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Патент USA US2051409

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'P;maa-m._1a 1936
‘ 2.051.409
UNITED ‘STATES
PATENT OFFICE .
3.0.51.4”
DION 0F NONSAPONM
AND PROCESS OF HAKING SAII
John A.Kenney,Plainileld.N.J.,a-lgnorto'!ho
Barrett-Company, New York, N. ‘2., a corpora
v
.us_,e,.
tion of New Jersey
No Drawing. Application January M, 193‘.
"
Serial No. 107.527
3 Olaims. (UL IN)
My invention relates to dispersed systems oi‘ typical formulae and the methods of pr
for producing dispersions of resins.
'
resinous materials and particularly to disper
sions, such as emulsions or suspensions of resins
of the coumarone-indene type..
g
V
Dispersions of saponi?able resins, such as
rosin, have been used heretofore in the form of
rosin size or rosin soaps, for the sizing of paper
and in the formation of paper board and simi
lar products. Resins such as paracoumarone,
1o para-indene, and similar resins derived from
coal tar distillates are cheap and form excel
lent sizing materials and binding agents but
such resins are not saponi?able. When it is de
sired to use resins of this type for sizing or
15 waterproo?ng materials, the resins have here
tofore been dissolved in an organic solvent
which is subsequently volatilized. The latter
process has the objection that solvents employed
for dissolving resins of the coumarone-indene
type are expensive and many are in?ammable.
Furthermore, their use usually requires the in
ure
In accordance with my invention, the resin is
dispersed to form an emulsion or suspension that
is relatively stable or which separates only very 5
slowly. The nature of the dispersion produced
is largely dependent upon the manner in which
the resin is treated. It seems probable that in
some instances, the resin is emulsi?ed, whereas
in other instances, the resin is probably sus- ‘10
pended in the form of minute solid particles.
I have found that dispersions of resins of the
coumarone-indene type can be produced by
melting the resin and distributing the molten
resin throughout a water solution of a dispers- 15
ing agent by grinding, stirring or whipping the
mixture of materials or by similar mechanical
treatment, as, for example, in a colloid mill, the
temperature of the solution being maintained
below its boiling point in the case where the
resin has a melting point below the boiling point
stallation of relatively costly solvent-recovery
of the solution.
apparatus.
desired, 1. e., one which it is desired to store for
I have discovered that unsaponiflable resins,
a and particularly resins of the coumarone-indene
type, can be dispersed or emulsi?ed directly in a
form satisfactory for use in a variety of ways,
and that such dispersions can be produced with
out employing large amounts of expensive and
3° in?ammable solvents for the resins.
Products obtained by the practice of my in
vention can be added to paper pulp or ?ber stock
If a more stable emulsion is
a considerable period of time upon formation, 7
a limited amount of saponi?able material may 25
be added to the dispersion to stabilize the same,
such material being added to either thedispers
ing agent or to the resin before mixing these
materials, or the saponi?able materialgmay be
added to the resin and dispersing agent during 30'
the agitation thereof.
My invention, as herein described, is applica
in a beater as sizing or binding agents for the' ble to the treatment of a wide range of resins of
?bers, or the dispersions may be used in treat
35 ing or impregnating ?ber board,‘ leather and
similar material, and for numerous other pur
poses. When the dispersions are used in treat
ing paper, ?brous pulp or the like, the products
obtained have increased resistance to the action
40 of water and alkali and can be made compara
tively ?exible or rigid, as desired.
Among the objects of my invention are to over
come di?iculties and objections heretofore pre
sented to the use of unsaponi?able resins of the
45 coumarone-indene type in the manufacture and
treatment of paper, ?ber, textiles and the like
and for various other purposes; to produce dis
persions of unsaponi?able resins, such as resin
of the coumarone-indene type, and to provide
simple and economical methods for producing
dispersions of such resins.
_
' These and other objects and features of my
invention will appear from the following de
“ scription thereof, in which reference is made to
the coumarone-indene type which have either
high or low melting points, i. e., which are of 35
either the hard or the soft grades.
