Note: Descriptions are shown in the official language in which they were submitted.
108S998
BACKGROUND OF THE INVENTION
Field of the Invention
This invention pertains to the field of urethane-
modified polyisocyanurate rigid foams. More particularly,
this invention pertains to the use of specific polyols
utilized in preparing said foams.
Description of the Prior Art
Urethane-modified polyisocyanurate rigid foams
are known in the art. Such foams are prepared by reacting
a polyol, polyisocyanate and optionally other ingredients
in the presence of a blowing agent. An isocyanurate group
formation catalyst is used to trimerize the isocyanate
groups to form the isocyanurate linkages. The polyol
essentially acts as a modifying or reactive plasticizing
agent in the overall polymeric scheme since a polymer
containing only isocyanurate groups is itself too friable.
Thus, the isocyanurate foam contains both isocyanurate
groups, as well as urethane linkages, with said urethane
linkages acting to plasticize the foam. Initially, the
reaction proceeds to give a urethane quasi-prepolymer
containing active isocyanate groups which during the sub-
sequent reaction time, trimerize to give a polymer rich in
isocyanurate linkages. This sequence ultimately produces a
urethane-modified polyisocyanurate polymer.
Some main uses of the resultant foam include
those of thermal insulation, and as building materials and
the like. Examples of some prior art, isocyanurate foams
and methods of preparation are described in U. S. Patent
Nos. 3,745,133; 3,644,232; 3,676,380; 3,168,483, and 3,519,95Q
to name a few.
- 1- ,; ,~,
: .
1085998
However, many known polyisocyanurate foams have
one or more disadvantages. In par~icular, rigid foams of
this type often have high friability or propensity to
break. Efforts to reduce friability have often resulted in
sacrifice of dimensional stability, and thermal stability
and flammability resistance. Lack of flammability resistance
is particularly characterized by flame spreadability. Yet
other prior art polyisocyanurate foams have suffered from
disadvantages of low adhesiveness, irregular cell structure
and the like.
One class of polyols disclosed as being useful in
preparing polyisocyanurates are novolak resins or derivatives
of novolak resins, including, alkoxylated novolak resins.
See, for example, U. S. Patent Nos. 3,723,364; 3,723,367;
3,728,293; 3,745,133; 3,842,036; and 3,849,349. In each
instance, the novolak resin is prepared by reacting an
excess of a phenolic compound such as phenol itself with an
aldehyde such as formaldehyde. The excess aromatic phenol
is then removed and the resin used as such or derivatized,
such as by preparing an oxyalkylated phenol-aldehyde resin.
However, it has been found here that such novolak polyols,
while useful in preparing rigid polyisocyanurate foams,
nevertheless, still do not have the requisite degree of low
friability necessary for a commercial application.
We have now found that it is now possible to
prepare modified polyisocyanurate foams involving use of
specific novolak polyols that do not exhibit any of the
aforesaid disadvantages. We have particularly found that
urethane-modified polyisocyanurate foams can be prepared
having suitable dimensional stability, low friability and
--` lV8S998
good flammability resistance. Such are achieved without sacrifice of other
sought-after properties such as thermal stability.
SUMMARY OF THE INVENTION
The present invention is an improved modified rigid polyisocyanurate
foam comprised of the reaction product formed by bringing together in the
presence of blowing agent, and an isocyanurate group formation catalyst, an
aromatic polyisocyanate and a polyol comprising an alkylene oxide adduct of
a novolak resin containing 5-25 weight percent of free phenol or substituted
phenol based on the weight of said resin. The rigid foams exhibit suprisingly
good dimensional stability, low friability, and good flammability resistance,
as well as good thermal stability.
The present invention provides a urethane-modified polyisocyanurate
rigid foam comprising a reaction product obtained by bringing together in the
presence of a blowing agent, an aromatic polyisocyanate, an isocyanurate
group formation catalyst and a polyol comprising the addition product of
an alkylene oxide to a mixture of a novolak resin and phenol or substituted
phenol wherein said phenol or substituted phenol is present in an amount of
5-25 weight percent based on the weight of said resin.
