Location via proxy:   [ UP ]  
[Report a bug]   [Manage cookies]                

United States Patent (19) : Naseem (45) Date of Patent: Jan. 9, 1990

Download as pdf or txt
Download as pdf or txt
You are on page 1of 8

United States Patent (19) 11) Patent Number: 4,892,683

Naseem (45) Date of Patent: Jan. 9, 1990


54) FLAME RETARDANT LOW SMOKE 4,462,831 7/1984 Raevsky et al. ................. 106/18.26
POLYOVNYL CHLORIDE) 4,544,685 10/1985 Hoelzer ............................... 523/200
THERMOPLASTC COMPOSITIONS 4,696,967 9/1987 Shedd et al. ........................ 524/437
(75) Inventor: Homaira Naseem, Leominster, Mass. OTHER PUBLICATIONS
(73) Assignee: Gary Chemical Corporation, Desai, Orig. Coating Appl. Polyn Sci. Proc., 48, pp.
Leominster, Mass. 806-810 (1983).
Appl. No.: 196,326
Moore, Soc. Plast. Eng. Tech. Rep., 23, pp. 216-227
21 (1977).
22 Filed: May 20, 1988 Moore, Fire Retard. Proc. Int. Sym., pp. 414-416
(1976).
51) Int. Cl. ........................ C09K 21A00; H01B 7/00; Price, J. Vinyl Tech., 1, pp. 98-106 (1979).
C08K9/00; C08L 27/00 Chem Abstracts, 87, 85704b.
52) U.S. C. ................................. 252/609; 106/18.24; Chem Abstracts, 87, 152861r.
106/18.25; 106/18.27; 106/18.35; 174/110 SR; Chem. Abstracts, 89, 111413u.
174/110 PM; 174/110 V; 174/113 R; 174/120 Chem Abstracts, 93, 169140b.
SR; 174/121 A; 174/121 SR 252/602; Chen Abstracts, 94, 137337a.
523/200; 523/206; 524/406; 524/423; 524/464; Chem Abstracts, 94, 176007n.
524/567
(58) Field of Search ............... 523/200; 260/DIG. 24; Chen Abstracts, 95, 204954k.
. 524/567,568, 569, 406; 174/110 SR, 110 PM, Chem Abstracts, 97, 24728x.
110 V, 113 R, 120 SR, 121 A, 121 SR; Chem Abstracts, 100, 122191s.
106/18.94, 18.25, 18.27, 18.35 Chem Abstracts, 100, 140139k.
Chem Abstracts, 100, 140259z.
56 References Cited Chem Abstracts, 100, 1402.60t.
U.S. PATENT DOCUMENTS Chem Abstracts, 100, 211026.
Chem Abstracts, 102, 79752c.
3,341,628 9/1967 Buning et al..... ... 260/899 American Stand. Test Method #D2863-77, pp.
3,566,009 2/1971. Lamond et al... ... 174/116 642-648.
3,576,940 5/1971 Stone et al. ...... ... 174/113
3,579,608 5/1971 De Coste ............. ... 260/837 American Stand. Test Method #D4100-82, pp.
3,623,940 1 1/1971 Gladstone et al. .................. 161/175 484-494.
3,745,233 7/1973 Lania et al. .......... ... 174/113 R American Stand. Test Method #E662-83, pp. 686-714.
3,823,255 7/1974 LaGase et al. ... ... 174/13 R Carmoin, J. Macromol. Sci. Phys, B14(2), pp. 307-320
3,845,166 0/1974 Betts et al. ....... ... 260/897 C (1977).
3,868,341 2/1975 Sauer et al. .................... 260/23 XA Clark, Polymer Eng. & Sci., 22, pp. 698-704 (1982).
3,869,420 3/1975 Mathis et al. .................. 260/30.6R Bohn, Rubber Chemistry and Technology, 41, pp.
3,900,533 8/1975 Kracketer et al. ... 260/897 A
3,928,210 12/1975 Peterson ........... ... 252/8. 495-513 (1968).
3,935,369 1/1976 George et al. ... 428/379 Primary Examiner-Howard J. Locker
3,941,908 3/976 Valia et al. .......................... 428/379 Attorney, Agent, or Firm-Weingarten, Schurgin,
3,943,087 3/1976 Leuchs ............. ... 260/30.6R Gagnebin & Hayes
3,944,717 3/1976 Hacker et al. .................... 174/23 C
3,998,715 12/1976 Bohm et al. ...... ... 204/159.6 57 ABSTRACT
4,008,368 2/1977 Leuchs ......... ... 174/120 R
4,018,983 4/1977 Pedlow ............................... 174/135 Flame retardant low smoke PVC-based thermoplastic
4,064,359 12/1977 Peterson et al. . ... 174/107 compositions for use in wire insulation and cable jacket
4,080,404 3/1978 Deets ................ ... 524/406 ing. The compositions include poly(vinyl chloride), an
4,098,748 7/1978 Moore et al. ... ... 260/30.6 additional chlorinated resin, tribasic lead sulfate, a
4,098,753 7/1978 Tsigdinos et al. ... ... 524/31.4 molybdenum-containing smoke suppressing material,
4,111,885 9/1978 Abu-Isa ............ ... 524/314
alumina trihydrate, a brominated aromatic ester plasti
4,225,649 9/1980 Peterson ........... ... 428/383
4,328,152 5/1982 Tsigdinos et al. o ... 524/406 cizer, at least one additional plasticizer, and at least one
