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Патент USA US2407107

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Patented Sept. 3, (1946
2,407,107
UNITED STATES PATENT’ OFFICE
-‘ PREPARATION oF STABLE DISPERSIONS 0F ‘
'
‘ ‘
ALKYL ALKACRYLATE POLYMERS
Joseph Edward Smith, Wilmington, DeL, assignorv
to E. I. du Pont de Nemours & Company, Wil
mington, Del., a corporation o'f‘Delaware
‘
No Drawing. Application May 5, 1943,
,
,
_Serial,No.485,757
‘
,12 Claims.v (Cl. 260—32)
5 productionit is difficult to obtain the required
‘ This invention relates to a- process for‘prepar
ing stable aqueous dispersions oi-alkyl alkacry
late polymers;
'
--
.
.
.
uniformity and'?‘n'eness of particle size in simple
equipment and within ' a reasonable length ‘of
j
‘In U. S. Patent 2,318,429 (issued ‘May 4, 1943)
time} Ordinarilythe‘emulsions are prepared by
and U. S. Patents 2,343,089 and 2,343,090 (issued
theu‘se ‘of high speed agitators, homogenizers, or
by'theuse of both, so that the alkyl alkacrylate
February 29,. 1944),‘ there has been described a
process for preparing highly stable-dispersions
of alkyl alk'acrylate polymers‘ particularly suit
monomer is dispersed in the aqueous phase in as
high a state ‘of ‘sub-‘division of the liquid particles
able for the treatment of textile ?bers, wherein
as possible. Inv the large scale commercial pro
the ‘preferred emulsifying and dispersing agent 10 duction, the particle size of the product has been
is a w‘ater‘soluble partially-saponi?ed polyvinyl
found to vary widely from batch to batch, with
acetate, or, what may be termed in other-Words,
sedimentation occurring in those batches that
awate'r soluble derivative of polyvinylal'cohol
have not been properly emulsi?ed. It has been
containing free hydroxyl groups." In U. S. Patent
found‘ that the average maximum particle size
permissible in the preparation of these highly
2,318,429, it is pointed out that vthe partially
saponi?ed polyvinyl acetate used in the prepara
_ stable allryl alkacrylate aqueous dispersions is
tion of stable dispersions of the alkyl alkacry
from'2 to 5 microns; and that the presence of a
lates ispreferably of the‘ type having a saponi
comparatively large number of particles with a;
?cation- number in the range of from 40 to 130,
diameter greater than 10_-microns is apt to prof
and a viscosity in a 4% aqueous solution at 20° C;
duce sedimentation as a result of the‘agglomera
of from 20 to 25 C; P. In U. S. Patents 2,343,089
tion, of these larger particles.‘ ‘It has‘ also been
found that the presence of a comparatively large
and 2,343,090,~a method is disclosed for preparing
textile treating compositions‘comprising an alkyl
number of particles of greater diameter than 10
alkacrylate ‘or other vinyl- compound, ‘held in
microns frequently leads to difliculties in the ap
stable dispersion by the water- solublei'partially
plication of the dispersions to textiles by either
saponi?ed polyvinyl acetate, which have'a‘sub
the padding operation ‘or by the process of ex
stantive a?inity for'?bers and which can be ap
haustion from dilute baths, for such dispersions
tend to break and deposit unevenly on the goods,
plied thereto by a processor exhaustion from
resulting in spotty effects. I
I
‘
dilute treating baths. In Us. application Serial
No.,4'71,577, a process is disclosed whereby the 30 While these difficulties can be overcome by the
? exercise of due care in the preparation of the
partially saponi?ed polyvinyl acetate may be pro
duced in a uniformly high degree of purity, par
emulsion to , assure complete and satisfactory
ticularly suitable for the preparation of stable
aqueous dispersions of' the alkyl alkacrylate
polymers.
.
W
.
'
.
.l
‘
.
It is generally recognized that, in the prepara
emulsi?cation ‘of the monomer prior to poly
merization, it requires a prolonged period‘of time
35 i'n‘the milling operations so that the output, from
‘ any particular homogenizing mill is limited.
