Note: Descriptions are shown in the official language in which they were submitted.
CA 02208602 2005-02-08
60557-5540
INTUMESCENT PUTTY
Field of the Invention
This invention relates too intumescent putty for
use in an opening as a firestop material to deter the spread
of flame, smoke, and vapors during a fire.
Description of Related Art
Firestop products are u:~ed to reduce or eliminate
the chimney effect at through-penetrations. Characteristics
of firestop materials suitable for typical commercial uses
include the ability to expand and to char. Further, the
charred material preferably has sufficient strength to
withstand a hose stream test.
An industry recognized fire endurance test used to
evaluate firestop materials is the American Society of
Testing Materials' test identified as "ASTM E-814-83". This
test includes subjecting the charred material to a stream of
water from a fire hose.
US-A-5,025,058 describes a flame-resistant non-
drying putty composition where the chief ingredients are an
unvulcanized rubber, intumescent material such as a metal
hydrate and liquid chloroprene as a liquid polymer resin.
JP-A-57-209980 relates to a putty composition
containing a liquid polychloropren.e as a key ingredient,
hydrated alumina as intumescent material and silicone
rubber.
GB-A-2 092 599 describes a fireproof putty
composition containing liquid chloroprene and a specific
unvulcanized chloroprene rubber with intumescent material.
1
CA 02208602 2005-02-08
60557-5540
Summary of the Invention
According to one aspect of the present invention,
there is provided an intumescent putty that remains soft and.
handleable for at least a month under ambient conditions
comprising a blend of intumescent material, vulcanized
rubber, and unvulcanized rubber, said vulcanized rubber and
said unvulcanized rubber together providing said putty with
a softness value of at least 4 mm,, wherein measurement of
the softness of the putty is described in ASTM D-1403-91,
containing less than 0.25 percent by weight halogen, said
putty containing less than 0.25 percent by weight water
other than bound water, wherein bound water is water that
does not come off until the putty is heated to at
least 100°C, and said putty containing less than 0.25
percent by weight rubber curing agent, based on the total
weight of the putty.
The present invention provides a non-aqueous,
indefinitely conformable, halogen-free, intumescent putty
comprising a blend of intumescent material, rubber, and
unvulcanized rubber, the rubber and unvulcanized rubber
together provide the putty with a softness value of at
least 4 mm (preferably, at least 9:.5 mm; more preferably at
least 5 mm; and even more preferably, at least 6 mm).
Further, the putty is
la
CA 02208602 1997-06-23
WO 96/20987 PCT/ITS95116633
essentially free (i.e., contains less than 0.25 percent
by weight) of a rubber curing agent.
In another aspect, the present invention provides
a non-aqueous, indefinitely conformable, halogen-free,
intumescent putty comprising a blend of intumescent
to material, rubber, and at least 5 percent (preferably, ,
at least 10 percent: more preferably, at least 15
percent) by weight unvulcanized rubber, based on the
total weight of the putty. The putty has a softness
value of at least 4 mm (preferably, at least 4.5 mm~
more preferably at least 5 mm~ and even more
preferably, at least 6 mm) and is essentially free of a
rubber curing agent.
Preferably, the rubber is selected from the group
consisting of natural rubber, butyl rubbers,
2o polybutadiene rubbers, synthetic isoprene rubbers,
styrene butadiene rubbers, ethylene acrylic rubbers,
nitrile rubbers, urethane rubbers, ethylene vinyl
acetate rubbers, and combinations thereof. Preferably,
the unvulcanized rubber is selected from the group
consisting of unvulcanized natural rubber, unvulcanized
butyl rubbers, unvulcanized polybutadiene rubbers,
unvulcanized synthetic isoprene rubbers, unvulcanized
styrene butadiene rubbers, unvulcanized ethylene
acrylic rubbers, unvulcanized nitrile rubbers,
unvulcanized urethane rubbers, unvulcanized ethylene
vinyl acetate rubbers, and combinations thereof.
Optionally, the intumescent putty according to the
invention further comprises one or more of a
plasticizes, a flame retardant, a char former, a
filler, a colorant, a wax, an antioxidant, and/or an '
antiozonant.
2
CA 02208602 1997-06-23
WO 96/20987 PCT/ITS95116633
In this application:
"putty" refers to a cohesive, moldable material
that does not substantially flow at ambient
temperatures (typically temperatures in the range from
about 0°C to about 50°C) ;
- l0 "indefinitely conformable" means the putty remains
soft and handleable for at least one month,
(preferably, one year; more preferably, at least five
years; even more preferably, at least ten years; and
most preferably, at least twenty years) under ambient
temperatures (typically temperatures in the range from
about 0°C to about 50°C) ;
"halogen-free" means essentially free of halogens
(i.e., contains less than 0.25 percent (preferably,
less than 0.1 percent; more preferably, less than 0.01
percent) by weight halogen calculated on an elemental
basis as C1, F, etc., based on the total weight of the
putty;
"non-aqueous" means essentially free of (i.e.,
contains less than 0.25 percent by weight) water, other
than bound water, wherein bound water is water that
does not come off until the material is heated to at
least 100°C (preferably, at least 150°C, more
preferably, at least 250°C) ;
"intumescent" refers to a material which expands
3o upon heating above about 100°C, although the temperature
at which a particular intumescent material intumesces
is dependent on the composition of that material;
"intumescent putty" refers to a putty that
intumeces to at least two times (preferably at least
three times) its (original) unexpanded volume (i.e.,
" its volume prior to intumescing);
3
CA 02208602 1997-06-23
WO 96120987 PCT/US95/16633
"rubber" refers to materials including natural
rubber and synthetic rubbers (or synthetic elastomers)
that exhibit stretch and recovery after being cured (or
vulcanized):
"unvulcanized rubber" refers to the precursor
to material that when vulcanized (or cured) provides
rubber:
"rubber curing agent" refers to a vulcanizing,
curing, or crosslinking agent such as sulfur, amines,
or difunctional acids, divinyl benzene, or a free
radical initiator such as dicumyl peroxide which when
compounded and activated with the unvulcanized rubber
produces rubber wherein the cure conditions and
concentration of agents) and/or free radical
initiators) determine the extent of vulcanization
"softness value" is a measure of the softness of
the putty and is determined as described below under
the heading "Softness Value Measurement":
"softness" refers to the ability of the putty to
be shaped or molded by hand with ease:
"moldable" means the putty is conformable (e. g.,
the putty can be wrapped around a pipe);
"cohesion" means that the putty adheres to itself and,
once molded, retains its shape until acted upon by an
external force:
"adhesion" refers to the ability of the putty to
adhere to a dissimilar material (i.e., the putty has
sufficient tack to stay in place when molded around
construction components (e. g., concrete, dry wall,
metal, plastic, and cables)), but not so much tack that
it adheres to skin: "
"reusable" refers to the ability of the putty
installed in one location to be removed and installed "
in another location, without substantially affecting
4
CA 02208602 1997-06-23
WO 96120987 PCT/US95116633
the intumescence, softness, and flame retardance
properties of the putty and
"char strength" is a measure of the strength of
the expanded carbonaceous residue ("char") formed from
the putty after exposure to temperatures above about
l0 350°C for about 15 minutes.