4,331,733 5/1982 Evans et al. ......... ... 428/379 lubricant.
4,381,364 4/1983 Georgacopoulos et al. ....... 524/373
4,430,384 2/1984 George ................................ 428/377 15 Claims, No Drawings
4,892,683
1. 2
other additives in PVC and with PVC itself in PVC
FLAME RETARDANT LOW SMOKE POLY(VINYL compositions exposed to high temperatures and/or
CHLORIDE) THERMOPLASTIC COMPOSITIONS flame. Accordingly, the preparation of PVC composi
tions having particular combinations of properties is
FIELD OF THE INVENTION largely an emperical art rather than a well developed
This invention relates to flame retardant plastic mate science.
rials, and more particularly, to flame retardant low In the area of PVC-based compositions for wire and
smoke poly(vinyl chloride) compositions. cable covering applications, it is very desirable to have
materials which are highly flame-retardant, tend to char
BACKGROUND OF THE INVENTION 10 rather than drip when burned or heated, produce a
Poly(vinyl chloride), hereafter referred to as PVC, is minimum amount of smoke when burned, and produce
extensively used in wire insulation and sheathing for light-colored smoke rather than dark smoke, while still
electric cables because of its ready availability, mechan possessing the good processing properties, mechanical
ical toughness, low cost, resistance to chemicals and 15
toughness, and resistance to environmental stresses for
weathering, and good dielectric properties. which PVC compositions are known.
In use, PVC is always plasticized to overcome its SUMMARY OF THE INVENTION
natural rigidity and permit it to be processed into a
flexible material. In addition, other additives such as The above-stated need is met in the present invention,
thermal stabilizers, lubricants, pigments, fillers, impact 20 which provides PVC-based thermoplastic compositions
modifiers, and flame retardants are generally employed which are strongly flame retardant, tend to char rather
to produce PVC compositions having desired proper than drip when burned, produce only relatively small
ties. amounts of light-colored smoke when burned, and still
Unmodified PVC is thermally unstable, decomposing possess good processing properties, toughness, and re
at about 150 C. to release HCl and produce sites of sistance to environmental stresses.
unsaturation in the polymer which lead to chain cross 25 The flame retardant low smoke PVC-based composi
linking and scission, resulting in degradation of the tions of the present invention include poly(vinyl chlo
polymer's properties. As the PVC decomposes, the ride), an additional chlorinated resin, tribasic lead sul
resin becomes discolored, brittle, and finally insoluble. fate, a molybdenum-containing smoke suppressing ma
To improve thermal stabilitY, various thermal stabi terial, alumina trihydrate, a brominated aromatic ester
lizers are nearly always employed in PVC composi 30
plasticizer, at least one additional plasticizer besides the
tions. The stabilizers generally used are metallic salts of brominated aromatic ester, and at least one lubricant.
inorganic and organic acids and phenols, organometal
lics, epoxy compounds, and phosphates. In wire and DETAILED DESCRIPTION OF THE
cable applications, lead stabilization systems are widely INVENTION
used. 35
Despite its thermal instability, unmodified PVC has The flame retardant low smoke compositions of the
relatively good flame retardant properties due to its present invention have as their base resin a mixture of
high chlorine content. However, the plasticizer neces PVC and an additional chlorinated resin. Throughout
sary for flexibility and good processing properties gen this specification, all amounts of composition ingredi
erally increases the flammability of PVC compositions, ents, including the amounts of PVC and the additional
especially if used at high levels. Moreover, when PVC chlorinated resin, will be expressed as parts per hundred
burns, it produces considerable smoke, and the addition of the sum of PVC and the additional chlorinated resin
of flame retardant to plasticized compositions to reduce in the composition.