‘ It is therefore an object of this invention to
tion of stable?uid aqueous emulsions and dis
persions, ‘the ‘average. particle. size of.‘ the . dis
persed phase should be below 3 to 5 microns. The
average pamue size in technical dispersions 40
which are offeredior use in the textile trade is ' :'
provide a process for preparing stable aqueous
dispersions of alkyl alkacrylate‘polymers by the
emulsion polymerization process, ‘wherein the al
kyl alkacrylate monomer is emulsi?ed in an aque
usually in the range of from. 0.1v to 5'microns.
ous solution in a much‘ shorter time than has
Experience shows that a dispersion which has
heretofore been required, and with a greater de
satisfactory stability to long storage has an
gree of uniformity ‘when the emulsi?cation is
average particlesize no greater than. 2 to 5 45 carried out inlarge scale commercial production.
microns.v It is of course understoodthat the great
majority of particles will fall within the range
L It is ‘a further object of the invention to provide
a. proeessior emulsifying alkyl alkacrylate mon
given for the average particle size, although there
omers in aqueous solution with a water soluble
may bea- relatively small percentage. of - larger
partially saponi?ed polyvinyl acetate as the
.50 emulsifying agent, and in the presence of a small
particles.
,
V
-
While in small scale operation, such as in
> amount of a petroleum hydrocarbon such as min
laboratory apparatus or small scale semi-works
eral oil and waxes, and‘in the presence of ‘a poly
equipment, the necessary particle size and uni
merization catalyst such as benzoyl peroxide or
formity of the emulsi?ed ‘ alkyl alkacrylate
other commonly employed catalyst. A further
monomer in the aqueous media can be obtained 55 object of the invention is to produce stable aque
with simple equipment and in a relatively short ' ous‘ dispersions of alkyl‘ alkacrylate polymers hav
time so that on polymerization of the alkyl
ing an average particle size of not more than 5
alkacrylate monomer in the emulsion the polymer
microns,‘ which ‘contain a partially saponi?ed
is obtained in the necessary degree of ?neness so
that it remains as a stable aqueous dispersion,
polyvinyl acetate as the dispersing agent and a
it has been ‘found that in large scale commercial '
refined petroleum hydrocarbon as a stabilizer.
I have found that new and stable'aqueous dis
2,407,107
3
4
persions of alkyl alkacrylate polymers can be
A similar preparation was carried out,‘ using
prepared by emulsifying the alkyl alkacrylate
1.25 parts of crude scale wax having a melting
point of about 50° C. as an addition to the 25
monomer in an aqueous solution of a partially
parts of n-butyl methacrylate. The particle size
saponi?ed polyvinyl acetate in the presence of
from 0.25% to 10% (based on the Weight of the UK range of the two emulsions at corresponding
stages of the operation was as follows:
alkyl alkacrylate) of a re?ned petroleum. hydro
carbon having a boiling point above approxi
Particle size in microns of
mately 110° C., and carrying out the polymeriza
emulsion containing
tion of the emulsi?ed monomer under the condi-
tions normally employed in the emulsion poly
10
Stage of'operation
No crude
Crude scale
scale wax
wax
merization processes of the prior art. The emul
si?cation may be carried out in the presence of
additional dispersing agents of the types more
30‘ minutes mixing with “Lightnin"
particularly disclosed in. my co-pending appli
agitator ___________________________ ._
2-60
One pass through homogenizing pump_
2-30
l-2
l~30
l-2
cations above-mentioned, and in the presence of 15 Two passes through homogenizing
ump ____________________________ -_
cationic surface active agents or‘ of water soluble
T ree passes through homogenizing
metal salts of polyvalent metals such’ as alumi
pump _____________________________ ._
Four. passes through homogenizing
num, barium, zinc, etc., which are used to im
pump _____________________________ __
part substantive aii‘inity for textile ?bers to the.
Polymerized dispersion__--___ ___ ___ ___
-
3-4
l~20
l-2
l-20
l-2
2~l4
1-2
resulting dispersed polymer. The petroleum. hy 20
drocarbon is preferably employed in an amount
equal to from 0.5% to 5%, based on the weight
of the alkyl alkacrylate monomer. The amount
of polyvinyl alcohol (water soluble partially sa
The product containing the crude scale. wax
has a much smaller and more uniform particle
size than the product that. does not contain the
poni?ed polyvinyl ester) that should be employed
wax, and it is easier to manufacture, requiring
less time and. energy. The polymerized disper
to maintain a stable aqueous dispersion of the
sion containing wax was stable without sedimen
alkyl alkacrylate: polymers should be above 6%‘,
tation on storage for a number of months, while
the sample without wax sedimented badly within
based on the weight of the polymer. ‘The top
limit is determined only by the viscosity desired
a week's time.
