USO08070990B2

(12) United States Patent (10) Patent No.: US 8,070,990 B2

H0 et al. (45) Date of Patent: Dec. 6, 2011

(54) SMOKE SUPPRESSANTS 4,670.494. A 6, 1987 Semenza

4,680,334 A 7, 1987 Wallace
i- 4,762,700 A 8/1988 Huggins
(75) Inventors: W SES t 3.
(US); Joseph K. Walker, Mentor,
4,965,309 A 10/1990
5,227,417 A
Batdorf
7/1993 Kroushl
(US) 5,494,718 A * 2/1996 Adams et al. ................ 428, 35.7
5,886,072 A * 3/1999 Linsky et al. ................. 524/145
(73) Assignee: J.M. Huber Corporation, Atlanta, GA 6,043,312 A 3/2000 Fagher
(US) 2004/O122149 A1 6/2004 Kakakia
2006, OO 14874 A1 1, 2006 Ito
(*) Notice: Subject to any disclaimer, the term of this FOREIGN PATENT DOCUMENTS
patent is extended or adjusted under 35 EP O708143 B1 1, 2000
U.S.C. 154(b) by 422 days. WO WO 2004O41930 A1 * 5, 2004
(21) Appl. No.: 11/934,427 OTHER PUBLICATIONS
(22) Filed: Nov. 2, 2007 Climax Molybdenum web site, 2004, accessed from http://web.
e Afs archive.org/web/20050306020006/www.climaximolybdenum.com/
(65) Prior Publication Data Products/Chemical? on Jul. 24, 2009.*
US 2011/0031454A1 Feb. 10, 2011 * cited by examiner
Related U.S. Application Data Primary Examiner — Peter F Godenschwager
(60) Provisional application No. 60/864.317, filed on Nov. (74) Attorney, Agent, or Firm — Ballard Spahr LLP
3, 2006. (57) ABSTRACT
(51) Int. Cl. The present invention is directed to Smoke Suppressants based
C09K2I/02 (2006.01) on ammonium octamolybdate chemistry. According to this
C09K2I/00 (2006.01) invention, the precipitation of ammonium octamolybdate in
CSK 3/I (2006.01) the presence of an inert mineral core produce a novel high
(52) U.S. Cl. ......................... 252/609; 252/601:524/406 Surface area ammonium octamolybdate Smoke Suppressant.
(58) Field of Classification Search ................... 252/609 The high Surface area significantly increases the Smoke Sup
See application file for complete search history. pression performance over a standard ammonium octamolyb
date. This invention is also directed to a process for making
(56) References Cited the high surface area ammonium octamolybdate Smoke Sup
pressant. The Smoke Suppressant of this invention is particu
U.S. PATENT DOCUMENTS larly suitable for smoke suppression in polyvinyl chloride
3,726,694 A 4, 1973 Moore (PVC) applications.
3.969,127 A 7, 1976 Robitalle
4,098,753. A 7/1978 Tsigdinos 11 Claims, 9 Drawing Sheets

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 US 8,070,990 B2
1. 2
SMOKE SUPPRESSANTS formulated with 30 phraluminum trihydrate and 5, 10 and 15
phr AOM of either commercial AOM or high surface area
CROSS-REFERENCE TO RELATED AOM.
APPLICATION FIG. 10 is a bar graph representing comparative NBS aver
age percent reduction in Smoke density results at 90 seconds
This application claims the benefit of U.S. provisional obtained from rigid PVC formulated with 6, 9 and 12 phr
patent application No. 60/864.317 filed on Nov. 3, 2006, the AOM of either commercial AOM or high surface area AOM.
entirety of which is hereby incorporated by reference. FIG. 11 is a bar graph representing comparative NBS aver
This invention generally relates to a novel high surface area age percent reduction in Smoke density results at 4 minutes
ammonium octamolybdate (AOM) based Smoke Suppressant 10
obtained from rigid PVC formulated with 6, 9 and 12 phr
that can be used in thermoplastic compositions and other AOM of either commercial AOM or high surface area AOM.
polymeric materials. The high surface area AOM material is FIG. 12 is a bar graph representing comparative NBS aver
prepared by controlled reaction of ammonium dimolybdate age percent reduction in maximum Smoke density obtained
and molybdenum trioxide in the presence of an inert core from rigid PVC formulated with 6, 9 and 12 phr AOM of
material. Precipitation of ammonium octamolybdate in the 15
presence of an inert core material promotes a rod-like mor either commercial AOM or high surface area AOM.
phology of AOM. The formation of discreet rods, rather than FIG. 13 is a graph representing of the total Smoke gener
agglomerates, results in a Surface area 1.5 to 2.5 times greater ated from the combustion of rigid PVC formulated with 6 and
than that of commercial ammonium octamolybdates. 9 phr of KG-STA and two commercial AOM materials.
