AN IMPROVED METHOD OR PROCESS OF DISTILLATION AND APPARATUS THEREFOR to be as follows:
Year: 1884

page_text: [Communicated from abroad by Messrs. Wirth & Company, of Frankfort on the
Main, in the Empire of Germany, acting as Agents of Doctor Franz König,
of Asti, in the Kingdom of Italy, Director of the Royal Oenological Assaying
Institution.]
I WILLIAM ROBERT LAKE of the firm of Haseltine Lake & Co Patent Agents
Southampton Buildings in the County of Middlesex do hereby declare the nature
of my invention for "AN IMPROVED METHOD OR PROCESS OF DISTILLATION AND
APPARATUS THEREFOR to be as follows:-
"
This invention relates to the distillation of liquids, and to apparatus therefor,
and is applicable in all cases where liquids having different boiling points are
required to be separated by fractional distillation, such as, for instance, to operations
carried on in braudy, spirit, petroleum, tar, and other distilleries.
According to the said invention the vapours of the boiling liquids are passed
through one or more chambers which are filled with substances such as stones,
pieces of metal, glass or porcelain, metallic wire, glass pipes, coke, or pumice stones,
Upon these substances which offer a great surface to the said vapours, condensation
takes place, the vapours of the least vaporizing liquid condensing first.
By reason of the intimate and extensive contact of the vapours with the liquid a
further separation of fluids having different boiling points is effected. The condensed
portions of the vapours of the least vaporizing liquids run back into the still or into
a rectifier which is placed between the still and the said chambers. The remaining
vapours then pass to the refrigerator where they are condensed. The above
mentioned receivers coutaining the cooling substances may, when necessary, be
cooled externally.
The process heretofore employed consisting in conveying alcoholic vapours
through a chamber containing small pieces of charcoal, has nothing in common with
the present process, as charcoal was only employed as means for freeing the alcohol
from fusel oil and could not be as efficiently used in the above described process as
other substances reduced to small pieces.
By combining in this new process, the rectification and dephlegmation operations
in a simple and suitable manner I am enabled to substitute for the complicated and
expensive apparatus heretofore employed, a much simpler and cheaper apparatus,

page_text: the operation of which is equivalent to that of the former and permits a considerable
reduction in the outlay required to construct such apparatus and also a saving of
time and fuel.
In constructing apparatus serving for the distillation of spirit according to this
invention I provide a still which is heated in the ordinary manner and to which is
connected a cylinder filled with suitable cooling substances. The said cylinder is
provided with an aperture at its side closed by a cover, and serves for the removal
of the said substances after the distillation is terminated. Upon the still is mounted
a rectifier. To the upper end of the cylinder is connected a pipe which leads into
the said rectifier at the lower part and has connected with it a perforated pipe
through which the vapours enter and come into intimate contact with the condensed
liquid in the rectifier.
At the upper extremity of the rectifier is arranged a second cylinder similar to
the first mentioned cylinder and filled with the same kind of substances as the
latter; the upper extremity of this cylinder is connected with a second rectifier by
means of a pipe provided at one end with perforations.
→
Upon the second rectifier is arranged a third cylinder filled with the same kind
of substances as the first and second cylinders, and the upper end of which is
connected with an ordinary refrigerator or cooling apparatus.
The still is supplied with alcohol or other liquid through a suitable aperture near
its top, the residues of which liquid, at the termination of the distillation, are
allowed to escape through a cock at the lower part thereof. The condensed liquids
in the rectifiers, which contain a certain amount of alcohol, are allowed to run back
into the still by raising valves in the bottom thereof, and are redistilled with a fresh
portion of liquid.
By using this apparatus it is easy (even from fermented mash) to produce rectified
alcohol of from 90 to 93 degrees in a proportionately shorter time and with a less
expense of heat than by any other apparatus.
The operation of this apparatus is greatly enhanced when, instead of one cylinder
being arranged upon the still, two or more are employed and communicate with the
perforated pipe. The number of cylinders, may be increased as desired.
By cooling, the concentration of the alcohol can be raised to from 95 to 90
degrees. The cooling may be effected, by surrounding the third cylinder with a
casing and filling the space between the said cylinder and casing with small pieces
of any suitable material. The cold water enters the said space at the top and runs
out through the pipe connected to the bottom.
In the distillation of petroleum, only one cylinder mounted upon the still and
filled with the cooling substances is necessary in order to obtain a sufficient
separation of the component parts of different liquids.
In most cases the arrangement of three cylinders will suffice; there is however
no objection to arranging a fourth cylinder when required.
The above described apparatus may be varied as regards form, and dimensions
without departing from the nature of the said invention. This process may also be
applied to apparatus heretofore employed, for instance upon the main column or
still in apparatus used for the distillation of alcohol may be placed a cylinder filled
with any of the above mentioned substances, the other parts of the apparatus being
retained.
HASELTINE, LAKE & Co.,
For the Applicant.

