Note: Descriptions are shown in the official language in which they were submitted.
fi;32
BACKGROUND OF THE INVENTION
This invention relates to fire-retardant putty-like
compositions for filling the spaces in bores penetrating
walls and floors of buildings and having electric wires
and cables extending therethrough or for filling the
clearance at the joints of interior finishing materials
of buildings.
Various fire-retardant putty-like compositions of
this type have heretofore been proposed. These compositions
must have such properties that when a fire breaks out in
a section of a building, the composition, exposed to a high
temperature in the initial stage of the fire, will not sag
due to softening and deformation per se or fall in molten
drops, without permitting flames and smoke to spread to an
adjacent section through a space which would otherwise be
formed. Additionally the putty like composition must remain
in shape free of large deformation or dripping even if heat
and wind pressure build up in the fire section due to fierce
flames and heavy smoke amidst of the fire. It is further
desired that even when the composition has been burned out,
carbonized and eventually ashed, the residual ashed
product has toughness without becoming brittle and falling,
thus completeIy preventing the spread of fire to the adja-
~.
" ~ , ,
~'~2l~fi3~
--2--
cent section to minimize the damage.
Published Unexamined Japanese Patent Application122895/1977 discloses a composition containing soybean oil
as a binder and consisting mainly of an inorganic filler
such as hydrated alumina and an inorganic fiber such as
asbestos. The composition softens and deforms with a rise
in temperature in the event of a fire, is not satisfactory
in non-sagging properties and fails to fully prevent the
spread of fire. Published Unexamined Japanese Patent
Applications 34150/1978 and 125552/1977 disclose compo-
sitions containing liquid chloroprene as a binder and
consisting predominently of an inorganic filler such as
hydrated alumina, and glass fiber or like inorganic fiber
of an organic fiber. Although having good non-sagging or
non-dripping properties, the compositions burn when subject-
ed to a fierce fire involving a heavy smoke and high wind
pressure, giving a brittle ash residue which cracks and
progressively breaks down into falling fragments to form
a hole where the composition has been applied. Thus the
compositions are unable to completely prevent the sp~ead
of fire.
whilethe putty-like compositions of this invention
comprise known materials which are individually employed
in the prior art reference mentioned above, the materials
are used in specified combination in specific proportions
as will be described later, so that the present composi-
tions exhibit outstanding performance, have excellent non-
X1
fig~2
--3--
sagging and non-dripping properties under the severe
conditions of fires and retain the original shape, or a
shape near to the original even when burned to an ashed
state because the ash residue has exceedingly high tough-
ness which has never been afforded by the conventionalputty-like compositions. The present compositions therefore
assure outstanding smoketightness and effectively prevent
the spread of fire. Needless to say, the compositions
are easy to handle especially for filling spaces.
SUMMARY OF THE INVENTION
The main object of the present invention is to over-
come the foregoing drawbacks of the conventional compo-
sitions and to provide novel putty-like compositions which
have suitable plasticity, and airtightness for filling
various spaces, joint clearances, etc. in buildings and
which retain non-sagging and non-dripping properties even
when subjected to severe conditions in the event of a fire,
the present composition, when burned and ashed, giving
a residual product having high toughness and retaining the
original shape or a shape near to the original.
The fire-retardant putty-like compositions of this
invention comprise (2) 100 parts by weight of a curable
polychloroprene in a liquid state at room temperature, (b)
about 200 to about 700 parts by welght of a hydrated metal-
lic oxide, and (c) about 20 to about 100 parts by weight
of a heat-resistant fibrous material, the compositions
1~2~fi3Z
--4--
containing the hydrated metallic oxide (b) and the heat-
resistant fibrous material (c) in a combined amount of at
least about 250 parts by weight per 100 parts by weight of
the polychloroprene (a).
DETAILED DESCRIPTION OF THE INVENTION
The polychloroprene in a liquid state at room tem-
perature and serving as the component (a) of the putty-like
compositions of the invention is used as a binder, and are
curable at room temperature or higher temperatures.
