AN IMPROVED METHOD AND APPARATUS FOR THE DISTILLATION OF CERTAIN OILS OR OILY SUBSTANCES FROM THE PETROLEUM, COMMONLY CALLED 'EARTH OIL,' FOUND IN CERTAIN DISTRICTS IN THE BIRMAN EMPIRE, AND AN IMPROVED METOD OF PURIFYING THE OILS OR OILY SUBSTANCES SO OBTAINED
Year: 1856

page_text: pool, in the County of Lancaster, Gentleman, for the Invention of "AN
IMPROVED METHOD AND APPARATUS FOR THE DISTILLATION OF CERTAIN OILS
OR OILY SUBSTANCES FROM THE PETROLEUM, COMMONLY CALLED 'EARTH OIL,'
FOUND IN CERTAIN DISTRICTS IN THE BIRMAN EMPIRE, AND AN IMPROVED
METOD OF PURIFYING THE OILS OR OILY SUBSTANCES SO OBTAINED."
Sealed the 9th December 1856, and dated the 10th September 1856.
PROVISIONAL SPECIFICATION left by the said Stephen White at the
Office of the Commissioners of Patents, with his Petition, on the 10th
September 1856.
I, STEPHEN WHITE, of Newlands Street, Everton, Liverpool, in the County
of Lancaster, Gentleman, do hereby declare the nature of the said Invention
for "AN IMPROVED METHOD AND APPARATUS FOR THE DISTILLATION OF CERTAIN
OILS OR OILY SUBSTANCES FROM THE PETROLEUM, COMMONLY CALLED EARTH OIL,'
FOUND IN CERTAIN DISTRICTS IN THE BIRMAN EMPIRE, AND AN IMPROVED METHOD
OF PURIFYING THE OILS OR OILY SUBSTANCES SO OBTAINED," to be as follows:-
My Invention consists, first, in distilling from the said petroleum three
several products, viz., eupion, an oil which I term eupion oil, and paraffine,
by one continuous operation conducted in several stills or boilers connected
and working one into the other, & kept at different temperatures suitable to
Price 81

page_text: ԱՂԵԼ ԵՆ
vaporizing points on The matters contained in the petroleum
which are convertible into the said three products.
The apparatus which I use, and find to answer, consists of three boilers or
stills. The first boiler or still I heat by means of an ordinary furnace, raising
the temperature gradually till the bottom of the still reaches a low red heat;
the second boiler or still I heat by means of oil of high boiling temperature,
or impure paraffine, surrounding the boiler or still, and maintained at a
uniform temperature of 450° Fahrenheit, or thereabouts; and the third boiler
or still I heat by means of steam, of about fifteen pounds pressure to the
square inch, applied externally to the bottom part and outside the boiler or
still. The nature of the process of distillation is as follows:- The petroleum
is put into the first boiler, and first gives off at a low temperature vapor of
eupion, which passes through the two other boilers, not being condensed
therein (by reason of their higher temperature), and passes from the last of
them into a condensing worm, and thence into a reservoir in the state of
eupion. As the heat of the first boiler is increased the petroleum gives off
vapor of eupion oil, and that passes into the second boiler without being
condensed therein, and thence into the third boiler, where it is condensed, and
is drawn off in the form of eupion oil. As the distillation continues, the
temperature of the first boiler continuing to be raised, vapor of paraffine is
given out by the petroleum, and is condensed in the first boiler by means of
mechanical arrangements, and flows into the second boiler, and is thence
drawn off in the form of impure paraffine. The distillation of the three
products thus goes on by means of the combination of boilers kept at different
temperatures (that of the first varying, while that of the two others is constant,
or nearly so,) as a continuous operation.
After this distillation the three products undergo purification, which is
performed as follows:-I purify the eupion and the oil which I call eupion
oil by means of a mixture of common salt, neutral chromate of potash, and
sulphuric acid combined with water maintained at a certain temperature.
The mass is then allowed to repose, and the oils are drawn off. I then re-
distil these partially purified products, by means of the apparatus before
mentioned of three combined boilers, in the same manner as in the first
distillation; after which the products thus rectified are washed with a mixture
of proto-sulphate of iron (green vitriol) and carbonate of soda or carbonate
of potash combined, dissolved in water. I purify the impure paraffine by
placing it in the first boiler, and redistilling first one half part of the charge,
the produce of which redistillation I sometimes mix with the impure eupion
oil obtained by the first distillation. Then I continue the redistillation of the

