Improvements relating to the Production of Pure Ethylic Alcohol from Crude Spirits.
Year: 1888

page_text: Date of Application, 26th Sept., 1888
Complete Specification Left, 26th June, 1889-Accepted, 17th Aug., 1889
PROVISIONAL SPECIFICATION.
Communicated from abroad by CARL EUDWIG THEODOR MÜLLER, of Berlin, in the
Empire of Germany, Engineer.]
Improvements relating to the Production of Pure Ethylic Alcohol
from Crude Spirits.
I, HENRY HARRIS LAKE, of the firm of Haseltine, Lake & Co., Patent Agents,
Southampton Buildings, in the County of Middlesex, do hereby declare the nature of
this invention to be as follows
This invention relates to an improved process of obtaining pure ethylic alcohol from
crude spirits, and is based on the fact that the aldehydes, amylic alcohols and the like
contained in the crude spirits, are less soluble than the ethylic alcohol, in solutions of
certain alkaline salts, of a certain concentration of temperature.
--
As salts which can be used in practical working, the following may be mentioned,
viz. carbonate of sodium or of potassium; oxyhydrate or hydroxide of sodium or of
potassium; phosphate of sodium; the sulphates of soda, ammonium, magnesium and
zine; potash or ammonia alum.
To carry the invention into practice, the crude spirits are conducted through one or
a series of vessels and a solution of either one or more of the above named salts is
injected into the spirit as a jet, or a number of jets, in such a manner as to pass the
liquid conducted into the vessel.
While passing the crude spirit the solution of one of said salts or of a mixture of
them will be saturated with pure ethylic alcohol and therefore provision must be
made to conduct the saturated jet or jets of the solution of salts into separate tanks
wherefrom the mixture is to be drawn off and the pure ethylie alcohol then obtained
in the usual manner by distillation, whilst the residue (the alkaline solution) may be
used again in the manner herein before mentioned.
After a sufficient quantity of the solution of salts aforesaid has passed the vessel or
vessels to which the crude spirit is conducted and in which the separation of the pure
ethylic alcohol is effected, finally the aldehydes, amylic alcohol and the like will be
retained therein in considerable proportions while the pure ethylic alcohol is obtained
as aforesaid.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, W.C., Agents for the Applicant.
COMPLETE SPECIFICATION.
Improvements relating to the Production of Pure Ethylic Alcohol
from Crude Spirits.
I, HENRY HARRIS LAKE, of the firm of Haseltine, Lake & Co., Patent Agents,
Southampton Buildings, in the County of Middlesex, do hereby declare the nature of
this invention 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 an improved process for obtaining pure ethylic alcohol
from crude spirits and is based on the fact that the aldehydes, amylic alcohols and the
like contained in the crude spirits, are less soluble than the ethylic alcohol in solutions
of certain alkaline salts of a certain concentration or temperature.
As salts which can be used in practical working the following may be mentioned
viz. carbonate of sodium, or of potassium, oxyhydrate or hydroxide of sodium or of
potassium phosphate of sodium; the sulphates of sodium; ammonium, magnesium
and zinc, potash or ammonia-alum.

page_text: To carry this invention into practice, apparatus such as illustrated in the
accompanying drawing may be used, in which,
Figure-1 is.a front. view of a series of vessels employed for mixing the crude spirits
with a solution of one or several of the above named salts.
Figure 2 is a sectional side elevation of Figure 1.
Figure 3 shows a top view of the mixing vessels (Figure 1) and
Figure 4a general view of the whole apparatus such as may be preferably used
for. continuous operation viz. -the mixing vessels (Figures 1-3) in combination
with a distilling and refining apparatus of usual construction..
Similar letters refer to similar parts throughout the several views.
A solution, having a specific gravity of from 1,190 to 1,240, of either one or more
of the above named salts is run through the conducting pipe a, three-way cock a¹,
branches a and by the aid of a screen or grating in fine jets into the first vessel A
containing crude spirit. The latter is conducted into the vessel A through the pipe e,
the cock e, a valve controlled by a float and numerous fine holes of an annular
pipe placed in horizontal plane, just above the level of the crude spirit first run into
the vessel.
