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Patent 2470783 Summary

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(12) Patent Application: (11) CA 2470783
(54) English Title: FIBERGLASS NONWOVEN BINDER
(54) French Title: LIANT DE FIBRE DE VERRE NON-TISSE
Status: Dead
Bibliographic Data
(51) International Patent Classification (IPC):
  • C08L 5/00 (2006.01)
  • B32B 27/04 (2006.01)
  • C08L 3/02 (2006.01)
  • C08L 3/04 (2006.01)
(72) Inventors :
  • RODRIGUES, KLEIN A. (United States of America)
  • SOLAREK, DANIEL B. (United States of America)
(73) Owners :
  • NATIONAL STARCH AND CHEMICAL INVESTMENT HOLDING CORPORATION (United States of America)
(71) Applicants :
  • NATIONAL STARCH AND CHEMICAL INVESTMENT HOLDING CORPORATION (United States of America)
(74) Agent: NORTON ROSE FULBRIGHT CANADA LLP/S.E.N.C.R.L., S.R.L.
(74) Associate agent:
(45) Issued:
(22) Filed Date: 2004-06-11
(41) Open to Public Inspection: 2004-12-12
Availability of licence: N/A
(25) Language of filing: English

Patent Cooperation Treaty (PCT): No

(30) Application Priority Data:
Application No. Country/Territory Date
60/478,132 United States of America 2003-06-12
10/860,103 United States of America 2004-06-03

Abstracts

English Abstract



A fiberglass non-woven binder composition containing a carboxy-functional
copolymer binder crosslinker and a compound capable of forming a hydrogen-
bonding
complex with the carboxy-functional copolymer binder. The binder composition
provides a strong, yet flexible bond that allows a compressed fiberglass mat
to easily
expand once the compression is released. The binder composition is capable of
being
cured at lower cure temperatures than those binders prepared using
conventional
crosslinkers.


Claims

Note: Claims are shown in the official language in which they were submitted.



What is claimed is:
1. A non-woven binder composition comprising:
a carboxyl polymer having one or more carboxylic acid functional monomer units
in an amount of 30 to 100 percent by weight of the carboxyl polymer; and
at least one compound capable of forming hydrogen-bonding complexes with the
carboxyl polymer.

2. The hydrogen-bonding complex forming compound of claim 1 further comprising
polyalkylene glycol, polyvinyl pyrrolidone, polyethylene amine, or a mixture
thereof.

3. The hydrogen-bonding complex forming compound of claim 1 further comprising
one
or more polysaccharides capable of forming hydrogen-bonding complexes with
itself
and/or other polysaccharides.

4. The one or more polysaccharides of claim 3 wherein the one or more
polysaccharides
is at least one starch having water fluidity ('WF') of 20 to 90.

5. The copolymer binder of claim 1 further comprising from 0 to 25 weight
percent of at
least one catalyst based on the weight of the carboxyl polymer.

6. The carboxyl polymer of claim 1 further comprising from 0.1 to 50 weight
percent of
ethylenically unsaturated monomers.

7. The carboxyl polymer of claim 1 further comprising from 0.01 to 10 weight
percent
of a monomer selected from the group consisting of substituted amide monomers,
silanol monomers, or amine oxide monomers.

8. A fiberglass sizing composition comprising the non-woven binder composition
of
claim 1.

9. A binder composition comprising:
at least one polysaccharide capable of forming hydrogen-bonding complexes with
itself.

-14-



10. The binder composition of claim 9 further comprising a crosslinker for
crosslinking
the polysaccharide.

-15-

Description

Note: Descriptions are shown in the official language in which they were submitted.