Intumescent putties according to the present
invention typically are reuseable, exhibit good
adhesion properties, and can be used to restore
acceptable fire ratings of floors and walls after
penetrations (or openings) are made in them. Such
penetrations are made, for example, to accommodate the
passage of cables, conduits, metal and plastic pipe,
and telephone installations. If the penetrations or
openings around the installations that pass through the
2o penetrations are not adequately sealed, flame, smoke,
and/or water may pass there through and extend the
destruction of a fire and/or water damage.
Description of Preferred Embodiments
The intumescent putty according to the present
invention remains in a soft, pliable, and unexpended
condition until it is exposed to heat at temperatures
in excess of about 100°C (212°F). When heated above
about 350°C (662°F), the putty readily intumesces
typically to about three times its original volume, and
begins to form char that further enhances the putty's
flame retardant characteristics. The putty seals voids
in through-penetrations caused by burning and/or
melting materials, effectively preventing the passage
of flame, smoke, vapors, and water from one location
(e. g., a room or floor) to another.
5
CA 02208602 1997-06-23
WO 96120987 PCT/ITS95/16633
In another aspect, the putty according to the
present invention typically resists flow when subjected
to heat. This resistance to flow allows the putty to
remain intact at elevated temperatures (i.e.,
temperatures normally encountered during combustion).
to If the temperature rises sufficiently (i.e., under the .
conditions of a fire) the putty may char as well as
intumesce.
The general effect of the amounts of materials
used to prepare a particular putty according to the
present invention on properties such as softness and
resistance to flow should be apparent to one skilled in
the art after review of the disclosure herein.
Preferably, the putty comprises in the range from
about 5 to about 50 percent (preferably, about 15 to
about 30 percent) by weight rubber and unvulcanized
rubber, based on the total weight of the putty.
In another aspect, the putty preferably comprises
in the range from about 10 to about 50 percent
(preferably, about 10 to about 25 percent) by weight
unvulcanized rubber, based on the total weight of the
putty.
In another aspect, the putty preferably comprises
in the range from about 1 to about 15 percent
(preferably, about 2 to about 8 percent) by weight
rubber, based on the total weight of the putty.
The putty can be made by, and is typically made by
a method that includes compounding rubber and
unvulcanized rubber. Although not wanting to be bound
by theory, it is believed that the rubber and the
unvulcanized rubber provide a balance between softness
and conformability and flow resistance at elevated
temperatures.
6
CA 02208602 2005-02-08
60557-5540
s A preferred rubber is a styrene butadiene rubber,
characterized by the manufacturer as having a high
degree of crosslinking (commercially available under
TM
the trade designation "POLYSAR S1018" from Polysar
Rubber Div. of Miles, Inc.). A styrene butadiene
1o rubber, characterized by the manufacturer as having a
low Mooney viscosity (commercially available from
Ameripol Synpol Co., a Division of Uniroyal GoodrYch
Tire Co. of Akron, OH) is the preferred unvulcanized
rubber. _
is In a preferred embodiment two types of rubbers
are used together with an unvulcanized rubber. The
first rubber is preferably a styrene butadiene rubber,
characterized by the manufacturer as having a high
degree of crosslinking ("POLYSAR 51018"j. The amount
20 of this rubber preferably ranges from about 10 to about
40 percent by weight of the total rubber and
unvulcanized rubber content of the putty. The second
rubber is preferably a butyl rubber characterized by
the manufacturer as "moderately" crossliriked"
2s (commercially available under the trade designation
TM
"POLYSAR BUTYL XL 68102" from Polysar Rubber Div. of
Miles, Inc. of Akron, OH). This second rubber is'
believed to provide a desirable level of stretch.
Preferably, the amount of this rubber ranges from about
30 1 percent by weight to about 5 percent (more
preferably, about 1 to about 2 percent) by weight of
the total rubber and unvulcanized rubber content of the
putty. If the amount of moderately crosslinked rubber
is greater than about 5 percent by weight, the material
35 tends to be undesirably tacky, and may be difficult to
install in some applications. At levels of less than 1
percent by weight, typically no benefit in stretch is
observed from its addition to the formulation.
7
CA 02208602 1997-06-23
WO 96/20987 PCTJUS9~/16633
Suitable intumescent materials include hydrated
alkali metal silicates (e. g., sodium silicate, lithium
silicate, and potassium silicate with bound water),
expandable graphite, unexpanded vermiculite, and
organic intumescent compounds such as melamine (i.e.,
l0 2, 4, 6-triamino-1, 3, 5-triazine), azocarbonamide, and ~
benzene sulfonyl hydrazide which decompose to give off
gases. The amount of intumescent material in the
formulation varies depending on the type of intumescent
chosen.
The preferred intumescent material is a granular
hydrated alkali metal silicate intumescent composition
comprising a mixture of bound water; at least one
alkali metal silicate having the formula MZO:xSi02
(e. g., sodium silicate, lithium silicate, and potassium
silicate), wherein M is an alkali metal and x ranges
from about 1.5 to about 4, and at least one oxy boron
compound selected from the group consisting of boric
acid and borate salts of group I and II elements (e. g.,
metaborate, tetraborate, perborate, polyborate
radicals, boric acid, colemanite, calcium metaborate,
magnesium borate, and zinc borate) (see, e.g., U.S.
Pat. No. 4,521,333 (Graham, et al.).
Preferably, the molar ratio of boron (present in
the oxy boron compound) to M is between about 0.2 and
about 0.9. The water preferably comprises about 5 to
15 percent by weight of the mixture of water, oxy boron
compound(s), and alkali metal silicate(s).
Preferably, the intumescent material is added in
particulate form to the rubber and unvulcanized rubber
in an amount sufficient to allow the putty to pass the
fire test described below under the heading "Flame
Through Test," but not so much that it makes the putty
non-pliable, or that it adversely affects the char that
8
CA 02208602 2005-02-08
60557-5540
forms in a fire such that heated putty does not pass the
Fire Hose Stream Test described below.