Because of its high surface area, the AOM precipitation tech DESCRIPTION OF THE INVENTION
nology is more effective at lower use levels than conventional
AOM in both flexible and rigid PVC compounds.
The present invention is directed to a novel high surface
BRIEF DESCRIPTION OF THE DRAWINGS area molybdate Smoke Suppressant. Inorganic molybdates are
25 the industry standard for Smoke Suppression based on their
Detailed Description of Illustrated Embodiments inherent capability of promoting char formation. According
to this invention, the effectiveness of Smoke Suppression can
FIG. 1 is a scanning electron micrograph image of a com be strongly enhanced by the increased Surface area of the
mercial AOM showing the AOM in the form of irregularly molybdate additive.
shaped agglomerates. 30 This invention is also directed to the preparation of a novel
FIG. 2 is a scanning electron micrograph image of a high high Surface area molybdate Smoke Suppressant. The process
surface area AOM-talc smoke suppressant showing the AOM involves controlled precipitation of AOM on an inert mineral
in the form of distinct rods. Precipitation of ammonium octa core. The AOM material on the inert core increases the Sur
molybdate in the presence of talc promotes the formation of face area of the active chemistry and reduces the total demand
rods rather than agglomerates. 35 for molybdenum in a polymer (for example, PVC) com
FIG. 3 is a bar graph representing comparative NBS aver pound. In accordance with this invention, the high Surface
age smoke density results at 90 seconds obtained from flex area AOM significantly increases the Smoke Suppression per
ible PVC formulated with 30 phraluminum trihydrate and 5, formance over a standard ammonium octamolybdate.
10 and 15 phr AOM of either commercial AOM or high High surface area AOM, hereinafter “KG-STA. can be
surface area AOM. 40 prepared by an in situ reaction of ammonium dimolybdate
FIG. 4 is a bar graph representing comparative NBS aver and molybdenum trioxide in the presence of an inert base
age Smoke density results at 4 minutes obtained from flexible pigment. Such as talc. In one embodiment, the Surface treat
PVC formulated with 30 phr aluminum trihydrate and 5, 10 ment of an inert core with AOM can include an in-situ reac
and 15 phr AOM of either commercial AOM or high surface tion comprising the steps of
area AOM. 45 (1) charging an inert base pigment into hot water;
FIG. 5 is a bar graph representing comparative NBS aver (2) addition of ammonium dimolybdate (ADM) and
age Smoke density results at maximum Smoke development molybdenum trioxide (MoO) in a stoichiometric molar
obtained from flexible PVC formulated with 30 phr alumi ratio of 2:4:
num trihydrate and 5, 10 and 15 phr AOM of either commer (3) holding the slurry at between about 88° C. and 95°C.
cial AOM or high surface area AOM. 50 for about 3-5 hours;
FIG. 6 is a bar graph representing comparative NBS aver (4) filtering;
age smoke density results at 90 seconds obtained from flex (5) drying; and
ible PVC formulated with 60 phraluminum trihydrate and 5, (6) grinding.
10 and 15 phr AOM of either commercial AOM or high Pigments that can be used for this invention include talc,
surface area AOM. 55 for example, MicrotalcR) powdered talc (available from Spe
FIG. 7 is a bar graph representing comparative NBS aver cialty Minerals, Inc., Bethlehem, Pa.), silica, clay, or any
age Smoke density results at 4 minutes obtained from flexible pigment that can be used as filler in polymers (such as PVC)
PVC formulated with 60 phr aluminum trihydrate and 5, 10 and do not interfere with the ammonium dimolybdate/molyb
and 15 phr AOM of either commercial AOM or high surface denum trioxide reaction. The incorporation of ammonium
area AOM. 60 dimolybdate (ADM) and molybdenum trioxide can be added
FIG. 8 is a bar graph representing comparative NBS aver in sequential order or simultaneously (i.e., regardless of
age Smoke density results at maximum Smoke development order) at specified rates.