_
In forming the dispersion, it is preferred to
employ silicate of soda, preferably containing a
high ratio of $102 to NazO, that is, a ratio of .
about 3 or more parts of $10: to 1 part of NazO 40
as ‘the dispersing agent. For example, I may
employ a silicate solution having a density of >
42.5“ Baumé and containing 39.6 per centby
weight of sodium silicate in which there is about
3.25 parts by weight of $10: to 1 part of NazO. 45
I have also employed a silicate solution having a
density of about 33.5° Baumé and containing 31.3 ,
per cent of silicate of soda having 3.86 parts by '
weight of S10: to 1 part of NazO. Although I
prefer to employ a solution containing 30 per 50’
cent or more by weight of silicate of soda which A
has a high ratio of S102 to NaaO, I may employ
other forms, grades or solutions of soluble sili
cates. Instead of the soluble silicate dispersing
agent, I may use sodium carbonate, caustic soda, 5;
._
2
_
a
.
.
I
.
~
.
I,‘
'
8,061,409
ammonium hydroxide or trisodium phosphate.
In the formation of more stable dispersions, i. e..
dispersionswhich will be stored for a considerable
period of time and‘will not be employed soon after
formation, a regulated amount, as hereinafter
pointed out, of saponi?able material may be added
to the dispersion to stabilize the same. The in
corporation of a‘ relatively large Proportion of
evaporatedwater (orsolvent-ifsuchisiued) to
the mixture. .
'
j
.
The products obtained bythe use of‘my inven
tion described above
vary considerably in
properties and composition.” For instance, I have 5
produced dispersions of resins by the use ofv the
methods of procedure suggested above that con
tain an amount ‘of resin equal to from about 5
saponi?able material in the dispersion deleteri
per cent to 70 per cent of the weight of water
ously affects the waterproo?ng properties of the . used in producing the dispersions and I have 10
sheets or boards made therefrom. In accordance produced dispersions of the resins without the
with this invention involving the incorporation use of any saponifiable material in the process.
of saponi?able material in the non-saponi?able
'l‘heproductsobtsinedinthepractlceofmy
resin emulsion or dispersion, the amount of sa
invention are adapted for use in the sizing of
.15 poni?able material added is carefully regulated paper, in the formation ‘of ?ber board and lami
with respect to the non-saponi?able resin con
nated products, for the impregnation or treat
tent. For example, in emulsifying paracouma
ment of paper, fabrics. leather and the like and
rone resin having a melting point below 40’ C., 1 for numerous other purposes where resins are
part of saponi?able material may be added for employed.
~
‘
20 every 50 parts of resin. In emulsifying harder
In using the products obtained for sizing paper 20
resins, more saponi?able material may be em
or for producing fiber board, the dispersion may
ployed. .In the emulsi?cation of paracoumarone be-added to a pulp of paper or ?ber'in a beater,
resin melting above 80° C., the amount of saponi-' the amount and character of the dispersion used
. ?able material added to the resin mixture is pref
25 erably one part or more saponi?able material to
25 parts paracoumarone resin. Suitable saponi?
able materials which may be employed include
rosin, rosin oil, rosin soap, linseed oil, linseed oil
fatty , acids, abietic acid, oleic acid and other
30 aliphatic acids and saponi?able materials. The
saponi?able material may be employed in con
junction with clays such as bentonite, kaolin, or
china clay. A non-aqueous solvent, e. g., toluene,
may also be added and stirred into the product,
35 but preferably this solvent should be added to
the resin before emulsi?cation.
The following example is illustrative of a pre
ferred method of practicing my invention to pro
duce dispersions or emulsions of the oil-in-water
40
type:
-
'
being regulated to obtain the desired proportions
of resin to ?ber. The dispersion is intimately 25
mixed with the pulp and a precipitant or floccu
lating agent such as alum or other electrolyte is
added to the materials to cause the resin to
precipitate on the ?ber. The addition of the
alum causes the breaking down of the dispersion. 30
the dispersed particles beingdeposited on the
?ber. In the case of higher melting point para
coumarone resins, e. g., resins melting above 25''
C., the dispersed particles will be deposited in
solid, non-adhesive condition onto the ?bers. 35
Hence, the mixture of ?brous material and para
coumarone resin particles canbe sheeted on a
paper-making machine without adherence of the
binder particles to the paper-making instrumen
talities. The binder particles are coalesced and
Resin of the coumarone-indene type having a substantially homogeneously distributed through
melting point below about 40° C. is melted and out the paper upon the drying and calendering
while the resin is still molten, I add 1 part by of the paper. The pulp may be formed into sheets
weight of the resin to 2 parts by weight of a solu
of desired thickness and the sheetsldried and
.45 tion ofv silicate of soda, whipping the materials pressed, if desired, to obtain the desired product.