Typically, the amount o.E intumescent material
(e. g. hydrated alkali metal silicate) used ranges from about
50 to about 200 percent (preferab:Ly about 100 to about 140
percent) by weight of the total vulcanized rubber and
unvulcanized rubber content of thES putty. In another
aspect, the hydrated alkali metal silicate preferable is
present in the range from about 5 to about 45 percent by
weight, based on the total weight of the putty.
The hydrated alkali metal silicate particles
typically range in size from about 75 micrometers to about
500 micrometers.
A silicate intumescent material such as hydrated
sodium silicate is preferably used together with a silicate
fluxing agent such as boric oxide. Such fluxing agents are
used to stabilize the char formed when the putty is
subjected to heat. A preferred silicate fluxing agent is
anhydrous boric oxide (B203) , commf~rcially available from
U.S. Borax of Valencia, CA. Boric: oxide can function as
both a flame retardant and a silicate fluxing agent.
If the intumescent material is intercalated
graphite, the putty preferably comprises in the range from
about 5 to about 30 percent by weight intumescent material,
based on the total weight of the putty.
It is within the scope of the present invention to
use combinations of intumescent material (e. g., to use both
hydrated alkali metal silicate and intercalated graphite).
Preferably, a sufficient amount of plasticizer is
included in the putty to obtain the desired level of
9
CA 02208602 2005-02-08
60557-5540
softness and moldability. Plasticizers are compounds that
increase the flexibility of a material and facilitate
processing. Suitable plasticizers include
9a
CA 02208602 2005-02-08
60557-5540
s aromatic oils, naphthenic oils, mineral oil, waxes,
phthalate esters such as dioctyl phthalate (DOP) or
dibutyl phthalate, and phosphate esters such as 2-
ethylhexyl diphenyl phosphate (commercially available,
for example, under the trade designation '"SANITIZER
141"' from Monsanto of St. Louis, MO), isodecyl diphenyl
phosphate, or triaryl phosphate ester (commercially
available, for example, under the trade designation
TM
"SANITIZ~R 143"' from Monsanto). A preferred
plasticizes is isobutylene/butene copolymer liquid
1s commercially available under the trade designation
°INDOPOL H100" from Amoco Oil Co. of Chicago, IL.
Suitable waxes include petrolatum (commercially
available, for example, under the trade designations'
"6916 WA7CM~ and '"PAXWAX 5324~ from National Wax Division
TM
of Dussek Campbell, Inc., Skokie, ~ IL: "'SR-172"' from .C.
TM
P. Hall Co. of Chicago, IL: and '"P~TROLATUM RP8"' from
Witco Chemical Corp. of New York, NY).
Typically, the plasticizes is present in the range
from about 30 to about 50 percent by weight
(preferably, from about 35 to about 45 percent by
weight, based on the total rubber and unvulcanized
rubber content of the putty. In another aspect, the
plasticizes typically is present, in the range from
about 2 to about 25 percent by weight, based on the .
3o total weight of the putty.
Other optional ingredients that can be included in
the putty formulation include flame retardants, char
formers (e.g., char forming resins), fillers,
colorants, antioxidants, and antiozonants.
3s Useful flame retardants include boric oxide: zinc
borate: alumina trihydrate: nitrogen phosphates such as
ethylene diamine phosphate (commercially available, for
TM
example, under the trade designation '~AMGUARD ~DiAP"
CA 02208602 2005-02-08
~ 60557-5540
from Allright & Wilson Ltd. of Richmond, VA),
dimelamine phosphate (commercially available, for
example, under the trade designation ~AMGUARD ND"' from
Allright & Wilson Ltd.), melamine phosphate
(commercially available, for example, under the trade
TM
to designation '"AMGUARD NH"' from Allright 6 Wilson Ltd. ) ,
ammonium polyphosphate (commercially available, for
TM
example, under the trade designations "PHOS CHEK'P30"'
TM
and "PROS CHEK P40~ from Monsan~o)~ and a blend of bis
melaminium pentate and polyhedric oxide (commercially
available, for example, under the trade designation
TM
"CHAR GUARD 329" from Great Lakes Chemical Corp. of
West Lafayette, IN).
Useful char forming resins include epoxy resins,
phenolic resins, polycarboimide resins, urea-
2o fonaaldehyde resins, and melamine-formaldehyde resins.
The general term "phenolic" refers to phenol-
formaldehyde resins as well as resins comprising other
phenol-derived compounds and formaldehydes. A
preferred char forming resin is an epoxy resin
commercially available under the trade designation
1M
"SCOTCHCRST SR 265"' from the 3M Company of St. Paul,
MN.
Fillers can used to adjust the hardness of the
putty (i.e., fillers typically make the putty stiffer
or harder), act as reinforcement, or reduce cost.
Fillers include fumed silica, clay, fly ash, colorants,
perlite, venaiculite, inorganic fibers (e. g., glass
fibers and mineral fibers), and organic fibers.
Melamine, which as discussed above is an organic
intumescent material, is also useful as a filler to
adjust the tack of the putty. A preferred filler is
milled glass fiber (commercially available as "731ED
TM
FIBERGLAS" from Owens-Corning Fiberglas Corp. of
11
CA 02208602 2005-02-08
~ 60557-5540
S Toledo, OH), or chopped fiberglass fibers (commercially
available, for example, under the trade designation
~799AB"' from Owens-Coming Fiberglas Corp. of Toledo,
OH ) .
Colorants ( a . g . , iron oxide such as FeaO, or FeZ03 D
1o are useful for product' identification.
Antioxidants are compounds added to rubbers to
protect the rubber against degradation by oxygen. Such
compounds are typically comprised of aromatic amines.
Antiozonants may be used to protect the putty from
15 degradation by ozone. Some compounds may perform as
antioxidants as well as antiozonants. A preferred
antioxidant is thiodiethylene bis-(3,5-di-tert-butyl-9-
hydroxy) hydrocinnamate (commercially available under
r", .
the trade designation "IRGANOX 1035" from the Additives
2o Division of Ciba-Geigy Corp. of Hawthorne, NY).
A preferred antiozonant is a mixture of diaryl p-
phenylene diamines (commercially available under the
trade designation "WINGSTAY 100" from Goodyear
Chemicals Division of Goodyear Tire and Rubber Co. of
25 Akron, OH) .
The putty can be made, by combining the ingredients
used to make the putty using conventional techniques
known in the art. Typically, the putty is made by
mixing the various ingredients using a mogul mixer
3o equipped with circulating cooling water. The cooling
water minimizes the build up of heat resulting from
exothermic reaction of the ingredients and/or the
action of mixing blades, therby preventing the
intumescent material from prematurely intumescing.
