U.S. patent number RE30,193 [Application Number 05/657,321] was granted by the patent office on 1980-01-15 for fire retardant agent.
Invention is credited to James D. O'Shaughnessy.
United States Patent |
RE30,193 |
O'Shaughnessy |
January 15, 1980 |
**Please see images for:
( Certificate of Correction ) ** |
Fire retardant agent
Abstract
A fire retardant agent comprising calcium or magnesium mineral
borates or calcium or magnesium meta borate and a halogen source; a
method of rendering organic materials generally of a hydrocarbon
nature, such as plastic and rubber polymers, cellulosics, resins
and oils, etc., fire retardant by introducing into said organic
materials calcium or magnesium mineral borates or calcium or
magnesium meta borate and a halide; articles, laminates, coatings,
foams, papers, fabrics, etc. containing calcium or magnesium
mineral borates or calcium or magnesium meta borate and a halide of
atomic weight greater than 19.
Inventors: |
O'Shaughnessy; James D.
(Gouverneur, NY) |
Family
ID: |
27001964 |
Appl.
No.: |
05/657,321 |
Filed: |
February 11, 1976 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
Issue Date |
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Reissue of: |
363212 |
May 23, 1973 |
03897387 |
Jul 29, 1975 |
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Current U.S.
Class: |
521/85;
106/18.26; 521/103; 524/165; 524/285; 524/359; 524/405;
524/467 |
Current CPC
Class: |
C08J
9/0095 (20130101); C08K 3/38 (20130101) |
Current International
Class: |
C08K
3/38 (20060101); C08K 3/00 (20060101); C08J
9/00 (20060101); C08C 011/04 () |
Field of
Search: |
;260/45.7R,29.7UA,28.5A,28.5B,28R,18.26 ;106/15FP |
References Cited
[Referenced By]
U.S. Patent Documents
Other References
Velea et al., "Materiale Plastice", vol. 3, No. 1966, pp. 9-13.
.
Kirk et al., "Encyclopedia of Chemical Technology," vol. 3, 1964,
pp. 649 and 650..
|
Primary Examiner: Marquis; Melvyn I.
Attorney, Agent or Firm: Sprung, Felfe, Horn, Lynch &
Kramer
Claims
What is claimed is:
1. A fire retardant agent comprising a calcium .[.or magnesium.].
mineral borate or a calcium .[.or magnesium.]. metaborate and a
halogen source, said halogen having an atomic weight greater than
19.
2. A composition according to claim 1 wherein the calcium .[.or
magnesium.]. mineral borate is selected from the group consisting
of 2CaO.B.sub.2 O.sub.3.H.sub.2 O; CaO.B.sub.2 O.sub.3.6H.sub.2 O;
CaO.B.sub.2 O.sub.3.4H.sub.2 O; CaO.B.sub.2 O.sub.3.3.65H.sub.2 O;
2CaO.3B.sub.2 O.sub.3.H.sub.2 O; 2CaO.3B.sub.2 O.sub.3.13H.sub.2 O;
2CaO.3B.sub.2 O.sub.3.9H.sub.2 ; 2CaO.3B.sub.2 O.sub.3.7H.sub.2 O;
CaO.B.sub.2 O.sub.3.2H.sub.2 O; Colemanite, .[.Boracite,.].
Sassolite, Ulexite, Tertschite, Probertite, Princeite, Pandermite,
Inyoite, Meyerhofferite, Nobleite, Gowerite, Ginorite, Calciborite,
.[.Inderborite, Hydroborocite,.]. K.sub.2 O.CaO.4B.sub.2
O.sub.3.12H.sub.2 O; (NH.sub.4).sub.2.CaO.4B.sub.2
O.sub.3.12H.sub.3 O and Na.sub.2 O.2CaO.5B.sub.2 O.sub.3.16H.sub.2
O.[.; Pinnoite, Ascherite, Szaibelyite, Inderite, Kurnakovite,
Preobrazlienskite, M.sub.g O.2B.sub.2 O.sub.3.8.5H.sub.2 O;
MgO.3B.sub.2 O.sub.3.7.5H.sub.2 O; MgO.3B.sub.2 O.sub.3.5H.sub.2 O;
Suanite, (NH.sub.4).sub.2 O.MgO.3B.sub.2 O.sub.3.15H.sub.2 O and
(NH.sub.4).sub.2 O.MgO.3B.sub.2 O.sub.3.7H.sub.2 O.]..
3. A composition according to claim 2 wherein the calcium .[.or
magnesium.]. borate preferably has a negligable solubility in water
at 25.degree. C.
4. A composition according to claim 2 wherein the halogen source is
selected from the group consisting of halogen-containing polymers,
halogen-containing rubbers, halogen-containing phenolics,
halogenated aliphatic compounds and halogenated aromatic
compounds.
5. A composition according to claim 4 wherein the halogen source is
selected from the group consisting of halogenated acids where the
halogen is on a non-carbonyl atom, said acid having between 3 and
24 carbon atoms and being saturated or unsaturated, polyethers,
ketones where at least one substituent attached to the carbonyl has
between 4 and 12 carbon atoms, aldehydes where the substituent
attached to the carbonyl group has between 4 and 12 carbon atoms,
anhydrides of halogenated acids where the halogen is on a
non-carbonyl atom and the group attached to the carbonyl atom has
between 3 and 24 carbon atoms, primary alcohols in which the group
attached to the OH radical has between 4 and 12 carbon atoms,
secondary alcohols in which at least one group attached to the
carbon atom to which the OH radical is attached has between 4 and
12 carbon atoms, acid halides of C.sub.2 to C.sub.12 atoms,
monosaccharides, polysaccharides, starch, cellulose, esters of said
acids, thio derivatives of said acids, aldehydes, ketones and
alcohols where the sulfur atom replaces the oxygen atom, aryl
compounds of C.sub.6 to C.sub.18 carbon atoms, aryl ethers where
the organic group attached to the oxygen contains at least 4 carbon
atoms, aryl aldehydes where the organic radical attached to the
oxygen atom contains between 4 and 12 carbon atoms, arylketones
where at one organic group attached to the oxygen atom has between
4 and 12 carbon atoms, alkenyl aryl compounds where the alkenyl
group contains between 4 and 12 carbon atoms, aryl alcohols where
at least one organic radical attached to the carbon bearing the
hydroxy group has between 4 and 12 carbon atoms, hydroxy aryl
compounds, sulfonated aryl compounds, nitrated aryl compounds, aryl
acid halides of C.sub.2 to C.sub.12 atoms in the acid halide group,
cyano aryl compounds, mercapto aryl compounds, amine aryl
compounds, aromatic dicarboxylicacids and their anhydrides, cyclic
and heterocyclic organic chemicals having between 5 and 10 members
in the ring.