their flammability generally increases smoke generation All ingredients comprising the compositions of this
upon burning. Smoke is particularly dangerous since it 45 invention are commercially available materials, the
not only contains toxic by-products of combustion and identities of which are listed below:
thermal decomposition of the plastic, but also restricts a GEON 102EP, a high viscosity, high molecular
visibility and disorients potential victims, resulting in weight PVC, Chemical Abstracts Registry No.
panic. 9002-86-2, purchased from the B.F. Goodrich Com
A further problem with burning olefin-based poly 50 pany;
mers generally and PVC in particular is that when they b. TEMPRITE 627X563, chlorinated poly(vinyl chlo
burn they frequently flow and drip combustible materi ride) resin, purchased from the B.F. Goodrich Com
als, thus feeding and spreading the fire. pany;
The plastics industry has long recognized that use of c. CPE 631, a chlorinated polyethylene containing ap
PVC in interior furnishings, building materials, and 55 proximately 42% chlorine, Chemical Abstracts Reg
coverings for wire and cable presents the hazards of istry No. 63231-66-3, purchased from the Dow
flame, toxic decomposition products, and smoke in the Chemical Company;
event of fire, as discussed above. It has therefore ex d. TRIBASE, tribasic lead sulfate, Chemical Abstracts
pended very considerable efforts to find additives for Registry No. 12202-17-4, a heat stabilizer purchased
PVC which reduce thermal decomposition, flammabil 60 from Associated Lead, Inc.;
ity, and smoke in the event that such PVC compositions e. Ammonium octamolybdate, abbreviated later as
are subjected to high temperatures or flame. AOM, a smoke suppressant having a Chemical Ab
Such research has yielded knowledge of several stracts Registry No. 12411-64-2, purchased from Cli
classes of stabilizers, flame retardants, smoke suppres max Molybdenum;
sants, plasticizers, etc., which function in PVC, and has 65 f. KEMGARD 911C, a smoke suppressant having a
disclosed many useful individual chemical compounds Chemical Abstracts Registry No. 76774-99-7, pur
within those classes, but it has not yet provided a full chased from Sherwin Williams Company and be
understanding of how various additives interact with lieved to be a zinc molybdate produced by a reaction
4,892,683
3 4.
of molybdenum oxide and zinc oxide although the diphenylphosphate can be employed. Such materials are
Chemical Abstracts computer record indicates that available from Monsanto. Similarly, dioctyl sebacate
the formula for this material is unknown; can be replaced with other ester-type plasticizers such
g. SOLEM 932, alumina trihydrate, a flame retardant as dioctyl adipate.
and smoke suppressant having a Chemical Abstracts 5 Besides the proprietary brominated aromatic ester
Registry No. 21645-51-2, purchased from Solem In DP45, other highly halogenated materials can in princi
dustries; ple be employed, among them decabromodiphenyl ox
h. DP 45, a proprietary brominated aromatic ester ide, and SAYTECH BT93 and SAYTECH 120 from
which is believed to be a brominated dioctyl phthal Ethyl Corporation.
ate and which is used as a flame retardant plasticizer, 10 A number of lubricants are known to be suitable for
purchased from the Great Lakes Chemical Company; use in PVC-based compositions, so besides stearic acid,
i. TOPANOL CA, an antioxidant having the chemical dibasic lead stearate, and the paraffin waxes, other ma
name 4,4,4'-(1-methyl-1-propanyl-3-ylidene)tris(2- terials such as AC 629A polyethylene wax may een
(1,1-dimethyl-ethyl)-5-methyl phenol, having the ployed.
Chemical Abstracts Registry No. 1843-03-4, pur 15 Similarly, in place of alumina trihydrate, materials
chased from ICI America; such as magnesium carbonate may be employed. Fur
j. LSFR antimony trioxide, a low smoke flame retardant ther, besides antimony trioxide, antimony oxide-con
having the Chemical Abstracts Registry No. taining materials such as ONGARD-2 of Anzon Inc.
1309-64.4, purchased from Lauryl Industries; may be employed.
k. ELVALOY 741, a plasticizer which is a terpolymer 20 Besides SP 33 clay filler, others may in principle also
