Improvements in Refining Crude Petroleum and its Products.
Year: 1899

page_text: Date of Application, 11th Apr., 1899-Accepted, 13th May, 1899
COMPLETE SPECIFICATION.
Improvements in Refining Crude Petroleum and its Products.
I, REGINALD HADDAN, of the Firm of Herbert Haddan & Co., of 18, Buckingham
Street, Strand, London, Patent Agent, do hereby declare the nature of this inven-
tion a communication to me from abroad by Friedrich Berg, of Cleveland, State of
Ohio, in the United States of America, Oil Refiner, and in what manner the same is
to be performed to be particularly described and ascertained in and by the follow-
ing statement:-
In carrying out my improved process place the crude petroleum as pumped
from the earth, (and I have taken the most inferior grade of oil) in a tank or
receptacle, and add alkali, preferably caustic soda, thereto, and stir and mix the alkali
and crude oil together in any approved manner. The alkali and crude oil are prefer-
ably mixed at the ordinary temperature. A mixture, in the proportions of about one
gallon of alkali to about one barrel of the oil is preferable. I then heat the mixture of
alkali and crude oil to about 200° Fahrenheit, or somewhat greater temperature,
and keep the mixture heated at this temperature for a few hours. A heat of 200°
Fahrenheit is preferable and the maintenance of the mixture at this temperature
for about five hours desirable. Of course, it is obvious that the lighter products
of petroleum, such, for instance, as naphtha, will vaporize at this temperature, but
these escaping vapors can be saved by any well known apparatus suitable for
the purpose, and the escaping products can be returned, if desired, to the body of the
oil that requires further treatment. The mixture of crude oil and alkali at the
aforesaid temperature should be stirred for about ten minutes every hour during
the time in which the mixture is maintained at the comparatively high temperature
indicated. The agitation of the mixture at intervals as aforesaid facilitates the work
of the alkali that is instrumental in decomposing the sulfurous compounds or
foreign matter contained in the oil, and is also instrumental in effecting the
destruction or removal of water contained in the oil. I would here remark that
all crude oil contains water in an undesirable quantity. The quantity of water
contained in the oil is generally about five per cent. All water should be removed
from the oil, if possible, in order to maintain a good illuminating oil. During this
treatment of the crude oil with the alkali, most of the impurities and water con-
tained in the oil are precipitated or destroyed. Of course, this treatment does not
entirely free the oil from impurities and water, and further treatment of the oil
is, therefore, required.
After the treatment of the oil with the alkali, in the manner herein before
described, I remove the oil from the tank or still, and consequently from the
alkali and foreign matter that have been precipitated or have settled in said tank
or still. The remaining alkali can be used in the treatment of another quantity
of raw crude oil. I then place the oil that has been removed from the alkali in
another tank wherein it is kept for a few days preferably six days, at a moderato
temperature (about 70° Fahrenheit) and during this time the alkali still remaining
in the oil, and that did not settle in the tank or still wherein the oil was treated
with the alkali, at the aforesaid comparatively high temperature, continues its
wark of destroying sulphurous compounds or impurities and water still contained
in the l

page_text: No expensive chemicals are required in my improved process to accomplish the
destruction or precipitation of the objectionable foreign matter and water, and I
have found that the work of the alkali still contained in the oil for several days is
invaluable in effecting the purification and deodorization of the oil.
The oil being treated is next removed from the tank, wherein it was lastly under-
going treatment, to a still, and is there subject to the ordinary process of distilla-
tion. The distillation of the oil after the removal of the larger percentage of the
sulfurous compounds, is important because it is obvious that a distilling apparatus
will last much longer if the larger percentage of the sulfurous compounds, that
would be highly destructive to said apparatus, are removed before the distillation.
