Process of Desulfurizing Oil or Distillate Page: 2 of 3
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764,099
tralizes any trace of acid that may be present
in the ferrous-sulfate solution, thereby insur-
ing a neutral ferrous solution.
The hydrate-of-iron and neutral iron solu-
5 tions readily take up oxygen from the air or
steam and acting as powerful oxidizing agents
convert the insoluble hydrosulfid of copper
into a soluble sulfate of copper. This may
easily be detected by the change of color.
10 The sulfate-of-copper and the iron solutions
are then drawn off, and after a thorough wash-
ing the oil is allowed. to settle or is filtered.
It is then ready for use. I have used man-
ganates and chromates to make the neutral
15 solution; but 1 prefer the ferrous sulfate, as
it is cheaper and just as effective.
It will be observed that the quantity of sa-
line copper solution used to effect desulfuriza-
tion is largely in excess of the quantity of
20 caustic and that while the quantity of caustic
employed is sufficient to neutralize any acid
present and to effect a partial precipitation of
the copper there remains an excess of neutral
saline copper solution. Therefore the action
25 of the caustic must be to first neutralize the
acid present, if there should be any, and then
to effect a partial precipitation of freshly-hy-
drated copper and the resulting sulfate of the
alkali applied, thereby producing of necessity
30 a neutral saline solution, which in consequence
of its specific gravity separates quickly from
the oil or distillate after agitation ceases.
I am aware that distillates have been treated
with copper and copper salts with an excess
35 of acid and with an excess of alkali, but have
found in both cases that the product so ob-
tained was so saturated with copper that it
was impossible to remove it with any ordinary
acid and alkali treatment and that the presence
40 of copper in the oil deprives it of value. I
am also aware that hydrated copper has been
used in the presence of heat; but it is well
known that hydrated copper plus heat pro-
duces an oxid of copper plus water, as the fol-
45 lowing formula will show:
Cu(OH)2+ heat=CuO+H20,
and the heat reaction so combines the copper
with the oil as to render it inseparable except
50 by redistillation.
The use of hydrated copper in a neutral so-
lution, as described in this application, makes
it possible to desulfurize the distillate with-
out combining copper with it, and what cop-
55 per is. taken up or held: in suspension is in-
soluble in sulfuric acid. and can be readily
eliminated: by the method employed in appli.-
cation Serial No. 145,072 or by the method
herein described for lubricating-oils.
6o I do not confine myself to the use of concen-
trated solutions of sulfate of copper and al-
kali, as very dilute solutions of the reagents
specified. if used in sufficient quantity will sat-
isfactorily desulfurize the distillates, the all-
65 important part being the use of a quantity ofthe copper and iron solutions in excess of the
alkali solutions and sufficiently so to produce
neutral saline solutions, as described. I pre-
fer the concentrated solutions, for the reason
that it is easier to separate and remove them 70
from the oil or distillate.
This process, as described, has been applied
to the desulfurization of Ohio, Canadian, and
Texas sulfur-bearing oils; but the most difll-
cult samples encountered and successfully re- 75
fined have been samples of thirty per cent.
straight-run plus thirty per cent. more of
cracked Findlay, Ohio, oil, making sixty per
cent. of the same distillation.
Having described my invention, what I claim 80
as new, and desire to secure by Letters Patent
of the United States, is-
1. The process of desulfurizing oil or distil-
late which consists: in removingthe sulfureted
hydrogen and neutralizing the fatty and or- 85
ganic acids contained therein; then in expos-
ing the oil or distillate with its sulfur or sulfur
compounds to the action of a soluble salt of
copper in the presence of an alkali; in remov-
ing the excess of copper and copper hydro- 90
sulfids and exposing the oil or distillate and
any hydrosulfid of copper remaining therein,
to the oxidizing effect of one or more oxidiz-
ing agents; in removing the resulting copper
sulfates and settling the oil, all substantially 95
as described.
2. The process of desulfurizing oil or distil-
late which consists: in neutralizing organic
acids contained therein; in exposing the oil or
distillate to the action of a soluble salt of cop- 100
per in the presence of an alkali in a neutral
saline solution; in removing the excess of cop-
per and copper hydrosulfids and exposing the
oil or distillate and any hydrosulfid of copper
remaining therein to the oxidizing action of 105
one or more oxidizing agents; in removing
the resulting copper sulfates and settling the
oil or distillate.
3. The process of desufurizing oil or distil-
late which consists: in neutralizing the acid 110
contained therein; in exposing the oil or dis-
tillate to. the action of a copper hydrate in a
neutral:saline solution; in removing the excess
of copper and copper hydrosulfids and expos-
ing the oil or distillate and any hydrosulfid of '15
copper remaining therein tothe oxidizing ac-
tion of one or more oxidizing agents; in re-
moving the resulting copper sulfates and set-
tling the oil or distillate, all substantially as
described. .1 2C
4. The process of desulfurizing oil or distil-
late which consists: in neutralizing the acids
contained therein; in exposing the oil or dis-
tillate with. the sulfur or sulfur compounds
therein contained to. the action of a copper hy- 125
drate in a neutral. saline solution; in exposing
the oil or distillate and the resulting copper
hydrosulfids to the oxidizing action of one or
more oxidizing agents; in removing the re-
sulting copper sulfate and residuum and set- 1302
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Amend, Otto P. Process of Desulfurizing Oil or Distillate, patent, July 5, 1904; [Washington D.C.]. (https://texashistory.unt.edu/ark:/67531/metapth508736/m1/2/?q=%22%22~1: accessed July 16, 2024), University of North Texas Libraries, The Portal to Texas History, https://texashistory.unt.edu.; crediting UNT Libraries Government Documents Department.