6. A composition according to claim 2 wherein said halogen source
is selected from the group consisting of a compound having the
formula ##STR2## its acids, mixed acids, bi-acids, mixed esters,
bi-esters and anhydrides, wherein R can be H, C.sub.1 -C.sub.12
alkyl or a halogenated derivative thereof,
1,2,3,4-tetrachloro-5,5-dimethoxycyclopentadiene,
1,2,3,4-tetrachlorocyclopentadiene,
nonachlorobicyclo[3.2.0]heptene-2,
1,2-dichloro-3,3,4,4,5,5-hexafluorocyclopentene,
decachloropentacyclo[5.3.0.0.sup.2,6.0.sup.4,10.0.sup.5,9
]decan-3-one, octachlorocyclopentene,
bis(pentachloro-2,4-cyclopentadiene-1-yl),
1,2,3,3,5,5-hexachloro-4-(dichloromethylene)-cyclopentene,
perchloropentacyclo[5.2.1.0.sup.2,6.0.sup.3,9.0.sup.5,8 ]-decane,
2,3,4,4,5-pentachloro-2-cyclopentene-1-one,
1,2,4-trichlorcyclopentene-3,5-dione,
1,2,3,4,7-hexachlorobicyclo[2.2.1]-2,5-heptadiene,
1,4,5,6,7,7-hexachlorobicyclo[2.2.1]-5-heptene-2,3-dicarboxylic
acid,
1,4,5,6,7,7-hexachloro-2,3-bis(chloromethyl)-bicyclo[2.2.1]-5-heptene,
1,4,5,6,7,7-hexachloro-2-(1,2-dichloroethyl)-bicyclo[2.2.1]-5-heptene,
1,4,5,6,7,7-hexachloro-2-carboxybicyclo[2.2.1]-5-heptene,
1,4,5,6,7,7-hexachloro-2,3-bis(hydroxymethyl)-bicyclo[2.2.1]-5-heptene,
undecachloropentacyclo [5.3.0.sup.2,6.0.sup.4,10.0.sup.5,9
]-3-decyclorosulfonate, 4,5,6,7,8,8-hexachloro-3a,
7a-dihydro-4,7-methano-indene,
1,2,3,4,10,10-hexachloro-1,4,4a,5,8,8a-hexahydro-1,4,-endo,
exo-5,8-dimethanonaphthalene,
1,4,5,6,7,7-hexachloro-2-formylbicyclo[2.2.1]-5-heptene,
1,4,5,6,7,7-hexachloro-2-cyanobicyclo[2.2.1]-5-heptene, and
hexachlorocyclopentenones.
7. A composition according to claim 4 wherein the mineral is
present together with the halogen such that the weight ratio of
mineral borate to halogen is between 1 and 8.
8. A composition according to claim 7 wherein said ratio is between
1 and 4.
9. A composition comprising a normally flammable organic material
and the fire-retardant composition of claim 2.
10. A flame-stabilized composition comprising a normally flammable
organic material and the fire retardant composition of claim 5.
11. A flame-stabilized composition comprising a normally flammable
organic material and the flame retardant composition of claim
6.
12. A flame-stabilized composition comprising a normally flammable
organic material and the flame retardant composition of claim 6,
the weight ratio of mineral to halogen source being between 1 and 8
and the mineral being present in the composition in an amount
between 2 and 400 parts per part of organic material.
13. A flame-stabilized composition according to claim 12 wherein
the amount of mineral introduced is between 5 and 50 parts per 100
parts of organic material and the weight ratio of mineral to
halogen is between 1 and 4.
14. A flame stabilized composition according to claim 13 wherein
the organic material is selected from the group consisting of
polymers of alpha olefins, vinyl polymers, polyamides, polyacetals,
polyurethanes, polyesters, rubbers and latexes.
15. A flame-stabilized composition according to claim 14 wherein
said organic material is a polymer of an alpha olefin.
16. A flame stabilized composition according to claim 15 wherein
said organic material is a polypropylene.
17. A flame-stabilized composition comprising a normally flammable
organic material selected from the group consisting of
polyethylene, polypropylene, polybutene-1, polyisobutylene,
polyvinyl chloride, polymethylmethacrylate, polyethylmethacrylate,
polyacrylonitrile, polyvinylalcohol, polyvinylacetate,
polyvinylbutyral, polystyrene, nylon 6, nylon 6/6, natural and
synthetic rubbers, natural and synthetic latexes,
polystyrene-butadiene, polyacrylonitrile acrylic polyethylenes,
chlorosulfonated polyethylenes, epichlorohydrin and its polymers,
ethylene-propylene copolymers, ethylene-propylene-diene
terpolymers, polyisoprene-acrylonitrile, polybutadiene,
polychloroprenes, polyisoprenes, polystyrene-isoprene and
polyurethane, said composition containing a flame retardant
composition which comprises a calcium or magnesium mineral borate
and a source of a halide of atomic weight greater than 19, said
source of halide being selected from the group consisting of a
compound having the formula ##STR3## its acids, mixed acids,
bi-acids, mixed esters, bi-esters and anhydrides, wherein R can be
H, C.sub.1 -C.sub.12 alkyl or a halogenated derivative thereof,
1,2,3,4-tetrachloro-5,5-dimethoxycyclopentadiene,
1,2,3,4-tetrachlorocyclopentadiene,
nonachlorobicyclo[3.2.0]heptene-2,
1,2-dichloro-3,3,4,4,5,5-hexafluorocyclopentene,
decachloropentacyclo[5.3.0.0.sup.2,6.0.sup.4,10.0.sup.5.9
]decan-3-one, octachlorocyclopentene,
bis(pentachloro-2,4-cyclopentadiene-1-yl),
1,2,3,3,5,5-hexachloro-4-(dichloromethylene)-cyclopentene,
perchloropentacyclo[5.2.1.0.sup.2,6.0.sup.3,9.0.sup.5,8 ]-decane,
2,3,4,4,5-pentachloro-2-cyclopentene-1-one,
1,2,4-trichlorocyclopentene-3,5-dione,
1,2,3,4,7-hexachlorobicyclo[2.2.1]-2.5-heptadiene,
1,4,5,6,7,7-hexachlorobicyclo[2.2.1]-5-heptene-2,3-dicarboxylic
acid, 1,4,5,6,7,7-hexachloro-2,3-bis(chloromethyl]-bicyclo
[2.2.1]-5-heptene,
1,4,5,6,7,7-hexachloro-2-(1,2-dichloroethyl)bicyclo
[2.2.1]-5-heptene, 1,4,5,6,7,7-hexachloro-2-carboxybicyclo
[2.2.1]-5-heptene,
1,4,5,6,7,7-hexachloro-2,3-bis(hydroxymethyl)-bicyclo[2.2.1]-5-heptene,
undecachloropentacyclo[5.3.0.sup.2,6.0.sup.4,10.0.sup.5,9
]-3-decyclorosulfonate, 4,5,6,7,8,8-hexachloro-3a,
7a-dihydro-4,7-methano-indene,
1,2,3,4,10,10-hexachloro-1,4,4a,5,8,8a-hexahydro-1,4,-endo,
exo-5,8-dimethanonaphthalene,
1,4,5,6,7,7-hexachloro-2-formylbicyclo[2.2.1]-5-heptene,
1,4,5,6,7,7-hexachloro-2-cyanobicyclo[2.2.1]-5-heptene, and
hexachlorocyclopentenones. .Iadd.