page_text: other half of the impure paraffine, and this half so redistilled being withdrawn,
I treat for purification with a mixture of bichromate of potash and sulphuric
acid; I then submit it to a pressure in an hydraulic press; it is then again
treated with the mixture of bichromate of potash and sulphuric acid, and,
lastly, washed with a mixture of proto-sulphate of iron (green vitriol) and
carbonate of soda or carbonate of potash combined, dissolved in water. It
is then nearly pure paraffine, fit for the manufacture of candles and other
purposes.
SPECIFICATION in pursuance of the conditions of the Letters Patent filed
by the said Stephen White in the Great Seal Patent Office on the
10th March 1857.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, STEPHEN
WHITE, of Newlands Street, Everton, Liverpool, in the County of Lancaster,
Gentleman, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Tenth day of September, in the year of our Lord
One thousand eight hundred and fifty-six, in the twentieth year of Her reign,
did, for Herself, Her heirs and successors, give and grant unto me, the said
Stephen White, Her special license that I, the said Stephen White, my
executors, administrators, and assigns, or such others as I, the said Stephen
White, my executors, administrators, and assigns, should at any time agree
with, and no others, from time to time and at all times thereafter during the
term therein expressed, should and lawfully might make, use, exercise, and
vend, within the United Kingdom of Great Britain and Ireland, the Channel
Islands, and Isle of Man, an Invention for "AN IMPROVED METHOD AND
APPARATUS FOR THE DISTILLATION OF CERTAIN OILS OR OILY SUBSTANCES FROM THE
PETROLEUM, COMMONLY CALLED EARTH OIL,' FOUND IN CERTAIN DISTRICTS IN THE
BIRMAN EMPIRE, AND AN IMPROVED METHOD OF PURIFYING THE OILS OR OILY
SUBSTANCES SO OBTAINED," upon the condition (amongst others) that I, the said
Stephen White, by an instrument in writing under my hand and seal, should
particularly describe and ascertain the nature of the said Invention, and in
what manner the same was to be performed, and cause the same to be filed
in the Great Seal Patent Office within six calendar months next and imme-.
diately after the date of the said Letters Patent.
NOW KNOW YE, that I, the said Stephen White, do hereby declare the
nature of my said Invention, and in what manner the same is to be per-

page_text: formed, to be particularly described and ascertained in and by the following
statement, reference being had to the Sheet of Drawings hereunto annexed,
and to the letters and figures marked thereon (that is to say):-
Whereas it has long been known that the petroleum, commonly called
"earth oil," found in certain districts in the Birman Empire, is capable of
being treated by distillation by the application of heat, so as to produce there-
from oils: And whereas it has been treated under several Patents, or other-
wise, so as to distil from it oils or oily substances, being volatile hydro-carbons,
being substantially the substances which I herein call eupion, eupion oil,
and paraffine; and in such processes, known in this country by virtue of such
Patents, or otherwise, such substances, when obtained, have been treated by
various processes of purification: And whereas the processes so known of
obtaining by distillation the substances which I call eupion, eupion oil, and
paraffine, consist of a series of detached and separate operations by which the
different substances are produced, whether the distillation has been effected
by the agency of external heat applied to the stills used, or by the agency of
steam brought into contact with the petroleum (as is described in several
Patents granted to Warren De la rue, dated respectively the Twenty-fifth day
of July, One thousand eight hundred and fifty-three, the Fourth day of
September, One thousand eight hundred and fifty-five, and the Twenty-third
day of December, One thousand eight hundred and fifty-four): And whereas
in the several processes of purification of the said substances to adapt them
for commercial purposes, which have been practised or made public under the
said Patent, or otherwise, the chemical agents used have been or directed to
be sulphuric, or muriatic, or nitric acid, and caustic soda, or potash, or lime,
applied in various ways and in various orders: Now I wish it to be under-
stood that my Invention does not consist in the simple distillation of the
Birman earth oil, such distillation having been long known as a chemical
process or experiment; nor in the purification thereof generally, nor in the use
of such chemical agents generally, as herein-before referred to; but my
Invention consists in the particular method, which I shall proceed to describe
minutely, of distilling the three several substances, which I call herein eupion,
cupion oil, and paraffine, by means of an apparatus consisting of several
boilers or stills working in connection with each other, so that the three
substances are produced by one continuous operation, and in the use, in the
processes of purifying the said oils or substances, when so produced, of common
salt, neutral chromate of potash, and sulphuric acid in combination, and proto-
sulphate of iron, or green vitriol, and carbonate of soda or carbonate of potash
in combination as chemical agents, and in the particular treatment and order

