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Патент USA US3084137

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United States- Patent O?ce
1
3,084,127
PROCESS FOR MAKING A CELLULAR MATE
RlAL FROM A VINYL CHLORIDE POLYMER
PLASTISOL
Walter J. Vakouslry, Seymour, Conm, assignor to The
B. F. Goodrich Company, New York, N.Y., a corpora
tion of New York
No Drawing. Filed Dec. 6, 1960, Ser. No. 73,986
9 Claims. (Cl. 260-25)
This invention relates to a process for the manufacture
of cellular vinyl chloride polymer materials from a plasti
sol using a metal borohydride and water to effect the ex
3,084,127
Patented Apr. 2, 1963
2
immediately thereafter, the desired delay in the reac
tion between metal borohydride and water is realized.
The isocyanates useful in this invention are those which
have the structural formula R(NCO)x wherein R is an
organic radical free of reactive hydrogen and x is an
integer. The organic radical R may be any aliphatic,
alicyclie or aromatic radical which is free of reactive
hydrogen since it is the (NCO)- radical of the isocyanate
which is responsible for delaying the reaction between
10 the metal borohydride and water. The number of termi
nal (NCO? groups in the isocyanate is not of conse
quence, although diisocyanate materials are desired, nor~
mally, because of their ready commercial availability.
pansion of the plastisol composition and pertains more
Representative isocyanates which conform to the above
particularly to the addition of an isocyanate to the plastisol 15 structural formula are methyl isocyanate, ethyl isocyanate,
composition to prevent the reaction between the borohy
phenyl isocyanate, m-naphthyl isocyanate, p-nitrophenyl
dride and water from occurring for a time su?lcient to
allow the plastisol composition to be charged into a mold
or deposited upon a conveyor belt before signi?cant ex
isocyanate, 4-diphenylisocyanate, 2,4-toluene diisocyanate,
2,6-toluene diisocyanate, 2,5-m-xylene diisocyanate, 4
chime-1,3 phenylene diisocyanate, 3,3'-dichloro-4,4'-bi~
pansion of the plastisol composition occurs.
phenylene diisocyanate, meta-phenylene diisocyanate,
In the co-pending application of Thomas F. Bush,
para-phenylene diisocyanate, LS-naphthalene diisccya
Serial No. 553,747, ?led December 19, 1955, now aban
nate, disphenylmethane-p'ediisocyanate, 4,4’-bipheny1ene
doned, a process for making a vinyl chloride polymer
diisocyanate, triphenylmethane-p,p’-diisocyanate, 1,4
cellular material from a plastisol utilizing certain metal
tetramethylene diisocyanate, 1,6-hexamethylene diisocya
borohydrides as blowing agents is described. In accord 25 nate, l,l0_decamethylene diisocyanste, 1,4-cyclohexylene
ance with the process, sodium borohydride, potassium
diisocyanate, 1,l-dimethyl-l,2-ethylene diisocyanate, tri
borohydride, rubidium borohydride or cesium borohy
phenylmethane-4,4',4"-triisocyanste, ‘benzene - 1,3,5 - tri
dride is added to the plastisol along with sut?cient water
isocyanate, monochlorobenzene-2,4,6-triisocyanate and
to react with the said borohydride. The hydrogen gas
diphenyl-Z,4,4’-triisocyanate. The isocyanate-modi?ed
evolved as a product of the reaction of the borohydride 30 polyesters having terminal (NCO)~ groups formed by
with the water expands the plastisol. The rate at which
the reaction of a polyester with an excess amount of a
the reaction proceeds can be accelerated by reducing
diisocyanate or triisocyanate, and the isocyanate-modi?ed
the pH of the water present in the plastisol and/or by
polyethers having terminal (NCO)- groups formed by
heating the plastisol. The reduction of the pH of the
the reaction of a polyether with an excess amount of a
water can be effected conveniently by the addition of a 35 diisocyanate or triisocyanate, also are illustrative of
water-soluble acidifying material to the plastisol just prior
to pouring the plastisol into a mold or onto a moving
isocyanates which may be used. For example, the iso
cyanate-modi?ed polyester formed by the reaction of
polytetramethylene adipate (having a molecular weight
conveyor belt. It will be appreciated‘ that expansion of
the plastisol normally will begin as soon as the horn
of about 400) with an excess amount of diphenyl methane
hydride and water (and acidifying material if it is neces 40 p,p'-diisocyanate may be used as the isocyanate which
sary to reduce the pH of the water in the composition)
is added to the plastisol composition to delay the reaction
have been added to the plastisol, and that, as a result,
between the metal borohydride and water.