Examples of such polychloroprenes are chloroprene
homopolymer; copolymers of chloroprene and at least one
monomer which is copolymerizable with chloroprene, such as
styrene, methacrylic acid, methyl methacrylate, acryloni-
trile or like vinyl compound, or 1,3-butadiene, isoprene,
2,3-dichloro-1,3-butadiene or like conjugated diene; and
chloroprene-sulfur copolymer. Exemplary of useful end
groups of these polychloroprenes are active halogen group,
hydroxyl group, carboxyl group, thiol group, alkylxanthate
group, or like groups being able to cause condensation,
addition reaction, etc.
The liquid polychloroprenes to be used in the present
invention are usually used together with a curing agent
described below, although the agent does not necessarily
need in the case where such a polychloroprene, for example,
those having alky~nthate end groups, carboxyl end groups
etc., is used which is curable at high temperatures without
~3~
--5--
the curing agent. Examples of useful curing agents are lead
peroxide and like metallic peroxides; tolylenediisocyanate
and like diisocyanates; tetraethylenepentamine, aminoethyl-
piperadine, 4-aminomethylpiperidine, N-aminopropylpipecolin,
N,N-dimethylpropane-1,3-diamine, methyliminobis-propylamine,
ketimine, methacrylate-amin adduct, epoxylamine adduct and
like amines; t-butylhydro peroxide, 2,4-dichlorodibenzoyl
peroxide, dicumyl peroxide and like organic peroxides; zinc
oxide, magnesium oxide, lead monoxide, red lead and like
metallic oxides; sulfur; n-b ~ylaldehydeaniline and like
aldehydeamines; N,N'-diphenylthiourea, N,N'-diethylthicurea
and like thioureas; di-orthotolylguanidine, di-orthotolyl-
guanidine salt of dicatechol borate and like guanidines;
sodium dimethylditiocarbonate and like dithiocarbamates;
and zinc butylxanthate and like xanthates. A suitable, if
necessary, two or more curing agent selected from the above
are used according to the end group of polychloroprene.
These curing agents are used in an amount of about
0.5 to about 20 parts by weight per 100 parts by weight of
the liquid polychloroprene.
Preferable among the liquid polychloroprenes exempli-
fied above are those having a viscosity of about 5,000 to
about 500,000 cps, especially about 10,000 to about 300,000
cps, at room temperature (25C). With respect to the end
group, preferable are those having an alkylxanthate group
in which the alkyl has 2 to about 10 carbon atoms such as
ethyl, propyl, butyl, etc. It is also desirable to use those
~'
fi3Z
--6--
having a hydroxyl end group conjointly with a diisocyanate
such as tolylenediisocyanate serving as a curing agent.
It is more desirable to use a liquid polychloroprene having
at least one kind of the alkylxanthate end groups as
admixed with a liquid polychloroprene having at least one
hydroxyl end group in an amount of up to about 100 parts by
weight per 100 parts by weight of the former.
According to this invention, the liquid polychloropren-
es given above are usable, with or without any of the curing
agents mentioned above when so desired. Preferable poly-
chloroprenes are those satisfying curing properties as
determined by the following test method.
Test method: 100 parts by weight of the component
(a) is admixed with 400 parts by weight
of A1203. 3H20 (mean particle size:
3.5 ~m) and 30 parts by weight of glass
fiber (mean diameter: 13 ~m, mean length;
6 mm) and the mixture is kneaded into a
putty-like composition, which is then
heated at 250C for 30 minutes. The
component (a) is acceptable when the
composition, after the heating, is up
to about 1, preferably up to about 0.5
in cone penetration value evaluated in
accordance with JIS A 5752-1966 (mm/
150g, 5 sec. at 20C).
3~2
--7--
The hydrated metallic oxide (or hydroxide of metal)
serving as the component (b) of the present compositions is
in the form of a fire-retardant or nonflammable powder having
a mean particle size of up to about 100 ~m, preferably up
to about 80 ~m, and having a heat loss of at least about 8%
by weight, preferably, at least about 20~ by weight obtained
by the following formula:
heat loss = A - B x 100
where A : initial weight of sample
B : constant weight of sample after heating
at a temperature of 400 + 20C.