obtained from flexible PVC formulated with 60 phr alumi The dried powder can be milled using a Netzch grinder.
num trihydrate and 5, 10 and 15 phr AOM of either commer The AOM content can be in the range of 20% to 85% by
cial AOM or high surface area AOM. 65 weight, and the inert core material can be range of 15% to
FIG. 9 is a bar graph representing comparative cone calo 80% by weight, based on the total weight of the smoke Sup
rimeter smoke density results obtained from flexible PVC pressant material.
 US 8,070,990 B2
3 4
The precipitation of ammonium octamolybdate in the pres Table 3 illustrates a rigid PVC formulation.
ence of talc promotes the formation of rods rather than irregu
larly shaped agglomerates. As measured by the BET method, TABLE 3
the rod-like structure of AOM in KG-STA has higher surface Rigid PVC formulation.
area than commercial AOM materials. The surface area of a 5
blended material can be considered an additive property. Oxvinyl 24OF PVC Resin
Mark 1900 thermal stabilizer
1O

For KG-STA, the experimentally determined BET surface Halstab 1214 acid scavenger
area is 7.0 m/gm, and the AOM contribution is calculated to Sb2O flame retardant
Calcium Stearate
be 4.09 m/gm. Therefore, the ammonium octamolybdate of 10 Paraloid K120N acrylic modifier
KG-STA is determined to have a surface area 1.5 to 2.5 times Paraloid K175 acrylic modifier
higher than the two commercial grades of AOM. Mg(OH)2
Talc 1
Table 1 shows the BET surface area values of KG-STA and
commercial AOM products (AOM #1 and AOM #2).
15 For example, flexible PVC containing the smoke suppres
TABLE 1. sant of this invention can be made by blending 30 phr or 60
phr (parts by weight per hundred parts of resin) of aluminum
trihydrate, and 5 phr or 10 phr or 15 phr of the high surface
BET Surface Area. Measurements area AOM with the blend of the base formula for flexible PVC
resin listed in Table 2. The components of the formulation are
KG-STA AOM #1 AOM #2 mixed in a Waring blender mixing vessel. The flexible PVC
(m/gm) (m/gm) (m/gm) specimens are fused using a 75-mL Brabender Plasticorder
Digisystem equipped with Type 6 roller blades (3:2 speed
ratio). The fusion process parameters include a mixing tem
7.0 1.6 2.9
25
perature of 160° C. and a mixing time of 5 min. The fused
samples are compression-molded to a "/8" thickness with a
Carver press at 300°F. Four plaques are produced per experi
Another aspect of this invention is a thermoplastic polymer ment for NBS Smoke Chamber and cone calorimetry tests.
comprising a high Surface area AOM. The thermoplastic As another example, rigid PVC containing the Smoke Sup
polymer composition comprises a chlorine-containing poly pressant of this invention can be made by blending 20 phr
30 (parts by weight per hundred parts of resin) of aluminum
merand a Smoke Suppressant compound comprising (a) from trihydrate, and 5 phr or 10 phr or 15 phr of the high surface
about 15% to about 80% by weight of an inert core material area AOM with the blend of the base formula for rigid PVC
such as talc, silica, or clay; and (b) from about 20% to about resin listed in Table 3. The components of the formulation are
85% by weight of an ammonium octamolybdate, both based mixed in a Waring blender mixing vessel. The rigid PVC
on the weight of the Smoke Suppressant compound. specimens are fused using a 75-mL Brabender Plasticorder
Digisystem equipped with Type 6 roller blades (3:2 speed
In yet another aspect of this invention is a method of ratio). The fusion process parameters include a mixing tem
improving the Smoke Suppressant characteristics of a poly perature of 190° C. and a mixing time of 5 min. The fused
meric composition. The method comprises (a) preparing a samples are compression-molded to a "/8" thickness with a
Smoke Suppressant material comprising from about 20% to 40 Carver press at 300°F. Four plaques are produced per experi
about 85% by weight of an ammonium octamolybdate, 15% ment for NBS Smoke Chamber and cone calorimetry tests.
