Polyurethane carpet backing ingredients
A summary of ingredients and processes described in polyurethane carpet backing
patents.
by Jim Vallette, Senior Researcher, Healthy Building Network, November 2010
Excerpted below –
Patent No. 7,794,814 (Sept. 24, 2010), “Polyurethane carpet backings made using
hydroxymethylated polyester polyols,” filed May 4, 2006, Randall Jenkines, Dow Global
Technologies (Midland, MI)
Patent No. 7,638,008 (Dec. 29, 2009), “Polyurethane roller coating process for carpet
backing,” filed October 8, 2004, Hamrick et al., New Spirit Backing LLC (Dalton, GA):
Patent No. 7,241,818 (July 10, 2007), “Filler Comprising Fly Ash for Use in Composites,”
filed Feb. 28, 2005, Raymond T. Hemmings, Russell L. Hill, Bruce Cornelius, Boral
Material Technologies Inc. (San Antonio, TX)
Patent No. 6,916,863 (July 1 2, 2005), “Fly ash for use in polymer composites,” filed
August 22, 2002, R. Hemmings, R. Hill, B. Cornelius, Boral Material Technologies
(San Antonio, TX) -- essentially same as 7,241,818
Patent No. 6,743,844 (June 1, 2004), “Spill resistant carpet backing,” filed Feb. 24,
2000, Tabor et al., Dow Global Technologies Inc. (Midland, MI)
Patent No. 6,555,199 (April 29, 2003), “Carpet backing precoats, laminate coats and
foam coats prepared from polyurethane formulations using fly ash,” J. Jenkines, Dow
Chemical (Midland, MI). Largely identical to Pat No. 6,096,401, not repeated here.
Patent No. 6,096,401 (August 1, 2000), “Carpet backing precoats, laminate coats, and
foam coats prepared from polyurethane formulations including fly ash,” filed Aug. 28,
1996, Randall Jenkines, Dow Global Technologies (Midland, MI)
Patent No. 5,908,701 (June 1, 1999), “Preparation of filled reactive polyurethane
carpet backing formulations using an in-line continuous mixing process,” filed Aug.
4, 1997, J. Jennings, R. Jenkines, L. Mobley, Dow Chemical Company (Midland, MI)
[patents in italics are available in data sources section of the Pharos record,
“Common polyurethane carpet backing components.”
First use of fly ash in carpet backing – Dow Patent No. 6096401: “The polyurethaneforming composition of the present invention comprises a polyol as described
herein, a chain extender, a polyisocyanate, a catalyst as described herein, a
surfactant, a filler wetting agent, and a filler that includes fly ash. The composition of
the present invention contains reactive components such as active hydrogen
containing compounds and compounds having isocyanate functionality. “
1. A+B:
“Conventional practice in the carpet manufacturing industry requires that the
precoat be prepared from an isocyanate formulation (A-side formulation) and a
polyol formulation (B-side formulation) at the carpet manufacturing site. This is
sometimes referred to as "A+B chemistry". Preparing a polyurethane precoat by
A+B chemistry can result in unpredictable loss of production and inefficiency due to
problems that can occur in carrying out the reaction at the manufacturing site, such
as premature gellation. “ . 6,743,844
Isocyanates and polyol blend mixed just prior to application, using catalyst.