Examples of useful hydrated metallic oxides are hy-
drated aluminas, represented by the formula A12O3.nH2O(n
being 0.5 - about 6), such as A12O3.2-H2O, A12O3.H2O,
A12O3.2H2O, A12O3. 3H2O(Al(OH)3), etc. and hydrated magnesias
such as Mg(OH)2, etc.
It is preferable to use a hydrated metallic oxide
comprising at least two portions which differ in particle
size, or to conjointly use at least two kinds of hydrated
metallic oxides which differ in particle size. Stated more
specifically, the component (b) comprises at least two
portions one of which has a mean particle size of about 10
to about 100 ~m, preferably about 10 to about 80 ~m,
the other portion being up to about 10 ~m in mean particle
size.
The hydrated metallic oxides serving as the component
1~2~fi3Z
--8--
(b) are used in an amount of about 200 to about 700 parts
by weight, preferably about 250 to about 450 parts by weight,
per 100 parts by weight of the component (a). With less than
about 200 parts by weight of the component (b) present, the
putty-like composition has greatly increased flowability,
is prone to deformation when applied even at room temperature,
is liable to soften and drop when subjected to the heat of
fires and gives a brittle residue when asked. With use of
more than about 700 parts by weight of the component (b),
the ingredients (a), (b) and (c) will have reduced compati-
bility when they are mixed, while the resulting composition
is not satisfactorily applicable to spaces, bores or the like
and affords low airtightness even at room temperature if
filled in place.
When the component (b) comprises at least two portions
of different particle sizes, the portion up to about 10 ~m
in mean particle size is used in an amount of about 10 to
about 500 parts by weight per 100 parts by weight of the
other portion with a mean particle size of 10 to about 100
~m.
According to this invention it is advantageous to use
the component (b) in combination with particles, smaller than
about 10 ~m, of at least one of clay, zinc borate, bentonite,
talc, diatomaceous earth, calcium carbonate and mica in an
amount of up to about 80% by weight, preferably up to about
50% by weight, based on the component (b). The composition
will then afford a residual product of enhanced toughness
63Z
when ashed. Among the above-mentioned materials, clay, zinc
borate and bentonite are especially advantageous to use.
The heat-resistant fibrous materials useful as the
component (c) of the present compositions are inorganic
fibers, and organic polymeric fibers which will not thermal-
ly deform at temperatures of lower than about 250C. Such
fibers are up to aboutloo~m preferably about 0.5 to about
~m, in average diameter and up to about 30mm, preferably
about 1 to about 2Omm, in average length.
Examples of useful inorganic fibers are glass fiber,
asbestos fiber, carbon fiber, etc. Examples of suitable
organic polymeric fibers are phenolic resin fibers, poly-
imide fiber, polyamide-imide fiber, etc. ~mong these
fibers, glass fiber and asbestos fiber are preferable. A
mixture of glass fiber and asbestos fiber is more preferable.
The heat-resistant fibers serving as the component (c)
are used in an amount of about 20 to about 100 parts by
weight, preferably about 20 to about 60 parts by weight,
per 100 parts by weight of the component (a). With less
than about 20 parts by weight of the component (c), the
putty-like composition, when exposed to the high temperature
of a fire, is liable to soften and sag, and also fails to
give a tough ashed product. If used in an amount of more
than about lOO parts by weight, the component (c) will be
less compatible with the other ingredients when formulated
into a putty-like composition, while the composition is
not satisfactorily applicable and provides impaired air-
fi3~
--10--
tightness at room temperature if used.
When the heat-resistant fibrous material (c) comprises
a mixture of glass fiber and asbestos fiber, it is suitable
to use about 10 to about 300 parts by weight of asbestos
S fiber per 100 parts by weight of glass fiber.
As described above, the fire-retardant putty-like
compositions of the present invention consist essentially of
100 parts by weight of the component (a), about 200 to about
700 parts by weight of the component (b) and about 20 to about
100 parts by weight of the component (c). It is also crit-
ical that the compositions contain the component (b) and the
component (c) in a ~ombined amount of at least about 250
parts by weight per 100 parts by weight of the component (a).