CA 02470783 2004-06-11
~'T~3ERGLASS NONWOVEN BINDER
The present invention is directed towards binder compositions. More
particularly,
the present invention is directed towards fiberglass non-woven binder
compositions
s having at least one carboxy-functional copolymer binder crosslinker and at
least one
compound capable of forming a hydrogen-bonding complex with the carboxy-
functional
copolymer binder.
Fiberglass insulation products are generally formed by bonding glass fibers
together with a polymeric binder. Typically, an aqueous polymer binder is
sprayed onto
matted glass fibers soon after they have been formed and while they are stih
hot. The
polymer binder tends to accumulate at the junctions where fibers cross each
other, thereby
holding the fibers together at these points. bleat from the hot fibers
vaporizes most of the
water in the binder. The fiberglass binder must be flexible so that the final
fiberglass
product can be compressed for packaging and shipping and later recover to its
full vertical
t 5 dimension when installed.
phenol-formaldehyde binders have lien the primary polymeric binders used in
the
past in manufacturing fiberglass insulation. These binders are low-cost, easy
to apply and
readily cured. They provide a strong bond while maintaining elasticity and
good
thickness recovery so that full insulating value is obtained. Still, phenol-
formaldehyde
2o binders release significant levels of forr~naldehyde into the environment
during
manufacture and therefore constitute an environmental and health risk. Once
cured, the
resin can continue to xelease formaldehyde in use, especially when exposed to
acidic
conditions.
As formaldehyde exposure can create adverse health effects in animals and
2s humans, fiberglass binders have been developed that provide reduced
emissions of
formaldehyde. These developments include a mixture of phenol formaldehyde
binders
with carboxylic acid polymer binders. Still, formaldehyde emissions remain a
concern.
Other formaldehyde-free binder systems have been developed using alternative
chemistries. These alternative chemistries have considered three different
parts. The first
3o part is a polymer that can be copolymerized with other ethylenically
unsaturated
monomers, e.g., a polycarboxyl, polyacid, polya~crylic, or anhydride. The
second part is a
crosslinker that includes an active hydrogen compound such as trihydrie
alcohol,
triethanolamine, beta-hydroxy alkyl amides or tzydroxy alkyl urea. The final
part
-1-
C


CA 02470783 2004-06-11
considered for providing a formaldehyde-free birder system is a catalyst or
accelerator
such as a phosphorous containing compound or a fluomboratc compound.
These alternative binder compositions work well; however, a deficiency of the
current cross-linker systems is that they require relatively high temperatures
to first drive
s off the water and then chemically convert the raw materials to a crosslinked
gel.
Temperatures needed to drive this esterification reaction can range 'from
about 200°C to
about 250°C. Accordingly, there is a need for a fiberglass binder
composition that cures
at lower temperatures. Fyn~ther, there is a net for alternative fiberglass
binder systems
that provide the performance advantages of phenol-formaldehyde resins in
formaldehyde
~ o free systems.
Polysaccharides such as starch have also been used in binder systems. These
polysacebiarides form hydrogen bonding complexes with polyacrylic acid, as
well as with
themselves. Additionally, these materials can be crosslinked by chemistries
known in the
art. However, these materials tend to have high molecular weights, which can
lead to
is clumping and sticking of the glass fibers during processing. As a
consequence of this
clumping and sticking of the fibers, insulation is produced that can be unfit
for
commercial use. Accordingly, there is a need for a hydrogen bonding coaoriplex
that does
not have the disadvamages of the above mentioned polysaccharides.
The binder composition of the present invention provides a strong, yet
flexible
2o bond allowing a compressed fiberglass mat to easily expand once compression
is
released. This binder composition can be a fiberglass non-woven binder
composition
having at least one carboxy-functional copolymer binder crosslinker and at
least one
compound capable of forming a hydrogen-bonding complex with the carboxy-
functional
copolymer binder. In this manner the binder composition is capable of being
cwled at
25 lower cure temperatures than with conventional cmsslinkers.
The binder composition can be in the form of an aqueous solution having a
polymeric binder and at least one compound capable of forming a hydrogen-
bonding
complex with the binder. The polymeric binder includes from about 30 to about
100
percent by weight of one or more acid functional monomer units.
3o The binder composition further includes at least one compound capable of
forming a hydrogen-bonding complex with the carboxy-functional copolymer
binder. In
one aspect those hydrogen-banding complex-forming compounds include
polysaccharides. It is desirable that the polysaccharides be of low molecular
weight so
that they form low viscosity solutions, thereby avoiding the problems detailed
above.
-2-