Polyurethane is gelled and foamed with carbon dioxide gas. “The balancing of these
two reactions is controlled by the natures of catalysts and auxiliary agents used in
the process.” 7,638,008
“It is customary in the carpet and rug industry to use various forms of filled and
unfilled latex or polyurethane to coat the back of carpet. The coating is used to
bond the face fibers to the primary backing and thereby creating good tuft bind or
fiber lock, and to bond secondary backing material to the greige (fibers/primary
backing). … 7,638,008
“Despite the [physical property] advantages of polyurethane, cost and technical
problems have kept it from widespread use in the industry as a coating, and even
more rarely as a flexible foam…. 7,638,008
“When chemical agents are added to control premature polymerization and
maintain viscosity to enable the polyurethane to penetrate the fibers and achieve
good tuft bond and maintain adhesiveness to affix the secondary backing, the
resulting mixture typically will not cure quickly without oven curing… 7,638,008
“To extend the coverage of a given quantity of pre-polymers, it is customary to add
filler material to the mixture. However, filler materials are generally abrasive and
complicate the application of the polyurethane mixture…. 7,638,008
“Contents of the polyol, iso and catalyst tanks are pumped to polyurethane coating
head 21…. 7,638,008
2. Aqueous dispersion
“Alternatively, the polyurethane precoat may be applied as an aqueous
polyurethane (PU) dispersion. Aqueous PU dispersions can be prepared by
polymerizing the polyurethane reactants in an organic solvent followed by
dispersion of the resulting solution in water, and optionally followed by removal of
organic solvent. See U.S. Pat. Nos. 3,437,624; 4,092,286; 4,237,264; 4,742,095;
4,857,565; 4,879,322; 5,037,864; and 5,221,710, which are incorporated herein by
reference. Also, an aqueous polyurethane dispersion may be prepared by first
forming a prepolymer, next dispersing the prepolymer in water, and finally
conducting a chain extension in the water as disclosed in WO 98/41552, published
Sep. 24, 1998, which is incorporated herein by reference. Preparations of aqueous
dispersions of polyurethane are also described in U.S. patent application Ser. Nos.
09/039,978 and 09/039,976. U.S. Pat. No. 4,296,159 to Jenkines, et al., discloses
preparing a tufted or woven article having a unitary backing prepared by applying a
polyurethane forming composition to the underside of the tufted or woven article. “
(6,743,844)
POLYOL MIXTURE
“Polyol tank contains polyol mixed with filler and surfactants, such as silicone…..
“Typically, there will be between 250 and 500 parts filler per hundred parts of
polyol …. “Thre may be other additives such as stabilizers, antioxidants,
antimicrobials, anti-mildew agents, colorants, flame retardants, penetrants, and
chain extenders, all depending upon the characteristics desired in the resulting
foam…
7,638,008
“The present invention can include other components, such as surfactants, blowing
agents, frothing agents, defoamers, fire retardants, pigments, antistatic agents,
reinforcing fibers, antioxidants, preservatives, acid scavengers, and the like.”
(6,743,844)
“Other additives may be used, including fire retardants, pigments, antistatic agents,
reinforcing fibers, antioxidants, preservatives, acid scavengers, and the like. It is
usually preferred not to include a blowing agent. Components are preferably dried
to remove residual water. The polyurethane-forming composition preferably
contains less than 0.1% by weight water, so as to avoid a gas-generating reaction
with the polyisocyanate. In order to provide a non-cellular coating, it is preferred to
eliminate or minimize the presence of surfactants and foam stabilizers. The
elimination of these materials permits the formulation to be frothed in order to
control coating weight, while then allowing the entrapped gases to escape before
the formulation is cured. “ (7,794,814)
“The present invention can include other optional components. For example, a
polyurethane-forming composition of the present invention can include a
surfactant, a blowing agent, a flame retardant, pigments, antistatic agents,
reinforcing fibers, antioxidants, preservatives, water scavengers, acid scavengers,
and the like.” (6.096,401)
Polyols:
“The polyol component includes a mixture of isocyanate-reactive compounds. For,
25 to 90%, such as from 25 to 75%, from 30 to 60% or from 30 to 50%, of the total
weight isocyanate-reactive compounds is one or more hydroxymethyl-containing
polyester polyols. … The additional high equivalent weight polyol may be a
polyether polyol, such as a polymer of ethylene oxide, propylene oxide,
tetrahydrofuran or butylene oxide, or a mixture of two or more of these. Particularly
suitable polyether polyols include polymers of propylene oxide, random copolymers
of propylene oxide and ethylene oxide, especially those containing up to about 16%
by weight randomly polymerized ethylene oxide, and oxyethylene-capped polymers
of propylene oxide or propylene oxide-ethylene oxide random copolymers. These
polyols are conveniently prepared by adding the corresponding alkylene oxide to an
initiator material such as a low molecular weight compound containing two or more
hydroxyl and/or primary or secondary amine groups. Polyester polyols such as
polycaprolactone and butanediol/adipate polyesters can also be used as an
additional high equivalent weight polyol. “ (7,794,814)
“Hydroxymethyl containing polyester polyol A (HMPP A) is prepared by reacting
2048.6 g (6.23 moles) of a hydroxymethylated soybean oil and 467.2 g (1.168
moles) of a difunctional, 400 molecular weight poly(ethylene oxide). HMPP A has an
OH number of 71.28 and a functionality of about 2.4.