18. A composition comprising rubber and a flame-retarding agent
selected from the group consisting of calcium mineral borate or a
calcium metaborate and a halogen source, said halogen having an
atomic weight greater than 19. .Iaddend. .Iadd.
19. A composition according to claim 18, in which the calcium
mineral borate or calcium metaborate is a natural mineral
comprising a hydrated salt. .Iaddend. .Iadd.
20. A composition according to claim 19, in which the inorganic
compound is colemanite. .Iaddend. .Iadd.21. A composition according
to claim 19, in which the inorganic compound is selected from
ulexite and pandermite.
.Iaddend. .Iadd.22. A composition according to claim 18, which
contains calcium carbonate. .Iaddend. .Iadd.23. A composition
according to claim 18 which is unfoamed. .Iaddend. .Iadd.24. A
composition according to claim 18, which is foamed. .Iaddend.
.Iadd.25. Carpet comprising a composition as claimed in claim 18
adhered to the undersurface of said carpet.
.Iaddend. .Iadd.26. A composition of a normally flammable organic
material selected from the group consisting of a polymer of an
alpha olefin, a polyamide, a polyacetal, a polyurethane, a
polyester, a rubber, rubber latex and an acrylic polymer, a calcium
or magnesium mineral borate or a calcium or magnesium metaborate
and a halogen source, said halogen
having an atomic weight greater than 19. .Iaddend. .Iadd.27. A
composition according to claim 26 wherein said mineral borate is a
calcium borate. .Iaddend. .Iadd.28. A composition according to
claim 27 wherein said borate is colemanite. .Iaddend. .Iadd.29. A
composition according to
claim 26 wherein said mineral borate is a magnesium borate.
.Iadd.30. A composition according to claim 26 wherein the calcium
mineral borate is selected from the group consisting of
2CaO.B.sub.2 O.sub.3.H.sub.2 O; CaO.B.sub.2 O.sub.3.6H.sub.2 O;
CaO.B.sub.2 O.sub.3.4H.sub.2 O; CaO.B.sub.2 O.sub.3.3.65H.sub.2 O;
2CaO.3B.sub.2 O.sub.3.H.sub.2 O; 2CaO.3B.sub.2 O.sub.3.13H.sub.2 O;
2CaO.3B.sub.2 O.sub.3.9H.sub.2 O; 2CaO.3B.sub.2 O.sub.3.7H.sub.2 O;
CaO.B.sub.2 O.sub.3.2H.sub.2 O; Colemanite, Sassolite, Ulexite,
Tertschite, Probertite, Princeite, Pandermite, Inyoite,
Meyerhofferite, Nobleite, Gowerite, Ginorite, Calciborite, K.sub.2
O.CaO.4B.sub.2 O.sub.3.12H.sub.2 O; (NH.sub.4).sub.2.CaO.4B.sub.2
O.sub.3.12H.sub.2 O and Na.sub.2 O.2CaO.5B.sub.2 O.sub.3.16H.sub.2
O. .Iaddend. .Iadd.31. A composition according to claim 30 wherein
the calcium borate preferably has a negligable solubility in water
at 25.degree. C. .Iaddend. .Iadd.32. A composition according to
claim 30 wherein the halogen source is selected from the group
consisting of halogen-containing polymers, halogen-containing
rubbers, halogen-containing phenolics, halogenated aliphatic
compounds and halogenated aromatic compounds. .Iaddend. .Iadd.33. A
composition according to claim 30 wherein the halogen source is
selected from the group consisting of halogenated acids where the
halogen is on a non-carbonyl atom, said acid having between 3 and
24 carbon atoms and being saturated or unsaturated, polyethers,
ketones where at least one substituent attached to the carbonyl has
between 4 and 12 carbon atoms, aldehydes where the substituent
attached to the carbonyl group has between 4 and 12 carbon atoms,
anhydrides of halogenated acids where the halogen is on a
non-carbonyl atom and the group attached to the carbonyl atom has
between 3 and 24 carbon atoms, primary alcohols in which the group
attached to the OH radical has between 4 and 12 carbon atoms,
secondary alcohols in which at least one group attached to the
carbon atom to which the OH radical is attached has between 4 and
12 carbon atoms, acid halides of C.sub.2 to C.sub.12 atoms,
monosaccharides, polysaccharides, starch, cellulose, esters of said
acids, thio derivatives of said acids, aldehydes, ketones and
alcohols where the sulfur atom replaces the oxygen atom, aryl
compounds of C.sub.6 to C.sub.18 carbon atoms, aryl ethers where
the organic group attached to the oxygen contains at least 4 carbon
atoms, aryl aldehydes where the organic radical attached to the
oxygen atom contains between 4 and 12 carbon atoms, arylketones
where at one organic group attached to the oxygen atom has between
4 and 12 carbon atoms, alkenyl aryl compounds where the alkenyl
group contains between 4 and 12 carbon atoms, aryl alcohols where
at least one organic radical attached to the carbon bearing the
hydroxy group has between 4 and 12 carbon atoms, hydroxy aryl
compounds, sulfonated aryl compounds, nitrated aryl compounds, aryl
acid halides of C.sub.2 to C.sub.12 atoms in the acid halide group,
cyano aryl compounds, mercapto aryl compounds, amine aryl
compounds, aromatic dicarboxylicacids and their anhydrides, cyclic
and heterocyclic organic chemicals having between 5 and 10
members
in the ring. .Iaddend. .Iadd.34. A composition according to claim
30 wherein said halogen source is selected from the group
consisting of a compound having the formula ##STR4## its acids,
mixed acids, bi-acids, mixed esters, bi-esters and anhydrides,
wherein R can be H, C.sub.1 -C.sub.12 alkyl or a halogenated
derivative thereof,
1,2,3,4-tetrachloro-5,5-dimethoxycyclopentadiene,
1,2,3,4-tetrachlorocyclopentadiene,
