AN IMPROVED METHOD OF TREATING COAL AND BITUMINOUS SUBSTANCES, AND FOR IMPROVEMENTS IN THE TREATMENT OF THEIR VOLATILE PRODUCTS
Year: 1853

page_text: LETTERS PATENT to William Brown, of the City of Glasgow,
Merchant, for the Invention of "AN IMPROVED METHOD OF TREATING
COAL AND BITUMINOUS SUBSTANCES, AND FOR IMPROVEMENTS IN THE
TREATMENT OF THEIR VOLATILE PRODUCTS.
Sealed the 16th March 1853, and dated the 13th January 1853.
PROVISIONAL SPECIFICATION left by the said William Brown
at the Office of the Commissioners of Patents, with his Petition,
on the 13th January 1858.
I, WILLIAM BROWN, of the City of Glasgow, Merchant, do hereby
declare the nature of the said Invention for "AN IMPROVED METHOD
OF TREATING COAL AND BITUMINOUS SUBSTANCES, AND FOR IMPROVEMENTS IN
THE TREATMENT OF THEIR VOLATILE PRODUCTS," to be as follows:-
It is well known to chemists and others that coal and other bitu-
minous substances distilled at a red heat suffer decomposition, and are
resolved into fixed and volatile compounds; the former consisting of
coke and ashes, the latter of gas and tar, which tar is known to contain
various compounds to which the names naptha, eupion, paraffine, &c.
have been given by chemists; and it has been found that the proportion
of these compounds capable of being produced from a given quantity of

page_text: coal or bituminous substances is much affected by the nature of the
process of distillation. Thus with a rapid operation and low tempera-
ture much volatile matter can be obtained; but with a slow operation
and high temperature little else than gas results. To hit the precise
point between these extremes is almost impossible in practice, and
hence great loss and destruction are produced by the process now in
use for obtaining the oily or volatile compounds derived from coal and
bituminous substances.
.
Now the first part of my Invention consists in an improved mode of
distilling coal and bituminous substances so as wholly or in great part
to prevent the decomposition of the volatile compounds alluded to
above. And the nature of my said Invention is as follows:-Having
provided a retort similar to those used in gas works, or of any other
convenient form, this retort is fixed or set in a furnace in such a
manner that a pipe or tube may be passed either within or without
the retort from its mouth to its farther end, and fixed so that it
terminates or opens into the furthest end of the retort, its other end
being without or exterior to the furnace as shown in the accompanying
Drawing. By this arrangement the tube is heated red hot when the
furnace is in action, and consequently if a current of steam be then
propelled through the tube it must become heated to a red heat ere
it leaves the tube to enter the retort. Now if we imagine that the
furnace and retort are in action, and have been charged with coal or
bitumen, and a current of steam is transmitted through the tube at the
time, it follows that the volatile products of the coal or bitumen will
be swept out of the retort as fast as they are formed, and carried at
once into the condenser, thus preventing their destruction in the retort
from the continued action of the fire. And in fact it has been found
that whereas by the greatest care no more than from 28 to 30 per cent.
in weight of volatile compounds can be obtained without steam from a
ton of coals, I find that more than 40 per cent. is easily procured by
my new process of the application of steam as above described; the
steam being generated in the first instance either by the waste heat of
the furnace or by a separate furnace applied to a steam boiler, and
in either case transmitted rapidly through the retort.