the plastisol must be shaped almost immediately after
As pointed out in the said Bush application Serial
it is compounded. If the plastisol is poured into molds, 45 No. 553,747, any plastisol may be used in the forma
the mold must be closed before appreciable expansion
tion of the cellular material. As is well understood in
of the plastisol occurs to prevent loss of the plastisol
the art, a plastisol is a dispersion of ?nely-divided vinyl
composition. If a continuous slab of cellular material
chloride polymer in a liquid plasticizer for the vinyl
is to be produced and the plastisol is to be spread onto
‘ chloride polymer. A plastisol normally contains at least
a moving conveyor belt and allowed to expand thereon, 50 35 parts by weight of the liquid plasticizer for every 100
the plastisol must be deposited on the conveyor belt and
parts by weight of vinyl chloride polymer but frequently
spread before expansion of the plastisol occurs, since the
comprises as much as 300 to 400 or more parts by weight
cellular structure of an expanded plastisol has a tendency
of the liquid plasticizer for every 100 parts by weight
to collapse if the plastisol is spread after appreciable
of vinyl chloride polymer. Dioctyl phthalate, butyl decyl
expansion has occurred. In view of these considerations, 55 phthalate, dioctyl adipate, dioctyl sebacate, tricresyl
the ?nal compounding of the plastisol composition here
phosphate, trioctyl phosphate, didecyl phthalate, and
tofore has been deferred until just prior to the time it
acetyl tributyl citrate are liquid plasticizers commonly
is to be used, and has been carried out in a place ad
used in the formation of plastisols. Plastisols may have
jacent to the place where it is to be utilized. Even then,
incorporated therein such additives as colorants, stabiliz
extreme diligence must be exercised by those handling 60 ers, fillers and other modifying agents. The most com
the composition in order that the plastisol is poured into
monly used plastisols contain polyvinyl chloride (a homo
the mold and the molds closed, or onto the conveyor
belt and spread, before appreciable expansion occurs. It
polymer of vinyl chloride) and/or copolymers of vinyl
chloride with vinyl acetate, vinylidene chloride or maleic
can be understood that it would be bene?cial if some
acid esters as the vinyl chloride polymer constituent.
means were available for preventing the reaction in the 65
As was mentioned in the said Bush application Se
plastisol between the metal borohydride and water from
rial No. 553,747, the amount of sodium borohydride,
occurring for a time suf?cient to allow the plastisol com
position to be charged into molds or spread onto a con
veyor belt before appreciable expansion takes place.
potassium borohydride, rubidium borohydride and/or
cesium borohydride used with water, as is blowing agent
for the plastisol will vary depending upon the amount
It now has been found that if any isocyanate is added 70 of the borohydride which must be reacted with water to
to the plastisol composition before the metal borohydride
form an expanded plastisol of the desired density, more
and water have been combined in the composition, or
of the borohydride being required to form a cellular ma
3,084,127
4
Example I-—Conlinued
terial of lower density than is required if a material of
greater density is desired. The borohydride can be added
in powder form directly to the plastisol, or may be dis
Material:
Parts by weight
Toluene diisocyanate ___________________ __
persed in the liquid plasticiser of the plastisol and the
2.0
50% dispersion of phthalic anbydride in di
dispersion added to the plastisol, or may be dissolved in
water and the resultant aqueous solution of the borohy
decyl phthalate ______________________ __
1.0
The vinyl chloride polymer and dioctyl phthalate are
mixed together to form the plastisol. The pH of the
water is adjusted to about 11 with sodium hydroxide and
solution, the pH of the solution must be raised by the 10 the potassium borohydride is dissolved therein. This
aqueous solution of potassium borohydride is added to
addition of an alkaline material to a pH at which the
the plastisol along with the toluene diisocyanate. Finally,
reaction between the borohydride and water does not tend
the acidifying material, phthalie anhydride, is added to the
to occur. Even when the borohydride is to be added to
plastisol. Whereas expansion of the composition would
the plastisol in the form of a dry powder or as a disper
sion of the borohydride in a liquid plasticiser, it is de 15 occur immediately after the lowering of the pH of the
system by the addition of the phthalic anhydride if the
sirable to add su?icient alkali to the plastisol composition,
isocyanate were not added, the presence of the toluene
or to the liquid plasticizer into which the borohydride
diisocyanate delays the expansion from beginning for
has been dispersed, to prevent the borohydride from pre
about 15 minutes. The composition was poured into a
maturely reacting with any water present with which it
20 mold and after the plastisol had attained the desired ex
might accidently come in contact.