“Soy Oil Polyol A is a 130-OH-number functional blown soy oil polyol transesterified
with a blend of sucrose and glycerin, sold as SoyOyl.TM. GC5N by Urethane Soy
Systems Corporation.
“Polyether Polyol A is a 2000 molecular weight, nominally difunctional
poly(propylene oxide). It is available commercially as Voranol.RTM. 9120A polyol
from Dow Chemical.
“Polyether Polyol B is a 2000 molecular weight, nominally difunctional
polypropylene oxide) end-capped with 12 percent ethylene oxide, available
commercially as Voranol.RTM. 9287A polyol from Dow Chemical. “ (7,794,814)
“Polyols of the present invention are prepared by known methods by reacting an
alkylene oxide with a suitable polyhydric initiator compound. The alkylene oxide
preferably has 2-8 carbon atoms. For example suitable alkylene oxides can be
ethylene oxide, propylene oxide, 1,2-butylene oxide, 2,3-butylene oxide, styrene
oxide, epichlorohydrin, 3-methyl-1,2-butylene oxide, like compounds and mixtures
thereof, with propylene oxide being the preferred oxide. The initiator compound can
be a polyhydric compound such as water, ethylene glycol, propylene glycol, 1,2butane diol, 1,3-butane diol, glycerine, trimethylol propane, p,p'-isopropylidine
diphenol, aniline, ammonia, ethylene diamine, aminoethylethanolamine, like
compounds and mixtures thereof. “ Dow’s example 5 includes Voranol 9741.
(6,096,401)
“ Polymers of propylene oxide which are at least partially end-capped with ethylene
oxide are particularly preferred. “ (5,908,701)
Filler:
The filler material can include conventional fillers such as milled glass, calcium
carbonate, aluminum trihydrate, barium sulfate, fly ash, dyes and pigments or fire
retardants (aluminum trihydrate and Tris polyolefin glyclol). Preferably the filler
can be present in an amount ranging from 0 to 600 parts, and more preferably
between 100 and 500 parts, per 100 parts of the polyol component. 7,638,008
“The present invention can include other filler materials. The filler material can
include conventional fillers such as milled glass, calcium carbonate, aluminum
trihydrate, talc, bentonite, antimony trioxide, kaolin, fly ash, or other known fillers.
A suitable filler loading in a polyurethane dispersion can be from about 100 to about
1000 parts of filler per 100 parts of the polyurethane compound. Preferably, the
filler material can be loaded in an amount of at least about 200 pph (phr), more
preferably at least about 300 pph, most preferably at least about 400 pph… The
inorganic fillers of the present invention include calcium carbonate, calcium sulfate,
kaolin, lignite fly ash, silica, talc, feldspar, mica, glass spheres, wollastonite,
aluminum trihydrate, aluminum oxide, fiber glass, similar compounds, and mixtures
thereof. In the present invention, the preferred inorganic filler is calcium carbonate.