3s Preferably, the rubber and unvulcanized rubber are
added to the mixing chamber and mixed until thoroughly
blended. Any fillers, silicate fluxing agents, char
forming resins. waxes, colorants, flame retardant,
lx
CA 02208602 1997-06-23
WO 96/20987 PCT/CTS95/16633
melamine, antioxidants, and antiozonants are then added
while the mixing operation continues. Plasticizer is
typically added and then mixed in for a few minutes.
The last ingredient added is usually the intumescent
material. The putty is typically mixed until
l0 homogeneous and smooth (i.e., not lumpy). After
mixing, the putty is ready to use.
For many firestop applications, the putty is
typically extruded into sheets or pads (usually about
0.635 cm (0.25 inch thick). The sheets or pads are cut
to provide the desired size or shape for a particular
application. For some applications, the putty is
formed into sticks or rope.
Objects and advantages of this invention are
further illustrated by the following examples, but the
particular materials and amounts thereof recited in
these examples, as well as other conditions and
details, should not be construed to unduly limit this
invention. All parts and percentages are by weight
unless otherwise indicated.
Softness Value Measurement
The softness of the putty is determined using a
penetrometer (available as Model 73510 from Precision
Instruments of Chicago, IL). Measurement of the
3o softness of the putty involves dropping a weighted
cone-shaped object into the putty, and then measuring
the distance the object penetrates the putty. The test
procedure is described in ASTM D-1403-91, which is
entitled "Standard Test Methods for Cone Penetration of
Lubricating Grease Using One-Quarter and One-Half Scale
Cone Equipment," wherein the penetration measurements
were made using a stainless steel, quarter scale cone
as specified in the ASTM test method.
13
CA 02208602 1997-06-23
WO 96/20987 PCT/US95/16633
Specifically, the softness value of the putty was
determined by packing the putty into a tube open at
each end such that the putty was flush with both ends
of the tube. The packed cylinder was allowed to stand ,
at room temperature (about 23°C) for a minimum of 12
to hours before the softness value was determined. -
The cone and the shaft connected thereto weighed
9.38_+0.025 grams. An additional 150 grams was added to
the top of the shaft. The tip of the cone-shaped
object was placed so it just touched the surface of the
putty packed into cylinder. For each measurement, the
shaft was released and the cone allowed to sink into
the putty for 5 seconds. The distance the cone sank
into the putty during the 5 seconds was recorded. The
softness values reported for Examples 1, 2, and 20 are
2o based on an average of 2 measurements. The softness
values reported for Examples 3-19 are based on an
average of 10 measurements.
Putty Flow Measurement
Putty was packed into a tube (2.5 cm diameters 2.5
cm long) open at each end such that it was flush with
both ends of the tube. The packed tube was then laid
on its curved side in an oven at 200°C for 30 minutes.
The amount of flow that occurred during the 30 minutes
of heating was determined visually to be excellent
(i.e., no flow), very good (i.e., slight flow), good
(i.e., some flow, but material did not flow onto the
surface on which the tube was placed in the oven),
fair, or very bad (i.e., material flowed freely out of
the tube and onto the surface on which the tube was
placed in the oven).
14
CA 02208602 2005-02-08
60557-5540
Flame Through Test
The Flame Through Test follows the procedure set
forth in ASTM'(American Society for Testing Materials)
Test '"E 819-83,"' entitled "Standard Test Method for
Fire Tests of Through-Penetration Fire Stops".
to This test is used to
evaluate the use of putty in a through-penetration tire
application.
For this test, a poured concrete slab, 11.4 cm
.(4.5 in) thick and approximately 30.5 cm (3 ft)
square, was prepared. Four 10.2 cm (9 in) diameter
circular openings were made in the slab. The openings
were evenly spaced. A 2.5 cm (1 in)) thick mineral
fiber insulation material (commercially available under
the trade designation. "USG 114 FIRE SAFING" from US .
2o Gypsum of Chicago, IL) was firmly packed into each .
opening in the slab. The mineral fiber was recessed
about 2.5 cm from the top surface of the concrete. The
putty was packed into the opening flush with the top
surface of the concrete. The thickness 'of the putty
was about 2.5 cm. The concrete slab was placed on the
top of a gas-fired furnace (commercially available from
Armil C.F.S. of South Iiolland, IL). The mineral fibers
faced the heat source (flame) of the furnace.
The time and temperature parameters outlined in
Figure 1 of ASTM E 819-B3 were followed for the test.
The test was run for 3 hours. unless flame through
occurred. Flame through is indicated by flames coming
through the opening to the "cold" side of the concrete
slab. If there is flame through in less than 3 hours,
then the material tested is deemed to have failed the
test. If the opening remained sealed for the.3 hours,
then the fire stop is given a passing designation
(referred in ASTM E 819-83 as having an "F" rating).
CA 02208602 1997-06-23
WO 96/20987 PCT/US95/16633
Fire Hose Stream Test
If a fire stop employing the putty of one of the
examples passed the "Flame Through Test," then the
following test, which is described in ASTM E 814-83,
l0 was conducted.
Immediately after the "Flame Through Test," the
slab was removed from the furnace and placed vertically
in a metal stand. From a distance of 6.1 meters (20
ft), a stream of water was propelled in a sweeping
motion against the material in the opening of the
concrete slab at a pressure of 0.21 MPa (30 lbs/in2 ).
To pass this test, the material sealing the through-
penetration, after having been subjected to the heat
from a fire thus producing a char, had to withstand the
2o hose stream and continue to seal the pipe for a period
of 1.5 seconds per 0.09 square meter,(i.e., 1.5 seconds
per square foot) of test structure. For example, a
0.84 m2 (9 ft2) assembly must withstand a hose stream
for 13.5 seconds.
16
CA 02208602 2005-02-08
~ 60557-5540
The ingredients used for the examples are listed
in Table 1, below.