If the combined amount of the components (b) and (c) is less
than about 250 parts by weight, the composition is unable to
exhibit high fibre retardancy and nonsagging and non-dripping
properties in the event of a fire and to yield a tough
ashed product.
The fire-retardant putty-like compositions of this
invention, when comprising the components (a), (b) and (c)
in the proport~ons specified above, have outstanding fire
retardancy, will not sag or drip even if exposed to a high
temperature and high wind pressure due to the intense flame
and smoke of fires but rather gain hardness with the lapse
of timel and afford a tough ashed product if burned and
ashed. The present compositions are therefore exceedingly
superior to any of the conventional putty-like compositions
K
in assuring high smoketightness and preventing the spread
of fire. Such remarkable effects are not achievable if
any one of the components (a), (b) and (c) is used in a
proportion outside the specified range.
The present compositions, which consist essentially of
the components (a), (b) and (c), may further incorporate
flame retardants, plasticizers, and silane coupling agents
or titanate coupling agents, such as given below, when so
desired.
Flame retardants:
Suitable flame retardants are those heretofore known
for use with rubbers and plastics. Examples are: (1) in-
organic flame retardants such as antimony trioxide, anti-
mony oxide, molybdenum trioxide, ammonium polyphosphate,
zirconium oxide, etc., and (ii) organic flame retardants
such as chlorinated paraffin, decabromodiphenyl ether and
like halogen-containing organic compounds, tris(aziridinyl)
phosphine oxide, phosphonyl amide and like phosphorus-
containing organic compounds, bromo cresyl phosphate,
tetrakis(hyroxymethyl)phosphonium chloride and like phos-
phorus - and halogen - containing organic compounds, etc.
These flame retardants are useful for imparting im-
proved flame retardancy to the putty-like composition dur-
ing the rise of temperature in the initial stage of a fire.
The above-mentioned flame retardants are used in an amount
of up to about 100 parts by weight per 100 parts by weIght
-12-
of the component (a).
Plasticizers:
Plasticizers usually used for polyvinylchloride are
usable. Examples are diisobutyl phthalate, dioctyl phthalate
and like phthalic acid derivatives, diisooctyl sebacate and
like sebacic acid derivatives, tricresyl phosphate and like
phosphoric acid derivatives. Other examples are process oil,
linseed oil, soybean oil and like oils, liquid, urethane
resin, liquid epoxy resin, liquid polybutene resin and like
liquid synthetic resin, etc.
Use of such plasticizers renders the resulting composi-
tion easily applicable. When the composition is used, for
example, for filling the space in a bore around a cable ex-
tending through the bore and sheathed as with polyvinylchlo-
ride, the plasticizer in the sheath can be held in equilib-
rium with the plasticizer in the composition at room temp-
erature a~d prevented from migrating into the composition
This inhibits the hardening of the cable sheath, hence desir-
able. The plasticizers nevertheless tend to impair the
non-sagging or non-dripping properties of the composition
at high temperatures, so that it is preferable to use
the plasticizers in an amount of up to about 50 parts by
weight, more preferably up to above 30 parts by weight, per
100 parts by weight of the component (a).
Silane coupling agents:
Useful silane coupling agents are those represented
by the formula
Y(CnH2n)siX3
63~
~13-
wherein n is zero or an integer of 1 to 6, X is chlorine,
alkoxy or acetoxy, and Y is chlorine, vinyl, methacryloxy,
cyclic epoxy, glycidoxy, mercapto, amino, diamino or ureido,
the organic groups exemplary of X and Y having about 2 to
about 30 carbon atoms. Examples of such silane coupling
agents are ~- chloropropyltrimethoxysilane, vinyltrichloro-
silane, vinyl-tris (~ -methoxyethoxy)silane, ~ -methacryloxy-
propyltrimethoxysilane, ~-(3,4-epoxycyclohexyl)ethyltrimeth-
oxysilane, ~-glycidoxypropyltrimethoxysilane, ~mercapto-
propyltrimethoxysilane, ~-aminopropyltriethoxysilane, N-
~ -(aminoethyl)- ~-aminopropyltrimethoxysilane, -ureido-
propyltriethoxysilane, etc.
