Process of Desulfurizing Oil or Distillate Page: 1 of 3
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Patented July 5, 1904.
UNITED
STATES
PATENT OFFICE.
OTTO P. AMEND, OF. NEW YORK, .N. Y.
PROCESS OF DESULFURIZING OIL OR DISTILLATE.
SPECIFICATION forming part of Letters Patent No. 764,099, dated July 5, 1904.
Application filed February 25, 1903. Serial No, 145,073. (No specimens.)To (ll whom it may coutern.-
Be it known that I, OrroP. AMEND, acitizen
of the United States, residing at New York, in
the county of New York and State of New
5 York, have invented new and useful Improve-
ments in Processes of Desulfurizing Oils or
Distillates, of which the following is a speci-
fication.
My invention relates to the desulfurization
10 of all sulfur-bearing oils, but especially to the
heavier grades of petroleum-oil used for lu-
bricating purposes.
Hitherto much difficulty has been experi-
enced in desulfurizing the heavy distillate
15 from which lubricating-oils are made. This
is especially true of Ohio, Texas, and Califor-
nia oils. I have found that these heavy oils
and distillates can be desulfurized as easily as
the naphthas and burning-oil, and to accom-
20 plish this I utilize a part of the process de-
scribed in the application for Letters Patent
filed simultaneously herewith, Serial No.
145,072, particularly that part of it which de-
scribes the use of a solution made with a solu-
25 ble copper salt; but as the faintest trace of
acid in a lubricating-oil is a fatal defect and
as the presence of caustic in any material quan-
tity is also objectionable, and, further, as it is
desirable to remove as much as possible of the
30 copper employed to effect desulfurization it
becomes imperative either to substitute an
after treatment to effect the removal of the
copper held in suspension in the oil in lieu of
the acid treatment used in application Serial
35 No. 145,072 or to redistil it. I prefer to use
the after treatment hereinafter described,
which may also be used to advantage with
lighter oils, to which the ordinary acid treat-
ment may be subsequently employed for fur-
40 there refinement.
In the desulfurization of heavy distillates I
have found that in the presence of neutral sa-
line solutions hydrates of the metals, espe-
cially hydrate of copper, will readily combine
45 with sulfur of the sulfur compounds in the
oils or distillates referred to, the latter form-
ing hydrosulfid of copper, which precipitates
and which may be easily separated from the
oil or distillate so treated, and after such sepa-
50 ration it can be shown that the oil or distillateis practically free of sulfur by testing it with
plumbate of soda, mercury, or with any of
the well-known means employed to indicate
sulfur reaction in oils.
In carrying out my invention I proceed as 55
follows: I first wash the oil or distillate and
blow it well with air, steam,.or with both to
remove as much sulfureted hydrogen as pos-
sible. I then remove the wash-water and add
enough caustic solution (preferably caustic- 6o
soda solution, as it is the cheapest) to neutral-
i tehteorganic acids found in portions of the
distillate. I usually employ of the solution
about one per cent. of the weight of oil, the
solution containing from three to five per 65
cent. of caustic soda. After thorough agita-
tion the caustic soda is drawn off, and with it
more or less coloring - matter separated or
taken up by it. I then apply an aqueous so-
lution of a soluble salt of copper in quantity 70
about five per cent. of the weight of the oil or
distillate and preferably one of 250 Baume
strength. The sulfate being the cheapest I em-
ploy it. After agitating the oil or distillate
with the copper solution I add of caustic-soda 75
or potash solution of 25 Baume strength one-
half of one per cent. of the weight of the dis-
tillate. The addition of this caustic solution
gives a freshly-precipitated hydrate of cop-
per and, with an excess of copper present, the 8o
resulting sulfate of the alkali. The hydrated
copper combining with the sulfur in the dis-
tillate forms hydrosulfid of copper, which with
the sulfate of the alkali settles to the bottom of
the oil or distillate and is removed. After such 85
removal the oil or distillate is thoroughly
washed with water and then when well settled
and the water is drawn off it is agitated in con-
tact withferrous hydrate in a neutral solution
of ferrous sulfate-say about five per cent., by 9o
weight, of the distillate treated and of about
250 Baume strength-by means of a strong cur-
rent of air or air and steam, the air being in-
troduced therein by a pump or blower and
communicating pipes or by any suitable me- 95
chanical device adapted to the purpose.
The ferrous hydrate is produced by adding
to the ferrous - sulfate solution about one-
quarter of one per cent. of caustic-soda solu-
tion of five per cent. strength, which also neu- IOUN\o. 764,099.
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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/m1/1/: accessed July 18, 2024), University of North Texas Libraries, The Portal to Texas History, https://texashistory.unt.edu; crediting UNT Libraries Government Documents Department.