use as backing
materials and base materials in flooring applications. In these
applications, the mat with the polymeric binder must have certain
strength properties. These strength properties are measured by dry
tensile, wet tensile, hot-wet tensile and tear strength of the mat with
the polymeric binder. A good mat and binder product must have adequate
tensile strength and adequate tear strength and wet strength. The
nonwoven, sheet-like mat and binder product of the present lnvention has
these adequate properties a~d even further improved values for some of
these properties as is shown in the examples of the present invention.
Preferred Embodiment of the Invention
_
The aqueous chemical treating composition preferably has one
cationic lubricant surfactant which is the fatty imidazoline derivative
formed as the reaction product of tetraethylene pentamine or mixtures
containing the same and stearic acid, which also may have enough dextrin
to prevent syneresis. Also the composition has the polyoxyethylene
homopolymer with a molecular weight of around 900,000. Also present as
the aldehyde-condensate-reactable, polymeric agent iq the urea-formal-
dehyde-reactable, polymeric agent which is preferably polyacrylamide for
non-polyacrylamide containing white water systems and which is polyamide
for polyacrylamide-containing white water systems. The nitrogen-
containing organosilane coupling agent is preferably the ethoxylated
gamma aminopropyltriethoxy silane for the non-acrylamide-containing white
water systems.
For the non or low polyacrylamide containing white water
systems, the glass fibers of the present invention preferably have an
- 23 -
~85434
aqueous chemical treating composition prepared in the following manner.
The polyoxyethylene homopolymer having a molecular weight of 900,000 is
added to water which is rapidly stirred with around a 2 horsepower motor
at 1800 rpm to make a solution which is less than 3 percent by weight of
the polyethylene oxide homopolymer. The initial water temperature is
around 65 to around 95F, and most preferably around 75 to around 80F
(23.9C to 26.7C) maximum and the polyoxyethylene homopolymer is added
within around 5 minutes and about 30 minutes later, the temperature is
raised to a temperature of around 115F, but to a temperature less than
that of boiling water until particles are no longer visible. Preferably,
the elevated temperature is around 120F. After dissolution of the
polyoxyethylene homopolymer in water, the solution is transferred to a
main mix tank. Water is added to a premix tank in a sufficient amount to
solubilize the polyacrylamide resin, 87D which is added to the water and
stirred for around 5 minutes and transferred to the main mix tank. Water
is added to a premix tank and the ethoxylated gamma aminopropyltriethoxy
silane is added and stirred for 5 minutes and transferred to a main mix
tank. Hot deionized water is added to a main mix tank and the cationic
lubricant (Cat-X) is added to the water dissolved and transferred to the
main mix tank. The formulation for the preferred sizing composition is
as follows: for a 5 gallon (18.9 liter) mix
Water 5,777 gms.
Polyethylene oxide 900,000 molecular weight 154.2 gms.
Water 500 gms.
Strength Resin 87D 45.8 gms.
Water 1,000 gms.
Ethoxylated gamma aminopropyltriethoxy silane 51.3 gms.
~2854~4
Water 500 gms.
Cationic lubricant (Cat-X) 49.9 gms.
The solids of the chemical treating composition is around 1.2
weight percent and the pH is around 9 and the average particle size is
around 0.5 microns.
For the acrylamide containing white water system, the aqueous
chemical treating composition preferably has in weight percent of the
nonaqueous components the following formulation:
Poly(ethylene oxide) homopolymer - 35 weight percent solids
Polyamide GP 2925 20 weight percent solids
Cationic lubricant (Cat-X) 15 weight percent solids
Ureido functional silane 30 weight percent solids
This aqueous chemical treating composition is prepared
similarly to the first aqueous chemical treating composition except the
polyamide resin ls substituted for the polyacrylamide strength resin 87D
and the ureido functional silane ls substituted for the ethoxylated gamma
aminopropyltrlethoxy sllane.
The aqueous treating composition is used to treat the glass
fibers preferably in a wet chop process, where the treated glass fibers
are gathered lnto strands and chopped durlng the flber formatlon and
aceenuatlon process. Preferably, the treated glass fibers are chopped
lnto lengths ranging from 1/2 lnch (12.7 mm) to a little over 1 inch
(25,4 mm). The treated glass flber strands have an amount of the
treatlng composltion ranglng in an amount from about 0.01 to about 1.5
percent, most preferably 0.05 to about 0.1 weight percent of the treated
glass fiber strands,
25 -
.