CA 02470783 2004-06-11
These polysaccharides have art additional benefit in that they are able to
form hydrogen-
bonding complexes with themselves. Ftuther, the polysaccharides can crosslink
with
themselves using techniques well lczrown in the art.
In one aspect, the polysaccharides are starches having water fluidity (' WF')
of
s about 20 to about 90 can be used as part of the fiberglass binder, (A
description of water
fluidity can be found in U.S. Patent No. 4,499,11b.) In another aspect,
starches having
WF of about 50 to about 90 can be used. In a third aspect, starches having WF
of about
70 to about 90 can be used. In addition, Ivw molecular weight starch
derivatives such as
dextrins, maltodextrins, corn syrups and combinations thereof can also be
used.
According to the invention lower temperature curing can be obtained by using a
crosslinker containing a compound capable of forming a hydrogen-bonding
complex with
the carboxy-functional copolymer binder. This hydrogen-bonding complex forms
erosslinks without chemical reaction and therefore can be cured at lower
temperatures,
e.g,, about 150°C. This results in both energy and time saving during
the xnanufaoturiztg
is process.
Conventional fiberglass binder systems using triethanol amine compounds are
hygroscopic and tend to adsorb moisture in the end-use application In
contrast, by using
the hydrogen-bonding complex according to the present invention, the novel
binder
composition overcomes this major problem.
zo 'The present invention is also directed towards a bonded fiberglass mat
bonded with
a polymer binder composition containing an acid-functional polymer binder and
a
compound capable of forming a hydrogen-bonding complex with the polymer.
The present invention provides a non-woven bindtr composition having a
carboxy-functional polymer and a compound capable of forming hydrogen-bonding
25 complexes with that polymer, The earboxy-functional polymer can be
synthesized from
one or more carboxylic acid monomers. Iz~ one embodiment, the acid monomer
makes up
from about 30 to about 100 molt percent of the carboxyl polymer. In another
embodiment, the acid monomer makes up from about 50 to about 95 mole percent
of the
carboxyl polymer. 1n an additional embodiment, the acid monomer makes up from
about
30 60 to about 90 mole percent of the carboxyl polymer.
Examples of carboxylic acid monomers useful in forming the polymer of the
invention include acrylic acid, methacrylic acid, crotonic acid, isocrotonic
acid, fumaric
acid, malefic acid, cinnamie acid, 2-methyl malefic acid, itaeonic acid, 2-
methy itaconic
acid, sorbic acid, a ~-methylene glutaric acid, malefic anhydride, itaconie
anhydride,
-3-


CA 02470783 2004-06-11
acrylic anhydride, methacrylic anhydride. In one aspect, the acid monomor used
in
synthesizing the polymer is malefic acid, acrylic acid, methacrylic acid or a
mixtwe
thereof. The carboxyl groups can also be formed tn situ, such as isopropyl
esters of
acrylates sad methacrylates that form acids by hydrolysis of the esters when
the isopropyl
group leaves. The carboxylic acid monomer also includes anhydrides that form
carboxyl
groups i~ situ.
Other ethylenically unsaturated monomers can also be used in forming the
carboxyl polymer at a level of up to about 70 weight percent based on total
monomer. In
another aspect, these ethylenically unsaturated monomers can be used at a
level of about
0.1 to about 50 weight percent. These monomers can be used to obtain desirable
properties of the copolymer in ways known in the art. For example, hydrophobic
monomers can be used to increase the water-resistance of the non-woven"
Monomers can also be use to adjust the glass transition temperature ('Ts') of
the
carboxyl polymer to meet end-use application requirements. Useful monomers
include
is but are not limited to (mcth)aerylates, maleates, (meth)acrylamides, vinyl
esters,
itaconates, styrenics, acrylonitrile, nitrogen functional monomers, vinyl
esters, alcohol
functional monomers, and unsaturated hydrocarbons.
Low levels of up to a few percent (e.g., up to about 2 weight % based on total
monomer) of crosslinking monomers can also tx used iu forming the carboxyl
polymer.
This extra crosslinking improves the strength of the bonding. However, at
higher levels
this can negatively affect the flexibility of the resultant material. The
erossli~~king
moieties cart be latent crosslinkers. By 'latent crosslinkers' it is meant
that the
crosslinking reaction takes place not during polymerization, but during curing
of the
binder.
Chain-transfer agents known in the art can also be used for regulating chain
length
and molecular weight. The chain transfer agents can be multifunctional whereby
star-
type polymers can bE produced.
The carboxyl polymer can also be co-synthesized with one or more substituted
amide, silanol, or amine oxide tonal monomers for improved glass adhesion.
These
3o functional monomers are used at a level of from about 0 to about 10 percent
by vvcight
based on tire total monomer. In another aspect the functional monomers arc
used at a
level of from about O.OI to about 10 percent. In one aspect the functional
monomers are
used at a level of from about 0.1 to about S percent. Examples of substituted
amide
monomers include, but are not limited to N-methylol acrylamide, N-ethanol
acrylamide,
-4-