In the following examples, the agitation and
for the resulting. aqueous suspension. Where too 30
homogenization employed has been adopted on
large an amount is employed, the suspension
the basis of experience as being reasonably equiv
will become too viscous to permit proper control.
during the polymerization process. Highly sta
alent to the larger scale agitation. and homoge
ble dispersions containing from 10% to 40% of
nization described in Example I. The technique
the alkyl alkacrylate, based on the total weight
used in the following examples is not intended
of the aqueous dispersion, may be prepared by
to represent the maximum e?'iciency which can
be obtained in a small scale operation, but has
been adopted to demonstrate the effectiveness of
the petroleum hydrocarbons as emulsifying as
in the emulsi?cation process as an emulsi?cation
assistant to decrease the time and energy re 40 sistants.
this process.
While the petroleum hydrocarbon is employed
quired in preparing the emulsion, the resulting
dispersion after polymerization also is a highly
Example II
Twenty-?ve parts of n-butylmethacrylate mon
stable dispersion and has a high degree of sta
omer, containing 0.25 part of benzoyl peroxide
bility which makes it possible to store the‘ prod
uct in warehouses for long periods of time for 45 and various amounts of a re?ned white mineral
oil with a viscosity of about 40 S. U. V.1oo from
commercial distribution, and it is therefore. con
sidered to act as a suspension stabilizer.
Generally, experience has indicated, wherever
a Pennsylvania crude as indicated in the table,
were mixed in each case, with 2.5 parts of par
tially saponi?ed polyvinyl acetate in water to
comparison can be made, that, where less energy
make a total of 100 parts. The partially saponi
is required to form an emulsion, such emulsion
fied polyvinyl acetate had a saponi?cation num
or resulting dispersion has higher stability than
ber of 110 and produced a viscosity of about 20
where more energy is required to effect reduction
C.
P. in a 4% aqueous solution at 20° C. The
to the same particle. size.
monomer solution was added to the aqueous solu
The following examples are given to illustrate
tion at- 25° C., while mixing with a Hamilton
the invention. The parts used are by weight.
55 Beach soda mixer, and agitation continued for
Example‘ I
3 minutes. The emulsion obtained was homo
genized by four passes through a Travis disper
Twenty-?ve parts of n-butyl methacrylate
»mill with the valve on the drain left open. The
monomer containing 0.25 part of benzoyl perox
ide were mixed with '15 parts of an aqueous solu 60 emulsion was aged (polymerized) for 16 hours
at I70” C. to obtain a polymer dispersion. The
tion containing 2.5 parts of partially saponi?ed
particle size of the dispersed particles after poly
polyvinyl acetate and 0.25 part of stearyl tri
merization was determined microscopically, and
methyl ammonium bromide at 25° to 30°C. The
found to be as given in the following table:
partially saponi?ed. polyvinyl acetate employed
had a viscosity in a 4% aqueous solution of 20
C. P. at 20° C. and had a saponi?cation. number
of about 110. The mixture was agitated, for 30
Average
Number
n-Butyl
40 S. U. V400 particle size
methacrylate white min- aged disper
minutes with two propeller type agitators, known
to the trade as “Lightnin” agitators, to obtain a
monomer
coarse emulsion. The emulsion was homogenized
Percent
by four passes through a disc type homogenizing
pump, known to the trade as a Wesco pump, and
then heated without agitation for 16 h'ours at
7 0° C. The monomer was completely polymerized
at the end of this period.
75
eral oil
sion in mi
crons
Percent
25
25
25
25
25
25
____________ __
4. 0-10
0. 06
0. 13
0. 5-8
0. 5—4
0. l9
0. 6
3. 3
0. 5-4
2. 0—3
(1.5-4
2,407,107
a?inic and cycloaliphatic hydrocarbons; the-pet
rolatum is composed largely of cycloalip'hatic
‘ These data show that as little as 0.06% ‘of the
white mineral oil in the composition or 0.25% on
the‘weight of the n-butylmethacrylate monomer
hydrocarbons.
