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Патент USA US2118915

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£118,915
Patented May 31, 1938
' UNITED STATES PATENT "OFFICE
Richard James Butz and Robert Charles vCantelo,
Whiting, Ind., assignors to Sinclair Re?ning
Company, New York, N. Y., a corporation of‘
Maine
No Drawing. Application September so. 1936,
Serial No. 103,367
3 Claims. I, (Cl. 260—116)
1
‘This invention relates to improvements in the . The wax acids are then saponi?ed by heating for
’ manufacture of so-called “wax acids”, the organic _ 1 hour at 172° F. with a 20° Baumé aqueous
, acids produced by oxidation of paraffin wax hav- solution of sodium hydroxide in proportion con
ing acid numbers approximating 120 or higher, taining about thatamount of sodium hydroxide
saponi?cation numbers approximating 130 or" theoretically required to react with the wax acids 5
higher and molecular weights in the. general and the temperature of the mixture is then ‘raised
neighborhood of 400. The invention is of special to _190° F. and maintained at 190° F. for 30 min
value in the manufacturevof wax acids for com
utes. The resulting mixture including the sodium.
pounding, as aluminum salts of the wax acids, salts of the wax acids is diluted with ?ve times its
0“) with petroleum lubricatingolls to lower the pour ' 'volume of water, suiiicient ‘acetone or other suit- 10
'
point of such oils as described in an application '
filed June 11, 1935, Serial Number 26,038 by Ed
win J. Barth and Ralph P. Corlew.
,
-
According to this invention, such wax acids
15 are prepared by blowing air through parailln
able organic solvent is added to resolve the re
sulting emulsion, and the aqueous soap solution.
is separated by decantation from the supernatant .
layer of unsaponi?able matter.
'
15'
Example II
wax of melting point approximating 130°-132° F.
at a rate ranging from 0.5 to 10.0 cubic feet per
The operation is the same as that described in
hour per pound of wax mixture while maintain. . Example I, except that the blowing is continued
ing a temperature of 220°-250° F., stopping the until the acid number and saponi?cation number
20
oxidation before the acid number and saponi?
of the wax mixture reach 45.5 and 92, respective- 2.0
cation number of the wax mixture exceeds 70
and 125, respectively, and separating the wax
‘ acids from the wax mixture. Separation of the
wax acids from the wax mixture can be effected
25 in any convenient manner, by saponi?cation and .
separation of the resulting soap or by‘extraction
with an appropriate solvent such as .isopropyl
, alcohol for example. A blowing rate approxi
" mating 2 cubic feet per hour per pound of wax
“9 mixture is particularly advantageous. The yield
1y.‘ A somewhat higher yield of wax acids some~ what more effective in the form of aluminum salts
as pour depressors is obtained.
Example III
2
'
25
» 21/2 kilograms of para?in wax having a melt- “
ing point of l30°-132° F. and 37.5 grams of stearic
acid are charged into a steam jacketed steel pot
. equipped with a paddle type stirrer. Air is blown
through the charge in the pot while maintain- 30
of wax acids is improved by blowing the wax while
ing a temperature of 250° F. until the saponi?ca» .
maintaining a temperature approximating 250° F.
until the saponi?cation number of the wax mix—
tion number of the wax mixture reaches 43.5, the
temperature is then reduced toabout 230° F. and
ture approximates 40-50 and then reducing the the blowing is continued at this lower tempera
35 temperature to about 230° F. and continuing ‘the ture until the acid number and saponi?cation 35
blowing at this lower temperature, the tempera 'numberreach’ 54.4,and 103, respectively. The
ture being reduced either in a single step or in wax acids produced are separated by saponi?ca
several steps.
4
_
tion with'sodium hydroxide as ‘in the ?rst ex
-
The following examples. will illustrate the
40 practice of the invention:
.
I
Example I .
2% kilograms of para?in wax having a nielt
ample A yield of wax. acids somewhat ‘higher
than that obtained in the second example is ob- 40
tained, these wax acids being about'as e?ective, .
in the formpf aluminum salts, as pour depressors
as those obtained in the first example.
ing point of 130L132‘ F. and 37.5 grams of stearic
45 acid are charged into a steam jacketed steel pot
application Serial No. 26,038 can be prepared by‘ 45
’ equipped with a paddle type stirrer. Air is blown
converting the sodium salts of the wax acids pro-_ .
through the charge in the pot at a rate of ‘about
llcublc feet per hour while maintaining a tem
The pour depressors described'in said prior
duced as described in the foregoing examples to
aluminum salts of these wax acids .by reaction
perature of 250° F., the mixture in the pot being with anappropriate aluminum salt, coagulation. ,
50 vigorously agitated throughout the blowing, care separation, washing, drying and extraction with 50
being taken to limit the agitation to a degree ‘ benzol as described in that prior application. The
avoiding the formation of an air emulsion with wax acids} produced as described herein are of
the wax mixture. The blowing is continued until special value in the manufacture of such pour.
the acid number and saponiilcation number of depressors.‘ For example, blowing rates substan
55 the mixture reaches 3'! and ‘19.3, respectively.
tially higher than those speci?ed, tend to produce 66_
_
_
,
2,118,915
‘wax acids which in ‘the form of aluminum salts
are less effective as pour depressors and the oxi
dation carried to a point such that the speci?ed
acid number and saponi?cation number (limits
‘
2. In the manufacture of wax acids, the im
provement which comprises blowing air through
param'n wax of melting point approximating
130°-132° F. at a rate approximating 2 cubic feet
per hour per pound of wax mixture while main
are substantially exceeded tends to produce wax
acids which in the form of aluminum salts are
less~e?ective as pour depressors. The aluminum
taining a temperature of 220°-250° F., stopping
‘salts of the wax acids prepared as described in
?cation number of the wax mixture exceed 70 '
the oxidation. before the acid number and saponi
the foregoing examples were effective, severally, and 125, respectively, and separating the wax
acids from the wax mixture.
10
to reduce the pour test of a Pennsylvania lubri
3. In the manufacture of wax acids, the im
cating oil originally having a pour test of 25° F. p
to -10° F. or lower added in amounts of 0.5% provement which‘ comprises blowing air through
para?in wax of melting point approximating
(by weight) on the oil.
;_
A
The addition of stearic' acid to the charge of 130°-l_32° F. at a rate of 0.5-1!) cubic feet per
paramn wax subjected to oxidation as in the hour per pound of wax» mixture while maintain 15
foregoing examples is not essential but does
ing a temperature approximating 250° F. until
facilitate the progress of the oxidation.
We claim:
1. In the manufacture of wax acids, the im
the saponi?cation number of the wax mixture ap
provement which comprises blowing air through
para?in wax of melting point approximating
130°~132° F. at a rate of 0.5-10 cubic feet per
hour per pound of wax mixture while maintain
proximates 40-50, reducing the temperature'to
about 230° F. and continuing the air blowing,
stopping the oxidation before the acid number
and saponi?cation number of the wax mixture
exceed '70 and 125, respectively, and separating
the wax acids from the‘ wax mixture.
ing a temperature of 220°-250° F., stopping the
oxidation before the acid number and saponi?
ROBERT CHARLES CANTEIlO.
cation number of the wax mixture exceed 70 and
RICHARD JAIWES BUTZ.
125, respectively, and separating the wax acids
'from the wax mixture. ,
25
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