CA 02470783 2004-06-11
N-propaaol acrylamide, N-methylol methacrylamide, N,N-dimcthyl acrylamide, N,N-

diethyl acrylamide, N-isopropyl aerylamide, N-hydroxyethyl acrylamide, N-
hydroxypropyl acrylanude, N-octyl aerylamide, N-lauryl aerylamide aad dimethyl
aminopropyl (meth)acrylamida 1n one aspect the substituted amide is di-
subststuDed, e.g:,
s N,N-dimethyl acrylamide and N,N-diethyl xcrylamide.
Examples of silanol monomers include vinyl trisisopropoxy silane, vinyl
trisethoxy silane, vinyl trlsmethoxy silane, vinyl trls(2-methoxyethoxy)
silane, vinyl
methyl dimethoxy silane, y-mcthacryl oxypropyl trimethoxysilane and vinyl
triaeetoxy
silane. These monomers ate typically copolymerized with acrylic acid in wator.
They
to hydrolyze in situ to form the silanol linkages and liberate the
corresponding alcohol,
which can then be distilled off.
The amine oxide monomers are typically incorporated by copolymerizing an
amine-containing monomer, e.g., 2-vixiyl pyridine, 4-vinyl pyridine, dimethyl
aminoethyl
methacrylate, and then oxidizing the amine functionality to the amine oxide.
The amine
l5 can also be oxidized to amine oxide prior to polymerization.
Similarly, the substituted amide and silanol funcdonalities can be introduced
into
the carboxyl polymer by other mtans. For example, the silanol functionality
can be
incorporated by using a chain transfer agent such as y-mereaptopropyl
trimethoxy silane.
Also, a polymer containing acrylamide groups can be functionalixed, for
example, with
2o dimethyl amine to give a substituted amide derivative. Copolymers of amino
acids, such
as a copolymer of aspartic acid and sodium aspartate as disclosed in
U.S.1'atant Number
5,981,691, are useful. These polymers contain amide functionality in the
backbone (e.g.,
Reactin AS 11 from Folia, Inc., Birmingham, Alabama). Furthermore, these
copolymers
have imide funcdonality. This imide functionality can be reacted with art
amine reagent
25 such as di-ethanol amine to form a polymer with amide side chains.
A carboxyl polymer can further be formed from the hydroxyl group of amine
monomers as described in U.S, Patent Publication Number 200410082240. Those
amine
monomers provide an internal cmsslinlcer and partially or fully eliminate the
need for
additional crosslinket. The binder composition can also be formulated with
erosslinker(s)
3o typically used in fiberglass binder compositions, such as hydroxyl, polyol,
or araine
components. Useful hydroxyl compounds include, but era not limitod to;
trihydric
alcohol; ~-hydroxy alkyl amides; polyols, especially those having molecular
weights of
less than 10,000; ethanol amines such as triethauol amine: hydroxy alkyl urea;
and
oxazolidone. UseRii amixles include triethanol amine, dicthylene triamine,
tetratGthylene
_5.


CA 02470783 2004-06-11
pentarnine, and polyethylene imine. In addition to providing additional
crosslinking, the
polyol or amine also serves in plasticizing the polymer film.
The carboxyl polymer can be synthesized by known polymerization methods suds
as solution, emulsion, suspension and Inverse emulsion ~lymerization methods.
In one
embodiment, the polymer is formed by solution polymcrixation in an aqueous
medium,
The aqueous medium can be water or a mixod water/water-miscible solvent system
such
as a water/alcohol solution. The polymerization cats be batch, sari-batch, or
continuous.
The polymers are typically prepared by free radical polymerization; however,
condensation polymerization can also be used to produce a polyrnscr containing
the
io desired moieties. The monomers can be added to the initial charge, added on
a delayed
basis, or a combination.
In one embodiment, the carboxyl polymer is formed at a solids level in the
range
of about 15 to about 60 peroctst. In another embodiment, the polymer is formed
at a
solids level in the range of about 25 to about 50 percent.
In one embodiment, the carboxyl polymer can have a pH in the range of from
about 1 to about 5. In another embodiment, the polymer can have a pH in the
range of
about 2 to about 4. Preferably, the pH is greater than 2 for the hazard
classi$cation it vSrill
be afforded.
The carboxyl polymer cars be partially neutralized, which is commonly done
with
2o sodium, potassium, or ammonium hydroxides. However, it is not necessary to
neutralize
the carboxyl polymer. The choice of base and the partial-salt formed affects
the glass
transition temperature ('T$'~ of the copolymer. The use of calcium or
magzsesiutn base
for neutratizadon produces partial salts having unique solubility
characteristics, making
them quite useful depending on end-use application.
2s The carboxyl polymer may be random, block, star, or other known polymer
architecture. Random polymers are preferred due to the economic advantages;
however
other architectures could be useful in certain end-uses. Copolymers useful as
fiberglass
binders have weight avers;e molecular weights in the range of about 1,000 to
about
300,000. In anc aspect, the weight average molecular weight of the copolymer
is in the
3o range of about 2,000 to about 15,000. In another aspect, the wtight average
molecular
weight of the copolymer is in the range of about 2,500 to about 10,000. In one
aspect, the
weight average molecular weight of the copolymer is in the range of about
3,400 to about
6,000.
-6-