page_text: The second part of my Invention consists in an improved mode of
purifying the volatile products or oily substances which result from the
first operation. These are redistilled at a lower temperature with steam,
but previous to such redistillation they are subjected to the action of sul-
phuric acid and peroxide of manganese in the proportion of about 10 per
cent. by weight of sulpuric acid, and 5 per cent. of peroxide of man-
ganese. After standing for a few minutes, the defecated oil is poured
off and distilled with steam as previously indicated, and this and the
application of the acid and manganese are repeated until the oil becomes
pure, after which it is treated in the usual way with an alkaline solution
and rendered fit for the market. And it must be observed, that since
during these redistillations the oily matter is separated into oily fluids
of different degrees of volatility, these different fluids are to be collected
separately at three different periods of the distillation, so as to obtain..
first, a light volatile oil; secondly, a heavy and loss volatile oil; and
thirdly, a heavy fatty oil, which, like butter, solidifies in cooling. From
the last paraffine may be obtained by pressure in a proper press, as is
well understood, and after this it must be purified by the action of
sulphuric acid at a boiling temperature which will be from 400° to
600° Fahr according to its purity.
SPECIFICATION in pursuance of the conditions of the Letters Patent,.
filed by the said William Brown in the Great Seal Patent Office
on the 12th July 1853.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I,
WILLIAM BROWN, of the City of Glasgow, Merchant, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her
Letters Patent, bearing date the Thirteenth day of January, in the
year of our Lord One thousand eight hundred and fifty-three, in the six-
teenth year of Her reign, did, for Herself, Her heirs and successors, give
and grant unto me, the said William Brown, Her special license that I;
the said William Brown, my executors, administrators, and assigns, or
such others as I, the said William Brown, my executors, administrators,
and assigns, should at any time agree with, and no others, from time to
:

page_text: 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 OF TREATING COAL AND
BITUMINOUS SUBSTANCES, AND FOR IMPROVEMENTS IN THE TREATMENT OF
THEIR VOLATILE PRODUCTS," upon the condition (amongst others) that I,
the said William Brown, by an instrument in writing under my hand
and seal, should partically 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 immediately after the date of the said.
Letters Patent.
NOW KNOW YE, that J, the said William Brown, do hereby declare
the nature of the said Invention, nda in what manner the same is to be
performed, to be particularly described and ascertained in and by the
following statement thereof (that is to say):
The first operation consists in distilling the coal or other bituminous
matter in conjunction with steam at a dull red heat, for which purpose
the coal or other bituminous matter is introduced into a retort fitted
with a steam pipe so situated as to become red hot by passing through
the furnace. This steam pipe terminates in the closed end of the retort,
so that when the retort is charged with coal or other bituminous
matter, and the furnace is in action, the steam pipe becomes red hot,
and steam being then passed along it, this also becomes red hot, and
in this state enters the end of the retort, and rapidly unites with and
expels the volatile matters arising from the coal or other bituminous
matter, by which their decomposition into gas is wholly or in great
measure prevented, and the amount of oily or condensible product
greatly increased. The annexed Drawing shews the disposition of the
retort and steam pipe allude to, or I pass the steam pipe through
a furnace distinct and separate from that which heats the retort, so
that I am enabled to withdraw the fire from the retort or diminish its
intensity at pleasure, without altering the temperature of the steam
pipe, by which means I can continue the distillation of the coal or
bituminous matter either altogether or in part with the retort at a

page_text: temperature below that of a dull red heat. The steam pipe may be of
cast iron, or of cast or wrought iron, glazed or enamelled, as it is
termed, or it may be of clay or earthenware. In distilling, I employ
a condenser as is usual, the temperature of which should not be lower
than 50° of Fahrenheit.
Having by this means obtained a quantity of volatile products from
coal or other bituminous matter, these are again subjected to dis-
tillation in a still or other convenient vessel, with or without the
employment of a steam pipe, though I prefer to use steam when a
large amount of paraffine is required, but where the production of oil
is the chief object steam may be dispensed with.
When steam is
used, this is to be brought into the still in a superheated state, by
passing it through a red hot steam pipe disposed in the furnace or flue
of the furnace which heats the still. The steam enters through the
upper part of the side of the still as shewn below, and promotes as
before the distillation of the volatile matters, whilst it rotards their
destruction or conversion into gaseous or other worthless compounds.
By this means the paraffine and heavy hydro-carbonaceous oils are.
preserved.
.
During the progress of the second distillation, it will be observed,
that the products vary at different periods of the distillation, and these
are therefore to be kept separate or received in different vessels. At
first a thin oil or impure cupione oil comes over to the extent of about
one eighth of the total fluid employed; after this a thicker and heavier
oil containing paraffine makes its appearance to the extent of from
forty to fifty per cent. of the fluid employed; and, lastly, a thick butyra-
ceous matter is evolved, consisting chiefly of paraffine, but mixed with
heavy oil; and this continues to the end of the operation, and con-
stitutes about one fourth of the bulk of the fluid originally used.
These three products are treated as follows:-The impure eupione oil
is mixed with from five to ten per cent. of its weight of oil of vitriol or
sulphuric acid to, which an equal bulk of water is added. Bichromate
of potash is next thrown in, equal in weight to one half of the sulphuric
acid employed. The whole is then heated in any convenient vessel of.
wood or lead or earthenware, and during the heating the materials