'- together
g'The product.
by{ means
resulting
of a highfrom
speedthe
stirring
process
device;
as. ' i, . The invention herein may be employed to form
stable emulsions or dispersions of other substan
described-min; the foregoing example is an oil-in ' tially non-saponi?able hard resinous materials.
watzer-di‘sper'siong'an' emulsion of resin in water For example, hard resins made from cracked
separate after standing for several petroleum, as well known in the petroleum art,
50;whl , ~wii
rodiictyhas su?'icientbodypto he‘: “Glyptal” resins‘, “Bakeiite,"v pitch resins, and
handle
{worked easily in a beater or‘" ‘they:vv “the substantially nonsaponi?able ester gum may
“ apparatus for‘ distributing the resin vonto-Pth’e be emulsi?ed in- the manner hereinabove de
fiber ofi'af pulp‘: such as paper stock. This disper
scribed for the emulsi?cation of hard resins of
‘sum 'is aiso'capable of dilution with water when... ; the coumarone-indene type. Resins made by the
'althinjdispers'ioniis desired.
,
'
polymerization of cracked distillates obtained
‘A'n‘y suitable type of apparatus may beemployed
. for agitating, mixing or whipping the materials
from petroleum and/or natural gas have proper
ties similar to the properties of paracoumarone
together or otherwise blending them to produce 'resins and for many purposes may be used iiiterchangeably with paracoumarone resins. The Oil
prefer to employ apparatus having a bladed pro
term “paracoumarone resin-like material” as
peller driven at high speed by means of a motor used in the claims herein is intended to ‘be a
or other suitable driving mechanism, or a suitable generic term to include both paracoumarone res
in and resin obtained by the polymerization of
colloid mill of well-known type.
60 the dispersions of the present invention, but I
65
When employing the above-described methods
of procedure for treating a resin having a melting
point appreciably above atmospheric temperature,
it may be preferable in some cases to heat the
70 materials during the formation of the dispersion.
This may easily be effected by heating the vessel
in which the materials are treated by means of
steam or hot water. The heating may be carried
out under pressure, when desirable, or in a closed
75 vessel ?tted with a re?ux condenser to return
such cracked distillates.
*
The term “dispersions" as used throughout the
speci?cation and claims in referring to the prod
ucts obtained in practicing my process is intend
ed to include all such products as I have de
scribed above whether they are suspensions or 10
emulsions.
I claim:
- -
1. The method which consists in melting a res
in of the coumarone indene type, having a melt
ing point‘below about 40° C., while the resin is 16
3
8,051,409
still molten adding one part by wei‘g'htof the
resin to two parts by weight of a solution of sili
cate oi soda, and whipping these materials to,
gether by means 0! a high speed stirring device
until a relatively stable emulsion is formed.
2. The method of producing a comparatively
tating the resultant
of resin and water
solution of alkali silicate to produce said com
paratively stable dispersion.
1
3. A comparatively stable dispersion of resin
oi the coumarone indene type, particularly
adapted for sizing and waterproo?ng ?brous
stable dispersion of a resin 0! the coumarone in! ' sheets during the manufacture thereof. said dis
dene type. free of saponi?able material, which , persion being free of saponi?able material and
dispersion is particularly adapted for sizing and consisting of lique?ed resin 0! the coumarone
indene type dispersed in a solution consisting oi 10
10 waterproo?ng paper, comprising the step of add
ing the said resin in lique?ed form to a solution alkali silicate and water.
consisting of alkali silicate and water and agi
'
'
'
JOHN A. KENNEY.
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