.” (6,743,844)
“The polyurethane-forming composition preferably contains a filler, which reduces
overall cost and may improve flame resistance and other physical properties. The
filler advantageously constitutes from about 20 to about 80 percent, such from 30 to
70, 50 to 65 or 55 to 60 percent, of the total weight of the polyurethane-forming
composition. Suitable fillers include talc, mica, montmorillonite, marble, milled glass
granite, milled glass, calcium carbonate, aluminum trihydrate, carbon, aramid, silica,
silica-alumina, zirconia, talc, bentonite, antimony trioxide, kaolin, coal based fly ash
and boron nitride. “ (7,794,814)
“Calcium carbonate A is a quarried calcium carbonate ground such that 70 weight
percent passes through a 325 mesh screen. It is available commercially as Georgia
Marble D70 from Georgia Marble Company. “ (7,794,814)
Boral: “The filler can be a filler blend including fly ash and at least one additional
mineral filler other than a fly ash. Suitable mineral fillers include calcium carbonate,
aluminum trihydrate (ATH), milled glass, glass spheres, glass flakes, silica, silica
fume, slate dust, amorphous carbon (e.g. carbon black), clays (e.g. kaolin), mica, talc,
wollastonite, alumina, feldspar, bentonite, quartz, garnet, saponite, beidellite,
calcium oxide, calcium hydroxide, antimony trioxide, barium sulfate, magnesium
oxide, titanium dioxide, zinc carbonate, zinc oxide, nepheline syenite, perlite,
diatomite, pyrophillite and the like, or blends thereof. In this embodiment, the
additional mineral filler is preferably calcium carbonate and the calcium carbonate
is preferably combined with a high fine particle content fly ash filler such as a lignite
or subbituminous fly ash (e.g. having a median particle size of 10 microns or less).”
(7,241,818)
“Increasing the amount of conventional fillers used in preparing carpet backing,
such as calcium carbonate (CaCO.sub.3) and aluminum trihydrate (ATH), can result
in an undesirable viscosity increase in a polyurethane formulation. While cost
reduction can be an incentive for introducing as much filler as possible into a
polyurethane formulation, it can be unacceptable to reduce the cost of production at
the expense of the quality of the article produced. The amount of filler incorporated
into a polyurethane formulation can be limited by the adverse effects that the filler
can have on the properties of a polyurethane, such as flexibility, resiliency, and
adhesion, for example. “ (6,096,401)
“The present invention includes a filler material. The filler material includes fly ash.
The filler can be exclusively fly ash, or it can optionally include conventional fillers
such as milled glass, calcium carbonate, ATH, talc, bentonite, antimony trioxide,
kaolin, or other known fillers. Preferably, fly ash makes up at least 50 percent by
total weight of the filler used in the present invention. More preferably, fly ash
makes up at least 75 percent of the filler, and even more preferably at least 90
percent of the filler used in the present invention. Most preferably fly ash makes up
substantially all of the filler material, i.e. at least 99 percent of the filler is fly ash. “
(6,096,401)
“The present invention includes a filler material added as a third stream (S3). In the
practice of the present invention, S3 is typically added as a dry stream. The filler
material can be a conventional filler, such as, for example: milled glass, calcium
carbonate, aluminum trihydrate (ATH), talc, bentonite, antimony trioxide, kaolin.
The filler material can also be recycled waste material from a carpet manufacturing
process. For example, recycled waste material can include: fibrous materials such as
lint from a fabric shearing process; and polymer waste that is ground to particle
sizes less than 2 mm, including rubber from tires, and polyurethane from carpet
underlays. The filler can be fly ash, or any filler or mixture of fillers known to be
useful in the art of preparing filled polymers.” (5,908,701)
Fly Ash Types:
(Boral) “ a filler blend that comprises multiple types of fly ash” ; “a high fine
particle content fly ash filler and a low fine particle content fly ash filler. “ ; “further
comprising calcium carbonate” ; “ wherein the fly ash is selected from the group
consisting of subbituminous coal fly ash, a lignite coal fly ash, a Class C fly ash, and a
Class F fly ash” ; a filler blend comprising a component selected from the group
