IMPROVEMENTS IN THE COKING OF PITCH, AND IN THE MANUFACTURE OF SOLID HYDROCARBONS THEREFROM.
Year: 1872

page_text: LETTERS PATENT to Ernst Friedrich Richard Lucas, of Pennfields,
Wolverhampton, in the County of Stafford, Chemist, for the In-
vention of "IMPROVEMENTS IN THE COKING OF PITCH, AND IN THE
MANUFACTURE OF SOLID HYDROCARBONS THEREFROM.'
"
Sealed the 9th July 1872, and dated the 11th March 1872.
t
PROVISIONAL SPECIFICATION left by the said Ernst Friedrich Richard
Lucas at the Office of the Commissioners of Patents, with his
Petition, on the 11th March 1872.
I, ERNST FRIEDRICH RICHARD Lucas, of Pennfields, Wolverhampton,
in the County of Stafford, Chemist, do hereby declare the nature of the
said Invention for "IMPROVEMENTS IN THE COKING OF PITCH, AND IN THE MANU-
PACTURE OF SOLID HYDROCARBONS THEREFROM," to be as follows:-
The first portion of this Invention relates to the treatment of pitch for
the purpose of producing coke of a superior quality therefrom. Pitch
is distilled in a muffle oven built of fire-bricks, and constructed in a

page_text: similar manner to a blind salt cake roaster, the bottom of the same being
heated by a number of flues, as well known and understood. The oven
as thus constructed is provided on opposite sides thereof with working
doors which are closed in an air-tight manner during the first part of the
process, which is the distillation of the oil. On the top of the oven are
a man-hole, iron pipes which convey the oil vapours into a condenser, an
opening which is closed with an iron door nearest to the firc-place, and
which connects by means of a flue the fire-place with the interior of the
oven, and a similar opening at the other end which is also closed by a
door, and which connects the interior of the oven with the main flue.
For the purposes of this Invention the oven is worked in the following
manner: The oven is charged with pitch in lumps (the quantity thereof
varying in proportion to the size of the oven) through the working
doors, or through the man-hole in the top of the oven, or the pitch is
run in a molten state through a tap. The fire is then lit and the
distillation soon commences. As soon as the distillation of the oil ceases,
the doors of the two openings at the top of the oven which connect the
interior thereof with the main flue and with the fire-place are opened.
The flame, heat, and gases derived from the fuel pass through the oven
and produce a coke of good quality. The working doors may be opened
and the coke occasionally raked about, so that all parts thereof may
come in contact with the heated gases until the coking process is
completed. The coke is then drawn from the oven through the
working doors and the oven charged again.
The second part of this Invention relates to the manufacture of solid
hydrocarbons. Coke oil or pitch oil obtained by the distillation of pitch
(either as it comes from the condensing pipes or after it has been
redistilled) is mixed in an agitator with naphtha, light oil, creosote oil,
or any other mineral oil until the gravity of the mixture is from 16° to
24° Twaddle, or until the mixture has the proper consistency for being
pressed. It is then well agitated and allowed to settle, or the mixture
is heated until all solid parts are dissolved and then cooled and
crystallised. The mass is afterwards filtered and subjected to the action
of a hydraulic press. The press cake thus obtained consists of a
mixture of solid hydrocarbons, mostly consisting of chrysene and
anthracene. In order to separate these hydrocarbons the press cake
is dissolved by heat in naphtha, light oil, creosote oil, or any other
mineral oil, and allowed to cool and crystallise, or the press cake is

page_text: mixed with a sufficient quantity of suitable mineral oil or oils to dissolve
the anthracene. The crystals of chrysene are separated from the liquid
by filtering and then subjected to pressure in a hydraulic press, the
press cake thus obtained consisting of crude chrysene. The quantity of
mineral oils necessary to be used will vary according to the quantity
of chrysene in the press cake. The liquid oil from the filter and press.
containing the anthracene and similar hydrocarbons is submitted to
distillation, either with or without the addition of superheated steam,
until anthracene begins to distil over. The fire may then be drawn and
the oil run off from the still and cooled, or the distillation may be
carried on until only coke remains in the still. The product obtained,
being the distillate containing the anthracene or the "bottoms" from
the still, is cooled and pressed in a hydraulic press, the press cake thus
obtained being crude anthracene, which may be purified in the usual
way.
SPECIFICATION in pursuance of the conditions of the Letters Patent,
filed by the said Ernst Friedrich Richard Lucas in the Great Seal
Patent Office on the 10th September 1872.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, ERNST
FRIEDRICH RICHARD LUCAS, of Pennfields, Wolverhampton, in the
County of Stafford, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her
Letters Patent, bearing date the Eleventh day of March, in the year
of our Lord One thousand eight hundred and seventy-two, in the thirty-
fifth year of Her reign, did, for Herself, Her heirs and successors, give
and grant unto me, the said Ernst Friedrich Richard Lucas, Her special
licence that I, the said Ernst Friedrich Richard Lucas, my executors,
administrators, and assigns, or such others as I, the said Ernst
Friedrich Richard Lucas, 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 "IMPROVEMENTS IN THE COKING OF PITCH, AND IN