CA 02470783 2004-06-11
The binder composition of the invention also contains compounds capable of
forming hydrogen bonding complexes with the carboxyl polymer. This allows for
crosslinking at lower temperatures. These cmsslinking compounds can be used in
conjunction with the functional copolymers of the presont invention, but are
also used
with polymer and copolymezs currently used as fiberglass binders. They can
also be used
in combination with the conventional crosslinking compounds listed
prc°viously.
Examples of hydrogen-bonding eomplexing agents include, but are not limited to
polyslkylene glycol, polyvinyl pyrrolidone, polysaccharides, polyethylene
amine, or
mixtures thtreof. In orse embodiment the polyalkylene glycol is polyethylene
glycol.
t o Polysaccharide that can be useful in the present invention can be derived
from
plant; animal and microbial sources. Examples of such polysaccharides include
starch,
cellulose, gums (e_g., gum arabic, guar and xanthan), alginates, pectin and
gellan.
Starches include those derived from maize and conventional hybrids of maize,
such as
waxy maize and high amylose (greater than 40"h amylose) maize, potato,
tapioca, wheat,
is rice, pea, sago, oat, barley, rye, amaranth including conventional hybrids
or genetically
engineered materials.
Also included are hemicellulose or plant cell wall polysaccharides such as ~
xylans. Examples of plant cell wall polysaccharides include arabino-xylans
such as corn
fiber gum, a component of com fiber. An important feature of these
polysaccharides is
2o the abundance of hydroxyl groups. These hydroxyl groups provide sites for
crosslinldng.
Some polysacchacidea also contain other functionality such as carboxyl groups,
which can
be ionically crosslinl~ed as well. Amylose containing starches can associate
through
hydrogen bonding or can complex with a wide variety of nnaterials including
polymers,
The polysaccharides can be modified or derivatizcd by ctherification (e.g.,
via
25 treatment with propylene oxide, ethylene oxide, 2,3-
epoxypropyltrimethylammonium
chloride), esterification (for example, via reaction with acetic anhydride,
oetenyl succinic
anhydride ('4SA')), acid hydrolysis, dextrinization, oxidation or enzyme
treatment (e.g.,
starch modified with a-amylase, ~-amylase, pullanase, isoamylase or
glucoamylase), or
various combinations of these treatments.
Other polysaccharides useful hydrogen-bonding materials include maltodcxtrins,
which are polymers having n-glucose units linked primarily by a-1,4 bonds and
have a
dextrose equivalent ('DE') of less than about 2Q. Maltodextrins are available
as a white
powder or concentrated solution and are prepared by the partial hydrolysis of
starch with
acid andlor enzymes.