consisting of subbituminous coal fly ash, a lignite coal fly ash, a Class C fly ash, a
Class F fly ash, and combinations thereof. “ and/or “the filler is a filler blend
comprising a first fly ash and at least one additional filler selected from the group
consisting of a second fly ash and calcium carbonate, and wherein the polymer
composite comprises at least one additional filler other than the fillers included in
the filler blend. … The inherent properties of fly ash, or modified fly ash, allow a
more economical polymer composite to be manufactured as well as one with
comparable or even superior mechanical properties and performance. “ (7,241,818)
(Dow) “Fly ash is a residue that results from the combustion of pulverized coal, and
can include various proportions of oxides of silicon (Si), aluminum (Al), iron (Fe),
calcium (Ca), and magnesium (Mg). The major portion of fly ash is composed of
oxides of aluminum and silicon. Fly ash can be classified as either Class C or Class F
type fly ash. Class C fly ash is obtained from subbituminous and lignite coals. Class F
fly ash is obtained from bituminous and anthracite coals. The fly ash of the present
invention is Class F fly ash. The fly ash used in the present invention can be treated
according to known processes to remove impurities or undesirable components. For
example, fly ash can be treated by water washing. Alternatively, fly ash can be
treated by direct acid leaching (DAL) as described in CS-4765. As another
alternative, fly ash suitable for use with the present invention can be purchased
commercially. “ Dow’s examples includes ALSIL, JTM Grade O1TR.(6,096,401)
Filler Wetting Agent:
“The present invention can include a filler wetting agent. A filler wetting agent
generally renders the filler material compatible with a polyurethane-forming
composition. Useful wetting agents include phosphate salts such as sodium
hexametaphosphate. A filler wetting agent can be included in a polyurethaneforming composition of the present invention at a concentration of at least about 0.5
parts per 100 parts of filler, by weight.” (6,743,844)
“filler wetting agent is an ethoxylated phosphate ester in an organic carrier… A filler
wetting agent generally performs the function of compatiblizing the filler and the
polyurethane-forming composition. Useful filler wetting agents can include
ethoxylated phosphate esters in an organic carrier. Examples of suitable filler
wetting agents include Maphos.TM. 56, Pegafax.TM. 410, and Code 5027 (available
from Fibro Chem, Inc.). ” Example uses Code 5027. (6,096,401, same in 5,908,701)
Surfactants:
Surfactants useful for preparing a stable dispersion can be.. preferably… silicone
surfactants such as Dow Corning DC-194 or Union Carbide’s L-540. A surfactant can
be included in a formulation of the present invention in an amount raning from
about 0.01 to about 7 parts per 100 parts by weight of polyurethane component….
7,638,008
“Useful surfactants include cationic and anionic surfactants. Examples of anionic
surfactants include sulfonates, carboxylates, and phosphates. Examples of cationic
surfactants include quaternary amines. Surfactants can be either external or
internal. External surfactants are surfactants are not chemically reacted into the
polymer during dispersion preparation. Internal surfactants are chemically reacted
into the polymer during dispersion preparation. A surfactant can be included in an
amount ranging from about 0.01 to about 20 parts per 100 parts by weight of
polyurethane component. “ (6,743,844)
“Suitable surfactants include block copolymers of ethylene oxide and silicone
surfactants” Example includes Niax L-5614. (6,096,401)
Blowing Agents:
“Examples of suitable blowing agents are gases such as air, carbon dioxide, nitrogen,
argon, and helium; liquids such as water and volatile halogenated alkanes; and azoblowing agents such as azobis(formamide). Volatile halogenated alkanes include the
various chlorofluoromethanes and chlorofluoroethanes. The use of a gas as a
blowing or frothing agent is preferred. Particularly preferable is the use of air as a
blowing or frothing agent. A frothing agent can differ from a blowing agent in that
frothing agents are typically introduced by mechanical introduction of a gas into a
liquid to froth the polymeric composition. “ (6,743,844)
“Examples of suitable blowing agents include gases such as air carbon dioxide,