;434
The treated glass fiber strands are added to water to form a
dispersion and it is preferred that a dispersing agent such as Katapol
VP532 dispersant in combination with the Natrasol HR 250 thickener be
used in amounts in the range of about 0.001 to about 0.05 weight percent
for each material based on the weight of the dispersion. The chopped
glass fibers are added to the aqueous solution with the dispersing agents
in a preferred amount of about 0.1 to 1.0 weight percent of the aqueous
dispersion and, thereafter, diluted with white water to about 0.01 to
about 0.05 weight percent of the aqueous dispersion. The preferred
polymeric material used to form the nonwoven, sheet-like mat is a urea
formaldehyde resin modified to have anionic functionality, either by a
blend of polymers or by the presence of anionic groups placed on the urea
formaldehyde resin. The mat is dried and cured in an oven after any
excess binder is removed by vacuum or suction means to produce the
nonwoven, sheet-like mat of the present invention.
Additional information and further illustrations of the
embodiments of the aqueous treating composition, treated glass fibers,
dispersion and nonwoven, sheet-like mat of the present invention are
presented in the following examples, although these examples do not limit
the scope of the invention to these specific embodiments.
Numerous examples of aqueous chemical treating compositions are
given in Table 1 which were prepared in a method similar to that of the
preferred embodiment.
~!.2~3S434
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-- 27 --
~85434
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-- 28---
~!.2~5434
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- 29 -
:~ '
~28S4;~4
The various aqueous chemical treating compositions of Table 1
were used to treat glass f ibers which were subsequently chopped and
prepared as hand sheets or tested on a mat line for making glass paper.
The results of the testing the hand sheets are given in Table 2. The
hand sheets were prepared and tested in accordance with the procedures
described at columns 18-20 of U.S. Patent 4,457,785 (Hsu et al.).
~ ~ ,
: - 30 -
~28sat~4
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~ ~285434
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-- 32 --
~ ~35a~34
In addition to the physical propertles for paper produced from
a ~lurry of glass fibers as indicated in Table 2, other glass fiber
papers were produced. A similar hand-sheet method of producing glass
flber papers as used for those examples in Table 2 was used with a white
water system having an amine oxide dispersant. The dispersion of the
glass fibers, the tensile strength, wet strength retentlon and tear
strength of the glass paper product are presented in Table 3. Also the
percent size retained after two hours at either 100F or 75F ls
indicated. The glass paper products that were tested were those produced
from Examples 1, 11, 14 and 19. The tensile strength and wet strength
retention and tear strength of the paper produced form an Example 1 glass
flbers are compared with the paper produced from the glass fibers of the
Illustrative Example. The values given are the percentage change from
those values obtalned for the Illustrative Example paper product.
Table 3
Physical Properties of Paper Produced from Slurry of Glass Fibers
Percent
~et X Size Retained
White Water Tensile Strength Tear2 hr/100F/in
Glass Flbers System Strength Retention Strength Deionized HgO
-% Change From Ill. Eg.
Example 11Amine oxlde 10 30 5 --
Example 11Amine oxide 11.13 -- 12 41
I1l. Eg. Amine oxide -- -- -~ 19 (75~F)
Example 11 ~ - -- 76
Example 142 -- -- -- -- 79
~xsmple 192 -- __ __ __ 79
2The paper bindèr used was Type B urea for~aldehyde resin.
Deionlzet water as white water.
~; - 33 -
'~
~ ~85434
Another test of the physical properties of the paper produced
from a slurry of glass fibers of the present invention were conducted on
a continuous mat maklng machine such as a Sandy Hill machine. The glass
paper produced was compared against paper produced from commercially
available glass flbers manufactured for use in making glass paper. The
white water system, the dispersion, the tensile strength in the machine
direction as well as the cross-directlon and the percent hot-wet
retention along with mat weight and LOI and tear strength are given in
Table 4.
Table 4
Phy~ical Propertles of Paper Produced from1a Slurry of Glass Flbers on a
Continuous Mat Llne
Whlte Dispersion Tensile Tear Percent
Glas~ Water Mat of Glass Strength Strength Hot-Wet
Fiber~ System Wt/LOI Flbers lb-force gms (MD) Retentlon
MD + CD MD + CD
Example 11 Separan 1.9/23 6.5 188 -- 69
dispersant
Katapol
thlckener
Example 11 Separan -- 6.5 224 894 (500~ --
dispersant
Katapol
thickener
other water
conditioning
~ agents
: Example 19 Separan 1.9/21.5 6.0 168 -- 71
dlspersant
Katapol
thickener
Commerclal Separan 1.89/22 7.0 183.5 -- 68.5
Owens- dispersant
Corning Katapol
Fiberglas thickener
:
- 34 -
~ 285434
Separan -- 7.0 210 866 (521) --
dispersant
Raeapol
thickener
and Water
Condltioning
Agents
l Type A urea formaldehyde resin was used as the paper blnder.
From Tables 3 and 4 it ls seen that good values of tensile
strength and tear strength and hot-wet retention are obtained with the
glass fibers of the present invention whlle the glass fibers of the
present lnventlon also provlde for a good percentage of slze retalned on
the glass fibers ln the process of maklng the glass paper.
': ~
;: :
, ~ ,
:~
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- 35 -