These data show that a wide
acts to improve appreciably the particle size
variety of petroleum hydrocarbons act in essen
reduction while the ‘use of 0.5% of the. white min 5 tially the same manner in markedly improving
eral oil on the weight of the monomer has a
marked effect in improving the efficiency of par
ticle size reduction where partially saponi?ed
polyvinyl acetate is used as the dispersing agent.
10
Example III
Example II was repeated. using ineach‘run'
a mixture of 0.25 part of stearyl trimethyl-am¢
the ease of particle size reduction when emulsi
fying n-butyl methacrylate monomer with a par
tially saponi?ed polyvinyl acetate and a repre
sentative cationic surface active agent as dispers
ing and emulsifying agents.
Example V
Twenty-?ve parts of n-butyl methacrylate mon
monium bromide and 2.5 parts of the partially ‘
saponi?ed polyvinyl acetate as emulsifying and
omer containing either 0.6 part of a 40 S. U. V400
dispersing agents. > The results obtained are sum
marized in the following table:
.
about 100 S. U. V400 were emulsi?ed as in Exam
‘
Number
white mineral oil or a blended mineral oil of
ple‘ II with an aqueous solution containing 2.5
parts of the partially saponi?ed polyvinyl acetate,
and in addition, 1.1 parts of basic aluminum
n-Butyl
40 S. U. V.m Average par
- niethacrylate white mineral ticle size in
monomer
oil
microns
20 formate. The emulsions‘were aged and examined
as in Example II.
follows:
Percent
_
Percent.
25
_
____________ __
25
25
25
25
25
3
The data obtained were as
'
a
-
'
>
‘
g
1. (H0
0. 06
0.13
0.19
0. 25
1. 25
0. 5- 2
0.5- 1
0.5- 1
1- 0- 2
1. 0- .2.
25
"n-Butyl
No.
White
methacrylate mineral
monomer
oil
. Per cent
This table shows that as little as ‘0.25% of the
white mineral oil' on the weight of the n-butyl
methacrylate produces a noticeable improvement,
while the use of 0.5% White mineral oil on the
weight of the n-butyl methacrylate produces a
Per cent
Blended Alumis
Particle
mineral
oil A
nnm
fonnate
size in
microns
Per cent
Per cent
__________________ __
25
25
,
.
0.6
________ __
........ __
0.6
1.1
1.1
1.1
4-10
~
2-3
2-3
The data show that the mineral oils produce a
marked
improvement in the particle size reduc-‘
marked improvement in the efficiency of particle
size reduction where. partially saponi?ed polyvinyl .35 tion of n-butyl methacrylate when partially sa
poni?ed polyvinyl acetate is used as the dispersing
acetate, together wi-tha representative cationic
agent in the presence of an aluminum salt, suc
agent, are used as. dispersing and emulsifying
agents.
'
'
'
as aluminum formate.
-
‘
Example IV
Experiments were run as in samples 11 and 12 ‘
of Example III, using in each run a mixture of
1“)
Example VI
> Twenty-?ve ‘parts of >isobutyl methacrylate
monomer containing 0.25 part of benzoyl peroxide
0.25 part of stearyl trimethyl ammonium bromide
and 2.5 parts of the partially saponi?ed polyvinyl
acetate as the emulsifying and dispersing agents,
alone or with 0.6 part of a blended mineral oil
of about 100 S. U. V400, as indicated in the fol
lowing table, were, emulsi?ed by mixing with an
aqueous solution containing 2.5 parts of the par
tially saponi?ed polyvinyl acetate, as employed
in the above examples, and additions of basic
and substituting two different blended mineral
oils with a viscosity of about 100 S. U. V400, petro
latum, and crude scale wax (M. P. 50°. C.) for the
40 S. U. V400 white mineral oil. The data obtained .
aluminumformate and stearyl trimethyl am
are summarized in the following table:
monium bromide, as indicated in the attached
‘
‘
r
n-Butyl
methac-
No.
rylate
monomer ,
Per cent
'
‘ 25
-
Whit
-
‘
.
e
mmieiral
-
011 A1
Crude
‘
0113 ’
Petrola-
tum.
o
Per cent
1
Average I
‘
: svelaage
I
Per cent
Per cent
'
Per cent
particle
Size in‘ ‘
microns
Per cent
‘
1. (H0
25
25
1. 0-2
1.0-2
25
25
1. 0-1.‘5 .