Titanate coupling agents:
Useful titanate coupling agents are represented by one
15 of the following fo:rmulae: :
(RO)n - Ti-~-0 - X- R - Y)m
iol
j ' Ti--~-- O--X--R2_ Y)2
2 o
CH2- O 2
¦ ~ Ti-~O -X_R _ Y)2
2 o
wherein RO is Cl 6 alkoxy, n is an integer of 1 or 4, m is
an integer of 2 or 3, X is carboxyl, phenyl, ethylene,
phosphate, pyrophosphate, phosphite or sulfonyl, R2 is
Cl 20 alkyl, and Y is hydrogen, allyl, vinyl or amino-
imino. Examples are isopropyltriisostearoyltitanate,
fi3~2
-14-
diisostearoyl ethylene titanate, titanium diacrylate
oxyacetate, etc.
The silane coupling agents or titanate coupling agents
give the component (b) or (c) improved affinity for the
component (a) and are effective for preparing suitable putty-
like compositions. Up to about 30 parts by weight, prefer-
ably about 2 to about 10 parts by weight, of such agents are
used per 100 parts by weight of the component (a).
According to this invention, the components (a), (b)
and (c) can be used conjointly with antioxidant, pigments,
carbon black, stabilizers, etc. which are usually used for
rubbers and plastics. Suitably these additives are used in
an amount of up to about 20 parts by weight per 100 parts
by weight of the component (a)..
The fire-retardant putty-like compositions of this
invention initially have a cone penetration value (mm/150
g. 5 sec, at 20C) of about 2 to about 40, preferably about
4 to about 15, as determined according to JIS A 5752-1966.
When having a cone penetration value within the above-
mentioned range, the putty-like compositions have suitable
softness for filling various spaces, joint clearance, etc.
The fire-retardant putty-like compositions of the
invention can be prepared by mixing the foregoing ingredients
with rolls usually used for mixing rubbers and plastics.
To effect dispersion of the ingredients, especially the
heat-resistant fiber, namely the component (c), in the compo-
sition with improved uniformity, the ingredients are pre-
-15-
ferably mixed together while being subjected to high-shear
friction with use of a kneader or the like.
The features of the fire-retardant putty-like compo-
sitions of this invention will be described below in greater
detail with reference to examples.
Examples 1-13 and Comparison Examples 1-6
The compositions listed in Table 1 were prepared with
use of a 2-liter experimental kneader and tested for mixing
workability, airtightness at room temperature, fire retard-
ancy, shape retentivity against heat and toughness ofashed product by the methods to be described later. The
properties of the compositions were evaluated according to
the criteria given below. The results are shown in Table 2.
The compositions of Examples 1 and 4, and Comparison Example
3 were filled in simulated cable bores and subjected to a
flame test under conditions similar to an actual fire as
will be described below to observe the burning process of
the compositions. Table 3 shows the results.
The above properties were determined by the following
test methods and evaluated according to the criteria given
below.
Mixing workability
The ingredients of each composition in specified
amounts were placed into a 2-liter test kneader equipped
with agitator blades and mixed together at room temperature
to 80C for 40 minutes. The resulting mixture was observed
with the unaided eye and touched with fingertips to evaluate
~r
!63~:
-16-
the homogeneity thereof according to the three criteria of:
excellent, good and poor.
Airtightness
An iron pipe, 300 mm in inside diameter and 600 mm in
length, was filled at its one end with the composition to a
thickness of 100 mm. While exposiing the outer surface of the
composition layer to the atmospheric pressure at 80C, air
was forced into the pipe from the other end at pressure of
0.8 kg/cm gauge for 5 minutes. If the leakage of air
through the composition layer was not larger than 5 liters/
min, the composition was evaluated as acceptable.