nonachlorobicyclo[3.2.0]heptene-2,
1,2-dichloro-3,3,4,4,5,5-hexafluorocyclopentene,
decachloropentacyclo[5.3.0.0.sup.2,6.0.sup.4,10.0.sup.5,9
]decan-3-one, octachlorocyclopentene,
bis(pentachloro-2,4-cyclopentadiene-1-yl),
1,2,3,3,5,5-hexachloro-4-(dichloromethylene)-cyclopentene,
perchloropentacyclo[5.2.1.0.sup.2,6.0.sup.3,9.0.sup.5,8 ]-decane,
2,3,4,4,5-pentachloro-2-cyclopentene-1-one,
1,2,4-trichlorocyclopentene-3,5-dione,
1,2,3,4,7-hexachlorobicyclo[2.2.1]-2,5-heptadiene,
1,4,5,6,7,7-hexachlorobicyclo[2.2.1]-5-heptene-2,3-dicarboxylic
acid,
1,4,5,6,7,7-hexachloro-2,3-bis(chloromethyl)-bicyclo[2.2.1]-5-heptene,
1,4,5,6,7,7-hexachloro-2-(1,2-dichloroethyl)-bicyclo[2.2.1]-5-heptene,
1,4,5,6,7,7-hexachloro-2-carboxybicyclo[2.2.1]-5-heptene,
1,4,5,6,7,7-hexachloro-2,3-bis(hydroxymethyl)-bicyclo[2.2.1]-5-heptene,
undecachloropentacyclo[5.3.0.sup.2,6.0.sup.4,10.0.sup.5,9
]-3-decyclorosulfonate, 4,5,6,7,8,8-hexachloro-3a,
7a-dihydro-4,7-methano-indene,
1,2,3,4,10,10-hexachloro-1,4,4a,5,8,8a-hexahydro-1,4,-endo,
exo-5,8-dimethanonaphthalene,
1,4,5,6,7,7-hexachloro-2-formylbicyclo[2.2.1]-5-heptene,
1,4,5,6,7,7-hexachloro-2-cyanobicyclo[2.2.1]-5-heptene, and
hexachlorocyclopentanones. .Iaddend. .Iadd.35. A composition
according to claim 32 wherein the mineral is present together with
the halogen such that the weight ratio of mineral borate to halogen
is between 1 and 8. .Iaddend. .Iadd.36. A composition according to
claim 33 wherein the mineral is present together with the halogen
such that the weight ratio of mineral borate to halogen is between
1 and 8. .Iaddend. .Iadd.37. A composition according to claim 36
wherein said ratio is between 1 and 4.
.Iaddend. .Iadd.38. A composition of a normally flammable organic
material comprising a vinyl polymer, a calcium or magnesium mineral
borate or a calcium or magnesium metaborate and a halogen source,
said halogen having an atomic weight greater than 19. .Iaddend.
Description
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention is directed to the use of certain specific types of
mineral borates, especially calcium or magnesium mineral borates of
a generally water-insoluble nature, as flame retardants for organic
materials, which borates are employed in a composition containing a
source of a halogen of an atomic weight greater than 19. This
invention is also directed to imparting to latex foam substances,
such as those substances used in carpet backing, increased
flame-retardancy by including in the latex foam a water-insoluble
mineral borate, such as colemanite or other calcium or magnesium
mineral borate. The latex foam contains a source of halide such as
chlorine, such as provided by polyvinyl chloride, or a chlorinated,
brominated, or iodated organic compound.
2. Discussion of the Prior Art
Borates including some of the mineral borates have been used as
fire retardant agents in the past, such as in extinguishing forest
fires. Borax and the sodium cation containing materials are
generally water-soluble, therefore causing incompatibility problems
in some systems.
There is also another major obstacle to their being used in that
they are leached out when in contact with a water environment or as
in washing or laundering. Hydrated zinc borates are effective fire
retardants. However, due to the cost of manufacturing these
products, they find application only in specialty products where
their high cost is justified. Halogenated materials have also been
used as fire retardant agents. Both borates and halogenated
materials, when used alone, however, require large amounts of
either to be effective.
What has now been discovered is that a composition comprising a
relatively crude, inexpensive mineral borate and a halogenated
organic material has a synergistic effect in that when only small
amounts of each component are employed, significant effective flame
retardancy is provided. Such composition, therefore, is an
efficient low-cost flame retarding agent.
Numerous fire retardant agents have been proposed for flammable
organic materials. Due to current and anticipated Government
regulations on items such as carpets there has been an
unprecedented desire and demand for effective, economical fire
retardants.
SUMMARY OF THE INVENTION
Broadly, this invention contemplates a composition for imparting
fire-retardant properties, which composition comprises a calcium or
magnesium mineral borate or a calcium magnesium meta borate and a
source of a halogen having an atomic weight greater than 19.
In a particularly desirable embodiment, this invention contemplates
a method for rendering a flammable material more fire retardant,
which method comprises introducing into said organic material a
calcium or magnesium mineral borate or a calcium or magnesium meta
borate and a source of a halogen of an atomic weight greater than
19.
This invention further contemplates a flame-retarded composition,
comprising a calcium or magnesiun mineral borate or calcium or
magnesium meta borate, a source of a halogen of an atomic weight
greater than 19 and a normally flammable organic material.
DESCRIPTION OF SPECIFIC EMBODIMENTS
It has now been found that a synergistic effect with respect to
flame-retardancy is provided through use of a two-component system.