Table 1
Iags~edibat Trades Desigiution loaroa of
Ingradieat
Uavulcaaised styrene'"AMERIP01. SYNPOb Ameripol Syapol
butadiene rubber 8107'x" Co. Division
bf
Uairoyal
Goodrich Tire
' Co., Akso~n,
OH
Styrene butadiene '"POLYSAR S lOlB"''"~Polysar Rubber
rubber ~ Division of
'
Milan,
Pittsburgh,
PA
Moderately "POLYSAR BUTYL Xh Polysar Rubber
~
crosslinked butyl 68102'T~ Division of
rubbez Idiles,
Pittaburgh,
PA
Mixture of diaryl '"wINGSTAY 100'T~ Goodyear .
p-
pheaylene diamine Chemicals
Division of
Goodyear Tise
and R~bbes Co,.,
Jv)cron,
Thiodiethyleae bin-"IRGANOX 1035' .W dditivea
(3,5-di-tert-butyl-~- Division of
hydroxy) Ciba-Geigy
hydrocianaaate Corp.,
Narrthorne,
NY
Fumed silica "CAB-O-SIL M-5" ~ Cabot Corp.,
.
Tuscola, II.
Epoxy resin po~rder'"SCOTCHCAST SR-265'The 3M Company,
St. Paul, 1~1
Pos~dered iron oxide"IRON OXIDE BF-95"' Bailey
(Fe=0>> Fagineers, Iae.,
Fairfield, AL
Soroa trioxide powder"ANHYDROUS BORIC tl.S. Borax,
ACID"' ~" Valencia, G
Melamine po~dtr "AFRO MEIJ~MINE" Cytec
(-60 ~
mesh) Industries,
west
Peterson, NJ
Milled glass '"?3~ED FIBERGLASS Oweas-Corafag,
filaments 1/e""""~ Fiberglas Corp.,
Toledo, OH
17
CA 02208602 2005-02-08
60557-5540
Table 1 Continued
Milled glaaa . "MFX-ll- 8 IN Phoenix
filaments Fiberglas, Inc.,
oakville,
Ontario, Canadi
Chopped fiberglass "799A8"'r' . Ovens-Corning
'
fibers, 1.25.cm Fiberglas Corp.,
(0.5
inch) lon Toledo, OH
Isobutylene butane '"INDOPOL H-~100"'~Amoco Chemical
c of r 1i d Co., Chica ,
Ib
Copolyaer of isobutyl'"POLYSAR BUTYL. Polysar Rubber
301"'
and isoprene Division of
Miles
Petrolatum '"6916 i~A7C"~" Nation: Wax
.
Division of
Dussek Campbell,
Ine., Skokie,
IL
Petrolatum '"PA)CWAX 532"'"" Natioat Wax
Division of
Dussek Campbell.
Inc.
Petrolatum "PEN~~ ~~"' ~" Peareco
zproducts C.;
Peateco
Division, ICarns
Cit , PA
Petrolatum '"PETROLATUM RP$'"7"'Witco Chemical
Corp., Nsw York,
NY
Blend of bis "CHARGUARD 32g'"" Grsat Lakes
melaminium pentate Chemical Corp.,
and polyhedric oxide West Lafayette,
(flame retardant)
Intercalated graphite"GRAPHITE TG 326"'x"UGR Carbon Co.,
,
flake ~ Inc., Danbury,
Granulated hydrated'"EXPANTROL ~811"'~The 3M Company
sodium silicate
Granulated hydrated"EXPANTROL 2"''". The 3M Company
sodium silicate
Hydrated zinc borate"FIREBRAKE Z8 FINE""U.S. Horax
18
i n. 1 II~.n~ I
CA 02208602 2005-02-08
a 60557-5540
Examples 1 and 2
The ingredients for Examples 1 and 2 are listed in
Table 2, below.
Table 2
llmonn! of Ingredients,
pgit~
Zagrediea! Example 1 P~cample
2
Unvulcanized atysene 76.50 76.50
butadiene
rubber ("AI~RIPOI. SYNPOI.
B107"')1""
Styrene butadiene rubber 20.00 20.00
("POhYSAR S 1018")1""
Moderately croaslinked yl 3.50 3.50
but
rubber ('POLYSAR XI. ~"
68102"'~
Mixture of diaryl p-phenylene 2.00 2.00
diamine ("NINGSTAY 100")s
Thiodiethylene bin-(3,5-di-tert- 2.00 2.00
butyl-4-hydroxy) hydrocinnamate
('"IRG~1NOX 1035")1'"
Fumed silica ('"CA8-O-SII. 13.00 13:00
M 5"'JTM
Epoxy resin powder ("SCOTCHCAST 15.00 15.00
8R 265")1""
Powdered iron oxide 5.00 5.00
(FeZO~)
("IRON OXIDE BF 95"')TM
Melamine powder ('"HERO 50.00 75.00
,
MELAMINE"' ) r"'
Boron Oxide 10.00 X0.00
(Anh roua)
Milled glass filaments 30.00 30.00
('"731ED
FI BERGIJ4SS" f"
Isobutylene butane copolysier X0.00 50.00
1i id ("INDOPOh H 100")TM
Petrolatum ('"6916 WAX"')' 60.00 60.00
Granulated hydrated.spdium 120.00
silicate ('"EXPANTROI.
481"')1'"
Intercalated graphite ?0.00
flake
("GRAPHITE TG 326"')r'"
* Parts per hundred based on the total rubber sad
unvulcanized rubber content of the putty.
The ingredients for each example were compounded
,15 using an internal mixer (Prep Mixer, Part # 02-2~-000,
350/420 cm' capacity: available from C. W. Hrabender
Instruments, Inc. of South Hackensack, NJ) equipped
with sigma mixing blades. The mixer was powered.by a
19
CA 02208602 2005-02-08
~ 60557-5540
3 Plasticorder, Model DR-2071, electronic torque
rheometer with a Model FE-2000 interface (each of which
are available from C. W. Brabender Instruments, Inc.).
The unvulcanized rubber ("Ameripol Synpol 8107")
and rubbers ("Polysar S 1018" and "POLYSAR BUTYL XL
TM
68102").were added to the mixing chamber of the mixer
and then blended for about 6 minutes at about 60 rpm.
The speed of the mixing blades was then reduced to 90
rpm, and the antioxidant (i.e., thiodiethylene bis-
(3,5-di-tert-butyl-9-hydroxy) hydrocinnamate),
1s antiozonant (i.e., mixture o;f diaryl p-phenylene
diamine), fumed silica, epoxy resin, iron oxide, boric
oxide, melamine, and milled~glass fibers were added
while mixing continued. The ingredients were mixed far
about 3 minutes, after which the mixing speed was '
ZO increased to about 60 rpm. The plasticizer ("INDOPOL
H-100"') was then added, and mixing continued for about
13 minutes. The petrolatum was then slowly added and
mixed in for about 5 minutes. Finally, the hydrated
sodium silicate was added and mixed in for about 5
25 minutes. The batch sizes for Examples 1 and 2 were
about 977 grams and about 462 grams, respectively.