of acrylic acid, ethylene, and vinyl acetate, Chemical be used, among them silicate fillers such as SATIN
Abstracts Registry No. 26713-18-8, purchased from TONE 2 and BURGESS 30 by Burgess.
DuPont; The flame retardant low smoke compositions of the
1. SANTICIZER 148, a plasticizer comprising isodecyl present invention include the following ingredients in
diphenylphosphate, this phosphate having the Chem 25 the amounts listed:
ical Abstracts Registry No. 29761-21-5, purchased poly(vinyl chloride) such as GEON 102EP, in an
from the Monsanto Chemical Company; amount from about 60 to about 90 parts per hundred,
m. Dioctyl sebacate, a plasticizer having the Chemical and preferrably about 75 to about 90 parts per hundred
Abstracts Registry No. 122-62-3, purchased from the of resin;
C.P. Hall Company; 30 an additional chlorinated resin such as chlorinated
n. PX 336, a plasticizer having the chemical name n poly(vinyl chloride) or chlorinated polyethylene, these
octyl-n-decyl trimellitate, Chemical Abstracts Regis materials not being equivalents for purposes of the wire
try No. 34870-88-7, purchased from Aristech; insulation and cable jacketing formulations disclosed
o. Stearic acid, a lubricant having the Chemical Ab below and claimed, the additional chlorinated resin
stracts Registry No. 57-11-4, purchased from Syn 35 being employed in an amount from about 40 to about 10
thetic Products, Inc.; parts per hundred, preferrably from about 25 to about
p. DS 207, a dibasic lead stearate lubricant, Chemical 10 parts per hundred of resin;
Abstracts Registry No. 56.189-09-4, purchased from tribasic lead sulfate, in an amount from about 6 to
Associated Lead, Inc.; about 12 parts per hundred, preferrably about 8 to about
q. ARISTOWAX 65, a paraffin wax lubricant having 40 12 parts per hundred of resin;
the Chemical Abstracts Registry No. 8002-74-2, pur a molybdenum-containing smoke suppressing mate
chased from the Ross Corporation; rial such as ammonium octamolybdate or zinc molyb
r. SP 33, a calcined aluminum silicate filler having the date, these materials not being equivalents for purposes
Chemical Abstracts Registry No. 39388-40-4, pur of the wire insulation and cable jacketing formulations
chased from the Englehard Corporation; 45 disclosed below and claimed, the molybdenum-contain
In PVC-based thermoplastic materials, lead com. ing smoke suppressing material being employed in an
pounds such as dibasic lead phthalate and tribasic lead amount from about 10 to about 30 parts per hundred,
Sulfate are frequently employed as heat stabilizers. preferrably about 15 to about 25 parts per hundred of
However, other heat stabilizers can in principle be used, resin;
among them various proprietary soaps containing bar 50 alumina trihydrate, in an amount from about 10 to
ium, cadmium, or zinc, such as MARKOHM, a barium about 50 parts per hundred, preferrably about 20 to
cadmium soap. Organotin compounds may also be em about 50 parts per hundred of resin;
ployed. a brominated aromatic ester plasticizer, in an amount
Similarly, other antioxidants besides TOPANOL CA from about 10 to about 30 parts per hundred, preferra
may in principle be used, among them various IR 55 bly about 15 to about 30 parts per hundred of resin;
GANOX materials, hindered phenols such as ETHYL at least one additional plasticizer besides the bromi
330 and bisphenol A, and hindered amines such as SEE nated aromatic ester, such additional plasticizer being
NOX 412S of Witco. efficacious in PVC-based plastic materials, the total
Likewise, besides ELVALOY 741, other plasticizers amount of such additional plasticizer being from about
may in principle be used, among them such materials as 60 20 to about 45 parts per hundred, preferrably about 25
trisooctyl trimellitate, HERCOFLEX 707, medium to about 40 parts per hundred of resin;
and high molecular weight polyester plasticizers such as and at least one lubricant efficacious in PVC-based
SANTICIZERS429 and DRAPEXP-1 by Witco, and plastic materials, the total amount of such lubricants