The preferred types of borates include calcium or magnesium meta
borate as well as calcium and magnesium mineral borates. Thus there
is included within the scope of this invention such mineral borates
as the following: 2CaO.B.sub.2 O.sub.3.H.sub.2 O; CaO.B.sub.2
O.sub.3.6H.sub.2 O; CaO.B.sub.2 O.sub.3.4H.sub.2 O; CaO.B.sub.2
O.sub.3.3.65H.sub.2 O; 2CaO.3B.sub.2 O.sub.3.H.sub.2 O;
2CaO.3B.sub.2 O.sub.3.7H.sub.2 O; 2CaO.3B.sub.2 O.sub.3.9H.sub.2 O;
2CaO.3B.sub.2 O.sub.3.13H.sub.2 O; CaO.B.sub.2 O.sub.3.2H.sub.2 O;
Colemanite (2CaO.3B.sub.2 O.sub.3.5H.sub.2 O); boracite, sassolite,
ulixite, tertschite (4CaO.5B.sub.2 O.sub.3.20H.sub.2 O); probertite
(Na.sub.2 O.2CaO.5B.sub.2 O.sub.3.10H.sub.2 O); priceite,
pandermite (4CaO.5B.sub.2 O.sub.3.7 H.sub.2 O); inyoite
(2CaO.B.sub.2 O.sub.3.13H.sub.2 O or 2C.sub.a O.3B.sub.2
O.sub.3.19H.sub.2 O); meyerhofferite (2CaO.3B.sub.2
O.sub.3.7H.sub.2 O); nobleite (CaO.3B.sub.2 O.sub.3.4H.sub.2 O);
goerite (CaO.3B.sub.2 O.sub.3.4H.sub.2 O); natural or synthetic
ginorite (2CaO.3B.sub.2 O.sub.3.8H.sub.2 O); calciborite
(CaO.B.sub.2 O.sub.3); inderborite (CaO.MgO.3B.sub.2
O.sub.3.11H.sub.2 O; hydroboracite (CaO.MgO.3B.sub.2
O.sub.3.6H.sub.2 O); K.sub.2 O.CaO.4B.sub.2 O.sub.3.12H.sub.2 O;
(NH.sub.4).sub.2 O.CaO.4B.sub.2 O.sub.3.12H.sub.2 O; Na.sub.2
0.2CaO.5B.sub.2 O.sub.3.16H.sub.2 O and CaO.2B.sub.2
O.sub.3.5H.sub.2 O. Most of these are complex polyboron borates
which contain recurring borate units in the mineral. They are
unlike the materials such as borax in that they are not readily
soluble in water and that, curiously, unless they are used in large
quantities, they have a small effect on an organic material with
respect to flame retardancy without the presence of a source of
halogen of an atomic weight of at least 19. Generally speaking,
these materials are insoluble to only slightly soluble in water at
25.degree. C. and are much less soluble than their sodium
counterparts.
The magnesium borates useful in the invention include magnesium
metaborate (Mg(BO.sub.2).sub.2.3H.sub.2 O), also known as pinnoite,
magnesium metaborate (Mg(BO.sub.2).sub.2.8H.sub.2 O), Mg.sub.2
B.sub.2 O.sub.5.H.sub.2 O, also known as ascharite; szaibelyite
(2MgO.B.sub.2 O.sub.3.H.sub.2 O or 2MgO.B.sub.2 O.sub.3.3H.sub.2
O); pinnoite (KgO.B.sub.2 O.sub.3.3H.sub.2 O); inderite and
kurnakovite each having the formula 2MgO.3B.sub.2 O.sub.3.15H.sub.2
O; preobrazlienskite (3MgO.5B.sub.2 O.sub.3.4.5H.sub.2 O;
MgO.2B.sub.2 O.sub.3.8.5H.sub.2 O; MgO.3B.sub.2 O.sub.3.7.5H.sub.2
O; MgO.3B.sub.2 O.sub.3.5H.sub.2 O; magnesium pyroborate
(MgO.B.sub.2 O.sub.3); suanite (2MgO.2B.sub.2 O.sub.3);
3MgO.B.sub.2 O.sub.3); (NH.sub.4).sub.3 O MgO.3B.sub.2
O.sub.3.15H.sub.2 O and 7H.sub.2 O.
The materials above similarly have low water-solubilities at
25.degree. C.
Moreover, it must be understood that the incorporation of the
halide is critical to the synergism whereby significantly greater
flame-retardant properties are obtained.
Halides which are particularly useful in the compositions of the
present invention and in the methods of improving flame retardancy
are those chlorinated, brominated, iodated, or mixed halogenated
compounds of aliphatic or aryl compositions such as paraffins,
fatty acids, starches, sugars, cellulosics, resins, polymers,
rubbers, phenolics and heterocyclics.
Included within this group are: polyvinyl chloride, chlorinated
polyethylene, halogenated paraffins where the alkyl group contains
between 6 and 36 carbon atoms in the chain, preferably between 12
and 24 carbon atoms in the chain. The halides contemplated within
the invention include, specifically, chlorine bromine and iodine.
Additional sources of halogen include halogenated aromatic
compounds, especially with aryl groups, such as C.sub.6 -C.sub.18.
Included within this group are phenyl naphthyl and anthracyl
compounds. Of these, halogenated phenyl compounds are desired. The
phenyl compound can be a polyhalogenated compound which supplies
one or more halide atoms to the composition. Indeed, the phenyl
compound can supply several types of halides such as would be
supplied by 2 bromo, 1,3 dichlorobenzene. It will be realized that
the aryl group, especially the phenyl group, can be substituted to
any desired extent provided there exists an available halide. Thus
the same can have other substitutes on the ring, such as amino,
imino, alkoxy, nitrile, nitroso, sulfono, alkyl, especially C.sub.1
-C.sub.8, acetyl and the like, including ortho, para and meta
directors.
Other halogenated organic compounds useful include:
Halogenated acids where the halogen is an anioncarbonyl atom
especially C.sub.3 -C.sub.24 saturated and unsaturated fatty
acids;
Polyethers such as polyethylene glycol derivatives;
Ketones where at least one substituent attached to the carbonyl has
at least 4 carbon atoms, preferably 4 to 12;
Aldehydes where the substituent attached to the carbonyl group is
at least 4 carbon atoms, especially C.sub.4 to C.sub.12 ;
Anhydrides of the halogenated acids;
Alcohols, both primary and secondary, which are the reduction
products of the aldehydes or ketones set forth above, i.e., having
4 to 12 carbon atoms or a group attached to the carbon atom bearing
the OH radical;
Acid halides, especially C.sub.2 to C.sub.10 acid halides;
Saccharides, especially mono- di- and polysaccharides, including
starch and cellulose.
There are also contemplated derivatives of the above, such as the
esters of the acids and the thio derivatives of the acids,
aldehydes, ketones and alcohols set forth above.
Additionally, the following aryl compounds in halogenated form can
be employed:
Aryl compounds having C.sub.6 to C.sub.18 aryl radicals, especially
phenyl. These can be substituted as follows or can be unsubstituted
(aside from the halogen): Substitutes include
Ether especially where the organic group attached to the oxygen
contains at least 4 carbon stoms;
Aldehyde especially where the organic radicals attached to the
oxygen atom contains at least 4 carbon atoms, e.g., C.sub.4
-C.sub.12 ;
Ketone, especially where at least one organic group attached to the
oxygen atom has at least 4 carbon atoms, e.g., C.sub.4 -C.sub.12
;
Alkenyl, especially C.sub.4 -C.sub.12 ;
Alcohol, especially C.sub.4 -C.sub.12, whether primary or
secondary;
Hydroxy, e.g., 1 hydroxy 2 chloro phenyl;
Sulfonate
Nitrate
Acid radical, especially C.sub.2 -C.sub.10 acid halide
Cyano
Mercapto
Amine
Dicarboxylic acid and its anhydride, especially phthalic acid
anhydride.