pansion the mold was heated to a temperature of about
The water for reacting with the borohydride may be
350° F. to gel and fuse the expanded plastisol. A cellular
added to the plastisol either before or after the boro~
material
having a density of about 12.5 pounds per cubic
hydride blowing agent is mixed into the plastisol or may
foot is formed.
be added simultaneously with the borohydride, either
dride added to the plastisol.
Since borohydrides and
water react together below a certain pH value, if the
borohydride is to be added to the plastisol in an aqueous
Example II
as a separate component or as a aqueous solution of the 25
borohydride as previously described. Alternatively, sepa
rate plastisol components can be formed and the boro
Parts by Weight
Material
hydride can be added to one of the plastisol components
and the water added to the other plastisol component.
The two plastisol compositions then can be mixed together 30
Vinyl chloride polymer __________________________ _.
to form a composite mixture just before they are to be
Oetyl hutyl phthalate __________________________ __
used. Sufficient water should be present in the plastisol
Methylene glycol dibonzoatc ____________________ ._
Cheutoell 3031 _______ _.
for reacting with the borohydride to form an expanded
Phthalic anhydride. _
material of the desired density, but an excess amount
Toluene dilsocyanate ............. ._
of water in the plastisol normally is not desirable.
The isocyanate can be added either directly to the
‘A composition composed of 7.5 parts by weight of water, 1.5 parts by
weight of sodium hydroxide, 1.0 port by weight of boric acid, 5.0 parts
plastisol. or mixed with a liquid plasticizer for the vinyl
by weight of sodium borohydride and 1.5 parts by weight of absolute
chloride polymer of the plastisol and the mixture of iso
cyanate and plasticizer can be added to the plastisol. If
the plastisol is formed into more than one compartment
for compounding (as described above), the isocyanate
methanol.
The A and B component plastisol compositions are
compounded separately in the usual manner and then
equal parts by weight thereof are combined by mixing
can be added to either or both of the plastisol com
them together by means of an air-driven three-bladed
propeller at 1600 r.p.m. for one minute. No foaming
the piastisol composition will vary depending upon the
occurs at this time. The plastisol is poured onto a moving
45
amount of borohydride being used. It is theorized that
conveyor belt and is spread evenly over the face of the
the isocyanate combines in some manner through its
belt. At room temperature, foaming of the plastisol for
(NC-O)~ group with the borohydride to form a com
mulation begins about three minutes after mixing and is
plex. but the mechanism is not understood. Normally,
virtually completed at the end of seven minutes. The ex
the addition of from 0.1 part to 50 parts by weight of 50 panded material is gelled and fused at 345° F. yielding a
isocyanate produces a sufficient delay in the reaction be
cellular slab material of uniform cell structure having a
ponents.
The amount of isocyanate desirable added to
tween the borohydride and water to provide ample time
to charge the plastisol composition into molds onto a
conveyor belt before the expansion, of the plastisol com
position begins.
As indicated above, the rate of reaction between the
borohydride and water in the plastisol can be accelerated
either by heat or by adding an acidifying material to the
density of about seven pounds per cubic foot.
Example III
55
Parts to W'cl ht.
Material
_
g
A
_.
B
plastisol. Any water-soluble acidic material may be used.
Such materials are well known and include inorganic
acids, carboxylic acids (particularly the stronger car 60
boxylic acids such as acetic acid), amino acids and acid
anhydrides. The amount of acidifying material added to
the plnstisoi in order to increase the rate of reaction be
tween the borohydride and water to the desired rate will
vary depending upon the amount of water present in the
plastisol and the drop in pH required.
The following examples are illustrative of the inven
tion, and are not intended to limit nor circumscribe
the scope thereof.
Examplel
Vinyl chloride polymer .......................... _.