PLASTOLEINS 9780 and 9790 by Emery. Alternative being from about 0.3 to about 1.5 parts per hundred,
trimellitate plasticizers include trioctyl trimellitate, and 65 preferrably about 0.4 to about 1.0 parts per hundred of
trisononyl trimellitate. S.
In place of SANTICIZER 148, other phosphate plas The composition of the invention may also include
ticizers such as triaryl phosphate and t-butylphenyl the following materials:
4,892,683
5 6
at least one antioxidant efficacious in PVC-based per hundred, preferrably about 15 to about 25 parts per
plastic materials, a preferred antioxidant being TOPA hundred of resin;
NOL CA, the total amount of such antioxidant being stearic acid, in an amount from about 0.15 to about 0.6
from about 0.15 to about 0.6 parts per hundred, and parts per hundred, preferrably about 0.15 to about 0.4
preferrably from about 0.15 to about 0.4 parts per hun parts per hundred of resin;
dred of resin; dibasic lead stearate such as DS 207, in an amount
antimony trioxide, in an amount -from about 2 to from about 0.15 to about 0.6 parts per hundred, prefer
about 8 parts per hundred, preferrably from about 3 to rably about 0.15 to about 0.4 parts per hundred of resin;
about 6 parts per hundred of resin; and 10
a paraffin wax such as ARISTOWAX 165, in an
a filler such as a calcined aluminum silicate, in an amount from about 0.15 to about 0.6 parts per hundred,
amount from about 10 to about 30 parts per hundred, preferrably about 0.15 to about 0.4 parts per hundred of
preferrably about 15 to about 25 parts per hundred of resin;
eS1 dioctyl sebacate, in an amount from about 4 to about
The additional plasticizer or plasticizers besides the 5
10 parts per hundred, preferrably about 6 to about 8
brominated aromatic ester are preferrably selected from parts per hundred of resin;
the group dioctyl sebacate, n-octyl-n-decyl trimellitate, n-octyl-n-decyl trimellitate, PX 336 for example, in
an isodecyl diphenyl phosphate material such as that an amount from about 10 to about 30 parts per hundred,
known commercially as SANTICIZER 148, and a ter preferrably from about 12 to about 20 parts per hundred
polymer of acrylic acid, ethylene, and vinyl acetate of resin; and
such as that known commercially as ELVALOY 741. antimony trioxide, in an amount from about 2 to
More particularly, the combination of dioctyl sebacate, about 8 parts per hundred, preferrably about 3 to about
n-octyl-n-decyl trimellitate, and DP 45 is advantageous, 6 parts per hundred of resin.
the DP 45 providing improved flame retardancy at the A cable jacketing formulation contains the following
cost of increasing brittleness of the compositions, while 25 ingredients in the amounts listed:
the dioctyl sebacate provides compensating increases in PVC such as GEON 102EP in an amount from about
flexibility at low temperatures and n-octyl-n-decyl tri 60 to about 90 parts per hundred, preferrably about 75
mellitate similarly increases flexibility at higher temper to about 90 parts per hundred of resin;
atures. a chlorinated PVC such as TEMPRITE 627X563, in
Lubricants useful in the composition of the invention 30 an amount from about 40 to about 10 parts per hundred,
are preferrably materials such as stearic acid, dibasic preferrably about 25 to about 10 parts per hundred of
lead stearate, and paraffin waxes. resun;
The compositions of the invention may be embodied a terpolymer of acrylic acid, ethylene, and vinyl ace
in formulations optimized for use as wire insulation and tate, ELVALOY 741 for example, in an amount from
as cable jacketing, as shown below. 35 about 10 to about 40 parts per hundred, preferrably
A wire insulation formula contains the following about 15 to about 25 parts per hundred of resin;
ingredients in the amounts listed: tribasic lead sulfate such as TRIBASE, in an amount
PVC such as GEON 102EP, in an amount from about from about 6 to about 12 parts per hundred, preferrably
60 to about 90 parts per hundred, preferrably about 75 about 8 to about 12 parts per hundred of resin;
to about 90 parts per hundred of resin; ammonium octamolybdate, in an amount from about
chlorinated polyethylene such as CPE 631, in an 10 to about 30 parts per hundred, preferrably about 15