page_text: or purnying processes, which I shan descrive, and which, together with tre
aforesaid combination of chemical agents, produce a better result than has yet
been produced by any of the processes of purification practised or known
hitherto.
י
And in order that the nature of my Invention may be more clearly under-
stood, I will first describe the apparatus by which the distillation is conducted.
Figures 1, 2, and 3 represent a section of three boilers, connected together
and working the one into the other by means of the conduit pipes g, r, w;
Figure 4 represents the condensing or worm tub. e, Figure 1, represents the
body of the first boiler, which should be of cast iron set in brickwork, and
having a groove or annular channel f, f, Figure 1, three inches deep, running
round within the inner circumference of the boiler to receive the condensed
vapours. b, Figure 1, is the outer dome of the boiler, made of copper, and
secured by flanches, bolts, and screws air-tight. c, d, Figure 1, are two smaller
domes, also of copper, placed within the larger dome to condense the heavy
vapours arising from the boiler, and all the condensed vapours sink and are
deposited into the inner circular groove or receptacle f, f, and thence pass into
the second boiler o, Figure 2, by means of the pipe g and spiral worm g¹ (also
of copper). a, Fig. 1, is the boiler head, being a circular vessel fixed over
the outer dome, and containing sand or some other similarly non-conducting
material. h, Figure 1, is a cock to draw off the residuum from the boiler;
o, Figure 2, represents a boiler made of copper, having a circular central
tube z, Figure 2, closed at the top, rising up from the bottom of the boiler,
and passing upwards into the body of the boiler, the more effectually to convey
heat from the heating medium which surrounds the boiler into the substance
under distillation. k, Figure 2, is the outer dome (also made of copper),
secured to the boiler o by flanches, bolts, and screws. b, m, Figure 2, are two
smaller inner domes; n, n, are the annular grooves or channels for receiving
the condensed vapours; i, Figure 2, is a circular vessel containing sand, in the
same manner and for the same purpose as before mentioned with reference to
the arrangement of the chapiter or head of the boiler in Figure 1. r, Figure 2,
is a pipe for conducting the vapours and condensed products (passing from the
boiler o, Figure 2) into the boiler s, Figure 3. p, p, Fig. 2, represents a
larger pan or boiler of cast iron, in which the boiler o, Figure 2, is fixed. The
intermediate space betwixt the two boilers is filled with a fixed oil of high
boiling temperature, or with impure paraffine (hereafter to be described), for
heating the boiler. q, Figure 2, is a cock to draw off the contents of the
boiler. s, Figure 3, is an elliptically-shaped boiler of copper, secured at the
half section by flanches, bolts, and screws; t, Figure 3, is an outer pan, also of

