IMPROVEMENTS IN THE METHOD OF PRODUCTION OF DISTILLATES FROM KIMMERIDGE SHALE
Year: 1882

page_text: LETTERS PATENT to Ebenezer Kennard Mitting of Rye in the County of
Sussex, Chemist for an Invention of IMPROVEMENTS IN THE METHOD OF
PRODUCTION OF DISTILLATES FROM KIMMERIDGE SHALE
PROVISIONAL SPECIFICATION left by the said Ebenezer Kennard Mitting
at the Office of the Commissioners of Patents on the 9th August 1882.
EBENEZER KENNARD MITTING of Rye, in the County of Sussex, Chemist
"IMPROVEMENTS IN THE METHOD OR PRODUCTION OF DISTILLATES
KIMMERIDGE SHALE"
FROM
My invention relates to the profitable distillation of bituminous shale known as
Kimmeridge Shale, and has for its object 1st The production of distillates with the
least proportion of permanent gas. 2nd The absorption or decomposition of noxious
bases by the injected aqueous portion of the distillate, which bases otherwise would
be absorbed by the distilled oils, rendering their purification a matter of great
difficulty. 3rd The cooling in closed vessels of the carbonaceous residue after
distillation to prevent absorption of gases from the atmosphere.
I carry my invention into practice as follows :-
:-
The bituminous shale is broken in a stone-breaker or other convenient manner
and placed in retorts, which may be of cast iron and of any suitable shape, arranged
either vertically or horizontally and set in brickwork as is usual. They may be
heated externally by fire or gas.
When the Kimmeridge Shale is thus gradually heated in the closed retorts the
first products of distillation are, Ammoniacal liquor, tar, and a small quantity of
permanent gas. These products are carried off, by a pipe, inserted conveniently at
the back of the retort, which particularly has no greater height than the top of the
retort.
This pipe leads to the coil of a condenser of ordinary construction, but with a
very considerable condensing surface, and a " drag or partial vacuum is created
in it by an exhausting steam jet, or by the usual mechanical gas exhauster.

page_text: The condensed or liquefied products from the condenser are carried off by a
suitable pipe, whilst the gaseous or uncondensed products are carried to a
"scrubber" of ordinary construction, and thence to a gas-holder for lighting or
heating purposes.
As soon as the temperature of the retort has reached from 210° C to 250° C., I
introduce steam into the retort at any convenient pressure; and so regulated in
quantity as not materially to reduce the temperature of the retort. I effect this
by means of a pipe which passes into the retort and is fitted outside with a stop-
cock for regulation. Inside the retort, the pipe is carried round the walls of the
retort in a spiral, zig-zag, or other convenient fashion, from the back to the front, or
from the top to the bottom, for about two-thirds of the length of the retort, so that
the steam may be thoroughly super-heated before escape into the retort. The end
of the pipe is perforated with several holes for the steam exit; or the steam may
be superheated before admission to the retort.
The steam is injected at this period of the distillation, and during the remainder
of the operation, in order to assist the distillation and to absorb or decompose
certain noxious bases and carry them over in solution, which otherwise would be
taken up by the distilled oils, rendering their purification a matter of great
difficulty.
When the temperature of the retort has reached a dull red heat, it will be found
that Tar ceases to come over, and the operation is then complete. The retort is
allowed to cool below visible red heat, and the carbonaceous residue is quickly
withdrawn and the retort recharged for another operation.
For receiving the carbonaceous residue I employ vessels, conveniently cylinders
of sheet iron, and closed with tightly fitting lids. The residue must be quickly
drawn from the retort into such a cylinder, to prevent contact with the atmosphere
and consequent absorption of gases and impurities during cooling. The retorts
may be arranged so that the process is continuous i.e. the shale may be fed in at
one end, and the carbonaceous residue taken out at the other.
By means of this apparatus and working in the manner described, I obtain a
large percentage of crude tar available for the manufacture of volatile spirit; also
oils free from noxious impurities for lubricating;-also wax for candles and other
purposes; Ammoniacal liquor for the manufacture of Ammonia salts ;-permanent
gas for lighting and heating;-and lastly, carbonaceous residue in a porous and
comparatively pure condition, especially well adapted for Filtration and disinfecting
purposes.