The distillate obtained could be used as, and is an illuminating oil, but has not
all the properties of what I consider first class illuminating oil and requires further
refinement in order to make it a first class illuminating oil. A small amount of
alkali is still in the oil during the distillation just referred to, and this remaining
alkali does effective work in destroying the lighter sulfurous compounds or
impurities still contained in the oil. The distillate obtained is then treated lightly
with sulfuric acid. This acid removes the water contained in the distillate. If freeh
acid is used, I prefer about three pounds of the acid to one barrel of the distillate;
if spent acid is employed, I prefer about five pounds of the acid to about one barrel
of the distillate. Spent acid would, of course, be generally employed. The acid
and oil are mixed at the ordinary temperature and are agitated or stirred in any
approved manner for about a half hour. The oil should not be washed after the
treatment of the distillate with the acid as has heretofore been practiced, because
I have found that the washing of the oil with water is attended by the liberation of
the hydrogen from the water and acid, and this hydrogen and the sulfur in the
acid and the impurities still contained in the oil, form new sulfurous_compounds.
and the oil, instead of being cleaned, is really made more impure. I would cal!
particular attention to the importance of removing as far as possible, every trace
of water contained in the oil. After having treated the distillate with the acid, as
hereinbefore described, I again treat the oil with an alkali in any approved manner
for the purpose of neutralizing and destroying the acid and impurities. I employ
preferably about one gallon of the alkali to one barrel of the oil, and mix or stir
the same together in a tank for about a half hour. After this second treatment of
the oil with an alkali I remove the oil into a still and again distill. Any vapours
escaping in this second distillation can, it is obvious, be saved by well known
apparatus suitable for the purpose.
After the second distillation, the oil now a second distillate is subject to a light
treatment with sulfuric acid, and in this treatment of the oil with acid about two
pounds of fresh acid are preferably used to about one barrel of the oil.
function of this last treatment of the oil with acid is to remove from the oil, or
second distillate, any water that is still contained in the oil.
The
The resulting product is an oil that is exceedingly clean, that is odourless, that
has superior illuminating properties and that costs much less, it will be observed
than the illuminating oils obtained by the refining
practiced or invented.
processes heretofore
Having now particularly described and ascertained the nature of this
invention and in what manner the same is to be performed I declare that what
I claim is :-
-
1) The petroleum refining process herein described, comprising firstly, a treat-
ment of the crude oil with an alkali at a comparatively high temperature, main-
taining this mixture at said temperature for several hours and stirring or agitating
the mixture, at intervals during this time; then removing or separating the alkali
and foreign matter that has been precipitated or settled during said alkali treat-
ment and permitting the alkali still contained in the oil by allowing the oil to
stand for several days at a moderate temperature to continue its work of destroying 5
sulfurous compounds and impurities still remaining in the oil then distilling the

page_text: oil, and finally treating the distillate with sulphuric acid for the
purpose of
removing the water contained in the distillate, substantially as hereinbefore
described.
2) The petroleum refining process herein described, comprising firstly a suitable
treatment of the crude oil with an alkali at a comparatively high temperature and
maintaining the mixture at such temperature for several hours; secondly the
removal or separation of the oil from the alkali and foreign matter that have been
precipitated or have settled during said alkali treatment, and permitting the alkali
still remaining in the oil to continue its work for several days at any suitable
temperature; thirdly distilling the oil; fourthly, subjecting the distillate to a
suitable treatment with sulphuric acid; fifthly, again suitably treating the oil with
an alkali for the purpose of neutralising and removing the acid and impurities;
sixthly again distilling the oil, and seventhly, subjecting the second distillate to a
suitable treatment with sulphuric acid in order to remove all water still contained
in the oil, substantially as hereinbefore described.