Octyl butyl
hthnlate. __
_
Diethylene 2 you! dlbenzo
Chernccll 303 _________ .c
_
100.0
40.0
100. 0
40.0
30. 0
30. 0
4. 5
________ r .
Phthalic ?t'lhytil'ltie_ ___
_._ ________ __
4. 0
Toluene dilsocyanatc ____________________________ __
1.0 ........ __
The component plastisols A and B are compounded
separately and are then admixed in equal proportions as
in Example II. At room temperature the resulting com
position did not begin to exp-and noticeably until about
15 minutes after the plastisol components (A and B) were
70 mixed together. However, an immediate expansion may
Parts by weight
be initiated by heating the composite piastisol mixture.
Vinyl chloride polymer _________________ __ 100.0
Dioctyi phthalate ______________________ __ 75.0
will start to expand immediately if heated to 130° F. and
Material:
Potassium
borohydride _________________ __
0.7
Water _______________________________ __
1.0
For example, a two-inch thick layer of the plastisoi mix
will be fully expanded after about ?ve minutes. Gela
tion and fusion then are accomplished by heating the
3,084,127’
5
6
expanded plastisol at 350° F. A foamed vinyl sheet of
line uniform cell structure having a density of 9.5 pounds
The plastisol mix thus formulated did not begin to ex
pand until about 15 minutes after the plastisol compo
nents were intermingled. The plastisol mix was spread
per cubic foot is obtained.
on a moving conveyor belt and after expansion was fused
Example IV
5 at 350° F. A cellular material 1 inch thick and having
a density of about 10 pounds per cubic foot resulted.
Parts by Weight
Material
*
__.___._
A
B
Example Example
___
X
Polyvinyl chloride polymer ________ __
100.
'llitiiloyl aillpate __________ h
200
ljll‘tilyll‘llc glycol dilicnzoate_.
Amyl iiocyl phthnlate__
(Tlll'lnPPil 30:5 _______ __
l’lithalic tl-tillyllrlt_le_ _ __
100. 0
__.__ _ ___
20.0
40.0
4_ 5
________ '_
_ _ _ _ _ _ _ __
Parts by it eight
Vinyl chloride polymer
4, 0
ninety! nhthahte"
6.5 ________ __
The component plastisol compositions A and B are com
'
’
100 0
100.0
80. 0
80. <1
_
'
phthahte4% aqueous so
‘
of acetic aci
50%ftgislpit1-rsion cesium borohydi
1-0
1- U
2.0
5.0
..---._...
________ ._
4% aqueous 891mm “mm m
_
pl
pounded separately and equal parts thereof are admixed
as in Example II.
,
15 Tolllefw diis?l‘yml?m25% dlspersion 0f rubl
mm Weight, biting about 12.543507,
I
Xi
Material
20 0
20.0
40.0
Mmiiliir Cit-75 (a pnlyisocyanate in ethyl acctat
solution, with the (N'CO)~ content, based upon
.
10
8
a
(l _ _ _ _ _ , _ _ _
w
_ _ _ _ _ _ _ _ , __
1,5
At room temperature, expansion of 20
the plastisol mixture begins about three minutes after the
two plastisol compositions are intermixed and is virtually
In each instance the polyvinyl chloride polymer, dioctyl
phthalate, toluene diisocyanate and alkali metal borohy‘
completed in seven minutes, yielding upon fusion at about
dride dispersion are mixed together in the usual manner
345° F. a vinyl foam of uniform cell structure having a
and the acetic acid solution is added to the resulting plas—
density of about seven pounds per cubic foot.
25 tisol composition. The compositions then are charged
Example V
Example VI
M atcrial
Dir-thyiene glycol dibcnzoate
(‘homcell303 ............ -.
A
B
A
B
A
B
A
100.0
50. 0
100.0
50. 0
100.0
50. 0
100.0
50.0
100.0
50.0
100.0
50.0
1000
50. 0
30. 0
30. 0
30. 0
30.0
30.0
30. 0
40. 0
40. 0
3.0
______ ._
4.0
unhyrlride . . . _ . . . . . .
Example VIII
Parts by Weight
\"iiiyl chloride polymer .................................... ._
Octyl butyl phthalntc _______ ._
i‘hthalic
Example VII
_ . _ . . .
. . . . . . _ .
______ __
4.0
______ ._
4.0
...... -_
4.0
...... __
Pont dz Co.) _____________________________________________________ ._
llylenc
Tat-S0 (a mixture of 80% 2,4-toluer1c dilsocyuriate
and 20% 2,6-toliicne dilsoeyanate, manufactured by Du
4. 5
______________________________________________ ._
Pont 8i C0.) ..................................................................... -.