page_text: copper, as a receptacle for steam for heating the boiler s; v is a steam pipe
leading from a common steam boiler for the supply of steam; w is the neck of
the boiler for conveying the vapours arising from it into the copper or lead
worm x, Figure 4, which is surrounded with cold water contained in the tub
for condensing. u, Figure 3, is a cock for drawing off the contents of the
boilers, Figure 3; t is a cock for removing the condensed steam.
For the purpose of obtaining the three several products above named,
(viz.), eupion, eupion oil, and paraffine, by one continuous operation, I fill the
boiler e, Figure 1, to three-fourths of its capacity with the petroleum, and I
heat it very gradually by means of the fire in the fire-place beneath. At the
same time the oil or impure paraffine contained in the vessel p, p, Figure 2, is
heated up to and regularly maintained at a temperature of about four hundred
and fifty degrees Fahrenheit, and steam of about fifteen pounds pressure to the
square inch is at the same time regularly supplied to the still s, Figure 3, by
means of the pipe v. When the heat is thus properly supplied to the three stills,
the distillation is carried on by the aid of the three boilers working at the
same time and in conjunction with each other. In the first part of the distilla-
tion, the more volatile parts of the petroleum, which will be impure eupion,
are first given off in vapour from the body of the petroleum in the still e,
Figure 1, and the greater part of that vapour will not condense in either of the
boilers, but will pass off from the boiler e, through the pipe g into the boiler o,
and from that will rise and pass through the pipe r into the boiler s, and will
pass over from that through the pipe into the worm x, Figure 4, where it
will be condensed into impure eupion, and will be discharged at the worm
end y, Figure 4, into an ordinary receiver A, from which it will be drawn off.
As the distillation is continued, the temperature of the boiler e, Fig. 1, is
gradually raised, and vapour of eupion oil being next chiefly given off, will pass
over into the boiler o, and through that boiler by the pipe r without being
condensed into the boiler s, and will there (by reason of the lower temperature
of that boiler) be condensed in it into eupion oil, which will be drawn off
through the cock u. The yield of impure eupion will gradually diminish as
the distillation proceeds, as will be observed by the discharge at y. Figure 4.
As the distillation continues, the fire under the boiler e, Figure 1, should
be gradually urged until the bottom of the boiler e becomes of a low red heat,
and it should be maintained at about this temperatnre until considerable
quantities of gaseous vapours are discharged at the worm end y, Figure 4,
when the fire of the boiler e should be gradually lowered. During the latter
part of the distillation, large quantities of vapours of paraffine, mixed with other
oils of high boiling temperature, pass off from the boiler e, Figure 1, and are

page_text: condensed in the dome
of the boiler e, Figure 1, and by the curved copper
plates c and d within that dome, and thence will sink into the annular channel
f, f, Figure 1, and flow into the conduit pipe g, and through it into the boiler o,
Figure 2.
At the end of the distillation, the paraffine is drawn off from the boiler o
through the cock q, to be purified in manner herein-after mentioned.
During the process of distillation, above described, it will be found that of
the vapours, which on passing over into the boiler o therein become at first
condensed, those which boil below four hundred and fifty degrees Fahrenheit
will be again converted into vapour, and will then on rising up to the dome
mostly be condensed by means of the dome and curved copper plates k, l, m,
Fig. 2. These condensed vapours will sink into the groove or channel n, n,
Fig. 2, and thence pass into the boiler s, Figure 3, and such portions as boil
below two hundred and twenty degrees Fahrenheit will be vaporized in the
third boiler, and thence pass over into the condensing worm x, Figure 4.
The object of this plan of distillation is to obtain by one continuous process
or operation with three boilers, maintained at the different temperatures indi-
cated, and working at the same time and into each other, first, the discharge
of impure eupion into the receiver A, Figure 4; next, the production of the
impure oil, which I term eupion oil, in the boiler s, Figure 3; and thirdly, the
production of impure paraffine in the boiler o, Fig. 2.
I now proceed to describe the purification of the substances distilled by the
process and apparatus above described.
I purify the impure eupion collected in the receiver A, Figure 4, in manner
following I put about one hundred gallons of impure eupion into a glazed
earthenware or glazed iron pan, enclosed in a steam jacket, heated by steam
to a temperature of about one hundred and twenty degrees Fahrenheit; I
then add to it fifty pounds weight of common salt, fifteen pounds weight of
neutral chromate of potash mixed with three gallons of water; the whole mass
is then to be well agitated; I then add very gradually, during a period of
about one to two hours, four gallons of strong sulphuric acid of commerce, of
specific gravity 1845. The whole is then thoroughly well agitated together for
one hour by means of a series of currents of atmospheric air proceeding
from a perforated coiled pipe of lead placed within the pan at the bottom,
and connected to a powerful blowing instrument of the ordinary construction.
I then allow it to settle for four hours, after which time the mixture of foreign
ingredients will have combined with portions of the impure eupion, and will
have settled at the bottom of the pan, leaving the upper stratum purified
eupion. I then draw off the purified eupion, and put it into the boiler s