3) The petroleum refining process herein described, comprising firstly the mixing
of an alkali with the crude oil in suitable proportions heating this mixture to a
comparatively high temperature, maintaining this mixture at a comparatively high
temperature for several hours and stirring or agitating the mixture at suitable
intervals during this time; secondly removing or separating the oil from the
alkali and foreign matter that have been precipitated or have settled in the afore-
said alkali treatment and permitting the oil, that still contains alkali, to stand for
several days at a moderate temperature; thirdly distilling the oil; fourthly sub-
jecting the distillate to a light treatment with sulphuric acid; fifthly again treat-
ing the oil with an alkali; for the purpose of neutralizing and removing the acid
and impurities, sixthly again distilling the oil, and seventhly subjecting the second
distillate to a light treatment with sulphuric acid, to remove all water still con-
tained in the oil, substantially as set forth.
4. The petroleum refining process herein described, comprising firstly, the mixing
of an alkali with the oil in suitable proportions, heating this mixture to about 2000
Fahrenheit and keeping the mixture heated at this temperature for a few hours
and stirring the mixture for a short time every hour during this treatment;
secondly, separating the oil from the alkali and foreign matter that have been
precipitated or have settled during the treatment of the oil with the alkali and
then permitting the alkali still contained in the oil to do work for several days at
a moderate temperature; thirdly distilling the oil, and finally treating the distil-
late in any approved manner with sulphuric acid, substantially as set forth.
5. The petroleum refining process herein described comprising firstly, the mixing
of an alkali with crude oil in suitable proportions, heating this mixture to a
comparatively high temperature and keeping the mixture heated at this tempera-
ture for about five hours, and stirring the mixture for a short time every hour,
during said alkali treatment; secondly separating the oil from the alkali and
foreign matter that have been precipitated or have settled during the aforesai
treatment of the oil with the alkali, and then permitting the alkali still contained
in the oil to continue its work for several days at a moderate temperature; thirdly,
distilling the oil; fourthly, subjecting the distillate to a light treatment with sul-
phuric acid in order to neutralize and destroy the acid and impurities: fifthly,
again treating the oil with an alkali; sixthly, again distilling the oil, and
Seventhly subjecting the second distillate to a light, treatment with sulphuric acid
for removing all water still contained in the oil, substantially as set forth.
6. The petroleum refining process herein described, comprising firstly the mix-
ture of an alkali with crude oil in suitable proportions, heating this mixture to a
comparatively high temperature and keeping the mixture heated at this tempera-
ture for a few hours, and stirring the mixture for a short time every hour during
this treatment; secondly, separating the oil from the alkali and foreign matter
that have been precipitated or have settled during the treatment of the aforesaid
il with the alkali, and then permitting the alkali still contained in the oil to

page_text: continue its work for about six days, at a moderate temperature; thirdly distilling
the oil, fourthly subjecting the distillate to a light treatment with sulphuric acid
in order to neutralize and destroy the acid and impurities; fifthly again treating
the oil with an alkali; sixthly again distilling the oil, and seventhly subjecting
the second distillate to a light treatment with sulphuric acid to remove all water
still contained in the oil, substantially as set forth.
7. The petroleum refining process herein described involving firstly the mixture
of the alkali with crude oil in the proportions of about one gallon of the alkali to
one barrel of the oil and heating this mixture to a comparatively high temperature
and maintaining the mixture at this temperature for a few hours and stirring
and agitating the mixture during this time for about ten minutes every hour
secondly separating the oil from the impurities and alkali that have been precipi-
tated or have settled during the preceding alkali treatment and permitting the
alkali that is still contained in the oil to continue its work for several days at a
moderate temperature, thirdly, distilling the oil, fourthly subjecting the distillate
to a light treatment with sulphuric acid in order to neutralize the acid and
impurities; fifthly again treating the oil with an alkali; sixthly again distilling
the oil, and seventhly treating the second distillate lightly with sulphuric acid, to
remove all the water still contained in the oil substantially as set forth.
S. As an improvement in refining petroleum, the treatment of the oil with an
alkali at a comparatively high temperature for several hours, and permtting the
alkali that is still contained in the oil after the expiration of the said time to con-
tinue its work of destroying sulphurous compounds and impurities or foreign matter
for a period of several days.