page_text: :
SPECIFICATION in pursuance of the conditions of the Letters Patent filed
by the said Ebenezer Kennard Mitting in the Great Seal Patent Office on the
9th February 1883.
EBENEZER KENNARD MITTING, of Rye, in the County of Sussex, Chemist,
"IMPROVEMENTS IN THE METHOD OF PRODUCTION OF DISTILLATES' FROM
KIMMERIDGE SHALE"
My invention relates to the profitable distillation of bituminous shale, known as
Kimmeridge shale, and has for its objects :-First, The production of distillates
with the least proportion of permanent gas. Second, The absorption or decom-
position of noxious bases by the injected aqueous portion of the distillate, which
bases would otherwise be absorbed by the distilled oils, rendering their purification
a matter of great difficulty. Third, The cooling in closed vessels of the
carbonaceous residue after distillation, to prevent absorption of gases from the
atmosphere.
I carry my invention into practice as follows :—
The bituminous shale is broken in a stone-breaker or other convenient manner,
and placed in retorts, which may conveniently be of cast iron, and of any suitable
shape, arranged either vertically or horizontally, and set in brickwork as is usual;
and is heated externally.
When the Kimmeridge shale is thus gradually heated in the closed retorts, the
first products of distillation are Ammoniacal liquor, tar, and a small quantity of
permanent gas. These products are carried off by a pipo, inserted conveniently at
the back of the retort when this is arranged horizontally. This orifice is preferably
placed at a low level.
This pipe leads to the coil of a condenser of ordinary construction, but with a
very considerable condensing surface, and a "drag" or partial vacuum is used in it,
created conveniently by an exhausting steam jet, or by the usual mechanical gas
exhauster, or other means.
The condensed or liquefied products from the condenser are carried off by
a suitable pipe, whilst the gaseous or uncondensed products are carried to a
"scrubber" of ordinary construction, and thence to a gasholder for lighting or
heating purposes.
:
As soon as the temperature of the retort has reached from 210° C. to 250° C., I
introduce steam into the retort at any convenient pressure, and so regulated in
quantity as not materially to reduce the temperature of the retort. I effect this
by means of a pipe, which passes into the retort, and is fitted outside with a stop
cock for regulation. Inside the retort the pipe is carried round the walls of the
retort in a spiral, zig-zag, or other convenient fashion, from the back to the front,
or from the top to the bottom, for about two thirds of the length of the retort, so
that the steam shall be thoroughly superheated before escape into the body of the
retort. The end of the pipe is perforated with several holes for the steam exit.
Alternatively, the steam may be previously superheated and directly admitted to
the retort, though I prefer the former method of heating in the coiled pipes.
The steam is injected at this period of the distillation, and during the remainder
of the operation, in order to assist the distillation, and to absorb or decompose
certain noxious nitrogenous bases such as the pyridine series and its homologues,
and to carry them over in solution. This treatment prevents their being taken up
by the distilled oils, and renders their purification a matter of much less difficulty.
In practice I find this adds to the quantity of ammonia in the aqueous portion of
the distillate,

page_text: When the temperature of the retort has reached a dull red heat, it will be found
that tar ceases to come over. The operation is then complete. The retort is now
allowed to cool below visible red heat, and the carbonaceous residue is quickly
withdrawn, and the retort charged for another operation.
For receiving the carbonaceous residue, I employ vessels, conveniently cylinders
of sheet iron, closed by tightly fitting lids. The residue must be quickly drawn
from the retort into such cylinders, to prevent contact with the atmosphere, and
consequent absorption of gases or impurities during cooling.-The retorts may be
arranged so that the process is continuous, i.c. the shale may be fed in at one end
or the top, while the carbonaceous residue is withdrawnat the other end or the
bottom.
By working in the manner described I obtain a large percentage of crude tar,
available for the manufacture of volatile spirit; oils, free from noxious impurities,
for lubricating etc.; wax for candles or other purposes; Ammoniacal liquor for the
manufacture of Ammonia salts; permanent gas for lighting or heating; and
carbonaceous residue in a porous and comparatively pure condition, especially well
adapted for filtration and disinfectant purposes.
Having now fully described and ascertained the nature and objects of my
invention and the manner of its performance, be it known that what I consider
novel and desire to protect by my Letters Patent is :-
First. The process of distillation of Kimmeridge shale by the introduction of
superheated steam when the retort is at a temperature of 210° C. to 250° C., to
effect the decomposition or absorption of various nitrogenous bases, and to add to
the quantity of ammonia in the aqueous portion of the distillate, substantially
as specified.
Second. The cooling of the carbonaceous residue in closed chambers or vessels
distinct from or forming part of the distilling retort, to prevent access of the
atmosphere or other gases, substantially as specified.
"
Third. The combination in a Kimmeridge shale distilling retort of a large
surfaced condenser, with a vacuum drag to produce the least proportion of
permanent gas in the first portion of distillate, substantially as specified.
In Witness whereof I the said Ebenezer Kennard Mitting have hereunto set
my hand and seal this seventh day of February in the year of our Lord
One thousand eight hundred and eighty-three.
Signed sealed and delivered by the
above named Ebenezer Kennard
Mitting in the presence of
FRED ATKINSON
Solicitor Rye.
EBENEZER KENNARD MITTING (L.S.)