page_text: through the moveable coverlid B, which is secured air-tight by means of lute
clamp and screw s, Figure 3, where it is rectified by redistillation by means of
the steam surrounding the lower part of the boiler s, as already described.
The eupion, after such rectification, is then drawn off from the receiver A,
Figure 4, and placed in a wooden or other suitable cistern, and I then add to
every one hundred gallons of the rectified eupion (resulting from the treatment
before mentioned) fifteen pounds of the proto-sulphate of iron (commonly
called green vitriol) dissolved in four gallons of water; the eupion and green
vitriol and water are well agitated together for half an hour; I then add
twenty-five pounds of carbonate of soda or carbonate of potash dissolved in
eight gallons of water. The whole is then thoroughly well agitated together
for one hour, and then allowed to repose for four hours, when the aqueous
solutions will be found at the lower part of the cistern, and the purified eupion
floating on the surface. The eupion thus purified is adapted for the purposes
of illumination, preserving metals from oxydation or corrosion, and other
useful purposes.
I purify the eupion oil or the oil containing eupion with paraffine in solution
produced as already described in the boiler s, Figure 3, in the first distillation,
in manner following: The oil drawn off from the cock u, Figure 3, is put into
an open iron vessel glazed on the inner surface and set in brickwork, and there
the oil is heated and maintained at about two hundred and forty degrees
Fahrenheit, and when so heated I add to every one hundred gallons of the oil
forty pounds of common salt, and twelve pounds of neutral chromate of potash
mixed with two gallons and a half of water; the oil and these added matters
are all well agitated together. I then add very gradually, and at different
times, extending over a period of about from one to two hours, four gallons of
sulphuric acid of commerce, specific gravity 1845; the whole is then well
agitated together for two hours by a proper agitating instrument. I then leave
the oil in contact with the re-agents before mentioned for twelve hours, during
which time the mixture is allowed gradually to cool, and the oil will then be
found floating on the surface, and the re-agents at the bottom. The eupion
oil thus treated is then drawn off and placed in the boiler o, Figure 2, where it
is redistilled over into the boiler s, Figure 3, by means of the oil bath p, p,
Figure 2, heated to four hundred and fifty degrees Fahrenheit, by the fire
beneath the boiler e, Figure 1, being filled with purified paraffine, and the boiler
s, Fig. 3, being filled with purified eupion, the redistillation is carried on
simultaneously, in manner similar to the first process of distilling the crude
petroleum; the oil is then drawn off from the boiler s, Figure 3, through the
cock u, and is then conveyed to a wooden cistern or other suitable vessel,

page_text: where it is mixed with twelve pounds of proto-sulphate of iron (green vitriol)
dissolved in three and a half gallons of water, and these are well and thoroughly
agitated together for a quarter of an hour. I then add twenty-four pounds of
carbonate of soda or carbonate of potash dissolved in six gallons of water, and
when the whole of these materials have been thoroughly well agitated together
for three hours, I allow the entire mass to settle for twenty-four hours; the
eupion oil or oil containing paraffine will have settled at the upper part of the
cistern, and is then drawn off for use, and is adapted to the purposes of illumi-
nation, lubricating machinery, or any other useful purpose to which it may be
applied.
When I desire to obtain an oil containing a large proportion of paraffine, I
draw off direct from the boiler o the impure paraffine or oil highly charged
with paraffine deposited in that boiler during the process of the first distillation
of the crude petroleum, and I purify it by the treatment similar to that already
mentioned in reference to the cupion oil, by means, firstly, of common salt,
neutral chromate of potash, and sulphuric acid; the paraffine, after being
treated by those re-agents, is allowed to settle, and is drawn off and placed
in the boiler e, Figure 1, where it is distilled and condensed in the boiler o,
Figure 2; it is then drawn off by the cock q into a wooden vessel, and the
distillate is there washed with the solution of proto-sulphate of iron and
carbonate of soda or carbonate of potash. The paraffine thus purified should
be then dissolved in the eupion, purified in manner before mentioned, and
when dissolved I mix it with the eupion oil, purified as before mentioned.
I find this mixture of oils (viz.) eupion, eupion oil, and paraffine, mixed
together in the several proportions as yielded by the first distillation, the best
suited for lubricating machinery.
I purify the impure paraffine or paraffine combined with other oils formed
in the boiler o, Figure 2, by the first distillation before described, in mauner
following: I fill the boiler e. Figure 1, to three-fourths of its capacity with
the impure paraffine, I then distil over one half by means of the fire beneath
into the boiler o, Figure 2, and when the one-half part is distilled I draw off the
distillate by means of the cock q. Figure 2, and I mix this first half of the
distilled paraffine with the impure eupion oil obtained by the first distillation;
I then continue the distillation until the remaining half part has been distilled
over; I then draw off this distillate, and place it in an open iron pan lined with
lead, and I then mix with it fifteen pounds of bichromate of potash in fine
powder, and thirteen gallons of sulphuric acid, specific gravity 1845, to every
one hundred gallons of the latter half of the distilled paraffine; I then heat it
to about one hundred and fifty, degrees Fahrenheit, and maintain it at that