The softness value of the putty was determined as-
described above under the heading "Softness Value
Measurement."' The softness value of both Examples 1
30 and 2 was 5.5 mm.
The char strength and expansion ratio (i~.e., the
char volume divided by the initial volume) of each
example was determined as follows. First, a portion of
each putty was pressed to a thickness of about 0.635 cm
33 (1/4"). Next, a 2.5 cm (1 inch) diameter disc was die
cut from each (pressed) sheet:.
The initial volume of each disc was determined by
weighing the disc, coating the disc with wax by dipping
CA 02208602 1997-06-23
R'O 96/20987 PCT/US95I16633
it in molten paraffin wax, submerging and weighing the
(coated) disc in deionized water, and then calculating
the volume using the following equation:
dry weight - submerged weight
l0 volume =
- (Equation 1)
density of water
The disc was then placed in a muffle furnace at about
350°C for about 15 minutes to intumesce and char. The
resulting charred, expanded disc was then weighed,
coated with wax, and then submerged and weighed in
deionized water. The volume of the charred, expanded
disc was calculated using Equation 1 (above).
The expansion ratio was calculated using the
following equation:
volume of charred, expanded disc
volume =
(Equation 2 )
volume of initial (uncharred) disc
The expansion ratios of Examples 1 and 2, based on
an average of two determinations, were 2.84 and 5.22,
respectively. The flow characteristics of the Example
1 and 2 putties were both excellent.
Examples 1 and 2 passed both the "Flame Through
Test" and the "Fire Hose Stream Test."
Examples 3-10
The ingredients for Examples 3-10 are listed in
Table 3, below.
21
CA 02208602 2005-02-08
60557-5540
0 0 0 0 0 0 0 0
o N o u~ 0 0 0 0 0
.-1 ~f1 Irl N N 1~1 Iff Uf
'
a ~ ,.~
O O O O O O O O
a ~1 O Uf O O O O O
1p O 1~1 N . Ir! Uf
N
p ~ ~
O O O O O O O O
'
Uf O ff O O O O O
W '
~i Nf N N Pf O If1
a ~ m .a .a r, .
y~ o 0 0 0 0 0 0 0
p ,..n o us o 0 0 0 0
1p O Nf N N PI .
U1
f~ N .i .1
O O O O O O O O
.~/ r ~f1 O off O O O O O
~ N N ~
'
N r1
O
f
~ 1 O Uf O O O O O
f
n1 1p ~ O !~ N N Al vf1 off
H O ~1 r1 .i
1
,~U1 O U1 O O O O O
,
~1 1'~1 N N ~'~f v1 ~I1
O
O O O O O O O O
Uf O off O O O O O
O O ~ N N wf h
~ ~ .a
~ N
o o .a 4 ~ ~. o
a ~
v V y w N h
~ i~ i~ o~r >
i
~ , 11G w
~ w o t o ao
v ' > r,. t~ w v~ a
a~ ,o Z se tb
> o
~n
c
ar
o
ar
m
b e.wa a H ~ w f.. o-m
wer ,
w
o
v~r~rrir0 '00~ wZ aa~ ua C wpA
v H o ~w > w .1
o w
~. c: ~,y ..irr ..~
.w a.w ~
a .~ .~.o ac o s ~ a w
.o ; s s w i m x
s ~ - ~c
c
x
~ c m - o .~ yh .iws . wwo
- a--N i ~
c0.
w o ~r o n o ~ w
~ o a f .a ~, ..r O a ~ w
ucw a~.,o o ..i i
w.-m..~ wca'= ..m ~
a
~
. aun o a~d~ wa~m ~n ~ b-..~o b >.o rood
~ a r~llo w vo tZ i G -.~
0 a i
' O
. . o w xCa: Z7oG...
a o, c b x a w i '~ o Ps
S .a o o >.~o ~ v,
o ~. o ..~ r~
a
,r
b
,,,
. ~ . . ~ , ..~
H i W = , f ,.,
N ~ _
t
~
.'i 0 V ~~'O H .ti w W 1
i1~ ri x L~ ~ ~ N 0
i '~' ~ O
7
A
i
22
CA 02208602 2005-02-08
60557-5540
0 0 0 0 0 0
0 0 0 0 0 0 0
.a
0 0 0 0 0 0
0 0 0 0 0 0
p O O 0 0 O O
. . . . .
O. O O O O O
h
O O O O O O
a o 0 0 0 0 0
0 0 0 0 0
i
o 0 o
p ~ 0 o o
0 0 0 0 0 0
~
o e ~o
.a
.d
0 0 0 0
" 0 o
.,., " 0 0 0 0 0 0
o ~ ~n ~ n~ .~ ~o
y
V
~ 0 0 0 0
"~0 0 0
' 0 0 0 0 0 0
1f~~ Nf 1~ 1p N
Q1
~i
O O 0 0 0 O
,~0 0 0 0 0 0
0 0 0 0 0 0
Iff~ PI 1~ O N
O O O O O O
A O O O O O O
O O O ~ ~ O
r1
~
Q i:
~ ~
~
11 I :
17 w~ i . ~
x O s a
~
o
, ~ ~ o
r ~p .r p
.a .
.i
~ ~ .
a~a b 4yv~Gds a o ''
a ~ g
~ ~
o ~W ov~ a~r~ r~.-aWa
~~Ca o a.a $o~ v a
a ox sac a xw o~
.., o a ~
aw
. . ..~
a ~ 4 ~ O d i~ A
. ~ 1 N W 'd
.1 r1
10
a . ~
. ~ ~
~
H ! m iww ~ u w=~ t9.c
. w
23
CA 02208602 1997-06-23
WO 96/20987 PCT/US95116633
Examples 3-10 were prepared as described for
Examples 1 and 2. The batch size of each example was
about 477 grams.
The expansion ratio of Examples 3-10 were ,
determined (as described in Examples 1 and 2) to be
3.06, 2.96, 3.05, 2.96, 3.02, 3.00, 3.07, and 3.10,
respectfully. The softness values of the Example 3-10
putties were determined as described above under the
heading "Softness Value Measurement." The softness
values for Examples 3-10 were 5.6 mm, 5.7 mm, 5.6 mm,
5.8 mm, 6.0 mm, 5.8 mm, 5.9 mm, and 5.9 mm. The flow
characteristic of the Examples 3-10 putties were
excellent, excellent, excellent, excellent, very good,
very good, good, and fair, respectively.