The present invention also provides a process for preparing a
urethane-modified polyisocyanurate rigid foam comprising the steps of mixing
and reacting in the presence of a blowing agent and an isocyanurate group
formation catalyst, an aromatic polyisocyanate and a polyol comprising the
addition product of an alkylene oxide to a mixture of a novolak resin and
phenol or substituted phenol wherein said phenol or substituted phenol is
present in an amount of 5-25 weight percent based on the weight of said
resin.
DETAILED DESCRIPTION OF THE INVENTION
The modified isocyanurate foams of the present invention in
rigid foam form are prepared by mixing in the presence of a blowing agent
~ _ 3 _
B
-
1085998
an isocyanurate group formation catalyst, an aromatic polyisocyanate and
a polyol comprising an alkylene oxide adduct of a novolak resin containing
5-25 weight percent of free phenol or substituted phenol based on
the weight of said resin. The mixing is carried out under conventional
foaming conditions utilizing conventional mixing devices employed in the
manufacture of polymer foams. The procedure for mixing of the materials
for the formation of the reaction product is not critical to the invention.
Examples of conventional polymer foam formation processes and equipment are
described in Ferrigno, "Rigid Plastic Foams", Reinhold Publishing Corporation,
New York, New York, 1963.
- 3a -
B
/ - -
108599~
In essence the novolak resin containing free
phenol is subjected to alkoxylation whereby both the resin
and free phenol are reacted with the alkylene oxide.
To provide the polyols described here, one first
prepares a novolak resin. These phenol-aldehyde resins are
polynuclear compounds having the structure:
OH OH OH
/~
Xn Xn Xn
wherein R is hydrogen or an alkyl radical having from 1 to
3 carbon atoms, X is hydrogen, hydroxy, chlorine, bromine or
an alkyl radical having from 1 to 12 carbon atoms, n is an
integer from 1 to 2 and m is an integer from 0 to 4.
The novolak resins are prepared by condensing
phenol or an ortho or para-substituted derivative thereof,
such as cresol, xylenol, resorcinol, chlorophenol, bromo-
- phenol, isopropylphenol, t-butylphenol, octylphenol, nonyl-
phenol, or dodecylphenol with an aldehyde in acidic solution
and at a reaction temperature between about 60 and 160C.
The novolak resins may contain from 2 to 6 aromatic rings
per molecule, but preferably contain an average of from 2.2
to 3.2 aromatic preferably, benzene rings.
The aldehydic reactant can be formaldehyde,
acetaldehyde, propionaldehyde, or butyraldehyde, but is
preferably formaldehyde, or a derivative, e.g. trioxane.
Suitable acidic catalysts for the novolak resin reaction are
oxalic acid, zinc acetate, hydrochloric acid, sulfuric acid
or stannous octoate.
1085998
The reaction for making the novolak resins is
carried out at the above temperature range and at atmospheric
pressure or thereabouts, employing the phenol or phenolic
derivative in amounts corresponding to from about 1.5 to
about 3.0 moles of phenolic compounds per mole of aldehyde.
In the usual case, in order to derivatize a
novolak resin or use it directly in some use such as a
polyol source for polyurethane or polyisocyanurate foams,
the novolak is first stripped of excess phenolic compound.
It has been thought that it is necessary to strip off
excess phenol in order to desirably increase the function-
ality and provide proper crosslinking. One would expect
that by leaving present in the resin excess phenolic compound,
overall functionality of the resin mixture would be undesir-
ably lowered to give a product of two or lower functionality
including monofunctional products, having unsuitable proper-
ties as a polyol for urethane resin formation or even other
uses. However, it has been found that a suitable, and in
fact greatly desirable polyol source for urethane-modified
polyisocyanurate rigid foams may be prepared directly from
a novolak resin containing excess phenol by leaving in the
resin the excess of phenol and avoiding a separate stripping
step. One thus achieves a considerable cost and time
savings particularly in terms of time savings. In addition,
it has been found that the friability of the resulting
rigid polyisocyanurate foam is desirably low due to presence
of a low functional polyol including monofunctional species,
namely, excess phenolic compound hereafter alkoxylated,
along with the novolak resin. As a still further advantage,
the unstripped novolak resin polyols has a lower viscosity
~08599~
than the conventional stripped novolak resin polyols,
resulting in easier handling. Lastly, due to the built-in-
chain stopper, i.e., the low functional alkoxylated phenol,
more isocyanurate linkages are allowed to be formed per
chain in a desirable manner. Usually, presence of mono-
functional compounds is avoided in cases of this type, due
to undesirable chain-stopping. However, presence of such
mono functional compounds can be tolerated, and in fact is
desirable here because the final rigid polyisocyanurate
polymer is cross-linked through the isocyanate group.