page_text: are diligently stirred together. As soon as the temperature has
reached 212° Fahrenheit the. heating means may be withdrawn, and
the whole permitted to cool and settle. The cupione oil is next to be
decanted from the acid fluid, and treated with a warm solution of
caustic soda, the whole being well mixed and afterwards left at rest
for some time to settle. Lastly, the cupione oil is decanted from the
alkaline fluid, and distilled either alone or with water or steam, as is
practised with respect to volatile oils generally.
The heavy oil containing paraffine is next treated either with strong
sulphuric acid and peroxide of manganese in the proportion of ten
per cent. of acid, and five per cent. of peroxide of manganese; or, what
I prefer, it is subjected like the eupione oil to the action of sulphuric
acid and bichromate of potash in the same manner and proportion as
indicated for the eupione oil, after which it is treated with soda ley, and
allowed to settle exactly as explained with regard to the cupione oil.
The heavy oil is then decanted and distilled in the usual way, the first
portions being added to the eupione oil, as consisting chiefly of that
substance; the second, and by far the larger portion of the whole, is
received apart under the name "lubricating oil," whilst the last por-
tions being thick and of the consistence of butter are mixed with the
impure paraffine which results. from the third stage of the second
distillation of the crude products, and which are next treated as
follows-Having allowed the impure paraffine to remain for twenty-
four hours or longer in a cool place to crystallize, the oily mixture is
placed in a bag or filter, similar to those in use for the separation of
spermaceti from sperm oil.. .When the oily fluid has drained away, the
paraffine must be removed to a press, and subjected to severe pressure,
as is practised with respect to stearic acid. by the makers of that sub-
stance; it must then be melted, and when cold again pressed; the oil
being in both cases added to the drainings, which are to be treated
as explained under the head heavy or lubricating oil. The paraffine
must now be melted, and the heat raised to about 400° Fahrenheit.
when strong sulphuric acid is to be carefully stirred into it in the pro-
portion of from one twentieth to one tenth of the weight of paraffine
operated upon.
After boiling for a few minutes, the fire must be

page_text: withdrawn, and the charred oil of the paraffine allowed to settle in
the form of a black powder from the melted paraffine. This being
separated, the paraffine must be boiled in water, or in a weak solution
of soda, after which it may be cooled, and is fit for the market.
I claim, first, the use of steam heated as indicated for the purpose
indicated.
Secondly, I claim the mode or modes described of purifying the
eupione oil, lubricating oil, and paraffine, obtained by the process or
processes above described.
In witness whereof, I, the said William Brown, have hereunto
set my hand and seal, this Eleventh day of July, in the year
of our Lord One thousand eight hundred and fifty-three.
indicated.
Secondly, I claim the mode or modes described of purifying the
eupione oil, lubricating oil, and paraffine, obtained by the process or
processes above described.
In witness whereof, I, the said William Brown, have hereunto
set my hand and seal, this Eleventh day of July, in the year
of our Lord One thousand eight hundred and fifty-three.
Witness,
S. CARPMAEL.
WILLIAM BROWN. (L.s.)