Other agents hexachloro and hexabromo benzene. Especially
contemplated are materials which are at least 50% halogenated by
weight. Decabromodiphenyl oxide [Dow FR-300-BA] a new fire
retardant agent. Especially included is hexachlorocyclopentadiene
and chloroprene.
Additionally, the following can be employed: ##STR1## its acids,
mixed acids, bi-acids, mixed esters, biesters and anhydrides.
In the formula R can be H, C.sub.1 -C.sub.12 alkyl or a halogenated
derivative thereof.
Examples of particularly suitable highly chlorinated materials
useful in the present invention include:
1,2,3,4-tetrachloro-5,5-dimethoxycyclopentadiene
1,2,3,4-tetrachlorocyclopentadiene
nonachlorobicyclo[3.2.0]heptene-2
1,2-dichloro-3,3,4,4,5,5-hexafluorocyclopentene
decachloropentacyclo[5.3.0.0.sup.2,6 0.sup.4,10 0.sup.5,9
]decan-3-one
octachlorocyclopentene
bis(pentachloro-2,4-cyclopentadien-1-yl)
1,2,3,3,5,5-hexachloro-4-(dichloromethylene)cyclopentene
perchloropentacyclo[5.2.1.0.sup.2,6.0.sup.3,9.0.sup.5,8
]-decane
2,3,4,4,5-pentachloro-2-cyclopentene-1-one
1,2,4-trichlorocyclopentene-3,5-dione
1,2,3,4,7,7-hexachlorobicyclo[2.2.1]-2.5 heptadiene
1,4,5,6,7,7-hexachlorobicyclo[2.2.1]-5-heptene-2,3-dicarboxylic
acid
1,4,5,6,7,7-hexachloro-2,3-bis(chloromethyl)bicyclo[2,2,1]-5-heptene
1,4,5,6,7,7-hexachloro-2-(1,2-dichloroethyl)-bicyclo[2.2.1]-5-heptene
1,4,5,6,7,7-hexachloro-2-carboxy-bicyclo[2.2.1]-5-heptene
1,4,5,6,7,7-hexachloro-2,3-bis(hydroxymethyl)-bicyclo[2.2.1]-5-heptene
undecachloropentacyclo[5.3.0.sup.2,6.0.sup.4,6.0.sup.5,9
]-3-decyclorosulfonate
4,5,6,7,8,8-hexachloro-3a, 7a-dihydro-4,7-methanoindene
1,2,3,4,10,10-hexachloro-1,4,4a, 5,8,8a-hexahydro-1,4-endo,
exo-5,8-dimethanonaphthalene
1,4,5,6,7,7-hexachloro-2-formylbicyclo[2.2.1]-5-heptene
1,4,5,6,7,7-hexachloro-2-cyanobicyclo[2.2.1]-5-heptene
hexachlorocyclopentenones
Halogenated heterocyclics, especially those containing between 5
and 8 members in the ring and containing, as a component of the
ring, a nitrogen, sulfur or oxygen atom, can be suitably employed.
Contemplated within these definitions are included materials such
as furan, pyridine and other nitrogen-containing heterocyclics such
as pyrimidine.
The synergistic composition of the present invention is useful in a
wide variety of flammable materials. Generally speaking, the
composition is useful in all organic materials which are flammable.
Most polymeric and resinous compositions are organic and are
therefore flammable.
The resinous compositions can be of any resin, including polymers
of alpha olefins, especially polyethylene, polypropylene,
polybutene-1, polyisobutylene, vinyl polymers, including polymers
of vinyl chloride, methyl methacrylate, ethyl methacrylate,
acrylonitrile, vinyl alcohol, vinyl adetate, vinyl butyral and
styrene, polyamide, especially nylon 6 and nylon 6/6, polyacetals,
polyurethanes, polyesters; also polymers classified as rubbers or
latexes such as natural rubber,
polystyrene-butadiene-acrylonitrile; acrylic, chlorosulfonated
polyethylenes, epichlorohydrin, ethylene-propylene copolymers,
ethylene-propylene-diene terpolymers, polyisoprene-acrylonitrile,
polybutadienes, polychloroprenes, polyisoprenes,
polystyrene-isoprene, and polyurethanes.
There are also included condensation polymers such as
phenol-formaldehyde and urea-formaldehyde polymers, polycarbonates
and, for that matter, all organic thermoplastic and thermosetting
resins and polymers such as epoxy resins.
A particular use of the composition of the present invention is in
the field of latex foams. Thus, it has been discovered a
styrene-butadiene rubber latex foam can be rendered flame-retardant
by removing a portion of the SBR latex and substituting for such
portion a polyvinyl chloride latex material. Such material not only
is compatible with the SBR latex to accomplish the purposes for
which the latex is used, but also the polyvinyl chloride
contributes the desired source of halogen, so that no additional
halide need be added to the composition. The composition is
complete when it contains the added calcium or magnesium mineral
borate. Latex foams which contain, initially, an adequate amount of
chlorine, bromine, or iodine need not have added thereto a material
which acts as a source of a halogen, it being sufficient that the
mineral borate be added thereto. Other latex materials which can be
treated include natural rubber, acrylic, isoprene, acrylonitrile,
nitrile, polybutadiene, polyisobutylene, polyisoprene, vinyl
pyridine, especially when they contain a source of halogen of
atomic weight of at least 19.
Other organic materials which can be rendered more flame-retardent
include fibrous materials such as cotton, polyester, nylon,
acrylics, non-woven and woven fabrics of natural and synthetic
fibers, paper, Kraft cardboards, adhesives, molded plastics,
compressed paper employed in the building industry in lieu of
plywood sheathing, and egg cartons.
The amount of mineral and source of halogen will vary depending
upon the type of mineral and the type of halogen source employed.
Generally speaking, the mineral will be present in the material to
be protected in an amount between 2 and 400 phm (parts per hundred
of organic material, e.g., resin) preferably in an amount between 5
and 50 phm. The parts are on a weight basis. Similarly, the source
of halogen will be present, such that the halogen itself is present
in an amount between 1 and 100 phm, preferably between 2 and 20
phm, based upon the weight of the resin being rendered
flame-retardant. The relation of mineral borate and halogen
generally satisfy the following ratios: 1 to 8 parts by weight
mineral borate; 1 part by weight halogen. Preferably the ratio is 1
to 4:1. Naturally, these ratios are satisfied in different manners
by different materials, owing to their different polymer systems,
the purity of the borate ore, and the atomic weight and
effectiveness of the different halogens and the number of halogen
atoms on the compound supplying the same.