Greatly preferred novolak resins containing
excess phenol or phenolic compound are those having a
hydroxyl number ranging from about 180 to about 325.
The novolak resin containing excess phenol or
phenolic compound is then condensed with alkylene oxide.
Such procedures are well known to those skilled in the art,
and such reaction is usually readily carried out in the
presence of a suitable catalyst.
Preferred oxyalkylating agents comprise alkylene
oxides having from 2 to 4 carbon atoms, and more preferable,
the 1, 2-oxides having 2 to 3 carbon atoms, i.e., ethylene
oxide and propylene oxide. Another useful agent of this
type is trichlorobutylene oxide.
The oxyalkylated novolak products here are chemically
tailored by the utilization of a specific alkylene oxide or
mixtures thereof in various quantities. The hydroxyl
number and viscosity of the final polyol product is determined
by various factors, such as temperature of reaction, particular
oxyalkylating agent used, its manner of addition to the
reaction media, and quantities used. The alkylene oxide
addition scheme is therefore somewhat emperical and depends
1085998
upon factors such as the product desired, the alkylene oxide
used, the type of addition, the order of addition, and the
temperatures at which the alkylene oxides are added. For
example, the alkylene oxide reagent can be added to the
novolak resin containing excess phenol in either a heteric
or a blocked manner or a combination thereof.
When blocked addition of the novolak resin con-
taining excess phenol is sought, as an example, ethylene
oxide may be first added, followed by addition of propylene
oxide. Various addition methods yield products of the
desired viscosity range with desirable hydroxyl numbers. As
another example, heteric-type addition can be employed
whereby a mixture of ethylene oxide and propylene oxide is
added. In such use, the relative concentrations of alkylene
oxides can be changed. Thus, the relative concentration of
ethylene oxide to propylene oxide may be varied in the
mixture as the reaction progresses. For example, an ethylene
oxide rich mixture may be initially metered into the reaction
mixture. As the addition progresses, the relative concen-
tration of propylene oxide may be increased. This can be
accomplished with, for example, a valved mixing nozzle
which is progressively regulated.
A greatly preferred polyoxyalkalene polyol com-
prising the alkoxylated adduct of a novolak resin containing
excess phenol or phenolic compound is the ethylene oxide or
propylene oxide of such mixture. Most preferable, the
polyol utilized here is an ethylene oxide adduct, propylene
oxide adduct or mixed ethylene oxide-propylene oxide adduct
of novolak resin, plus excess phenol, prepared by reacting
1-4 moles of the alkoxylating agent per hydroxyl group of
the novolak and the phenol.
~O~S998
It has been found here that the above described
polyol is specifically tailored for use in rigid polyiso-
cyanurate foams, and must be exactly constituted as directed
to provide foams of desired and necessary physical properties.
First, for example, if one does not alkoxylate the novolak
resin containing excess phenol, a resultant rigid isocyanurate
foam is obtained which is not sufficiently stable. On the
other hand, foams prepared from the polyols described here
have excellent dimensional stability and exhibit minimal
volume, weight and linear changes. Again, the polyols here
are so constituted to impart the proper amount of cross-
linking to the rigid foams, and yet, have a proper overall
functionality to provide desirable physical properties.
As used above, the hydroxyl number is defined as
the number of milligrams of potassium hydroxide required for
the complete neutralization of the hydrolysis product of the
fully acetylated derivative prepared from one gram of polyol.
The hydroxyl number can also be defined by the equation:
OH = 56.1 X l,000 X F
MW
where
OH = hydroxyl number of the
polyol
F = average functionality, that
is the average number of hydroxyl
groups per molecule of polyol.
MW = average molecular weight
of the polyol.