page_text: I WILLIAM ROBERT LAKE, of the firm of Haseltine, Lake, and Co Patent
Agents, Southampton Buildings, in the County of Middlesex do hereby declare the
nature of my invention for "AN IMPROVED METHOD OR PROCESS OF DISTILLATION,
AND APPARATUS THEREFOR," and in what manner the same is to be performed,
to be particularly described and ascertained in and by the following statement:-
This invention relates to the distillation of liquids, and to apparatus therefor.
The process hereinafter described and the apparatus required for carrying the
same into effect can advantageously be employed in the following branches of
industry.
1st In the manufacture of brandy, raw and distilled spirit.
2nd In the production of wood spirit (methyl alcohol).
3rd In the manufacture of ether, and for the production of other neutral, volatile
bodies, such as ethyl bromide.
4th For the separation and production of the ingredients of fusel oils.
5th In the fractional distillation of petroleum.
6th For the separation and production of the pure ingredients of coal-oils (benzol,
toluol, phenol, etc) and their derivatives, and
7th For the extraction of ammonia and ammonia salts from gas-water, urine and
other refuse.
The process is as follows: The vapours of boiling mixtures are passed through
one or more chambers of suitable form (having one or more partitions in the
interior), the said chambers containing divided substances which are unaffected
by the vapours, such as stones or pieces of metal, fragments of glass or porcelain,
pieces of glass or metal tubing, pieces of coke or pumice stone, metallic wire,
small pieces of wood or cork, vegetable fibres, etc. Upon these substances which
present a very large surface to the vapours, condensation takes place, so that.
the less volatile portions thereof condense and flow back into the still.
By reason of the extremely intimate contact between the vapours and the
condensed liquid a most thorough separation of fluids having different boiling
points takes place, so that the vapours of the more volatile substances to be
extracted, having passed a sufficiently high layer of the divided substances, enter
the cooler or refrigerator in a very pure state.
In a few cases, say with substances boiling at high temperatures, the cooling of
the chambers by the exterior air is sufficient; but in the greater number of cases
and in the most important ones, such as in the extraction of alcohol, a thorough
cooling is very essential for the process, if the distillation is carried out on a large
scale and the chambers are of considerable height, or when several of them are
employed. This cooling is preferably effected internally by tubes placed in contact
with the divided substances through which tubes passes the cooling fluid. The said
chambers having the divided substances can also be cooled, if necessary externally
by means of a jacket through which a cooling agent flows.

page_text: In order that my invention shall be well understood I will proceed to describe
an apparatus which serves for carrying the said invention into practice.
The drawing illustrates several modifications of the said apparatus all as herein-
after described.
In suitable connection with a distilling vessel (with or without a singlings (low
wine) receptacle, for periodical or continuous distillation), is placed the dephlegmator
or rectifying column A (Figure 1) which is a chamber having the form of a column.
This column has a perforated bottom, and contains in its interior fragments or
pieces of material as before described. .
A lateral opening 8 is provided at the lower end and is closed by a lid. This
opening enables the filling material to be removed from the chamber when it is to
be replaced by fresh filling material as before described.
For cooling the divided substances, within the chamber one or more tubes m
extend in numerous convolutions, the diameters of which alternately increase and
diminish through the column. Through the said tube or tubes passes the cooling
fluid from above downwards.
Inasmuch as dephlegmation predominates above, whilst rectification prevails
more and more towards the bottom, the cooling tubes need not necessarily extend
to the lower end of the dephlegmator or rectifying column. The convolutions can
advantageously be made to incline slightly towards one side, in order to prevent
the ascent of the lower layers of the cooling liquid which are first heated.
If the incrustation of the internal walls of the cooling tube by salts of lime is
to be obviated, boiled water, rain-water, distilled water, or other suitable liquids
can be used. They are passed after leaving the lower end of the column, in a more
or less heated state through an ordinary cooler B and are conveyed by a pump to
the upper end again, thus proceeding in a continuous circuit.
A thermometer o is provided by means of which the operation of the apparatus
can be observed.
A series of straight, horizontal or inclined cooling tubes may be used, these tubes
being arranged beside each other and passed in several superposed bends m m
through the divided substances so that the connections of these tubes are situated
either on the outside of the chamber as shown in Figure 2 or on the inside as
shown in Figure 3.
In every other respect the remarks made with reference to Figure 1 apply to
this case.
The cooling may also be effected by a series of vertical tubes such as are
represented in Figure 4. In order to prevent the rapid mixing of the lower layers
of the cooling-liquid with the upper and cooler layers, the tubes, when they are of
large diameter, can be filled with divided substances.
If desired two or more of the arrangements of cooling pipes shown may be
combined and used simultaneously, for instance the form shown in Figure 1 may be
combined with that shown in Figures 2 and 3.
All these arrangements have the same effect, namely the cooling of the divided
substances.
Instead of causing a liquid cooling substance to flow through the tubes, a gaseous
agent may be used, say a current of air which passes freely through the tubes or is
forced through by a fan from the top downwards.
The column may be circular, oblong, quadrilateral, or of any other suitable shape
in cross section, and in order to increase the surface it may also assume re-entrant
forms, for instance as shown in Figure 5 or Figure 6.
The internal cooling will in most cases be sufficient, but if it is intended to cool
externally as well, the receptacle is surrounded by a jacket M (Figure 7). The
cooling liquid flows through a cock from above, and leaves through the tube 2. In
order to render the ascent of the warmer lower layers of the cooling liquid into tho
upper colder layers difficult, the intermediate space between the chamber and the
jacket M is filled with divided substances.

page_text: Having now particularly described and ascertained the nature of my said
invention and in what manner the same is to be performed, I declare that what
I claim is
First. The process of extracting one or more volatile ingredients from a mixture
by fractional distillation, the vapours from the said mixture being passed through
one or more chambers containing pieces or fragments of material not affected by
the said vapours, which materials are cooled by coils or tubes, or by a jacket
through which a cooling fluid is caused to pass.
Second. A column of any suitable section, containing fragments or pieces of
material unaffected by the vapours of the liquids being distilled, and which are
cooled internally by coils or tubes or externally by a jacket through which a
cooling fluid flows for the purpose specified.
HASELTINE, LAKE & Co.,
For the Applicant.