CA 02470783 2004-06-11
Polysaccharides have the additional advantage of forming hydrogen bonding
complexes) with themselves. Accordingly, tha binder composition can include
the
polysaccharides) without the carboxyl polymer. 'This polysaccharide can be
further
crosslinkcd using crossiinking agents known in the art. Such crosslanking
agents include
s but are not limited to phosphorus oxychloride, epichlorohydrin, sadiutn
trimetaphosphate,
or adipic-acetic anhydride.
The hydrogcn~bonding complex to polymer binder weight xatio is from about 1:99
to about 99;1. In one aspect the hydrogen-bonding complex to polymer hinder
weight
ratio is from about 1 ~0 to about 20:1. ~ another aspect the hydrogen-bonding
catnplac
to polymer binder weight ratio is from about 5: 1 to about 1:5.
The binder composition can form strong bonds without the need for a catalyst
or
accelerator. One advantage of not using a catalyst in the binder composition
is that
catalysts tend to produce films that cast discolor and/or release phosphorous-
containing
vapors. An accelerator or catalyst can be combined with the copolymer binder
in oz~der to
is decrease the cure time, increase the crosslinking density, and/or decrease
the water
sensitivity of the cured binder. Catalysts useful with the binder are known in
the art, such
as allcali metal salts of a phosphorous-containing organic acid, e_g., sodium
hypophosphate, sodium phosphate, potassium phosphate, disodium pyrophosphate,
tetrasodium pyrophosphate, sodium tripolyphosphate, sodium hexamctaphosphate,
2o potassium polyphosphate, potassium tripolyphospate, sodium
trimetaphosphate, sodium
tetrametaphosphate; fluoroborates, and mixtures thereof. The catalyst could
also be a
Lewis acid, such as magnesium cattate or magnesium chloride; a Lcwis bast; or
a fret
radical generator, such as a peroxide. The catalyst is present in the binder
formulation at
from Q to 25 percent by weight, $nd more preferably from 1 to 10 percent by
weight
25 based on the copolymer binder.
The carboxyl polymer, compound capable of forming hydrogen-bonding, and
optional catalyst are blended together to form a f bcrglsss binder
composition.
The binder composition can optionally be formulated with one or more adjuvants
such a5 coupling agents, dyes, pigments, oils, fillers, tl~ert~nal
stabilizers, emulsifiers,
3o curing agents, wetting agents, biocides, plasticizers, anti-foaming agents,
waxes,
enzymes, surfactants, release agents, corrosion inhibitors, additives to
t:ninimiu leaching
of glass, flame-retarding agents, and lubricants. The adjuvants are generally
added at
levels of less than 20 percent based on the weight of the copolymer binder.
-g_


CA 02470783 2004-06-11
The poiymer binder composition is useful for bonding fibrous substrates to
form a
formaldehyde-free non-woven material. The copolymer bitader of the invention
is
especially usefirl as a binder fox heat-resistant non-wovens, e.g., aramid
fibers, ceramic
fibers, metal fibers, polyrayon fibers, polyester fibers, carbon fibers,
polyimide fibers, and
mineral fibers such as glass fibers.
The copolymer binder composition is generally applied to a fiber glass mat as
it is
being formed by means of a suitable spray applicator, The spray applicator
aids in
distributing the binder solution evenly throughout the formed fiberglass mat.
Solids are
typically present in the aqueous solution in amounts of about 5 to 25 percent
by weight of
1o total solution. The binder may also be applied by other means known in the
art,
including, but not limited to, airless spray, air spray, padding, saturating,
and roll coating.
Residual heat from the fibers volatiz~es water away from the binder. The
resultant
high-solids binder-coated fiberglass mat is allowed to expand vertically due
to the
resiliency of the glass fibers. The fiberglass mat is then heatod to cure the
binder.
is Typically, curing ovens operate at a temperature of from 130°C to
325°C. However, the
binder composition of the present invention can be cored at lower temperatures
of from
about 110°C to about 1 SO°C. In one aspect, the binder
composition can be cured at about
120°C. The fiberglass mat is typically cured Exam about 5 seconds to
about 15 minutes.
In one aspect the fiberglass mat is cured from about 30 seconds to about 3
minutes. Tlte
2o cure temperature anti aura time also depend on both the temperature and
level of catalyst
used. The fiberglass mat can then be compressed or rolled for shipping. An
important
property of the fiberglass mat is that it returns substantially to its full
vertical height once
the compression is removed. The copolymer binder produces a flexible film that
allows
the fiberglass insulation to bounce back when the roll is unwrapped and placed
in walls
z5 andlor ceilings.
Fiberglass or other non-woven treated with the copolymer binder composition is
useful as insulation for heat or sound in the form of rolls or baits; as a
reinforcing mat for
roofing and flooring products, ceiling tiles, flooring tiles, as a mieroglass-
based substrate
for printed circwit boards and 'battexy separators; for filter stock and tape
stock and for
3o reinforcements in both non-cementatious and cementatious masonry coatings.
The following examples are presented to further illustrate and explain the
present
invention and should not be taken as limiting in any regard.
_g.