Fire retardancy
The oxygen index of the composition was determined in
accordance with JIS K 7201-1976 to evaluate the fire retard-
ancy based on the following criteria:
Not smaller than 80 in oxygen index -------excellent
60 to less than 80 in oxygen index ------- good
Less than 60 in oxygen index ------------- poor
Shape retentivity against heat:
The composition was shaped into a pillar, 3cm x 3cm x
7cm, which was then allowed to stand in its upright position
within an oven at 250 C for-30 minutes and thereafter withdrawn from
the oven. The resulting variation in the height of the pillar was mea-
sured to evaluate the shape retentivity based on the variation and
according to the following criteria:
Less than 5% in variation -------------- excellent
5% to less than 10~ in variation ------- good
fi3;~
-17-
Not less than 10% in variation, or
overturned or cracked pillar ------------ poor
Toughness of ashed product:
The composition was shaped into a cube, 3cm x 3cm x
3cm, which was then heated in an electric furnace at 1,000C
for 3 hours to a completely ashed state, thereafter with-
drawn and allowed to cool. The ashed residue was checked
for appearance and touched with fingertips to evaluate the
toughness according to the following criteria:
Uncollapsible with a strong pressing touch---excellent
Slightly collapsible with a strong
pressing touch --------------------- good
Easily collapsible with a light touch --------- poor
Flame test
The following flame test was conducted for the putty-
like compositions of Examples 1 and 4, and Comparison
Example 3 with use of bore penetrating cables simulating
those in actual buildings to observe the burning process of
the compositions as applied to the penetrating cable por-
tions.
A rectangular bore, 45 cm x 12 cm, was formed in the
center of a concrete board, 1 m x 1 m x 10 cm. Ten 600 V
polyvinylchloride-sheathed polyvinylchloride-insulated
cables, 34 mm in sheath outside diameter and 1.6 m in
length were passed through the bore as arranged side by side
at right angles to the concrete board, with equal lengths
of the cables projecting from opposite sides of the board.
.
63~
One of the above-mentioned compositions was filled in the
space within the bore around the cables to prepare a speci-
men. The lower side only of the specimen including the
cable portions projecting therefrom was assembled into a
vertical heating furnace measuring 1 m x 1 m x 1.5 m and
was sealed off. The interior of the furnace was heated with
propane ~as with its flame in direct contact with the bored
portion of the concrete board on its lower side. The speci-
men was heated for 2 hours in conformity with the heating
curve (room temperature to 1,010C, max.) provided in JIS A
1304-1975 and approximately representing the rise of temp-
erature in actual f~res. The same procedure as above was
repeated with use oX the other two compositions. The results
are given in Table 3.
32
-19-
Table 1
Examples No.
Material 1 2 3 4 5 6 7
. _ _ _ _
Polychloroprenel 100 70 50 100 100 100
Polychloroprene2 - 30 50 100
Polychloroprene3 ---- -
Zinc oxide - - 10
Tolylenediisocyanate - - - - 3
Aluminium hydroxide 60 ~m* 50 100 100 100 100 100 100
Aluminium hydroxide 25 ~m* 50 150 150 150 100 150 150
Aluminium hydroxide 35 ~m* 100 150 - 100 150
Aluminium hydroxide 10 ~m* 100
Magnesium hydroxide 10 ~m* - - - 150
Clay 30 ~m* 150
Zinc borate 30 ~m* -- 150 - -
Bentonite 10 ~m* - 30
Glass fiber 30 20 15 30 30 30 30
Asbestos fiber5 1010 10 10 1010
Phenolic fiber6 - -
Dioctylphthalate 3030 30 - 30
Antimony trioxide 10 - 10
Chlorinated paraffin7 - -
-Chloropropyltri- - 10 - - 10
methoxysilane
32
-20-
Table 1 (Continued)
Examples No.
Material 8 9 10 11 12 13
Polychloroprenel 70 80 100 100 100
Polychloroprene2 30 - 100
Polychloroprene3 - 20 - -
Zinc oxide - - 10
Tolylenediisocyanate - - 3
Aluminium hydroxide 60 ~m* 100 100 - 300
Aluminium hydroxide 25 ~m* 200 100 - -
Aluminium hydroxide 35 ~m* 200 100 300
Aluminium hydroxide 10 ~m*
Magnesium hydroxide 10 ~m* - - - 300 250
Clay 30 ~m* - - 100
Zinc borate 30 ~m* -
Bentonite lO~m*
Glass fiber4 20 30 30 60 ~30 30
Asbestos fiber5
Phenolic fiber6 10
Dioctylphthalate 30
Antimony trioxide - 10 - -
Chlorinated paraffin7 30 - -
~-Chloropropyltri-10
methoxysilane
~1 .
fi3~
-21-
Table 1 (Continued)
Comparison Examples No.