nitrogen, argon, helium, and the like; liquids such as water, volatile halogenated
alkanes such as the various chlorfluoromethanes and chlorfluoroethanes; azoblowing agents such as azobis(formamide). Preferred in the practice of this
invention is the use of a gas as a blowing agent. Particularly preferable is the use of
air as a blowing agent. “ (6,096,401)
Chain Extenders:
“When the polymeric material is a polyurethane compound, the aqueous dispersed
polymeric composition can include a chain extender. A chain extender is used herein
to build the molecular weight of the polyurethane prepolymer by reaction of the
chain extender with the isocyanate functionality in the polyurethane prepolymer,
i.e., chain extend, the polyurethane prepolymer. A suitable chain extender is
typically a low equivalent weight active hydrogen containing compound, having
about 2 or more active hydrogen groups per molecule. The active hydrogen groups
can be hydroxyl, mercaptyl, or amino groups. An amine chain extender can be
blocked, encapsulated, or otherwise rendered less reactive. Other materials,
particularly water, can function to extend chain length and so are chain extenders
for purposes of the present invention. Polyamines are preferred chain extenders. It
is particularly preferred that the chain extender be selected from the group
consisting of amine terminated polyethers such as, for example, Jeffamine D400
from Huntsman Chemical Company, amino ethyl piperazine, 2-methyl piperazine,
1,5-diamino-3-methyl-pentane, isophorone diamine, ethylene diamine, diethylene
triamine, triethylene tetramine, triethylene pentamine, ethanol amine, lysine in any
of its stereoisomeric forms and salts thereof, hexane diamine, hydrazine and
piperazine. In the practice of the present invention, the chain extender is often used
as a solution of chain extender in water. “ 6,743,844
“A chain extender is also preferably present in the polyol composition. For purposes
of this invention, a chain extender is a material other than the hydroxymethylcontaining polyester polyol and the additional high equivalent weight polyols
discussed above, having two isocyanate-reactive groups/molecule and an
equivalent weight per isocyanate-reactive group of from about 30 to 150. Chain
extenders having two hydroxyl groups are preferred. Examples of suitable chain
extenders include ethylene glycol, diethylene glycol, triethylene glycol, propylene
glycol, dipropylene glycol, tripropylene glycol, 1,4-dimethylolcyclohexane,
diethyltoluene diamine, 1,4-butane diol, 1,6-hexane diol, 1,3-propane diol, amineterminated polyethers such as Jeffamine D-400 (from Huntsman Chemical
Company), amino ethyl piperazine, 2-methyl piperazine, 1,5-diamino-3-methylpentane, isophorone diamine, ethylene diamine, hexane diamine, hydrazine,
piperazine, mixtures thereof and the like. Amine chain extenders can be blocked,
encapsulated, or otherwise rendered less reactive. Chain extenders advantageously
constitute up to about 20%, especially up to about 15% of the combined weight of
all isocyanate-reactive materials.” 7,794,814
“Preferred chain extenders include glycols and glycol ethers such as: ethylene
glycol; 1,4-butane diol; 1,6-hexamethylene glycol; dipropylene glycol; tripropylene
glycol; diethylene glycol; triethylene glycol; cyclohexanedimethanol; the diverse
bisphenols; like compounds and mixtures thereof. Suitable amine chain extenders
include: methylene bis(o-chloroaniline); NaCl-blocked methylene dianiline;
diethyltoluenediamine; like compounds, and mixtures thereof.” Examples used
diethylene glycol or dipropylene glycol. 6,096,401
Cross-linkers
“It is also within the scope of the invention to include a crosslinker in the polyol
composition. A crosslinker, for purposes of this invention, is a compound having
three or more isocyanate reactive groups and an equivalent weight per isocyanatereactive group of 150 or less. However, the use of crosslinkers is generally
discouraged because their use tends to increase edge curl. Therefore, crosslinkers
are most preferably eliminated or used in small quantities. The isocyanate-reactive
groups may be hydroxyl, primary amine or secondary amine groups.” (7,794,814)
ISOCYANATES
“The iso tank contains isocyanate…. Any organic polyisocyanates, modified
polyisocyanates, isocyanate based prepolymers and mixtures thereof…. Preferably
methyl diisocyanates such as Bayer’s 142L or Dow p901 or blends of equal type.