CA 02470783 2004-06-11
E~,1~PLE 1
The following farmulataons ware mined together to form insulation sizing
resins.
50 grams of a 50% solids solution of polyacrylic acid was blended with 26
grams of 50°l0
solutions of the listed crossliaker producing 7f> grams of a 50% solids
nonwovezt binder
s composition. Curing was measured by qualitatively measuring the strength of
the
resulting film.
The testing protocol was as follows, 20 grams of each of solution was poured
into
PMP petri dishes and placed vverniglat in a forced air oven set at
60°C. The film was
then cured by being placed fox 10 minutes in a forced air oven set at
150°C. After
1 o cooling, the cure of the resulting films was evaluated in terms of
physical appearance,
flexibility, and tensile strength.
TAELE 1
FacampiaAmount co-ingredientAmount Performance of
# of of insulation


polyacrylic co-ingredientsizing re:in
acid


i5o96 solution


1 a 50 Triethanol 13 Control (cured
amine at 220C)



nom bve


_ 50 Polyethylene 13 Cured better compared
1 b glycol to


800 conventional main
in 1a


1 c 50 Polyethylene 13 Cured better compared
glycol to


6000 conventional resin
in is


id 50 Polyvinyl 10 Cured better compared
pyrrolidone to


conventional resin
in 1 a


_ 50 Polyethylene 10 Cured better compared
1e amine to


conventional resin
in 1a


While not being bound by any theory, it is bolieved that the resins in lb to
1e form
15 hydrogen bonding complexes. Hence, they cure at much lower temperatures
than the
conventional resin in la. This is because the conventional resin needs to
undergo an
esterification reaction beivvecn the polyacrylic acid and the TEA after all
the water in the
system is driven off. In contrast, after driving the water off in 1b to lc,
hydrogen-
bonding complexes are formed, which lower energy costs and save processing
time:
-10-


CA 02470783 2004-06-11
F.X,AMPLE 2
Copolymer binders containing glass-adhesion promoting comonomers were
synthesized as follows --
EXAMPLE 2A
A reactor containing 200 grams of water and 244 grams of isopmpanol was heated
to 85°C. A monomer solution containing 295 grams of acrylic acid and
4.1 grams of
N,N-dimethyl acrylamide was added to the reactor over a period of 3.0 hours.
An
initiator solution comprising 15 grams of sodium persulfate in 100 grams of
deioniud
water was simultaneously added to the reactor over a period of 3.5 hours. The
reaction
product was held at 85°C far an additional hour. The isopropanol was
then distilled using
a Dean-Stark trap.
is ~ 2B
A reactor containing 200 grams of water and 244 grams of isopropanol was
heated
to 85°C. A monomer solution containing 295 grams of acrylic acid and 5
grams of vinyl
trisisopropoxy silane (available as CoatOSil~ 170b from GE Silicones, Wiltvn,
Connecticut) was added to the reactor over a period of 3.0 hours. An initiator
solution
2o comprising of 15 grams of sodium persulfate in 100 grams of deionized water
was
simultaneously added to the reactor over a period of 3.5 hours. The reaction
product was
held at 85°C for as additional hour, Tho isopropanol was then distilled
using a Dean-Stark
trap. The isopmpdxy silane is attached to the copolymer via the vinyl linkage.
I~owever,
it hydrolyzes during the reaction forming silanol groups and isopropanol. The
2s isopropanol formed is distilled with the rest of tl~ isoprapanol added to
the initial charge.
Additional water is added to the reaction to dilute it to 50% solids.
EXAMPLE,E 2C
A reactor containing 200 grams of water and 244 gams of isopmpanol was heated
30 tv 85°C. A monomer solution containing 295 grams of acrylic acid and
5 grams of vinyl
triethoxy silane (available as Silquest~ A 151 from GE Silicones, Wilton,
Gonnecticut)
was added to the reactor over a period of 3.0 hours. An initiator solution
comprising of
grams of sodium persulfate in 100 grams of deionized water was simultsaeously
added
to the reactor over a period of 3.5 hours. The reaction product was held at
85°C for an
-11-


