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Патент USA US2105511

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Patented Jan. 18, 1938
Robert Dewey' Snow and Harold Joseph Hepp,
Bartlesville. Okla., assignors to Phillips Petro
leum Company, Bartlesville, Okla., a corpora
tion of Delaware
Application April 18, 1934, Serial No. 721,203
3 Claims. (Cl. 10G-22)
'I‘his invention relates to the manufacture of
multicellular heat and sound insulating mate
rials from the high molecular weight reaction
composition products to expand the resin to a
cellular form when the pressure is released. Im
mediate cooling is then provided to prevent fur
ther fiow of resin in the intercellular films.
The products produced by either of the above
_ products of sulfur dioxide and unsaturated com
pounds, all as more fully hereinafter described
and claimed.
It is well known that cellular material having
processes are light inn weight, but quite strong
and resistant to physical damage and disinte
gration. From the foregoing, it is evident that
a large volume percentage of dead gas space in
10 the form of small cells generally has good heat
they can be produced either by controlled elimi
nation of excess sulfur
insulating and sound proofing properties. ` Such
the resinous material in sulfur dioxide, or by
heating the solid resinous material under pres
sure to a temperature above its softening point,
quickly releasing the pressure and cooling the
and thus takes advantage of the very low heat
conductivity of still gases.
We have found that such a material of cellular
structure, suitable for sound proo?lng, and heat
insulation at low or moderately elevated tem
peratures, can be manufactured from the resinous
or high molecular weight polymeric compounds
formed by the reaction of sulfur dioxide with
unsaturated compounds. Such compounds have
been described, for example, in British Patent
Serial No. 599,350, ñled
expanded product so produced.15
The methods of practicing the processes of
the present invention are illustrated by the fol
lowing examples and the accompanying drawing..
Example I
One mol. of butene-Z and one and one-quarter
mois of SO2 -are mixed with a quantity of AgNOs,
LiNOa. NHiNOa or other suitable catalyst. cor->
those described, the most suitable for the manu ' responding to 0.01-0.1 per cent of the weight
of SO2 and olefin, and are allowed to react in
facture of our product are the complexes of those
oleiins containing more than three carbon atoms a pressure vessel. When reaction is complete,
the product is warmed to the desired degree of
to the molecule.
>fluidity and is then forced by pressure through
Such complexes will absorb considerable quan
tities of sulfur dioxide and form agelatinous or an oriiic into anexpansion chamber where the
viscous solution. If the excess sulfur dioxide in evaporation of SO2 is controlled by pressure. In 30
the gel’be'limited to a small amount, and the l general the cooling effect due tothe evapora
gel heated under pressure till it becomes fluid, tion of SO2 is suiiicient and the expansion cham
ber need not be further cooled. The same pur
a rapid release of the pressure will cause the
gel to expand, assuming a. light, fairly uniform,
cellular form whose structure is preserved by
~ cooling.
The expanded material may thus be
»formed by controlled elimination of excess sulfur
We have also found another way in which ex
panded, cellular material may be manufactured
from these complexes of sulfur dioxide and un
saturated compounds. Virtually all such com
plexes begin to decompose even below the tem
peratures at which they soften appreciably, re
generating sulfur dioxide and the unsaturated
compound. 'I'his decompositionreaction is gen-'
erally slow below the softening temperatures, but
increases rapidly as the temperature increases.
If the solid, resinous material, free from excess
sulfur dioxide, is heated a short time at a tem
perature at which it is Huid, and under pres
sure suiiicient -to prevent the formation of a
gaseous phase. it ssen accumulates enough de
pose may be accomplished by dissolving the dry,
solid resin in SO2 and extruding, and the tem
perature and partial pressure of~SOa in the ex
pansion chamber may be varied over wide ranges
depending upon the product desired. Apparatus
suitable for carrying out this process is shown
in Figure I.
Example II
Resin formed by the reaction of SO2 with an
unsaturated compound is ground or pulverized
and the excess SO2 and other volatile materials
are allowed to evaporate. 'I'he resin is then
charged to a cylinder fitted with a plunger for
applying pressure tothe resin and with steam
coils, electric resistance elements or other means
of heating. 'I'he resin is heated under pressure
until it is iiuid. An orifice is opened in the end 50
of the cylinder and the resin is extruded into
an expansion chamber Where it is quickly cooled
in the expanded form. Apparatus suitable for
-carrying out this process is shownin Figuren.
Resin formed by the reaction o! SO2 with an
unsaturated compound is groundor pulverized
2. A substantially cellular material, light in
weight, and suitable for heat and sound insu
lation, the said material containing small gas
pockets surrounded> by retaining walls oi a resin
and is charged to a cylinder fitted with two
ous, polymeric compound formed by the-reaction
drawn and the resin isquickly cooled in the
expanded form. That remaining in the cylinder
polymeric compound is essentially non-plastic at
plungers. Heat and pressure are applied until «of sulfur dioxide with 4an olefin of more than
the resin is iluid. One plunger is suddenly with f three carbon atoms to the molecule, and which
is pushed out with the second plunger. y Appa
.1.0 ratus suitable for carrying out this process is
shown in Figure III.
What we claim and desire to secure by Letters
3. A substantially cellular material, light in 10
weight, and suitable for heat and sound insu
lation, thevsaid material containing small gas
pockets surrounded by'retaining walls of a resin
1. A material suitable for heat and sound in
ous, polymeric compound formed by the reaction
of sulfur dioxide with olefins predominantly of
sulation comprising a> resinous reaction product
essentially non-plastic at atmospheric tem
Patent is:
atmospheric temperatures.
/ `
of sulfur dioxide and an olefin containing three
f orv more carbon atoms in expanded, cellular form,
and essentially non-plastic at atmospheric tem
20 peratures.
three or more carbon atoms per molecule and
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