24
CA 02208602 2005-02-08
60557-5540
Examples 11-14
The ingredients for Examples 1l-14 are listed in Table
4, below.
Table 4
llmouat of ingredieata,
P8R
Iags~edieat ?s.. ?~c. lac. l~c.
11 12 19
11
Unwlcanized styrene butadiene76.50 76.50 76.50 76.50
( "AMERI POL SYNPOL 8107
"' ) r""
Styrene butadiene rubber 20:00 20.00 20.00 20.00
("POLYSAR ~S 1018' )'"'
Moderately crosalinked butyl3.50 3.50 3.50 3.50
rubber (POLYSAR XL 68102"')1""
Mixture of diaryl p-phenylene2.00 2.00 2.00 2.00
diamine ('"WINGSTAY 100"')T~
Thiodiethylene bia-(3,5-di-2.00 2.00 2.00 2.00
tart-butyl-4-hydroxy)
hydrocinnamate ("IRGANOX
1035")TM
Fumed silica ('CAB-O-SIL 13.00 13.00 13.00 13.00
M 5"')TM.
Epoxy resin powder 7.5.00 15.00 15.00 15.00
("SCOTCHCAST SR 265"')TM
Powdered iron oxide (FezO~)5.00 5.00 5.00 5.00
("IRON OXIDE BF 95"') T""
Melamine powder ("HERO 50.00 50.00 50.00 50.00
MELAMINE" ) T""
Boron Oxide 90.00
(anh roua)
Hydrated Zinc Borate 40.00 83.25
("FIREBRAKE ZB FINE"')1M
Milled glass filaments ('"731ED30.00 30.00 30.00 30.00
FI BERGIJ~SS "' ) T""
Isobutylene butane copolymer,40.00 40.00 40.00 40.00
1i id ('"INDOPOL H 100"')1""
Petrolatum ("PAXWAX 5324"')T~~60.00 60.00 60.00 60.00
Granulated hydrated sodium 120.00 120.00 120.00 120.0
silicate ('"EXPANTROL 4BW"')TM 0
to Examples 11-14 were prepared by blending the
styrene butadiene rubbers ("POLYSAR S 1018"r""and
"POLYSAR XL 68102")1; and about 4.35% of the
unvulcanized styrene butadiene rubber ("AMERIPOL SYNPOL
8107")TM on a 40.6 cm (16 inch) rubber mill, and then
mixing for about 30 minutes at about 20 rpm. About
3.75% of the plasticizer ("INDOPOL H-100")'Mesas then
added to the rubber/unvulcanized rubber mixture while
milling continued.
CA 02208602 2005-02-08
~ 60557-5540
The resulting "prebatch" was removed from the
rubber mill and charged into a mogul mixer (No. 59821:
available from APV Chemical Machinery Inc. of Saginaw,
MI) along with the balance of the unvulcanized styrene
butadiene rubber("AMERIPOL SYNPOL 8107")T;and then mixed
1o for about 2 minutes.
While mixing continued, antioxidant (i.e., ,
thiodiethylene bis-(3,5-di-test-butyl-4-hydroxy)
hydrocinnamate), antiozonant (i.e., the mixture of
diaryl p-phenylene diamine), fumed silica, epoxy resin,
13 iron oxide, boron oxide (if in the formulation), zinc
borate (if in the formulation), melamine, and milled
glass fibers were added to the mixer over a 10 minute
period. Plasticizes ("INDOPO:L H-100"Tj was then added
and mixed in for about 5 minutes. Next, hydrated
20 sodium silicate ("EXPANTROL 48W") was added and mixed
in for about S~minutes. Finally, the petrolatum
("PAXWAX 5324"'jMwas added and mixed in for about 10
minutes, until the putty was smooth. The batch sizes
' of Examples 11-14 were about :L.35 kg, about 1.35 kg,
25 about 1.24 kg, and about 1.47 kg, respectively.
The expansion ratio of Examples 11-l4 were
determined (as described in Examples 1 and 2) to be
2.77, 2.77, 3.20, and 2.64, respectively. The softness
values of the Example 11-14 putties were determined as
3o described above under the heading "Softness Value
Measurement." The softness values for Examples 11-14
were 5.4 mm, 5.5 mm, 5.5 mm, and 5.10 mm, respectfully.
The flow characteristic of the Examples 11-14 putties
were excellent, good, good, and very good.
33 The "Flame Through Test" and the "Hose Stream
Test" were run on four samples of each lot. All four
samples for Examples 11, 13, and 14 passed the "Flame
Through Test." Only two of the four Example 12
26
i i . I I I"~ I
CA 02208602 2005-02-08
~ 60557-5540
samples, however, passed the "Flame Through Test."' For
the "Hose Stream Test," four of the Example 11 samples
passed, one of the Example 12 samples passed, none of
the Example 13 samples passed,. and three of the Example
14 samples passed.
1o
Examples. 15-19
The ingredients for Examples 15-19 are listed in
Table 5, below.
TABLE 5 .
lvmonat f ingredients
o , Pit
Ingredient l~c. l~c. lac. ~c. 18 ?ac.
15 16 17 19
Unvulcanized 76.50 76.50 76.50 76.50 76.50
styrene ,
butadiene rubber
'"AMERI POI.
SYNPOI. 8107"'
)T""
Styrene 20.00 20.00 20.00 20.00 20:00
butadiene rubber
('" POLYSAR
S
lore-jTM
Moderately 3.50 3.50 3.50 3.50 3.50
croaslinked
butyl rubber
('"POLYS1\R
XI.
68102"'jT""
Mixture of 2.00 2.00 2.00 2.00 2.00
diaryl p-
phenylene
diamine
(WINGSTAY 100')TM
Thiodiethylene 2.00 2.00 2.00 2.00 2.00
bis-(3,5-di-
tert-butyl-4-
hydroxy)
hydrocinnamate
("IRGANOX 1035"')""
Fumed silica 13.00 13.00 13.00 13.00 13.00
('" CAB-O-S
I I. M
5.j,~
Epoxy resin 15.00 15.00 15.00 15.00 15.00
powder
('"SCOTCHCAST
SR
265"')T""
Powdered iron 5.00 5.00 5.00 5.00 5.00
oxide (FeiO~)
("IRON OXIDE
BF
95"')rra
Z7
CA 02208602 2005-02-08
~ 60557-5540
Table 5 Continued
I~lelamine powder50.00 50.00 50.00 50.00 50.00
("~
Z'~L~MII~iL""
)'"
Boson oxide 10.00 40.00 10.00 10.00 10.00
lanh rows)
Killed glass -30.00
filamenta 30.00 30.00 30.00 30.00
("731LrD
FTBERGI~'1SS"
) "''
Iso~tyle~ 55.00 50.00 10.00 0.0 25.00
buteae ex~poiys~er
liquid ("hIDOPO3.