Any aromatic polyisocyanate may be used in the
practice of the instant invention. Typical aromatic poly-
isocyanates include m-phenylene diisocyanate, p-phenylene
diisocyanate, polymethylene polyphenylisocyanate, 2, 4-tolylene
1085998
diisocyanate, 2, 6-tolylene diisocyanate, dianisidine
diisocyanate, bitolylene diisocyanate, naphthalene-l, 4-
d~isocyanate, diphenylene-4, 4'-diisocyanate, aliphatic-
aromatic diisocyanates, such as xylylene-1, 4-diisocyanate,
xylylene-l, 3-diisocyanates, bis(4-isocyanatophenyl)methane,
bis(3-methyl-4-isocyanatophenyl)methane, and 4, 4'-diphenyl-
propane diisocyanate.
Greatly preferred aromatic polyisocyanates used
in the practice of the invention are methylene-bridged
polyphenyl polyisocyanate mixtures. These latter isocyanate
compounds are generally produced by the phosgenation of
corresponding methylene-bridged polyphenyl polyamines,
which are conventionally produced by the reaction of formal-
dehyde and primary aromatic amines, such as aniline, in the
presence of hydrochloric acid and/or other acidic catalysts.
Known process for preparing the methylene-bridged polyphenyl
polyamines and corresponding methylene-bridged polyphenyl
polyisocyanates therefrom are described in the literature
and in many patents, for example, U. S. Patent Nos. 2,683,730;
2,950,263; 3,012,008; 3,44,162 and 3,362,979.
Most preferred methylene-bridged polyphenyl
polyisocyanate mixtures used here contain from about 20 to
about 100 weight percent methylene diphenylisocyanate
isomers with the remainder being polymethylene polyphenyl
isocy~nates having higher functionalities and higher molecular
weights. Typical of these are polyphenyl polyisocyanate
mi~tures containing about 20 to 100 weight percent methylene
diphenylisocyanate isomers, of which 2 to about 40 weight
percent thereof is the 2, 4'-isomer, with the remainder
being polymethylene polyphenyl polyisocyanates of higher
molecular weight and functionality such that they have an
_g_
~V~5998
average functionality of from about 2.1 to about 3.5.
The isocyanate mixtures are known, commercially available
materials and can be prepared by the process described in ~ -
U. S. Patent No. 3,362,979, issued January 9, 1968, to
Floyd E. Bentley.
Foaming is accomplished by employing in a minor
amount (for example, from about 5 to 25 weight percent,
based on total weight of the reaction mixture), of blowing
agents which are vaporized by the exotherm of the isocyanato-
reactive hydrogen reaction. The preferred blowing agents
are certain halogen-substituted aliphatic hydrocarbons
which have boiling points between about -40C., and 70C.,
and which vaporize at or below the temperature of the
foaming mass. The blowing agents include, for example,
trichloromonofluoromethane, dichlorodifluoromethane, dichlo-
romonofluoromethane, dichloromethane, trichloromethane,
bromotrifluoromethane, chlorodifluoromethane, chloromethane,
l, l-dichloro-l-fluoroethane, l, l-difluoro-l, 2, 2-
trichloro-ethane l, 1, l-trichloro-2, 2, 2-trifluoroethane,
2-chloro, l, 1, l, 2, 3, 3, 4, 4, 4, -nonafluorobutane,
hexafluorocyclobutane, and octofluorocyclobutane. Other
useful blowing agents include water and low-boiling hydro-
carbons such as butane, pentane, hexane, cyclohexane, and
the like. Many other compounds easily volatilized by the
exotherm of the isocyanate-reactive hydrogen reaction also
can be employed. A further class of blowing agents includes
the thermally unstable compounds which liberate gases upon
heating, such as N, N'-dimethyl-N, N-dinitrosoterephthalamide.
The amount of blowing agent used will vary with
the density desired in the foamed product. In general, it
--10--
10~9~8
may be stated that for 100 grams of reaction mixture con-
taining an average ratio of isocyanate group-reactive
hydrogen of from about 1:1, to 20:1, about 0.05 to 0.3
mole of gas is used to provide densitites ranging from 30
to 1 pound per cubic foot respectively.