amount from about 40 to about 10 parts per hundred, to about 25 parts per hundred of resin;
preferrably from about 25 to about 10 parts per hundred alumina trihydrate such as SOLEM 932M, in an
of resin; amount from about 10 to about 50 parts per hundred,
tribasic lead sulfate such as TRIBASE, in an amount 45 preferrably about 20 to about 50 parts per hundred of
from about 6 to about 12 parts per hundred, preferrably resin;
about 8 to about 12 parts per hundred of resin; . a brominated aromatic ester such as DP 45, in an
a zinc molybdate such as KEMGARD 911C, in an amount from about 10 to about 30 parts per hundred,
amount from about 10 to about 30 parts per hundred, preferrably about 15 to about 30 parts per hundred of
preferrably about 15 to about 25 parts per hundred of 50
resin; resin;
alumina trihydrate such as SOLEM 932M, in an isodecyl diphenyl phosphate material, SANTI
amount from about 10 to about 30 parts per hundred, CIZER 148 for example, in an amount from about 5 to
preferrably about 20 to about 30 parts per hundred of about 20 parts per hundred, preferrably about 6 to about
resin; 55 15 parts per hundred of resin;
a brominated aromatic ester such as DP 45, in an an antioxidant such as TOPANOL CA, in an amount
amount from about 10 to about 30 parts per hundred, from about 0.15 to about 0.6 parts per hundred, prefer
preferrably about 15 to about 20 parts per hundred of rably about 0.15 to about 0.4 parts per hundred of resin;
resin; stearic acid, in an amount from about 0.15 to about 0.6
isodecyl diphenyl phosphate such as SANTICIZER 60 parts per hundred, preferrably about 0.15 to about 0.4
148, in an amount from about 5 to about 20 parts per parts hundred of resin;
hundred, preferrably about 10 to about 15 parts per dibasic lead stearate such as DS 207, in an amount
hundred of resin; from about 0.15 to about 0.6 parts per hundred, prefera
an antioxidant such as TOPANOL CA, in an amount bly about 0.15 to about 0.4 parts per hundred of resin;
from about 0.15 to about 0.6 parts per hundred, prefer 65 a paraffin wax such as ARISTOWAX 165, in an
rably about 0.15 to about 0.4 parts per hundred of resin; amount from about 0.15 to about 0.6 parts per hundred,
a filler such as a calcined aluminum silicate, SP 33 for preferrably about 0.15 to about 0.4 parts per hundred of
example, in an amount from about 10 to about 30 parts resin;
4,892,683
7 8
dioctyl sebacate, in an amount from about 3 to about Next, 25 phr of SOLEM 932M, 20 phr of KEMGARD
10 parts per hundred, preferrably about 6 to about 8 911C, 20 phr of SP 33, 3 phr of LSFR antimony triox
parts per hundred of resin; ide, 0.2 phr of TOPANOL CA, 0.2 phr of stearic acid,
n-octyl-n-decyl trimelitate, PX 336 for example, in 0.2 phr of DS 207,and 0.2 phr of ARISTOWAX 165
an amount from about 8 to about 25 parts per hundred, 5 were added and mixed for ten minutes. Finally, 10 phr
preferrably about 10 to about 20 parts per hundred of of CPE 631 was added and the blend was processed on
resin; and a Banbury mixer for approximately 150 seconds at 350
antimony trioxide, in an amount from about 2 to F. then dropped on a hot two-roll mill, subsequently
about 8 parts per hundred, preferrably about 3 to about stripped off, and diced.
6 parts per hundred of resin. O The resulting composition exhibited an oxygen index
The compositions of the invention are prepared using of 41.3% and maximum smoke specific optical densities
steps that are individually known to those skilled in the of 260 (flaming) and 290 (smoldering).
art, in a manner known to the art. A steam heated PREPARATION OF CABLE JACKETING
blender is employed to mix the ingredients, then the FORMULATION
initial blend is further processed in a Banbury high 15
intensity mixer for a predetermined time at a predeter Initially, 25 phr of DP 45, 5 phr of dioctyl sebacate,
mined temperature. Finally, the blend is dropped onto a 12 phr of PX336, and 8 phr of SANTICIZER 148 were
hot two-roll mill, and ultimately stripped off the roll preheated at 150 F. in a suitable container. This mix