to 80% of an inert core material Such as talc, silica, or clay, While the present invention has been illustrated by the
and (b) compounding the Smoke Suppressant material with a description of embodiments thereof, and while the embodi
formula of a polymeric formulation. An example of a poly ments have been described in considerable detail, it is not the
meric formulation is polyvinyl chloride. In one embodiment, 45
intention of the applicants to restrict or in any way limit the
the thermoplastic polymer is a flexible polyvinylchloride Scope of the appended claims to such detail. Additional
(PVC). Although polyvinylchloride is inherently flame advantages and modifications will readily appear to those
skilled in the art. Therefore, the invention, in its broader
retarding, the use of plasticizers to achieve PVC flexibility aspects, is not limited to the specific details, the representative
has resulted in increased flammability of the material. In apparatus, and illustrative examples shown and described.
another embodiment, the thermoplastic polymer is a rigid 50 Accordingly, departures may be made from Such details with
polyvinylchloride. out departing from the spirit or scope of the applicant's gen
A base formula of a typical flexible polyvinyl chloride is eral inventive concept.
shown in Table 2: EXAMPLE 1.
55
TABLE 2
Method for Producing AOM Treated Talc
Base formula of a typical flexible PVC.
To 400 parts deionized water is added 30 parts talc and
Oxyvinyl 240 F PVC Resin 100 mixed to form a slurry. 51 parts ammonium dimolybdate and
Halstab H-695 thermal 7
stabilizer 60 42 parts molybdenum trioxide are then added. The slurry is
Sb2O flame retardant 3 heated to 88° C. and held for 3 hours while stirring. The
(synergist) reaction of the ammonium dimolybdate and the molybdenum
Micral 94.00 (Aluminum 30 trioxide occurs at the elevated temperature. Water can be
trihydrate)
Santicizer 2148 Plasticizer 2O added during the reaction to keep the volume above the mix
Uniplex FRP-45 Plasticizer 2O 65 ing blade, if necessary. After 3 hours, the slurry is filtered hot,
the filtered slurry is dried at 150°C., and then the filter mass
is ground in a centrifugal grinder.
 US 8,070,990 B2
5 6
EXAMPLE 2 COMPARATIVE EXAMPLES

Method for Producing AOM Treated Talc Commercial AOM #1 and AOM #2 vs. KG-STA

To 400 parts deionized water is added 30 parts talc and 5 Flexible PVS-NBS Smoke
mixed to form a slurry. 51 parts ammonium dimolybdate is
added at 6 grams per minute, and then 42 parts molybdenum The NBS Smoke results of flexible PVC are presented in
trioxide is added at 5 grams per minute. The slurry is heated FIGS. 3-8, and cone calorimeter results of flexible PVC are
to 88° C. and held for 3 hours while stirring. Optionally, the presented in FIG. 9. All samples are tested at total AOM
slurry can be cooled to 66° C. and then held for 1 hour. The
10 content levels of 5 phr, 10 phr and 15 phr (parts per hundred
reaction of the ammonium dimolybdate and the molybdenum PVC resin) with talc levels adjusted to maintain a fixed total
trioxide occurs at the elevated temperature. Water can be filler content, and either 30 phr or 60 phraluminum trihydrate
added during the reaction to keep Volume above mixing (ATH).
blade. After 3 hours, the hot or cooled slurry is filtered, the The data clearly demonstrate that at all use levels and all
15 times, the KG-STA far exceeds the performance of commer
filtered slurry is dried at 150° C., and then the filter mass is cial AOM #1 and #2 samples. In terms of maximum smoke
ground in a centrifugal grinder. density, KG-STA shows the greatest performance advantage
The following examples demonstrate the results obtained at the lower use levels. The results demonstrate that the per
utilizing AOM smoke suppressant PVC compounds of this formance of KG-STA at 5 phr is comparable to the perfor
invention. Plasticized flexible and rigid PVC plaques (100x mance of the best commercial AOM at 10 phr, resulting in
100x3 mm) containing the KG-STA are prepared and tested much more efficient use of the AOM chemistry.