While passing the crude spirit, the solution of salt or salts will mix with nearly
pure ethylic alcohol in quantity of about 15 per cent. and precipitate while the mixture
of impure spirit retaining aldehydes amylic alcohol &c. with the solution of salts as
aforesaid will float upon the one containing nearly pure ethylic alcohol which is
caused by the proportionally larger quantity of spirit (about 55 per cent.) contained
in this above floating mixture.
The precipitated solution which still contains traces of aldehydes and other
impurities is then conducted from the bottom of the vessel A through the three-way
cock pipe, three-way cock b', branches 62 and a screen or grating to distribute
the mixture in fine jets, into a second vessel B, into which refined spirit is conducted
from a reservoir or directly from the refining apparatus through the pipe d, a cock d²,
a valve e controlled by a float and a perforated annular pipe e, both the latter similar
to such as are employed in the vessel A. This refined spirit mixes with the solution
of salt mixed in the vessel A with ethylic alcohol but still containing aldehydes and
other like impurities. The process then taking place in the second vessel will be
analogous to that performed in the first vessel viz. the refined spirit having greater
affinity to the alkaline solution is taken up by the latter while the aldehydes and other
impurities are separated in the upper part of the vessel exactly as in the foregoing
vessel A.
This operation may be a third or more times repeated in conducting the mixture
precipitating in the vessel B for instance into a third vessel through the three-way
cock g, stand pipe g, three-way cock c', branches c &c. while refined spirit may be
conducted through the cock d³ and distributed by the aid of a perforated annular pipe
just as previously set forth. The product to be obtained from this last vessel consists
of a mixture of pure ethylic alcohol and an aqueous solution of the salt or salts above
mentioned and it is finally conducted from the bottom of the vessel C through the
three-way cock and tube i to a preferably continuously working distilling apparatus
of known construction (Figure 4) by the aid of which the pure ethylic alcohol
is obtained from its mixture with the salt solution as will be hereafter described.
In the beginning of the operation the upper layer of the mixing vessel still contains
considerable quantities of ethylic alcohol, but in the proportion as the quantity of
amylic alcohol, aldehydes &c. increases. in this layer, when the process is continued
for some time, the ethylic alcohol first retained in the upper floating layer will
gradually be received entirely from the solution of salt or salts continuously injected
therein and will settle with the latter until finally the upper layer contains only the,
impurities in mixture with about 45 per cent. of the alkaline solution.
This construction of apparatus will allow a continuous working and the operation.
of which will be easily understood as by way of example from the following
explanations.
In the first vessel A suppose that into the crude spirit an alkaline solution, is run

page_text: as aforesaid, the proportions of aldehydes &c. therein increase very rapidly first in the
upper layer and then in the lower layers of the contents of the vessel, so that after.a
determined time the entire vessel requires to be emptied, which is done through a
cock and pipe l.. The liquid drawn off may be discharged as waste or it may be
distilled separately and the products thereby obtained may be used for several other
purposes.
foregoing vessel A.
At the samo moment, however, when the cock is opened the three-way cock a¹
must be turned so as to stop the supply of the alkaline solution to the vessel A and
to establish communication between the pipe h and the branches a², whilst the
three-way cock was directed so as to conduct now the alkaline solution through the
branches 62 into the following vessel B. While this is done the supply of refined
spirit into this vessel B must be discontinued by closing the cock d² and the cock e
opened, in order to allow the crude spirit to enter into the vessel B through the
valve ex. At this stage the vessel B is acting in the manner as and instead of the
During the discharge of the vessel A the mixture of alkaline solution and pure
ethylic alcohol, contained from a former period in the third vessel C, is continuously
conducted through the three-way cock into the discharge pipe i and in an uniform
state of purity into the distilling apparatus (Figure 4). As soon as the vessel A is
entirely emptied, the three-way cock h' at the bottom of the vessel C is turned so as
to stop the discharge into the pipe i and to establish communication between the vessel C
and the conducting pipe h. The contents of the vessel C must now be discharged
through this pipe h, the three-way cock a' and the branches a² into the vessel A
first started with, into which refined spirit is run during this period by opening the .
cock d'.