mill and diced. Twin screw extruders, continuous mix ture was added to a mixture of 85 phr of GEON 102EP,
ers, or other mixing equipment known to the art will 20 15 phr of TEMPRITE 627X563, and 10 phr of TRI
also serve in place of the Banbury mixer. BASE in a blender, which was heated with steam and
EXPERIMENTAL run until the mixture was dry. The blender was cooled
by circulating water through it, then 45 phr of SOLEM
Formulations of the compositions of the invention 932M, 25 phr of ammonium octamolybdate, 3 phr of
optimized respectively for wire insulation and for cable 25 LSFR antimony trioxide, 0.2 phr of TOPANOL CA,
jacketing were prepared as shown below. Ingredient 0.2 phr of stearic acid, 0.2 phr of DS 207, and 0.2 phr of
amounts are shown as parts per hundred of the sum of ARISTOWAX 165 were added, and mixed for ten
PVC and the additional chlorinated resin employed, the minutes. The blend was then transferred to a Banbury
units being abbreviated phr. mixer along with 12 phr of ELVALOY 741 and mixed
Tests for Oxygen Index and Specific Optical Density 30 for approximately 150 seconds at temperature of ap
of Smoke were performed using ASTM standard test proximately 340 F., then dropped on a hot two-roll
procedures D-2863 and E-662 respectively, and these mill, subsequently stripped off, and diced.
test methods are expressly incorporated herein by refer The resulting composition exhibited an oxygen index
eCe. of 50% and maximum smoke specific optical densities of
35 233 (flaming) and 275 (smoldering).
PREPARATION OF WIRE INSULATION
FORMULATION TEST FORMULATIONS OF THE COMPOSITION
Initially, 11 phr of SANTICIZER 148 plasticizer, 18 OF THE INVENTION
phr of DP45plasticizer, 6 phr of dioctyl sebacate plasti The compositions shown in Tables I and II below
cizer, and 15 phr of PX 336 plasticizer were mixed and 40 were prepared according to the above procedures em
preheated to 100 F. in a suitable container. This was ploying the listed relative amounts of ingredients. Table
added to 90 phr of GEON 102EPPVC in a blender, no I shows a number of experimental preparations of wire
additional heat being provided to the blender. Next, 10 insulation formulation of the above composition. Table
phr of TRIBASE was added and the blender was II similarly shows several experimental preparations of
heated with steam to dry the mixture, after which the 45 cable jacketing formulations of the basic composition.
blender was cooled by circulating water through it.
TABLE I
WIRE INSULATION FORMULATIONS:
Ingredients A. B C D E F G
GEON 102EP 90 80 90 90 90 90 70
CPE 631 10 20 10 O 10 O 30
TRIBASE 10 10 10 10 10 O O
KEMGARD 91C 20 20 2O O 20 35 25
SP33 2O 20 10 10 20 20 2O
SOLEM 932M 25 25 25 35 25 5 35
TOPANOL CA O.2 0.2 O.2 0.2 0.2 0.2 0.2
Stearic Acid 0.2 0.2 0.2 0.2 0.2 0.2 0.2
DS 207 0.2 0.2 0.2 0.2 0.2 O.2 0.2
ARISTOWAX 165 O.2 0.2 0.2 0.2 0.2 0.2 O.2
SANTICIZER 148 1 11 11 7
DP 45 8 8 18 18 22 18 18
Dioctyl Sebacate 6 6 6 6 6 6 6
PX336 15 5 5 15 15 15 5
LSFR Antimony Oxide 3 3 3 3 3 3 3
Oxygen Index 4.3 40.5 40.0 43.0 42.5 39.5 41.0
Smoke Optical Density (sample thickness 100 mils):
D (corr.) Flaming 260 245 268 270 275 250 250
Din (cort.) Smoldering 290 28O 295 300 296 275 285
"Amounts of ingredients are expressed as parts per hundred of the sum of PVC and CPE employed.
4,892,683
9 10
TABLE II
CABLE JACKETING FORMULATIONS
Ingredients A. B C D E F G
GEON 102 EP 85 85 85 85 100 70 80
TEMPRITE 62TX563 15 15 15 15 -- 30 20
ELVALOY 741 12 18 18 2 22 12 2
TRIBASE 10 10 10 O 10 10 10
AOM 25 20 20 20 25 25
SOLEM 932M 45 35 35 35 45 45 45
TOPANOL CA 0.2 0.2 0.2 0.2 0.2 0.2 0.2
Stearic Acid 0.2 0.2 0.2 0.2 0.3 0.2 0.2
DS 207 0.2 0.2 0.2 0.2 0.2 0.2 0.2
ARISTOWAX 16S 0.2 0.2 O2 0.2 0.2 0.2 0.2
SANTICIZER 148 8 10 10 10 O 8 2
DP 45 25 22 18 25 18 25 8
Dioctyl Sebacate 5 5 5 5 5 5 8
PX336 12 15 15 15 15 2 2
LSFR Antimony Oxide 3 3 3 3 3 3 3
Oxygen Index 50 48 45 49 45 50.5 47
Snoke Optical Density (sample thickness 100 mils):
D (corr.) Flaming 233 250 248 255 210 240 215
Dn (corr.) Smoldering 275 290 280 288 250 280 248
*Amounts of ingredients are expressed as parts per hundred of the sum of PVC and chlorinated PVC
employed.