H 100"') T~"
Petroiat~m 60.00 60.00 60.00 60.00 60.00
("PAX~PA)C 532!")T"
Granulated 120.00 120.00 120.00 120.00 120.00
hydrated~sodium
silicate
"EXPI~iTWOI~
4 B11" )" .
Examples 15-19 were prepared as described for
Examples l and 2. The batch size for Examples 15, 1-6,
17, 18, and 19, was about 992 grams, about 48? grams,
about 977 grams, about 467 grams, and about 462 grams,
to respectively.
The expansion ratio of Examples 15, 16, 17, 18,
and 19 were determined (as described in Examples 1 and
2) to be 2.97, 2.93, 3.02, 2.97, and 2.93,
respectively. The softness~values of the Example 3-10
putties were determined as described above under the
heading '"Softness Value Measurement."' The softness
values for Examples 15, 16, 17, 18, and 19 were 6.1 mm,
5.9 mm, 6.0 mm, 5.9 mm, and 5.1. mm, respectfully. The
flow characteristic of the Examples 15, 16, 17, 18, and
19 putties were fairy good, very good, very good, and
very good, respectively.
The following observations were made when handling
each of Examples 15-19. Example 15 was very tacky and
left residue on the skin. Example 16 was tacky and
Z5 left some residue on the skin. Examples 17, 18, and 19
2E
CA 02208602 2005-02-08
~ 60557-5540
all had a good level of tackiness and left no visible
residue on the skin.
Example 20
The ingredients for Example 20 are listed in Table
6, below.
Table 6
7lmonat o! ingredients,
Ingredfeat gamble 20
Non-crosslinked 80.00
styrene
butadiene
rubber
('"AMERIPOL
SYNPOL
8107"')""'
Cross-linked 20.00
styrene
butadiene
rubber
('"POLYSI\R
S
1018")
T''"
Fumed 13.00
silica
("CAB-O-SIL
M-5"')T""
Epoxy 15.00
resin
powder
("SCOTCIiCAST
SR
265"'
)
T""'
Powdered 5.00
iron
oxide
(FeZO~)
("IRON
OXIDE
BF
95')T""
Hydrated 50.00
zinc
borate
("FIREBRAKE
ZB
FINE"')T"'
Choed fiber lass fibers 20.00
("799AB"')T""
Isobutylene 71.00
butene
copolymer
liquid
("INDOPOL
H
100"'
)
TM
Blend 15.00
of
bis
melaminium
pentate
and
of
hedric
oxide
('"C~iARGUARD
329"')x"
Petrolatum TM 50.00
('"PETROLATUM
RPB"'T
Granulated 100.00
hydrated
sodium
silicate
('"EXPANTROL
2")'"'
Example 20 was prepared as described for Examples
1 and 2. The batch size was about 439 grams.
The expansion ratio of Example -20 was determined
(as described in Examples 1 and 2) to be 7.05. The
softness value was determined as described above under
the heading "Softness Value Measurement" to be 5.6 mm.
The flow characteristic of the putty was good.
Example 20 passed both the "Flame Through Test"
and the "Fire Hose Stream Test.."
29
CA 02208602 2005-02-08
60557-5540
Example 21
The ingredients for Example 21 are listed in Table
~7, below.
Table 7
Amount of '
Ingredieats
PHR*
Ingredient Example 21
tlnvulcaaised styrene 74.02
butadiene rubber
("AMERIPOL SYNPOL 8109"ITM
Styzene butadiene rubber 22.11
("Polysar S
1018") ""
Moderately crosslinked 3.8?
butyl rubber
( POLYSAR XL 68102")'"'
Thiodiethylene bas-(3,5-di-tart- 3.32
butyl-4-hydroxy) hydrocinnamate
("IRGANOX 1035")T""
Flamed silica ("CAB-O-SIL"!~" 14.3?
E ox resin owder ("SCOTCHCAST 16.59
265" T""
Powdered iron oxide ( 5. 53
F'e203 ) ( "IRON
OXIDE BF-1")'~"
Melamine oWder ("HERO 55.29
MELAMINE")T""
Boron Oxide Anhydrous 44.23
("BORIC OXIDE
60 MESH)T""
Milled filaments ("MFX-1/8'TM 33.1?
IN")
Iaobutylene butane copolymer 44.23
liqisid
( "INDOPOL H 100" )T""
Petrolatum ("PENRECO AMBER")TM- 66.34
Granulated hydrated sodium 132.68
silicate
"EXPANTROL 4B~" ) r''"
Parts pu hundred based on the fatal robber and unvulcaaized
rubber cf the pnay. '
The ingredients were compounded using the internal
mixer described in Example 1.
The unwlcanized rubber ("Ameripol Synpol 810?N),M
and rubbers ("Polysar S 1018" and "POLYSAR BUTYL XL
68102~') were added to the mixing chamber of the mixer
and then blended for about 6 minutes at about 60 rpm.
2o The speed of the mixing blades was then reduced to 90
rpm, and the antioxidant (i.e., thiodiethylene bis-
(3,5-di-tart-butyl-4-hydroxy) hydrocinnamate), fumed
silica, epoxy resin, iron oxide, boric oxide, melamine,
CA 02208602 2005-02-08
60557-5540
s and milled glass fibers were added while mixing
continued. The ingredients were mixed for about 3
minutes, after which the mixing speed was increased to
. about 60 rpm. The plasticizes ("INDOPOL H-100")'was
then added, and mixing continued for about 13 minutes.
The petrolatum was then slowly added and mixed in for
about 5 minutes. Finally, the hydrated sodium silicate
was added and mixed in for about 5 minutes. The bhtch
size was about 466.44 grams.
The softness value of the putty, as determined
is using the method described above under the heading
"Softness Value Measurement"',was 6.32 mm. The
expansion ratio of Example 21,, based on an average of
two determinations, was 2.76. The flow characteristic
of the putty. was excellent. ,'E~rther, the '"Flame
2o Through Test"' and the '"Fire Hose Stream Test."'
Various modifications and alterations of this
invention will become apparent to those skilled in the
art without departing from the scope and spirit of this
25 invention. and it should be understood that this
invention is not to be unduly limited to the
illustrative embodiments set forth herein.
31