page_text: THE MANUFACTURE OF SOLID HYDROCARBONS THEREFROM," upon the condition
(amongst others) that I, the said Ernst Friedrich Richard Lucas, my
executors or administrators, by an instrument in writing under my, or
their, or one of their hands and seals, 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 immediately
after the date of the said Letters Patent.
NOW KNOW YE, that I, the said Ernst Friedrich Richard Lucas, do
hereby declare the nature of my said Invention, and in what manner
the same is to be performed, to be particularly described and ascertained
in and by the following statement, that is to say :—
The first portion of my said Invention relates to the treatment of
pitch for the purpose of producing coke of a superior quality therefrom.
The pitch is distilled in a muffle oven built of fire-bricks, bound with
iron plates. I have found that a suitable oven for this purpose is one
constructed in a similar manner to a blind salt cake roaster, the bottom
of the oven being heated by a number of flues on the bottom thereof.
This method of heating has been suggested and practised before, but
the coke obtained in the ordinary ovens is not of a good quality,
whereas I obtain coke of a very superior description by the use of an
oven such as herein described, and by conducting the flame and heat
of the fuel in a direct manner through the said oven after the distillation
of the coke oil has ceased. On two opposite sides of the oven are
working doors which are closed in an air-tight manner during the first
part of the operation, that is to say, the distillation of the oils. On the
top of the oven is a man-hole, iron pipes which convey the oil vapours
into a condenser, an opening which is closed with an iron door nearest to
the fire-place and which opening connects by a flue the fire-place with
the interior of the oven. A similar opening closed with an iron door
is provided at the other end of the top of the oven, and which connects
the interior of the oven with the main flue.
For the purposes of this Invention the oven is worked in the follow-
ing manner: The oven is charged with pitch in lumps (the quantity
of the charge varying with the size of the oven, as will be well under-
stood) through the working doors, or through the man-hole on the top
of the oven, or the pitch may be run into the oven in a molten state

page_text: through a tap provided for that purpose. The fire having been lighted,:
the distillation soon commences. In order to prevent the condensing,
pipe becoming choked, especially in cold weather, a small jet of. steam
may be injected into the same. When the distillation ceases, the doors:
of the two openings in the top of the oven which connect the interior
thereof with the main flue and with the fire-place are opened. To avoid.
an explosion, care must be taken to close the condensing pipe by means
of a tap or a water joint before the doors which connect the interior of >
the oven with the main flue and the fire-place are opened. The flame,
heat, and gases derived from the fuel now pass through the oven and
produce a good coke. In this part of the operation, the working doors:
may be opened and the coke occasionally raked about so that all parts
of the same may come in contact with the hot gases until the coking
is complete, or as soon as the distillation of the oil ceases the condensing ›
pipe is closed, the working doors opened, and the vapours contained in
the oven ignited. The two doors of the openings which connect the
interior of the oven with the main flue and with the fire-place are then
opened and heat applied until the coking is concluded.
I should here observe that I do not claim the construction of the
oven employed as above mentioned for the purposes of my said In-
vention, as the same may be altered and varied without interfering
with the methods of treatment of pitch before described.
The second part of my said Invention relates to the manufacture of,
solid hydrocarbons. The coke oil or pitch oil obtained by the dis-
tillation of pitch (as before described), either as it comes from the
condensing pipe or after it has been re-distilled, is mixed in an agitator
with naptha, light oil, creosote oil, or any other mineral oil, until the
mixture has a gravity of 16° to 24° Twaddle, or until the mixture has
the proper consistency for being pressed; and the whole is then well
agitated and allowed to settle, or the mixture is heated until all solid
parts thereof are dissolved and then allowed to cool and crystallize.
The mass is now filtered, and then pressed in a hydraulic or other
suitable press. The press cake thus obtained consists of a mixture of
solid hydrocarbons, mostly of chrysen and anthracene.
In order to obtain crude chrysen and anthracene from this mixture
of solid hydrocarbons I proceed as follows:-I dissolve the press cake
by means of heat in naptha, light oil, creosote oil, or any other mineral
oil, using for this purpose as much naptha or oil as may be necessary.
1

page_text: for the dissolving of the press cake. I have found that about five gallons
of naptha or oil to ten pounds of press cake suitable proportions for this
purpose. When the press cake is dissolved I allow the mixture to cool,
and the chrysen thus to crystalize; or I mix the press cake with a
sufficient quantity of mineral oils to dissolve the anthracene. The
crystals of chrysen are separated from the liquid by filtering, and then
pressed in a hydraulic or other suitable press, the press cake thereby
obtained being a "crude chrysen." The quantity of mineral oils used
varies according to the quantity of chrysen in the press cake. The
liquid oil from the filter and press containing the anthracene and other
similar hydrocarbons is submitted to distillation, either with or without
the addition of superheated steam, until anthracene begins to distil over.
The fire may now be drawn from the still and the still allowed to cool,
or the distillation may be carried on until only coke remains in the still.
The product obtained, that is to say, the distillate containing the
anthracene or the. "bottoms " from the still is cooled, and then
pressed by hydraulic or other suitable
pressure, the press cake
obtained being "crude anthracene," which may be purified in the

page_text: And, Secondly. The modes or methods herein-before set forth and
lescribed for the manufacture of solid hydrocarbons, or any mere modi-
ications of the same modes or methods.
In witness whereof, I, the said Ernst Friedrick Richard Lucas,
have hereunto set my hand and seal, this Seventh day of Sep-
tember, in the year of our Lord One thousand eight hundred and
seventy-two.
ERNST FRIEDRICH RICHARD LUCAS. (L.S.)