Aii‘inrmic L (a glycol-based rtriolcouleY chaincxtendod, ter
5.0
______ ._
4.0
100.0
50. 0
_ _ . _ . _ --
llyleno Till-05 (a mixture of 65% 2,4-toluene diisocyanate
and 35% 2,6—tolucne diisocyanate, manufactured by Du
4. 0
B
______ __
______________________________ __
minated with reactive isocyanate groups, manufactured by
i’ont dz (.70.) _________________________________________________________________________________ ._
(Alln
polymeric
material rnsuiting from the reaction or 100.0
parts by weight of polypropylene glycol being a dial of
molecular weight 2025 and having a hydroxyl number 50,
and 40.0 parts by weight oi Hylerie ‘PM-65, and 4.0 parts
20.0
.............. __
by Weight oilicxitne trial) ................................................................................ ._
10.0
______ __
in Examples V, VI, VII and VIII, the plastisol cominto separate molds. The formulations thus formed did
ponents of each example are compounded in the usual
not begin to expand until about 15 minutes after being
manner and equal proportions of each component are 50 mixed. The expanded plastisols are fused at 325° F.
admixed as in Example II. The plastisol mixture did not
and cellular products of ?ne uniform cell structure hav_
begin to expand at room temperature for aboutS minutes
ing a density of about 12 pounds per cubic foot are
after mixing, although expansion thereof could be initiated
obtained.
at any prescribed time by heating the mixture at a temFrom the foregoing examples it becomes readily ap
perature for example between 100-200° F. Gelation 55 parent that the addition of an isocyanate to a plastisol
and fusion of the plastisol material in molds maintained
delays the reaction of the alkali metal borohydride and
at about 360° F. produced in each instance a cellular
water in the plastisol and thereby provides more time
material of ?ne uniform cell size having a density of
for the operator to charge the plastisol into molds or
about 6 pounds per cubic foot.
onto a moving conveyor belt before appreciable expan'
Example IX
60 sion of the plastisol composition has occurred._ '
M
_
It is clear that obvious modi?cations and variations of
this invention may be made without departing from the
Parts by Weight
Mmml
spirit and scope of the invention as de?ned in the ap
A
B
pended claims.
..
65
Vinyl chloride polymer __________________________ ._
I claim:
Vinylclilnriilc-vlnylideno chloride cnpolyiiicn
60. 0
100.0
40.0 ________ __
llt'tt'lltliivllilltlmlillt‘ ........................... -.
80.0
30.0
vinyl chloride polymer plastisol composition containing
1.8 ........ --
vinyl chloride polymer which comprises adding to said
30 ‘)tll'lS b
wi-iuiit smiiiiiii boroiiyilriilc and T0
-
( {tirts by syvc-iulit 5% aqueous solution of sodium
liyilroxitlol ____________________________________ __
-
-
,1‘ A pr‘fcess for making ,a cellular miitenal min? 3'
-
-
~
-
-
_
a'_vmyl chlqnde polymer mid a hqmd.plasnclz.cr for Said
50'? ulhtllmlil" "mln‘llfi'll‘ ‘ii-WNW 1" my‘ WW1
6 D 70 plastisOl composition (1) a chemical blowing agent se
TL‘JIUL'HU (llla‘ilCXllllillL‘ ...................................... --
1.0
iitui
1m‘ ___________ _.
a
.
.
.
.
lected from the group consisting of sodium borohydride,
potassium borohydride, rubidium borohydride and cesium
The materials of each plastisol component are com-
borohydride, (2) water for reacting with the said chemi
pounded together, following which equal parts of the
cal blowing agent to produce hydrogen gas for expand
A and B compositions are admixed in the usual manner. 75 ing the said plastisol composition and (3) an isocyanale
3,084,127
to delay the reaction between the said chemical blowing
agent and the water to allow additional time before said
plastisol composition commences to expand, said iso
cyanate having the structural formula R(NCO)x where
R is an organic radical free of reactive hydrogen and x
is an integer, said chemical blowing agent and water
being intermixed in said plastisol composition in the
presence of said isocyanate, allowing said chemical blow
ing agent and water to react in said plastisol composition
to expand said plastisol composition into a cellular mass,
and heating the expanded plastisol composition to gel
and fuse said expanded plastisol composition.
2. A process for making a cellular material from a
8
composition into a cellular mass, and heating the ex
panded plastisol composition to gel and fuse said ex
panded plastisol composition.