It has been found, surprisingly, that mined mineral borates having
a relatively high concentrate of nonborate materials can be used as
such, i.e., in a nonrefined state, pursuant to the present
invention. The concentraton of borates are normally reported as to
their percentage of boric oxide (B.sub.2 O.sub.3). Thus it has been
found that the borate can be present together with other minerals
in an amount between 15 and 55 percent by weight, based upon the
weight of the boric oxide. For example, gangue materials which can
be present together with the borate include earth (soil), bentonite
clay, and other normally associated mineral silicates and
carbonates.
However, in certain instances, it is preferred that the mined
mineral borate be refined, so that it has a purity of at least 45
percent B.sub.2 O.sub.3. Different mineral types and grades to be
employed are dependent on such factors as type of borate ore, mine
location, purity and assay of ore, as well as other processing
refinements.
In order to more fully illustrate the nature of the invention and
the manner of practising the same, the following examples are
presented:
EXAMPLE I ______________________________________ FIRE RETARDANT NO
GEL LATEX FOAM FOR- MULA A B ______________________________________
(Pliolite LPE3717E (5) (NO GEL (SBR latex) 129.0 129.0 (Geon 354
(2) (polyvinyl chloride IA (latex) 19.0 19.0 (Supex OLS (6) (alkyl
sulfonate)(a (wetting agent) 3.75 3.75 (Sodium tripolyphosphate 4.0
4.0 (NH,OH) 5.0 5.0 (Acrysol GS (3) (polacrylamide 3 3 IB
(thickener) drops drops (Sparta fil (7) (Feldspar) 200.0 160.0 II
(Colemanite = calcium borate of (formula 2 CaO B.sub.2 O.sub.4
5H.sub.2 O -- 40.0 III (Cure Paste (sulfur & rubber
(accelerators) 10.0 10.0 370.75 370.75
______________________________________
NO GEL LATEX FOAM PROCEDURE
Mixed slowly part IA until thoroughly blended. Added part IB,
thickener, to desired viscosity. Added Part II, fillers, flame
retarders, and pigments with intermediate stirring until dispersed.
Added Part III, with stirring. Foamed with 6 minutes at high speed
on blender, poured out onto substrate and drawn down to desired
thickness, generally three eighths inches thick. Cured 20 min. at
150.degree. C.
FIRE RETARDANT TEST - HORIZONTAL MATCH TEST
Foam samples of the above materials, 1 inch .times. 5 inches
.times. 5/8 inch, were supported horizontally and a burning match
was positioned under the leading edge of the foam samples for 5
seconds.
Failure to self-extinguish within 1 inch of the edge is considered
failing.
TEST RESULTS:
The A samples had to be extinguished after burning for more than 1
inch and therefore failed.
The B samples self-extinguished in less than 1 inch and therefore
passed.
EXAMPLE II
__________________________________________________________________________
FIRE RETARDANT TYPE LATEX FOAM A B C
__________________________________________________________________________
(Pholite 5352D (5) (SBR Latex) 119.0 119.0 119.0 (Geon 354 (2) (PVC
copolymer 27.0 27.0 27.0 (PTPP (potassium tripolyphosphate) 2.0 2.0
2.0 (Alipal CD436 (8) (Wetting agent) 2.0 2.0 2.0 (50% K.sub.2
CO.sub.1 2.0 2.00 2.00 (10% KOH 4.0 4.0 4.0 II ( (Cure Paste
(Sulfur & rubber ( accelerators) 20.5 20.5 20.5 (20% Potassium
oleate 20.0 20.0 20.0 (Water to Balance 2.0 2.0 2.0 (Spartalil (7)
(Feldspar) 160.0 179.0 197.0 III (Colemanite 40.0 20.0 --
(Thermogard S (Sb.sub.2 O.sub.1) (21) -- 1.0 3.0 (NH.sub.1 O.sub.1
H 2.0 2.0 2.0 (Afquad T 50 (g) (Quaternary ( Ammonium Compound 3.0
3.0 3.0 IV (Water 4.0 4.0 4.0 (20% Potassium Oleate (3 (3 (3 drops)
drops) drops) V (25% Ammonium Acetate 10.0 10.0 10.0 416.5 416.5
416.5
__________________________________________________________________________
PROCEDURE FOR LATEX FOAM
Part I was stirred slowly as Part II was added and mixed in. Part
III was then added gradually, and foamed for 21/2 minutes at high
speed.
Part IV is added and mixed one minute, then Part V is added and
mixed for 40 seconds.
The foam is poured onto the substrate, drawn down, gelled for 30
seconds under heat lamps, and then cured for 20 min. at 150.degree.
C.
TEST AND RESULTS
Samples from A, B, and C were exposed to the 5 second horizontal
match test.
Sample A (Colemanite and PVC) Passed Sample B (Colemanite, Sb.sub.2
O.sub.3 and PVC) Passed Sample C (Sb.sub.2 O.sub.3 and PVC)
Failed
EXAMPLE III
__________________________________________________________________________
FLAME RETARDANT PLASTISOL FORMULA A B
__________________________________________________________________________
(Dioctyl) phthalate 350 350 (Paraplex G62 (3) epoxy plasticizer) 25
25 I (Nuostabe V1216 (4) (Ba & Cd (fatty acid stabilizer) 15 15
(Aleolee S (Sulfonated wetting agent) 5 5 (Gerstly Borate (1)
(Ulexite & (Colemanite) -- 75 II (Atomite (22) (Calcium
Carbonate) 75 -- (Geon 121 (2) (Polyvinyl chloride III (dispersion
grade) 500 500 IV (30% CaO paste 5 5 975 grams 975 grams
__________________________________________________________________________
PLASTISOL PROCEDURE
Part II was added to Part I and dispersed with a Cowles Dissolver.
Part III was then added and dispersed followed by Part IV. The
plastisol was evacuated, drawn down, and fused.
TEST AND RESULTS:
Film samples of the above materials 0.5 inches wide and 0.14 inches
thick, were supported horizontally and a burning match was
positioned under the leading edge of the plastisol samples for 5
seconds. Upon removal of the flame, the B samples self-extinguished
within 8 seconds, and burned less than 1/16 inch, passing the test.
The A samples burned over 1 inch (completely) and were considered
to have failed.