via the NBS smoke chamber and cone calorimetry test meth FIGS. 6-8 present the NBS smoke results obtained from a
ods as described below. The examples are intended to be 60 phr ATH-containing formula. The smoke density is shown
representative of the formulations that can be made and are as a function of use level for the various compounds. FIG. 6
not intended to limit the scope of the invention. All test 25 shows the 90 second smoke, FIG. 7 shows the smoke devel
compounds are mixed using a Brabender Plasticorder and test opment at 4 minutes and FIG. 8 shows the maximum Smoke
plaques are prepared by compression molding. The Smoke development for the various compounds.
generated by combustion of the PVC plaques are determined The results in FIG.9 demonstrate that the performance of
in the NBS Smoke chamber according to ASTM E662-06 KG-STA again far exceeds the performance of AOM #1 at all
“Standard Test Method for Specific Optical Density of Smoke 30 use levels. The total smoke numbers with 5 phr KG-STA were
Generated by Solid Materials”, incorporated herein by refer comparable to those obtained with AOM #1 at 10 phr. Sig
CCC. nificantly, the total smoke obtained with 10 phr KG-STA was
nearly the same as that obtained with 15 phr of AOM #2.
Test Methods Thus, both the Cone Calorimeter and NBS Smoke results
35 demonstrate that in flexible PVC, KG-STA offers perfor
ASTM E662 NBS Smoke Chamber mance advantages over commercial AOM. Depending on the
The release of smoke generated by the combustion of plas system, the use of KG-STA allows for the reduction of 25% to
tic materials can be determined using the National Bureau of 50% total AOM while retaining equal or better smoke Sup
pression.
Standards (NBS) smoke chamber method, standardized in the 40
U.S. as ASTM E662-06. This test was originally developed to Rigid PVC-NBS Smoke
determine the Smoke generating characteristics of plastic
materials used in aircraft construction. A model rigid PVC formula is selected for the comparison
The NBS Smoke chamber measures smoke density accu of KG-STA and commercial AOM. In this formula, the total
mulated when a specimen of specified form and thickness is 45 filler content is fixed at 20 phr. In the negative control, the
exposed to a radiant heat source of 25kW/m . Depending on filler is made up of 8 phr of magnesium hydroxide and 12 phr
the application, either the maximum Smoke density or the talc. Smoke Suppressants are studied at 6, 9, and 12 phr. In
Smoke density at a set time (usually 4 minutes) can be speci these samples, the talc level is reduced to maintain the fixed
fied. The test can be run with or without the application of a total filler level. In these examples, the comparison of KG
pilot flame (flaming and Smoldering mode, respectively). 50 STA and AOM is on an equal weight basis, rather than equal
ASTM E1354-04a Cone Calorimeter AOM content. In other words, the samples with KG-STA
The cone calorimeter is a laboratory instrument that mea contain only 70% of the molybdate content of the samples
Sures combustibility and Smoke generation of materials under containing commercial AOM.
a wide range of conditions. For building materials that must NBS results at 90 seconds, 4 minutes and the maximum
pass the E-84 Steiner Tunnel test, the cone calorimeter is
55 smoke development are shown in FIGS. 10-12. These figures
often used as a screening test. demonstrate the percent reduction in Smoke when compared
In the cone calorimeter test, described by ASTM E1354 to a control system with no Smoke Suppressant (talc and
04a “Standard Test Method for Heat and Visible Smoke Rates Mg(OH) as the only fillers). As can be seen in FIGS. 10-12,
at all use levels and all times, KG-STA significantly outper
for Materials and Products Using an Oxygen Consumption 60 forms both AOM smoke suppressants. Significantly, KG
Calorimeter, incorporated herein by reference, a square STA at 6 phr exceeds the performance of the commercial
sample of 100x100 mm (4x4 in.) is exposed to the radiant flux AOM #2 at 12 phr. The KG-STA contains only 70% AOM
of an electric heater. The heater has the shape of a truncated based on the total weight of KG-STA (i.e., equal or enhanced
cone and is capable of providing heat fluxes in the range of performance is achieved at an AOM level 65% lower than
10-110kW/m, but most typically from 50-75kW/m. This is 65 when using the pure commercial materials).