5. A process for making a cellular material from a
vinyl chloride polymer plastisol composition containing a
vinyl chloride polymer and a liquid plasticizer for said
vinyl chloride polymer which comprises adding to said
plastisol composition (1) a chemical blowing agent se
lected from the group consisting of sodium borohydride,
potassium borohydride, rubidium borohydride and cesium
borohydride, (2) water for reacting with the said chemical
blowing agent to produce hydrogen gas for expanding the
said plastisol composition and (3) an isocyanate to delay
the reaction between the said chemical blowing agent and
vinyl chloride polymer and a liquid plasticizer for said 15 the water to allow additional time before said plastisol
composition commences to expand, said isocyanate hav
vinyl chloride polymer which comprises adding to said
ing the structural formula R(NCO)x where R is an or
plastisol composition (1) a chemical blowing agent se
ganic radical free of reactive hydrogen and x is an integer,
lected from the group consisting of sodium borohydride,
said chemical blowing agent and water being intermixed
potassium borohydride, rubidium borohydride and cesium
in said plastisol composition in the presence of said isocya
borohydride, (2) water for reacting with the said chemi
nate, heating said plastisol composition to a temperature
cal blowing agent to produce hydrogen gas for expand
below the temperature at which the said plastisol composi
ing the said plastisol composition and (3) an isocyanate
tion ‘gels to catalyze the reaction between the said chemi
to delay the reaction between the said chemical blow
cal blowing agent and water in said plastisol composition
ing agent and the water to allow additional time before
said plastisol composition commences to expand, said iso 25 to expand the said plastisol composition into a cellular
mass, and heating the expanded plastisol composition to
cyanate having the structural formula R(NCO)x where
gel and fuse said expanded plastisol composition.
R is selected from the group consisting of polyvalent
vinyl chloride polymer plastisol composition containing a
aromatic organic radicals, polyvalent aliphatic organic
6. A process for making a cellular material from a
radicals and polyvalent alicyclic organic radicals and x
vinyl chloride polymer plastisol composition containing a
being intermixed in said plastisol composition in the
vinyl chloride polymer which comprises adding to said
plastisol composition (1) a chemical blowing agent se
is an integer, said chemical blowing agent and water 30 vinyl chloride polymer and a liquid plasticizer for said
presence of said isocyanate, allowing said chemical blow
ing agent and water to react in said plastisol composition
to expand said plastisol composition into a cellular mass,
lected from the group consisting of sodium borohydride,
potassium borohydride, rubidium borohydride and cesium
and heating the expanded plastisol composition to gel 35 borohydride, (2) water for reacting with the said chemi
cal blowing agent to produce hydrogen gas for expand
and fuse said expanded plastisol composition.
3. A process for making a cellular material from a
vinyl chloride polymer plastisol composition containing
a vinyl chloride polymer and a liquid plasticizer for said
vinyl chloride polymer which comprises adding to said
plastisol composition (l) a chemical blowing agent se
lected from the group consisting of sodium borohydride,
potassium borohydride, rubidium borohydride and cesium
ing the said plastisol composition and (3) an isocyanate
to delay the reaction between the said chemical blowing
agent and the water to allow additional time before said
plastisol composition commences to expand, said isocya
nate having the structural formula R(NCO)a where R is
an organic radical free of reactive hydrogen and x is an
integer. said chemical blowing agent and water being
intermixed in said plastisol composition in the presence of
borohydride, (2) water for reacting with the said chemical
blowing agent to produce hydrogen gas for expanding 45 said isocyanate, adding an acidifying material to the said
plastisol composition to catalyze the reaction between the
the said plastisol composition and (3) an isocyanate to
said chemical blowing agent and water in said plastisol
delay the reaction between the said chemical blowing
agent and the water to allow additional time before said
plastisol composition commences to exp-and, said isocya
nate having the structural formula R(NCO)x where R
is a divalent aromatic organic radical and x is the integer
2. said chemical blowing agent and water being intermixed
in said plastisol composition in the presence of said
isocyanate, allowing said chemical blowing agent and
water to react in said plastisol composition to expand said
plastisol composition into a cellular mass, and heating
the expanded plastisol composition to gel and fuse said
composition to expand the said plastisol composition into
a cellular mass, and heating the expanded plastisol com
position to gel and fuse said expanded plastisol composi
tron.