page_text: temperature for twenty-four hours; it is agitated for twenty hours, and allowed
to repose for the last four hours, and then allowed to cool. The paraffine,
which will be found on the upper part of the vessel in a compact mass, is then
removed and placed in strong canvass or caya bags, is therein subjected to
a pressure of about one hundred and twenty pounds to the square inch in an
horizontal hydraulic or other suitable press, whereby most of the oily or fluid
part will be expelled, and cakes of paraffine of harder consistence will be
found in the bags.
The pressed cakes of paraffine are then removed from the bags, and are again.
placed back in the open pan, and submitted to the same treatment of mace-
ration (with the bichromate of potash and sulphuric acid), agitation, cooling,
and pressing as before mentioned; and, lastly, the cakes of paraffine are
removed from the bags and placed in a glazed open pan, where it is mixed
with five pounds of proto-sulphate of iron (green vitriol) dissolved in two gallons
of water, and ten pounds of carbonate of soda or carbonate of potash dissolved
in three gallons of water to every nine hundredweight of the paraffine; these
are then well agitated together for two hours at a temperature of about one
hundred and eighty degrees Fahrenheit; it is then allowed to repose at the
same temperature for six hours, when the heat is withdrawn, and the paraffine
allowed to cool gradually, when it is removed, and will be found pure or nearly
so, and fit for use for the manufacture of candles and other useful purposes.
In that part of the processes of purification herein-before described, which
consists of redistillation of the three several products of the petroleum, I have
already partially pointed out, and I wish it to be distinctly understood, that such
redistillation proceeds as the first distillation did, in one continuous operation
in the three boilers, the boilers having been first discharged of their contents
after the first distillation described, and being then charged thus: the boiler e,
with the paraffine partially purified; the boiler o, with eupion oil partially
purified; and the boiler s, with eupion partially purified; and the process of
redistillation goes on in the three boilers at once, by reason and by means of
their different temperatures, as herein-before described; the eupion being dis-
charged into and drawn off from the vessel A; the eupion oil being discharged
into and drawn off from the boiler s; and the paraffine being discharged into
and drawn off from the boiler o.
Having now described the nature of my Invention, and the manner in which
the same is to be performed, I declare that I claim the process or method
which I have described of distilling and redistilling the petroleum or earth oil,
herein-before referred to, and its products, by means of an apparatus composed
of several boilers or stills acting in combination, so as to produce and afterwards

page_text: to redistil the three substances, herein-before described as eupion, eupion oll,
and paraffine, by one continuous operation. I claim the use of an apparatus
composed of several boilers or stills so acting in combination, in the manner
herein-before described. I claim the particular order or series of purifying
processes which I have particularly described; and I claim, as applied to those
processes, the use of common salt and neutral chromate of potash with sulphuric
acid in, combination, and proto-sulphate of iron or green vitriol, and carbonate
of soda or carbonate of potash in combination. I do not claim the distillation
of the earth oil simply, nor the use of boilers or stills used separately, nor any
of the processes of purification described used separately, nor the use of any of
the chemical agents described or referred to in reference to such processes used
separately, but only common salt, neutral chromate of potash, and sulphuric
acid combined, and proto-sulphate of iron or green vitriol. and carbonate of
soda or carbonate of potash combined, nor, save as aforesaid, do I claim any of
the matters or things herein-before described.
In witness whereof, I, the said Stephen White, have hereunto set my
hand and seal, the Ninth day of March, in the year of our Lord One
thousand eight hundred and fifty-seven.
Witness,
JULIAN STEPHEN HAWKINS,
60, Newlands Street, Everton,
Liverpool.
STEPHEN WHITE. (L.S.)