two to three times the heat flux used in the NBS Smoke At 90 seconds and 4 minutes, there is very little depen
chamber. dence on use level with KG-STA. This is in striking contrast
 US 8,070,990 B2
7 8
to the commercial AOM, which definitely show increasing 5. The smoke suppressant of claim 1, wherein the ammo
performance with increasing use levels. The maximum nium octamolybdate is about 70% to about 75% by weight,
smoke density developed with KG-STA does, however, dem based on the weight of the Smoke Suppressant, and the inert
onstrate a dependence on use level. At all levels, the reduction core material is about 25% to about 30% by weight, based on
in smoke generation achieved with KG-STA far exceeds that 5 the weight of the Smoke Suppressant.
of the commercial products. 6. A thermoplastic polymer composition comprising:
a) a chlorine-containing polymer; and
Rigid PVC Cone Calorimeter b) a Smoke Suppressant compound comprising:
(a) from about 15% to about 80% by weight of an inert
Using the same model rigid PVC formula shown above, 10 core material;
cone calorimeter testing (ASTM E-135404a) is performed to (b) from about 20% to about 85% by weight of an ammo
further compare the smoke suppression effectiveness of KG nium octamolybdate;
STA and the two commercial AOM materials. Product com wherein the ammonium octamolybdate is obtained from an
parisons were conducted at 6 and 9 phr, with talc levels in situ reaction of ammonium dimolybdate and molyb
adjusted to maintain a fixed total filler level. FIG. 13 presents 15 denum trioxide;
the total Smoke generated from combustion of the various and wherein the in situ reaction occurs in the presence of
PVC samples as a function of use level. the inert core material; and
In both NBS Smoke and Cone Calorimeter testing, KG wherein the ammonium octamolybdate obtained from the
STA has consistently demonstrated its performance advan in situ reaction is in the form of particles having Sub
tages over the commercial ammonium octamolybdate. Ana stantially rod-shaped morphology.
lytical results indicate that the significant performance 7. The thermoplastic polymer composition of claim 6,
improvements are primarily attributed to the increased Sur wherein the polymeric formulation comprises polyvinyl
face area of KG-STA. NBS Smoke and Cone Calorimetry chloride.
results demonstrate that KG-STA outperforms both AOM #1 8. The thermoplastic polymer composition of claim 6, fur
and #2 in decreasing Smoke. Thus, both commercial 25 ther comprising aluminum trihydrate.
examples of AOM #1 and #2 can be replaced with KG-STA at 9. A method of improving the Smoke Suppressant charac
equivalent or up to 50% less AOM content while retaining teristics of a polymeric composition, comprising:
equal or better Smoke reduction. (a) preparing a Smoke Suppressant material comprising:
We claim: 1. from about 15% to about 80% by weight, based on the
1. A Smoke Suppressant comprising: 30 weight of the Smoke Suppressant material, of an inert
a) from about 15% to about 80% by weight of an inert core core material; and
material; 2.from about 20% to about 85% by weight, based on the
b) from about 20% to about 85% by weight of ammonium weight of the Smoke Suppressant material, of an
octamolybdate; ammonium octamolybdate;
wherein the ammonium octamolybdate is obtained from an 35 wherein the ammonium octamolybdate is obtained from an
in situ reaction of ammonium dimolybdate and molyb in situ reaction of ammonium dimolybdate and molyb
denum trioxide; denum trioxide;
and wherein the in situ reaction occurs in the presence of and wherein the in situ reaction occurs in the presence of
the inert core material the inert core material, and wherein the ammonium octa
wherein the ammonium octamolybdate obtained from the 40 molybdate obtained from the in situ reaction is in the
in situ reaction is in the form of particles having Sub form of particles having Substantially rod-shaped mor
stantially rod-shaped morphology. phology;
2. The Smoke Suppressant of claim 1, wherein the inert core (b) compounding the Smoke Suppressant material with a
material is selected from the group consisting of a talc, clay, polymeric formulation.
silica, and extender pigment. 45 10. The method of claim 9, wherein the polymeric formu
3. The smoke suppressant of claim 2, wherein the talc is lation comprises polyvinyl chloride formulation.
Surface-treated with the ammonium octamolybdate. 11. The method of claim 9, wherein the inert core material
4. The Smoke Suppressant of claim 1, wherein the ammo is selected from the group consisting of talc, clay, silica, and
nium octamolybdate is about 65% to about 80% by weight, extender pigment.
based on the weight of the Smoke Suppressant, and the inert 50
core material is about 20% to about 35% by weight, based on
the weight of the Smoke Suppressant.