The isocyanurate group formation catalyst or
catalysts employed to promote trimerization may be chosen
from a variety of known materials. Such catalysts include
strong bases, alkali metal salts of carboxylic acids,
nonbasic metal salts of carboxylic acids and aliphatic
tertiary amines. For example, suitable strong bases include
guaternary ammonium hydroxide, alkali metal hydroxide, and
alkali metal alkoxides. Suitable alkali metal salts of
carboxylic acids include, for example, sodium acetate,
potassium octoate, potassium acetate, sodium benzoate, and
the like. Examples of suitable tertiary amines are N,
N'diethylpiperazine, N, N'-dimethylpiperazine, trialkylamines
such as trimethylamine, triethylenediamine, tributylamine,
2, 4, 6-tris~dimethylaminopropyl)hexhydro-s-triazine, 2, 4,
6-tris-(dimethylaminomethyl)-phenol and the like. Mixtures
of catalysts may also be employed.
~he particular amount of catalyst employed can
vary over a wide range and is not critical so long as it is
present in an amount sufficient to promote trimerization of
the isocyanate mi~ture. Preferably, the catalyst is added
in an amount of about 0.0005 to about 0.025 equivalents for
each ~quivalent of isocyanate employed. An optimum amount
would be from about 0.001 to 0.01 equivalents per equivalent
of isocyanate. Expressed in other terms, the catalyst or
~085998
catalyst mixture is preferably added in an amount of from
about 0.03 up to about 5.0 parts by weight, based upon the
total foam formulation, i.e., 100 parts by weight.
Though not necessary, as will be seen hereafter,
the isocyanurate foams of the invention can be formulated
to include flame retardant components to improve the fire
retardancy of the foams. Any known flre retardant component
compatible with rigid isocyanurate foams can be employed.
This would include both the reactive and additive type fire
retardants. Representatives of the additive types include
halogenated organic phosphates such as tris~chloroethyl)
phosphate, tris(2, 3-dibromopropyl)phosphate, triphenyl
phosphite, diammonium phosphate, and antimony oxide.
Representatives of the chemically bound types are diethyl-
N, N'-bis(2-hydroxyethyl)aminomethyl phosphonate, chlorendic
acid derivatives, and phosphorous-containing polyols. When
employed, the fire retardant component is added to the
above-described isocyanate mixture with some other component
or as a preformed mixture with some other component described
hereinbefore, in an amount of about 1 to about 20 weight
percent of the total foam formulation.
Furthermore, fillers can be employed in the
preparation of the isocyanurate foams, if desired in amounts
within the range of about 0.1 to about 20 weight percent of
the total foam formulation. Any conventional filler known
in the art to be compatible with isocyanurate foam manufac-
ture can be employed, such as hydrated alumina, polyethylene,
aluminum powder, and various clays and talcs.
108S998
An emulsifier or stabilizing agent may also be
used in the preparation of the isocyanurate foams of this
invention including, for example, sulfonated castor oil or
the like. One preferred foam stabilizer is that based on
silicon such as, for example a polyoxyalkylene block co-
polymer of a silane. The latter type of silicone surfactant
is disclosed in U. S. Patent No. 2,834,748. Other surfac-
tants or emulsifying or dispersing agents which may be used
include ethylene oxide modified sorbitan, monopalmitate or
ethylene oxide modified polypropylene ether glycol.
The amount of novolak polyether polyol employed
in relation to the organic aromatic polyisocyanate is not
critical, but preferably ranges in an amount of from about
0.05 to about 0.5 equivalents per equivalent of polyiso-
cyanate. Optimally, about 0.1 to about 0.25 equivalents
per equivalents of polyisocyanate is employed. Moreover,
the polyol can be added to the polyisocyanate as a separate
component or as a preformed mixture with one or more of the
other components.
To prepare the isocyanurate foams of the invention,
the above discussed ingredients may be simultaneously, or
independently intimately mixed with each other by the so-
called "one shot" method to provide a foam by a one-step
process. Proportions of ingredients are properly adjusted
to give rigid foams. In addition to the "one shot" method
the "quasi-prepolymer method", may also be employed. Here,
a portion of the polyol is reacted in the absence of a
cataly~t with the polyisocyanate component. Thereafter, to
prepare a suitable foam, the remaining portion of the
polyol is added and reaction allowed to go to completion in
-13-
:' ' , . ' : .
1085998
the presence of catalyst along with other appropriate
additives such as blowing agents, foam stabilizing agents,
fire retardants, etc.
Again, the isocyanurate foams of the present
invention may be prepared over a wide range of temperatures.
However, normally, the reaction is initiated at room temper-
ature, and the only heat involved is that generated by the
polymerization itself.