1. 0—2
25
25
25
25
0. 2—0. 8
0. 2-0. 8
0. 2-0. 8
0. 5-1. 0.
25 _
25
1. 0-2. 0
0. 5-1. 0
‘
l Blended mineral oil A was obtained from the Atlantic‘Re?ning 00. nnder the
code 1225 mineral 011.
l Blended mineral oil B was obtained from the Atlantic Re?ning 0'». under the
code 1268 textile oil.
The 40 S. U. V400 white mineral oil and crude
para?ln wax are preponderantly para?lnic hydro
table, to‘ make‘ a total‘ ‘pr 100‘ parts, including an
ingredients. ‘The emulsi?cation and polymeriza
carbons; the blended oils are mixtures of par 75 tion to obtain dispersions ‘of the polymer were
anon-107
7
8
carried? out as in Example II. The results were
alkacrylate-monomer and from 0.25% to 10.0%,
based on the weight of the alkacrylate, of a re
as follows:
?ned petroleum hydrocarbon boiling about 110°
Isobutyl
No.
Blended
gtearyl
monomer
_
Per cent
25
25
25
25
25
25
011 A
Per cent
formate - microns
Per cent
Per cent
._r..___-_____.___._ ___.
______________________ _ _
0. 6
____________ __
________ _ _
0. 25
0. 6
polyvinyl acetate having a saponi?cation number
size in
bromide
________________________________ _-
0.6
C. in an aqueous solution of a partially saponi?ed
Basic 21- Particle
“gags: ‘ mineral atgllglggtilglln uminum
of from 40 to 130 and a viscosity in a 4% aqueous
solution at 20° C. of from 20 to 25 C‘. P., and e?ect~
ing polymerization of the monomer, the partially
4. 0-8
saponi?ed polyvinyl acetate being present in an
2.0-3
10 amount equal to at least 6% of the weight of the
l. 1
4. 0-8
l. l
2.0-3
________ _ _
2. 0-3
0. 25 ________ ._
0. 5-1
dispersed alkacrylate.
2. A process for‘ preparing stable aqueous dis
persions of polymerized alkyl alkacrylates con
taining from 10% to 40% of the dispersed alkac
These comparisons show that the dispersions
containing the relatively small amount of min
eralvoil all had a markedly smaller particle. size
than the corresponding dispersions without min
eral oil;
‘
rylate, which comprises emulsifying the alkyl
alkacrylate monomer and from- 0.25 % to 10.0%,
based on the weight of the alkacrylate, of a 40
S. U. V.1oo white mineral oil in an aqueous solu
tion of a partially saponi?ed polyvinyl acetate
20 having a saponi?cation number of from 40 to 130
Example VII
and‘ a viscosity in a 4% aqueous solution at 20° C.
Methyl methacrylate monomer was substituted
for the isobutyl methacrylate monomer and the
40 S. U. V400 white mineral oil from a Pennsyl
vania crude for the blended mineral oil in Exam
ple VI. The data obtained are summarized in the
of from 20 to 25 C. P., and effecting polymeriza
tion, the partially saponi?ed polyvinyl acetate be
ing present in an amount equal to at least 6% of
the weight of the dispersed alkacrylate.
3. A process for preparing stable aqueous dis
following. table:
persions of polymerized n-butyl methacrylate
Methyl
N0‘
.
Stearyl tri-
Basic
methyl am-
alumi
oil
monium
bromide
num
formate
Per cent
Per cent
Per cent
methacryl- 31111:;
ate monomer
' Percent
25'
containing from 10% to 40% of the dispersed n
-
microns
butyl methacrylate. which comprises emulsifying
30 the n-butyl methacrylate monomer and from
0.25% to 10.0%, based on the weight of the meth
acrylate, of a re?ned petroleum hydrocarbon boil
ing above 110° C. in an aqueous solution of a par
4.0-8
1.0-2
3.0-4
1.0-2
tially saponi?ed polyvinyl acetate having a sa
poni?cation number of from 40 to 130 and a vis
cosity in a 4% aqueous solution at 20° C. of from
1.0-2
0. 2—0.4
1.0-3
0.1-0.4
20 to 25 C. P., and effecting polymerization, the
partially saponi?ed polyvinyl acetate being pres
ent in an amount equal to at least 6% of the
weight of the dispersed n-butyl methacrylate.