Material 1 2 3 4 5 6
Polychloroprenel 100 100100 100
Polychloroprene2 _ 100 - 100
Polychloroprene3 - - -
Zinc oxide 10
Tolylenediisocyanate - 3
Aluminium hydroxide 60~ m* 50 200 100 100 50 100
Aluminium hydroxide 25 ~m* - 300 100 150 100 150
Aluminium hydroxide 35 ~m* 130 300 100 50 50 150
Aluminium hydroxide 10 ~m* 100 -
Magnesium hydroxide 10 ~m*
Clay 30 ~m*
Zinc borate 30 ~m*
Bentonite 10 ~m*
Glass fiber4 30 30 5 1515 30
Asbestos fiber5 10 5 ~- 5 10
Phenolic fiber6
Dioctylphthalate 30 - - 30
Antimony trioxide - - -
Chlorinated paraffin
~-Chloropropyltri- - -
methoxysilane
æ
~ 2~3%
-22_
Notes for Table l
1, Viscosity at 25C; 100,000 c.p.s.,
End group; Alkylxanthate group
2, Viscosity at 25C; 57,000 c.p.s.,
End group; Hydroxyl group
3, Viscosity at 25C; 300,000 c.p.s.,
End group; Car~oxyl group
4, Diameter; 13 ~ m, Length; 6 mm
5, Diameter; 0.07~ m, Length; 13 mm
6, Diameter; 14 ~ m, Length; 6 mm
7, Chlorine Content; 70 w%
*, Mean particle size
3~
-23-
Table 2
Examples No.
1 2 3 4 5 6 7 8 9 10 11 12 13
Mixing
workability: E EEEEEE G EE G G G
Airtightness: A A A A A A A A A A A A A
Fire retardancy: EEEEEEEEEE E E E
Shape retentivity
against heat: EEEEEEEEE G E G E
Toughness of
ashed product: E E E E E E E E E G G G E
Comparison Examples No.
1 2 3 4 5 6
Mixing
workability: G P E E G E
Airtightness: U U A A U A
Fire retardancy: P EEE G E
Shape retentivity
against heat: P P P G P P
Toughness of
ashed produc~: P P P P P P
E: Excellent, G: Good P: Poor, A: Acceptable,
U: Unacceptable,
:
, ..
fi3~
-24-
Table 3
Burning process
.. . . _ _
Examples 1 No smoke leaked through the bore to the upper
and 4 side of the specimen outside the furnace even
two hours after the start of heating. The
cable sheaths on the upper side remained free
of burning although slightly thermally ex-
panded.
No portion of the composition in the bore
dropped. Inside the furnace, the composition
was found to have been ashed as held in place
without falling, and maintaining the original
shape thus very effectively preventing the
spread of fire.
Comp. Ex. One hour after the start of heating, the com-
3 position, burned and ashed on the inner side
of the furnace, began to release part of the
ashed product. Ashed portions thereafter
dropped in an increasing amount, permitting
marked outflow of smoke through the bore to
the upper side. The cable sheaths burned in
the vicinity of the bore on the upper side of
the specimen outside the furnace.
;: ' ~
1~2~3~
-25-
As will be apparent from the above examples, the
fire-retardant putty-like compositions of this invention can
be prepared with sood mixing workability, are usable with
extreme ease because of suitable softness, retain high
airtightness at room temperature, will not soften, sag or
drop unlike conventional compositions even when exposed to
the high temperature of a fire, and give a hard, compact
and tough residue even if ashed to very effectively prevent
the spread of fire.
Of these outstanding properties, the present composi-
tions are distinct from the conventional compositions in
that they will not become softened and form a tough residue
when burned and ashed. Thus these are remarkable features
for the present invention.
, - . , ~ ,,