The invention will be illustrated further with
respect to the following examples, which are given by way
of illustration and not as limitation on the scope of this
invention.
EXAMPLES I-XI
Here, preferred polyols of the invention were
. first prepared. A typical procedure for the preparation o~
these polyols is described below.
To a 15 gallon kettle was charged 28.2 pounds
(.30 pound moles) phenol. A condensation reaction catalyst,
oxalic acid dihydrate in an amount of 115 grams was then
added. Upon heating to 90C., 37 percent aqueous formal-
dehyde was added (13 pounds, .16 pound moles) over a period
of fifteen minutes. The mixture was then digested at 100-
150C. for 2 hours. Water was distilled from the mixture
together with some phenol which carried over while the
temperature was raised to 180C. The remaining resin and
phenol (28.75 pounds, .287 pound moles), was cooled to 80-
90C., and an aqueous alkoxylation catalyst was added.
After removing water, the mixture was heated to 140C., and
16.6 pounds of propylene oxide (.287 pound moles), was added
and then digested to constant pressure. While holding the
mixture at 140C., ethylene oxide (12.6 pounds, .287
~.o~S998
pound moles), was added and then digested to constant
pressure. After neutralizing the alkoxylation catalyst, the
product was recovered to yield 52.5 pounds. This product is
designated polyol Number 9 in Table I below.
A number of other polyols of the invention were
prepared which are listed in Table I below, as well as their
characteristics and method of formation.
Polyols No. 4 and 5 represent extremes of free
phenol content. Polyol No. 4 with a functionality of
3.4 has a free phenol content prior to alkoxylation of 7%
while Polyol No. 5 with a functionality of 1.7 has a free
phenol content of 25%.
-15-
.
1085998
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-16-
108S998
EXAMPLES 12-39
In these examples, 600 g. handmix box pour foams
were made to determine foaming behavior utilizing typical
novolak polyols. A pre-blended B-component was combined
with the isocyanate (A-component), stirred 2-3 seconds and
poured. Stirring was accomplished with a drill press motor
with an attached stirrer made by assembling one Conn mixer
and two medium lift impellers on a steel shaft. The motor
was operated at 4200 rpm.
The formulation of these rigid foams is shown
below:
-component
Polyol
DC-193 Silicone( )
Potassium Octoate(2)
DMAPAT(3)
FYROL CEF(4)
R-llB(5)
A-Component -
PAPI-901(6)
(l). Silicone-polyether; Dow Corning Corporation
(2). Potassium octoate was prepared from potassium hydroxide
(1.0 mole) and 2-ethylhexanoic acid (1.1 mole) as a
50% solution in a propylene oxide adduct of glycerin,
molecular weight 700; Jefferson Chemical Company, Inc.
(3). Tris [N, N-dimethyl-3-aminopropyl] sym hexahydro
triazine.
(4). Tris (chloroethyl) phosphate; Stauffer Chemical Company.
and Company.
(5). Trichloromonofluoromethane, E. I. duPont de Nemours
and Company.
(6). Methylene-bridged polyphenyl polyisocyanate mixture
obtained from Upjohn Company.
-17-
10~3S998
T A B L E II
Formulation, pbw. 12 13 14 15 16
B-Component
Polyoll 21.2 21.2 20.9 21.3 21.0
DC-193 0.5 0.5 0 5
Potassium octoate1.0 ---- ---- 0.5 0.5
ATl 2.5 ____ 1.0 ----
DMP-30 ---- ---- 4.0 ---- 2.0
FYROL CEF 6.0 6.0 6.0 6.0 6.0
R-llB 12.0 12.0 12.0 12.0 12.0
A-Component
PAPI-901 59.3 57.8 56.6 58.7 58.0
Reactivity values, sec.
CT 5 2 2 3 3
RT 35 60 120 27 38
NCO/OH index 5.0 5.0 5.0 5.0 5.0
_am Properties
Density, pcf 2.17 1.91 1.98 2.09 2.03
Closed Cells,% 90.9 90.6 92.0 90.8 91.8
K-Factor .128 .129 .128 .125 .126
Heat distortion, C. >225 204 204 219 184
Friability 48 33 9 57 29
Compressive strength
with rise, psi 39 27 41 38 43
cross rise, psi16 10 19 12 15
Butler Chimney*
Wt. retained, %96.7 93.5 92.9 95.6 94.9
Flame height, in. 3.3 6.5 6.3 4.2 5.4
Dimensional stability
~V ~W ~L, 1 wk
158F, 100~ rel.
hum. 4-3 3 8-5 6 5 0 45-3 4 4-2 3
2, 4, 6-tris-[dimethylaminomethyl] phenol, a product of
Rohm and Haas.