The data clearly show that the dispersions con
4. A process for preparing stable aqueous dis
taining the relatively small amount of 40 S. U.
V400 white mineral oil all had ‘markedly smaller
particle sizes than did the corresponding dis
persions without the mineral oil.
It is of course torbe understood that other types
of petroleum oils and petroleum hydrocarbon
persions of polymerizedv n-butyl methacrylate
containing from 10% to 40% of the dispersed n
butyl methacrylate, which comprises emulsifying
the n-butyl methacrylate monomer and from
0.25% to 10%, based on the weight of the meth
acrylate, of a 40 S. U. V.1oo white mineral oil in
an aqueous solution of a partially saponi?ed poly
vinyl‘ acetate having a saponi?cation number of
from 40 to 130 and a viscosity in a 4% aqueous
solution at 20° C. of from 20 to 25 C. P., and effect
waxes, either of the para?inic or cycloaliphatic
types or mixtures of the same, may be substituted
for those speci?cally disclosed in the above ex
amples. As above pointed out, those re?ned pe- '
troleum hydrocarbons having a boiling point
above 110° C. are preferred.
ing polymerization, the partially saponi?ed poly
'
vinyl acetate being present in an amount equal to
at least 6% of the weight of the dispersed n
The invention also contemplates the prepara
tion of stable emulsions and dispersions of alkyl
alkacrylate interpolymers and copolymers. Plas- -
ticizers and other resins may be dissolved in the
monomers before polymerization to give modi?ed
polymers, as more particularly described in U. S.
P. 2,318,429 and 2,343,089 to 2,343,093, inclusive.
While the preferred dispersing and emulsifying
agents are water soluble partially saponi?ed poly
vinyl acetates having a saponi?cation number in
the range of from 40 to 130, and having a viscosity
in a 4% aqueous solution of from about 20 to 25
C. P. at 20° C., it will of course be obvious that
other water soluble derivatives of polyvinyl alco
hol, containing hydroxyl groups such as may be
produced by partially saponifying other polyvinyl
esters, may be substituted for those speci?cally
described in the above examples.
I claim:
1. A process for preparing stable aqueous dis
persions of polymerized alkyl alkacrylates con
taining from 10% to 40% 0f the dispersed alkac
rylate, which comprises emulsifying the alkyl
.
butyl-methacrylate.
'
5. A process for preparing stable aqueous dis
persions of polymerized alkyl methacrylates con_
taining from 10% to 40% of the dispersed alkyl
methacrylate, which comprises emulsifying the
alkyl methacrylate monomer and from 0.25% to
10.0%, based on the weight of the alkacrylate, of
a re?ned petroleum hydrocarbon boiling above
110° C. in an aqueous solution of a partially sa
poni?ed polyvinyl acetate having a saponi?cation
number of from 40 to 130 and a viscosity in a 4%
aqueous solution at 20° C. of from 20 to 25 C. P.,
and e?ecting polymerization, the partially sa
poni?ed polyvinyl acetate being present in an
amount equal to at least 6% of the weight of the
dispersed alkyl methacrylate.
6. A stable aqueous dispersion of a polymerized
alkyl alkacrylate containing from 10% to 40% of
the dispersed alkacrylate which has been pro
duced by the emulsion polymerization of the alkyl
alkacrylate monomer dispersed in an aqueous so
9,407,107
lution of a water soluble partially saponi?ed poly- '
10
partially saponi?ed polyvinyl acetate being pres
vinyl acetate having a saponi?cation number of
ent in an amount equal to at least 6% of the
from 40 to 130 and a viscosity in a 4% aqueous
solution at 20° C. of from 20 to 25 C. P. and in
the presence of from 0.25% to 10.0%, based on the
weight of the dispersed alkyl methacrylate.
weight of the alkacrylate, of a re?ned petroleum
hydrocarbon boiling above 110° C., the partially
saponi?ed polyvinyl acetate being present in an
10. A stable aqueous dispersion of a polymerized
n-butyl-methacrylate containing from 10% to
40% of the dispersed n-butyl methacrylate which
has been produced by the emulsion polymerization
of the n-butyl methacrylate monomer dispersed in
amount equal to at least 6% of the weight of the
an aqueous solution of a water soluble partially
10 saponi?ed polyvinyl acetate having a saponi?ca
7. A stable aqueous dispersion of a polymerized
tion number of from 40 to 130 and a viscosity in a
dispersed alkacrylate.