An experimental preparation like preparation A of


Table II except that 25 phr of KEMGARD 911C was
employed in place of the AOM gave a composition 25 consisting of dioctyl sebacate, n-octyl-n-decyl trimelli
having an Oxygen Index of 49.5%, and Smoke Optical tate, and isodecyl diphenyl phosphate.
Densities as follows: Dn (corr.) flaming-255; Dn 6. The composition of claim 1 wherein said at least
(corr.) smoldering-290. This was judged unsuitable for one lubricant is selected from the group consisting of
the intended purpose. stearic acid, dibasic lead stearate, and paraffin waxes.
What is claimed is: 30 7. The composition of claim 1 further comprising at
1. A flame retardant smoke-suppressed thermoplastic least one filler suitable for use in PVC-based plastic
composition comprising the below-listed materials, materials, the total amount of said fillers in said thermo
amounts being expressed as parts per hundred of the plastic composition being from about 10 to about 30
sum of poly(vinyl chloride) and chlorinated polyethyl parts per hundred of resin.
ene resins in the composition: 35 8. A flame retardant smoke-suppressed thermoplastic
poly(vinyl chloride), in an amount from about 60 to composition comprising the below-listed materials,
about 90 parts per hundred of resin; amounts being expressed as parts per hundred of the
chlorinated polyethylene, in an amount from about 40 sum of poly(vinyl chloride) and chlorinated poly(vinyl
to about 10 parts per hundred of resin; chloride) resins in the composition:
tribasic lead sulfate, in an amount from about 6 to poly(vinyl chloride), in an amount from about 60 to
about 12 parts per hundred of resin; about 90 parts per hundred resin; w
a zinc molybdate, in an amount from about 10 to chlorinated poly(vinyl chloride), in an amount from
about 30 parts per hundred of resin; about 40 to about 10 parts per hundred of resin;
alumina trihydrate, in an amount from about 10 to a plasticizer which is a terpolymer of acrylic acid,
about 30 parts per hundred of resin; 45 ethylene, and vinyl acetate, in an amount from
a brominated aromatic ester plasticizer, in an amount about 10 to about 40 parts per hundred of resin;
from about 10 to about 30 parts per hundred of tribasic lead sulfate, in an amount from about 6 to
resin; about 12 parts per hundred of resin;
at least one additional plasticizer besides said bromi ammonium octamolybdate, in an amount from about
nated aromatic ester, said at least one additional 50 10 to about 30 parts per hundred of resin;
plasticizer being efficacious in PVC-based plastic alumina trihydrate, in an amount from about 10 to
materials; and about 50 parts per hundred of resin;
at least one lubricant efficacious in PVC-based plastic a brominated aromatic ester plasticizer, in an amount
materials. from about 10 to about 30 parts per hundred of
2. The composition of claim 1 further comprising at 55 resin;
least one antioxidant efficacious in PVC-based plastic at least one additional plasticizer besides said bromi
materials, the amount of said at least one antioxidant nated aromatic ester and said terpolymer of acrylic
being from about 0.15 to about 0.6 parts per hundred of acid, ethylene, and vinyl acetate, said at least one
eS additional plasticizer being efficacious in PVC
3. The composition of claim 2 wherein said at least 60 based plastic materials; and
one antioxidant comprises 4,4',4'-(1-methyl-1-propa at least one lubricant efficacious in PVC-based plastic
nyl-3-ylidene) tris(2-(1,1-dimethylethyl)-5-methyl phe materials.
nol. 9. The composition of claim 8, further comprising:
4. The composition of claim 1 further comprising at least one antioxidant efficacious in PVC-based
antimony trioxide in an amount from about 2 to about 8 65 material, in an amount from about 0.15 to about
parts per hundred of resin. 0.15 to about 0.6 parts per hundred of resin.
5. The composition of claim 1 wherein said at least 10. The composition of claim 9 wherein said at least
one additional plasticizer is selected from the group one antioxidant comprises 4,4', 4'-(1-methyl-1-propa
W 4,892,683
11 12
c1 1?t a 13. The composition of claim 8 wherein said lubricant
nyl-3-ylidene) tris(2-(1,1-dimethylethyl)-5-methyl phe is selected from the group consisting of stearic acid,
nol. dibasic lead stearate, and paraffin waxes.
11. The composition of claim 8 further comprising 14. An insulated wire comprising:
5 at least one electrically conductive wire and an insu
antimony trioxide in an amount from about 2 to about 8 lation about said at least one wire, said insulation
parts per hundred of resin. imprising the thermoplastic composition of claim
12. The composition of claim 8 wherein said addi- 15. A jacketed electrical cable comprising:
tional plasticizer is selected from the group consisting of 10 at least one electrical cable and cable jacketing about
dioctyl sebacate, n-octyl-n-decyl trimellitate, and iso said at least one cable, said cable jacketing compris
ing the thermoplastic composition of claim 8.
decyl diphenyl phosphate. ck k : : :

15

20

25

30

35

40

45

50

55

60

65
UNITED STATES PATENT AND TRADEMARK OFFICE
CERTIFICATE OF CORRECTION
PATENT NO. : 4,892,683
DATED : January 9, 1990
INVENTOR(S) ; Homaira Naseem
it is certified that error appears in the above-identified patent and that said Letters Patent is hereby
corrected as shown below:

Column 1, line 29, "stability," should read --stability--.


Column 3, line 13, "4, 4, 4"" should read --4, 47, 4"--.
Column 4, line 13, "may e" should read --may be--.
Column 5, line 7, "-from" should read --from--.

Signed and Sealed this


Ninth Day of November, 1993

(a teen
BRUCELEHMAN

Attesting Officer Commissioner of Patents and Trademarks

You might also like