7,638,008
“The polyisocyanate component includes at least one organic polyisocyanate, which
may be an aromatic, cycloaliphatic, or aliphatic isocyanate. Examples of suitable
polyisocyanates include m-phenylene diisocyanate, tolylene-2-4-diisocyanate,
tolylene-2-6-diisocyanate, hexamethylene-1,6-diisocyanate, tetramethylene-1,4diisocyanate, cyclohexane-1,4-diisocyanate, hexahydrotolylene diisocyanate,
naphthylene-1,5-diisocyanate, methoxyphenyl-2,4-diisocyanate, diphenylmethane4,4'-diisocyanate, 4,4'-biphenylene diisocyanate, 3,3'-dimethoxy-4,4'-biphenyl
diisocyanate, 3,3'-dimethyl-4-4'-biphenyl diisocyanate, 3,3'-dimethyldiphenyl
methane-4,4'-diisocyanate, 4,4',4''-triphenyl methane triisocyanate, a
polymethylene polyphenylisocyanate (PMDI), tolylene-2,4,6-triisocyanate and 4,4'dimethyldiphenylmethane-2,2',5,5'-tetraisocyanate. Preferably the polyisocyanate is
diphenylmethane-4,4'-diisocyanate, diphenylmethane-2,4'-diisocyanate, PMDI,
tolylene-2-4-diisocyanate, tolylene-2-6-diisocyanate or mixtures thereof.
Diphenylmethane-4,4'-diisocyanate, diphenylmethane-2,4'-diisocyanate and
mixtures thereof are generically referred to as MDI, and all can be used. Tolylene2,4-diisocyanate, tolylene-2,6-diisocyanate and mixtures thereof are generically
referred to as TDI, and all can be used.” (7,794,814)
“Polyisocyanate A is a 50/50 blend of a 2.3 functional, 32%-NCO polymeric MDI and
an MDI prepolymer (181 I.E.). 2,4'-MDI constitutes 14% of the total weight of the
polymeric MDI. The MDI prepolymer is made from dipropylene glycol, tripropylene
glycol and a pure MDI containing 2.6 weight percent of the 2,4'-isomer.
Polyisocyanate A is commercially available as Isonate.RTM.7594A isocyanate from
Dow Chemical. “ (7,794,814)
“The polyisocyanate can be aliphatic or aromatic. Aromatic polyisocyanates suitable
for use herein include: phenyl diisocyanate; 2,4-toluene diisocyanate; 2,6-toluene
diisocyanate; ditoluene diisocyanate; naphthalene 1,4-diisocyanate; 2,4'- and/or
4,4'-diphenylmethane diisocyanate (MDI); polymethylene
polyphenylenepolyisocyanates (polymeric MDI); like compounds, and mixtures
thereof. Suitable aliphatic polyisocyanates include: the hydrogenated derivatives of
suitable aromatic polyisocyanates such as 1,6-hexamethylene diisocyanate;
isophorone diisocyanate; 1,4-cyclohexyl diisocyanate; like compounds and mixtures
thereof.” Example includes Isonate 7045. (6,096,401; same in 5,908,701)
CATALYSTS
“The catalyst tank contains one or more catalysts and a small amount of water….