CA 02470783 2004-06-11
additional hour, The isopmpanol was then distilled using a Dean,Stark trap.
The
isopmpoxy silane is attached to the copolymer via the vinyl linkage. ~Iowever,
it
hydrolyzes during the reaction to form sila~tol groups and ethanol. The
ethanol formed is
distilled with the rest of the isopropanol added to the inititat charge.
Additional water is
s added to the reaction to dilute it to 50 percent solids.
EX~PLE 2D
A reactor containing 200 grams of water and 244 grams of isopropanol was
heated
to 85°C. A monomer solution containing 295 grams of acrylic acid and S
grams of 4
t 0 vinyl pyridine was added to the reactor over a period of 3.0 hours. An
initiator solution
comprising of 15 grams of sodium persulfate in 100 grams of deioni~ed water
was
simultaneously added to the reactor over a period of 3.5 hours. The reaction
product was
held at 85°C for an additional hour. The isopropanol was then distilled
using a Dean-Stark
trap. The vinyl pyridine moiety was then oxidized to amine oxide by treating
tl~e polymer
~ 5 with hydrogen peroxide in the presence of sodium molybdate.
EXAMPLE 3
Solutions were prepared by dissolving 25 gxams of a polyecrylic acid
(available as
Alcosperse~ 602A from Alco Chemical, Chattanooga, Tennessee), and a low
viscosity
2o starch solution in the amount detailed in Table 2 below. The solutions were
diluted to
10%, and the viscosities of these 10% starch-containing solutions were
measured. As a
comparison, the viscosity of a similar solution containing triethanol amiae (a
conventional crosslinker known in tho art) was also measured,
-12-


CA 02470783 2004-06-11
ExamploCrosslinking agent rams of orosslinkingscosity WF of
of a


agent added 10% fiberglassstarch
to


polyacrylic sizing solution
avid


solution


3a Triethanol amine 4.3 18 '
-


3b Acid corwerted waxy28.9 19.7 85
mafiz!


substituted with
hydroxypropyl


rou 30 % solids


3c Ac converted waxy 18 19.6 85
maize


substituted with
hydroxypropyl


rou 50 % solids


3d Acid converted waxy2fi.8 18.8 Bknd
mane of


octenyl svccinabe 40 WF
I waxy maize


dextrin blend (30% g~mh
solids)


and


dextrin


p~ ~n~~ ~y ~~ 1g 20.8 Blend
of


octenyi succinate 40 WF
I waxy maize


dextrin blend (5096 $~~h
solids]


and


dextrin


3f AGd converted waxy 16 _ B3
maize 20.0


octen I succinate
50% solids


3g Beta amylase converted16 16.5 85
waxy


m8ize octenyl succinate
(50%


solids


3h Acid converted waxy28.9 45.3 40
mains


substituted with
hydroxypropyl


rou s 30 % solids


3i Regular high molecular3 2000 5
weight


starch


The data indicate that the viacosities of the starch/polyacrylic acid
solutions with
water fluiditics ('WF') from 40 to 85 are in the range of the viscosity of the
conventional
polyacrylic acid-triethanol amine system, However, a traditional unmodified
starch has a
very high viscosity and cannot be used in this system.
-13-

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Administrative Status

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Administrative Status

Title Date
Forecasted Issue Date Unavailable
(22) Filed 2004-06-11
(41) Open to Public Inspection 2004-12-12
Dead Application 2009-06-11

Abandonment History

Abandonment Date Reason Reinstatement Date
2008-06-11 FAILURE TO PAY APPLICATION MAINTENANCE FEE

Payment History

Fee Type Anniversary Year Due Date Amount Paid Paid Date
Application Fee $400.00 2004-06-11
Registration of a document - section 124 $100.00 2004-11-25
Maintenance Fee - Application - New Act 2 2006-06-12 $100.00 2006-05-04
Maintenance Fee - Application - New Act 3 2007-06-11 $100.00 2007-05-22
Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
NATIONAL STARCH AND CHEMICAL INVESTMENT HOLDING CORPORATION
Past Owners on Record
RODRIGUES, KLEIN A.
SOLAREK, DANIEL B.
Past Owners that do not appear in the "Owners on Record" listing will appear in other documentation within the application.
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Document
Description 
Date
(yyyy-mm-dd) 
Number of pages   Size of Image (KB) 
Abstract 2004-06-11 1 15
Claims 2004-06-11 2 43
Description 2004-06-11 13 726
Cover Page 2004-11-19 1 28
Correspondence 2004-07-16 1 32
Assignment 2004-06-11 2 82
Correspondence 2004-12-01 1 28
Assignment 2004-11-25 5 138
Correspondence 2004-12-22 1 12
Correspondence 2005-03-14 1 10