7. A process for making a cellular material from a
vinyl chloride polymer plastisol composition containing
a vinyl chloride polymer and a liquid plasticizer for said
vinyl chloride polymer which comprises adding to said
plastisol composition ( 1) a chemical blowing agent se~
lected from the group consisting of sodium borohydride,
potassium borohydride, rubidium borohydride and cesium
borohydride, (2) water for reacting with the said chemi
vinyl chloride polymer plastisol composition containing 60 cal blowing agent to produce hydrogen gas for expanding
the said plastisol composition, said chemical blowing
a vinyl chloride polymer and a liquid plasticizer for said
agent and water being added to said plastisol composi
vinyl chloride polymer which comprises adding to said
tion as an aqueous solution having a pH sufficiently high
plastisol composition (l) a chemical blowing agent se—
lected front the group consisting of sodium borohydride,
that the said solution is essentially stable, and (3) an
potassium borohydride, rubidium borohydride and cesium
isocyanate to delay the reaction between the said chemi
borohydride, (2) water for reacting with the said chemi
cal blowing agent and water when catalyzed to allow
cal blowing agent to produce hydrogen gas for expand
additional time before said plastisol composition com
ing the said plastisol composition and (3) toluene-2,4
mences to expand, said isocyanate having the structural
expanded plastisol composition.
4. A process for making a cellular material from a
diisocyanatc to delay the reaction between the said chemi
cal blowing agent and the water to allow additional time
before said plastisol composition commences to expand,
said chemical blowing agent and water being intermixed
in said plastisol composition in the presence of said isocy
anatct allowing said chemical blowing agent and water to
react in said plastisol composition to expand said plastisol
formula R(NCO)x where R is an organic radical free
of reactive hydrogen and x is an integer, adding an
acidifying material to the said plastisol composition to
catalyze the reaction between the said chemical blowing
agent and water in said plastisol composition to expand
the said plastisol composition into a cellular mass, and
3,084,127
heating the expanded plastisol composition to gel and
fuse said expanded plastisol composition.
8. A process for making a cellular material from a
vinyl chloride polymer plastisol composition containing
a vinyl chloride polymer and a liquid plasticizcr for said
vinyl chloride polymer which comprises adding a chemi
cal blowing agent selected from the class consisting of
10
blowing agent selected from the group consisting of 50.
dium borohydride, potassium borohydride, rubidium boro
hydride and cesium borohydride, (2) water for reacting
with the said chemical blowing agent to produce hydrogen
gas, said chemical blowing agent and water being added
to said plastisol composition as an aqueous solution hav
ing a pH su?’iciently high that the said solution is essen
tially stable, and (3) an isocyanate to delay the reaction
between the said chemical blowing agent and water when
polymer plastisol composition, adding (1) water for 10 catalyzed to allow additional time before expansion com
reacting with the said chemical blowing agent to produce
mences, said isocyanate having the structural formula
hydrogen gas and (2) an isocyanate having the structural
R(NCO),, where R is an organic radical free of reactive
formula R(NCO), where R is an organic radical free
hydrogen and x is an integer, adding an acidifying mate~
of reactive hydrogen and x is an integer to a second
rial to a second vinyl chloride polymer plastisol compo
vinyl chloride polymer plastisol composition, admixing 15 sition, admixing the two plastisol compositions together
the two plastisol compositions together to produce a
to produce a plastisol blend, allowing said plastisol blend
plastisol blend, said isocyanate delaying the reaction be
to expand into a cellular mass, and heating the expanded
tween the said chemical blowing agent and water when
plastisol composition to gel and fuse the expanded mass.
admixed to allow additional time before said plastisol
blend commences to expand, allowing said plastisol blend 20
References Cited in the ?le of this patent
to expand into a cellular mass, and heating the expanded
UNITED STATES PATENTS
plastisol composition to gel and fuse the expanded mass.
sodium borohydride, potassium borohydride, rubidium
borohydride and cesium borohydride to a vinyl chloride
9. A process for making a cellular material from a
vinyl chloride polymer plastisol composition containing
a vinyl chloride polymer and a liquid plasticizcr for said 25
vinyl chloride polymer which comprises adding to a vinyl
chloride polymer plastisol composition (1) a chemical
2,909,493
2,915,496
Bush ________________ __ Oct. 20, 1959
Swort et al. _________ __ Dec. 1, 1959
785,256
805,167
Great Britain __________ _- Oct. 23, 1957
Great Britain __________ __ Dec. 3, l958
FOREIGN PATENTS
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