*Numerical or other data from this test are not intended
to reflect hazards presented by this or any other material
under actual fire conditions. The data represents the
behavior of the tested material under specific controlled
test conditions~
-18-
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--20--
- 1085998
EXAMPLES 40-48
Here runs were made by machine performed by conven-
tional spray techniques utilizing a Gusmer spray machine to
prepare the rigid foams. Both, A and B-components were pre-
blended and charged to the machine. Then spray was applied
in both single layer and multi-layer fashion for test purposes.
The foams thus prepared had unifoam fine cells and good ~-
appearance. In addition, the thermal stability was excellent
as shown by heat distortion and flammability resistance as
evidenced by the Butler Chimney and Monsanto Tunnel values.
The values in parenthesis in the Monsanto test represent the
values obtained with a control standard foam. This foam was
a Clasg I polyisocyanurate foam which was purchased com-
mercially.
Results are given in Table III below.
-21
o o co o o r~ 1~.,1 h¦co ~ ~ ~ o ~ o lV8S998
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--22--
:
c~o ~ ~ o~ 1~8S998
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m ~ :3 ~ 0 ~ 0
--23--
1085998 :;
o o ~r o o o ~ I h~ 1 O ~ o o --I , '
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a) ~n C~1 ,1 h
ndP a) ~ ~
C U r~ h ~ .C C O
O O O o ~ O O o ~ ~ ~ ~ ~ ~ U
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U ~ ~ ~ h ~ ~ a) ~ a) C C ~ -I V
O I ,1 :3 a) ~-,1 U _l h ~ al a) u~ h 0 ,1
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~ a) ~: a) ~ q ~ h a) ~ ~-,1 rl h ~ ~ S h ,1
O ~ ; ~ O N O a) Ul Q~-,l o ~ U h cO ,~ ~n h C~ a) -I a) U
Orlrl ~O ~1 h U ~ Q ~ O-,~ n h a) 0 ~ a
X ~ ~ U~ ~ ~ a) ~ o ~ ~ ~ a) ,1~ o 0
0 0 a~ u~ ~ m ~ ~: a) . _1 ~ h ~ ~1 a) U ~ h ~ O a) 0 ,~
I 0 ~ ~1 0 Z ~: C ~ ~ a) N ~ ~4tq ~n 0 ~J 0 Q,-,l h ~ I h
O ~ ¢ O rl Ei Ei 5:: N U~ C 0 ~ 4 a) h h
~ ~ O c~ O ~ I ~ 5; ~ S I a) ,1 o ,1 ~a)--l I al h O ~ E~ a) a
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Z ~ * O
--24--
10859g8
l a) ~ .
'~ ~ ~r ~
~ ~ ~ _ o
co a~ D
~r ~ ~
a) _~ 1 o
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~ ~1 ,_~--~ --O
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t- C~ ~ ~ .
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H ~ dO ~i a~ O
H U~ ~7 t~ I eP _I
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m ~ l ~ .
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D _ _
~ _ j _ j ~ .
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u
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u~ ~ co ~ ~ t~
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O tn~1
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ri ~ ~ ~ ~ ~ ~ o
tn ~ ~ ,c ~r ~ x ~o _l
3-i *
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O ~ 1
Z o 3 ~ o
o ~ 3 ~1 ~4 3 ~
~ ~ a
O ~rl O * ~
* F
--25--
1085998
While the formulations described above were
intended primarily for spray application, other types of
application are possible utilizing the polyols here, in-
cluding use as short rise laminated panels, slab stock
foam, high rise molding, and pour-in-place applications.
As can be seen from the above Examples, the
polyols described here are uniquely tailored to provide
rigid polyisocyanurate foams possessing high resistance to
deformation and exposure to heat, low friability, low flame
spreadability, low smoke evolution, excellent dimensional
stability and other sought after properties.
3n
-26-