Catalysts suitable for use in preparing the polyurethane of the present invention
include tertiary amines, and organometallic compounds and mixtures thereof. For
example, suitable catalysts include stannous octoate, triethylenediamine, N-methyl
morpholine…. 7,638,008
“A catalyst can be used to promote the reaction between a chain extender and an
isocyanate. Suitable catalysts include tertiary amines, organometallic compounds,
similar compounds, and mixtures thereof. For example, suitable catalysts include din-butyl tin bis(mercaptoacetic acid isooctyl ester), dimethyltin dilaurate, dibutyltin
dilaurate, dibutyltin sulfide, stannous octoate, lead octoate, ferric acetylacetonate,
bismuth carboxylates, triethylenediamine, N-methyl morpholine, similar
compounds, and mixtures thereof. An amount of catalyst is advantageously
employed such that a relatively rapid cure to a tack-free state can be obtained. If an
organometallic catalyst is employed, such a cure can be obtained by using from
about 0.01 to about 0.5 parts per 100 parts of the polyurethane-forming
composition, by weight. If a tertiary amine catalyst is employed, the catalyst
preferably provides a suitable cure using from about 0.01 to about 3 parts of
tertiary amine catalyst per 100 parts of the polyurethane-forming composition, by
weight. Both an amine type catalyst and an organometallic catalyst can be employed
in combination. “ 6,743,844
“The polyurethane-forming composition also preferably contains one or more
catalysts, which promote the reaction of the polyisocyanate with the isocyanatereactive materials. Suitable catalysts include tertiary amines, organometallic
compounds, or mixtures thereof. Specific examples of these include di-n-butyl tin
bis(mercaptoacetic acid isooctyl ester), dimethyltin dilaurate, dibutyltin dilaurate,
dibutyltin diacetate, dibutyltin sulfide, stannous octoate, lead octoate, ferric
acetylacetonate, bismuth carboxylates, triethylenediamine, N-methyl morpholine,
like compounds and mixtures thereof. An amine-blocked tin (IV) catalyst, such as
those described in U.S. Pat. No. 5,491,174, can be used. An amount of catalyst is
advantageously employed such that a relatively rapid cure to a tack-free state can be
obtained, while providing enough open time that the polyurethane composition can
be dispensed and spread over the carpet back before curing. If an organometallic
catalyst is employed, such a cure can be obtained using from about 0.01 to about 0.5
parts per 100 parts of the polyurethane-forming composition, by weight. If a tertiary
amine catalyst is employed, the catalyst preferably provides a suitable cure using
from about 0.01 to about 3 parts of tertiary amine catalyst per 100 parts of the
polyurethane-forming composition, by weight. An amine type catalyst and an
organometallic catalyst can be employed in combination. “ 7,794,814
“Catalyst A is a blend of 10% of a dibutyltin diisooctylmercaptoacetate delayed
action catalyst, commercially available as Fomrez.TM. UL6 from OSI Specialties, in
Polyether Polyol B Catalyst B is a blend of 20% dibutyltin dilaurate (Dabco.TM. T12,
from Air Products and Chemicals, Inc.) in Polyether Polyol B. “ (7,794,814)
“Suitable catalysts include tertiary amines, and organometallic compounds, like
compounds and mixtures thereof. For example, suitable catalysts include di-n-butyl
tin bis(mercaptoacetic acid isooctyl ester), dimethyltin dilaurate, dibutyltin
dilaurate, dibutyltin sulfide, stannous octoate, lead octoate, ferric acetylacetonate,
bismuth carboxylates, triethylenediamine, N-methyl morpholine, like compounds
and mixtures thereof.” Example includes dibutyltin sulfide. (6,096,401)
Example %s:
Component
Example 1
Example 2
45 pbw (12%)
0
40 (11%)
0
15 (4%)
Comp Sample
B
0 pbw
25 (9%)
0
64 (20%)
5.5 (2%)
30 pbw (8%)
0
55 (15%)
15 (4%)
Comp Sample
B
0 pbw
30 (8%)
57.8 (16%)
12.2 (3%)
HMPP A (Soy and
Soy Oil Polyol A
Polyether polyol A
Polyether polyol B
Dipropylene
glycol
Tripropylene
glycol
Carlcium
Carbonate A
Catalyst A
Organotin
Catalyst A
Organotin
Catalyst B
Polyisocyanate A
Water content
(est.)
Vegetable oilbased polyol as %
of reactants
Vegetable oilbased polyol as %
of formulation
% Polyols from
Vegetable oils
% Filler
FROM Dow Patent
7,794,814
0
5.5 (2%)
-
-
205 (56%)
160 (52%)
205 (56%)
205 (56%)
0.45 (0.1%)
0.60 (0.2%)
0.45 (0.1%)
-
0.45 (0.1%)
-
0
0.60 (0.2%)
-
-
60.1 (16%)
-
48.75 (16%)
-
59.5 (16%)
0.06
58.18 (16%)
0.06
-
-
18.76%
18.91%
-
-
8.22%
8.25%
28%
16.8%
-
-
56.1%
51.8%
56.16%
56.37%