Valkyl alkacrylate containing from 10% to 40% of
the dispersed alkacrylate which has been pro
duced by the emulsion polymerization of the alkyl
4% aqueous solution at 20° C. of from 20 to 25
C. P., and in the presence of from 0.25% to 10.0%,
based on the weight of the methacrylate, of a
alkacrylate monomer dispersed in an aqueous so‘ 15 re?ned petroleum hydrocarbon boiling above 110°
lution of a water soluble partially saponi?ed poly
(3., the partially saponi?ed polyvinyl acetate being
vinyl acetate having a saponi?cation number of
present in an amount equal to at least 6% of the
from 40 to 130 and a viscosity in a ‘4% aqueous
weight of the dispersed n-butyl methacrylate.
solution at 20° C. of from 20 to 25 C. P. and in
11. A stable aqueous dispersion of a polymerized
the presence of from 0.25% to 10.0%, based on the 20 methyl methacrylate containing from 10% to 40%
weight of the alkacrylate, of a 40 S. U. V.1o0 white
of the dispersed methyl methacrylate which has
mineral oil, the partially saponi?ed polyvinyl ace
been produced by the emulsion polymerization of
tate being present in an amount equal to at least
the methyl methacrylate monomer dispersed in an
6% of the weight of the dispersed alkacrylate.
aqueous solution of a water soluble partially sa~~
8. A stable aqueous dispersion of a polymerized 25 poni?ed polyvinyl acetate having a saponi?cation
n-butyl-methacrylate containing from 10% to
number of from 40 to 130 and a viscosity in a 4%
40% of the dispersed n-butyl methacrylate which
aqueous solution at 20° C. of from 20 to 25 C. P.,
has been produced by the emulsion polymerization
and in the presence of from 0.25% to 10.0%, based
of the n-butyl methacrylate monomer dispersed
on the weight of the methacrylate, of a re?ned
in an aqueous solution of a water‘soluble partially 30 petroleum hydrocarbon boiling above 110° 0., the
saponi?ed polyvinyl acetate having a saponi?ca
partially saponi?ed polyvinyl acetate being pres
tion number of from 40 to 130 and a viscosity in a
4% aqueous solution at 20° C. of from 20 to 25
ent in an amount equal to at least 6% of the
weight of the dispersed methylmethacrylate.
C. P. and in the presence of from 0.25% to 10.0%,
12. A stable aqueous dispersion of a polymerized
based on the weight of the methacrylate, of a 40 35 isobutyl methacrylate containing from 10% to
S. U. V400 white mineral oil, the partially sa
40% of the dispersed isobutylmethacrylate which
poni?ed polyvinyl acetate being present in an
amount equal to at least 6% of the weight of the
dispersed n-butyl methacrylate.
9. A stable aqueous dispersion of a polymerized
alkyl methacrylate containing from.10% to 40%
of the dispersed alkyl methacrylate which has
been produced by the emulsion polymerization of
has been produced by the emulsion polymeriza
tion of the isobutyl methacrylate monomer dis
persed in an aqueous solution of a water soluble
partially saponi?ed polyvinyl acetate having a sa
poni?cation number of from 40 to 130 and a vis
cosity in a 4% aqueous solution at 20° C. of from
20 to 25 C. P., and in the presence of from 0.25
the alkyl methacrylate monomer dispersed in an
to 10.0%, based on the weight of the methacrylate,
aqueous solution of a water soluble partially sa 45 of a re?ned petroleum hydrocarbon boiling above
poni?ed polyvinyl acetate having a saponi?cation
number of from 40 to 130 and a viscosity in a 4%
aqueous solution at 20° C. of from 20 to 25 C. P.,
110° C., the partially saponi?ed polyvinyl acetate
being present in an amount equal to at least 6%
of the weight or the dispersed isobutylmethacry
and in the presence of from 0.25% to 10.0%, based
on the weight of the alkacrylate, of a de?ned pe 50 late.
JOSEPH EDWARD SMITH.
troleum hydrocarbon boiling above 110° C., the
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