EXAMPLE IV ______________________________________ FLAME RETARDANT
POLYESTER FORMULAS A B ______________________________________
Polylite 31-586(polyester resin) (22) 34.1 34.1 Dion BR6399
(chlorinated polyester resin (14) 5.0 5.0 BPO Paste (Benzoyl
peroxide) (22) 0.9 0.9 80 WSA (Talc) (16) 60.0 35.0 Colemanite --
25.0 100.0 100.0 ______________________________________
PROCEDURE:
The materials were mixed, molded into one quarter inch rods, cured
for 15 min. at 300.degree. F.
The samples were exposed to a modified match test. The samples were
positioned at 45.degree. down from the horizontal to increase the
severity of the flame test. Otherwise the match was again held at
the leading edge of the sample for 20 seconds.
The sample passes if it self-extinguishes before burning 1
inch.
RESULTS:
Formula A failed the match test. Formula B passed.
EXAMPLE V
Flame Retardance and Prevention of Dripping of Polypropylene
Polyolefins are very flammable due to their wax like structure.
Also, when they are ignited they melt and run or drip, thereby
carrying and spreading the flame.
It is therefore advantageous that where flame retardance is
necessary that the resin also be prevented from running and
spreading the flames.
The following compositions were tested:
______________________________________ A B C D
______________________________________ Profax 6523 (24)
(POLYPROPYLENE RESIN) 100 g 100 g 100 g 100 g CHEX BC 26 (20)
(Organic Chemical containing Cl and Br) -- 3 g 3 g 6 g COLEMANITE
-- -- 40 g -- 80 WSA TALC (16) -- -- -- 40 g 100 g 103 g 143 g 146
g ______________________________________
PROCEDURE
The extruded samples were cut into strips, held in a vertical
position and the top edge was ignited by holding a match to it for
20 seconds. Failure results from not self-extinguishing within an
inch.
RESULTS
Sample A failed and ran.
Sample B failed and ran.
Sample C passed and no running.
Sample D failed and ran.
CONCLUSIONS:
The addition of the Citex at this level was not sufficient to make
the polypropylene flame retardant and non-dripping. The addition of
the Colemanite effected both desired results. The addition of the
inert talc effected neither of the desired results when added with
double the amount of Citex, which is an organic chemical containing
both aliphatic bromine and chlorine.
EXAMPLE VI
Flame Retardant Paper
Brown Kraft paper was made flame retardant and self-extinguishing
by the addition of Colemanite and vinyl chloride-vinylidene
chloride copolymer, whereas the paper containing double the amount
of either material alone remains flammable.
PROCEDURE FOR SAMPLE PREPARATION:
3 grams of brown kraft paper was refiberized with 450 cc of water
in a Waring Blender. Two coats of the paper was then reformed on a
screen, press dried on felt and finally dried in an oven for 30
min. at 100.degree. C. and stored in a dessicator until testing for
flame resistance. Three other papers were made by adding the
following per coat:
______________________________________ MATERIALS CONTROL A B C
______________________________________ Kraft Paper 3 g 3 g 3 g 3 g
Colemanite -- 2.4 g 1.2 g -- Geon 652 (2) (x) -- -- 2.4 g 4.8 g
______________________________________
TEST PROCEDURE:
The dry paper sample materials are cut into 1 inch wide strips.
These strips are suspended horizontally in a draft free hood and
the leading edge of each strip when tested is ignited with a
burning match. The material passes if the sample self-extinguishes
within an inch of the ignited edge. The material fails if it's
samples do not extinguish themselves within this limit.
______________________________________ RESULTS SAMPLE Variable Fire
Test ______________________________________ Control Paper Only
Failed A Double Colemanite Failed B Colemanite & Copolymer
Passed C Double Copolymer Failed
______________________________________
CONCLUSIONS:
The Colemanite with the halogenated polymer is effective as a fire
retarder in Kraft paper. The combination is synergistic as the
combination is effective, whereas double the amounts of either of
the materials alone are ineffective.
EXAMPLE VII
Flame Retardance of Polystyrene
The following materials were heated, blended, molded, and cooled.
They were then exposed to the 20 second horizontal match test.
______________________________________ A B
______________________________________ Piccolastic D 150
(10)(Polystyrene Resin) 100 100 Hexabromobenzene (II) 1 1
Colemanite -- 10 101 111 Match test results Failed Passed
______________________________________
EXAMPLE VIII
Flame Retardance of Rubber
The following formulas were made by combining their ingredients on
a 2-roll rubber mill, calendaring and curing in a mold for 20 min.
at 300.degree. F. The cured rubber specimens were cut into 1 inch
.times. 6 inch .times. 3/8 inch samples and were exposed to flame
tests.
______________________________________ FORMULAS B Chlorowax A 70 20
phm Chlorowax Colemanite MATERIALS 70 20 phm 60 phm
______________________________________ Natural Rubber (NR) 30 30
Plioflex 1502 (SBR)(5) 30 30 Epsin 40 (BPDM) (12) 20 20 Chlorobutyl
10-68 (HR) (13) 20 20 Chlorowax 70 (14)(Chlor- inated Paraffin) 20
20 Protox 166 (XnO) (15) 5 5 Colemanite -- 60 P-725 Talc (16) 40 --
Inpure 1 W (TiO.sub.1) (17) 35 15 Sulfur Tire RM (18) 2.65 2.65
MBTS (17)(Benzothrazyl) disulfide 0.75 0.75 Vultax No. 5
(19)(Curing 1.25 1.25 Agent) 204.65 204.65
______________________________________
The flame test consisted of laying the samples flat horizontally
and lighting the leading edge of the sample with a match held to
the sample for 20 seconds. The sample is judged to pass if it
self-extinguishes within one inch of the edge.
RESULTS:
Formula A consistently failed the flame test, whereas Formula B
passed.
RAW MATERIAL SUPPLIERS
1. U.S. Borax & Chemical Corp.
2. B. F. Goodrich Chemical Co.
3. Rohm and Haas Co.
4. Tenneco Chemicals Inc.
5. Goodyear Co.
6. Alcolac Chemical Corp.
7. Spartan Minerals Co.
8. GAF
9. Armak Company
10. Pennsylvania Industrial Chemical Corp.
11. East Coast Chemicals Inc.
12. Copolymer Rubber and Chemical Corp.
13. Enjay Chemical Co.
14. Diamond Shamrock Chemical Co.
15. New Jersey Zinc Co.
16. International Talc Co., Inc.
17. E. I. du Pont de Nemours and Co.
18. Stauffer Chemical Co.
19. Pennsalt Chemicals Corp.
20. Cities Service Co.
21. M and T Chemicals, Inc.
22. Reichhold Chemicals Inc.
23. Thompson, Weinman and Co.
24. Hercules Inc.
* * * * *