The vessel A which during the first mentione.l period has served for mixing the
crude spirit with the alkaline solution is now adapted to receive a mixture, previously
treated in the vessels B and C, and the latter is at the present period employed in
the same manner as has been heretofore described in relation to the vessel B during
the first mentioned period. For this reason the vessel A will act now just as and in
place of the vessel C during the first period and the three-way cock f¹ must therefore
be directed so as to allow the finally treated liquid of that vessel A to discharge into
the pipe and into the distilling apparatus as before mentioned.
In the next period it will then be started with the vessel C and the process
continuously carried forward hereafter, just as before explained.
It must however be mentioned that for the purpose of a regular working of the
apparatus it is advisable to control the supply of crude spirit as well as that of refined
spirit of the purifying or settling vessels (A, B, C) according to the density of the
different layers of liquid within the vessels. For this reason the supply valve in
question (ex) is connected to a float (k) which is accordingly adjusted and serves to
regulate the supply of spirit through the said valve (ex) in all the purifying or settling
vessels.
From the conducting pipe of the settling battery A, B, C, the mixture of alkaline
solution and pure ethylic alcohol is conducted through the pipe after passing a
serpentine placed in the condenser m and warmed therein by the aid of the volatilized
spirit evaporated in the rectifying column p, into the distilling apparatus n of known
construction.
In this distilling apparatus n the ethylic alcohol by the aid of heat generated from
steam supplied through the valve n¹, is separated from the alkaline solution, but
while evaporating the ethylic alcohol will still be accompanied by a part of the water
of the alkaline solution, which will be entirely separated by conducting the vapors
produced in the distilling apparatus through the pipe p¹ into the rectifying column p.
As the latter is also of known construction it may only be mentioned, that on
evaporation the volatile alcohol is condensed by means of the condensor m, wherein the
specifically lightest parts are again separated and then conducted through the pipe q to
the refrigerator, while the heavier parts return through the piper into the rectifying
column for repeated evaporation.

page_text: The alkaline solution separated by means of the distilling apparatus from the mixture
coming from the settling battery A, B, C is run through the cock n³ and pipe n³ into
a vessels in which it may be diluted when required by water stored in the reservoir t
from which it is conducted through the pipe u. A pump then serves to elevate the
alkaline solution and to discharge it through the pipe a* into the conducting-pipe a of
the settling-battery.
Although in the foregoing specification three vessels are mentioned as forming a
settling battery, it must be understood that a greater or less number of vessels may
be employed to carry the present invention into effect and that also any other
distilling and rectifying apparatus in combination with the former may be employed
without departing from the limits of this invention.
Having now particularly described and ascertained the nature of the said inven-
tion and in what manner the same is to be performed as communicated to me
by my foreign correspondent I declare that what I claim is:
First. The method of obtaining pure ethylic alcohol from crude spirits by conducting
the latter successively into one or more vessels through which an aqueous solution of
one or more alkaline salt or salts, such as carbonate of sodium or potassium,
oxyhydrate of sodium or of potassium, phosphate of sodium, the sulphates of sodium,
ammonium, magnesium and zinc, potash or ammonium-alum are simultaneously
distributed under sufficient pressure, all substantially as and for the purpose,
specified.
Second. In the process of separating amylic alcohols, aldehydes and other
impurities from a mixture of spirits and an aqueous solution of alkaline salt or salts
the addition of refined spirit to said mixture, substantially as, and for the purpose,
specified.
Third. In the process of obtaining pure ethylic alcohol from crude spirits by the
aid of an aqueous solution of alkaline salt or salts the reverse application of the latter
in comparison with that substantially explained in the first and second claim.
Fourth. An apparatus for obtaining pure ethylic alcohol from crude spirit by the
aid of an aqueous solution of alkaline salt or salts, consisting of one or more settling
vessels such as A, B, C, a distilling and rectifying-column and their appliances, such
as illustrated by Figure 4, all substantially as, and for the purpose, set forth.
Fifth. In an apparatus for producing pure ethylic alcohol from crude spirits by
the aid of aqueous solution of one or more alkaline salts, the combination of the
settling vessels A, B, C, with their pipe-system for continuous working of the
distilling column n, the reservoirs pump and the condenser m and rectifying
column P, all substantially as specified.
Dated this 26th day of Inno 1880.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, Agents for the Applicant.