Improvements relating to the Separation of Mixtures of Ethyl, Alcohol, and Water from Fusel Oil and other Impurities, and to Apparatus therefor.
Year: 1888

page_text: Date of Application, 8th Dec., 1889
Complete Specification Left, 26th Aug., 1889-Accepted, 5th Oct., 1889
PROVISIONAL SPECIFICATION.
Improvements relating to the Separation of Mixtures of Ethyl,
Alcohol, and Water from Fusel Oil and other Impurities, and to
Apparatus therefor.
I, ISIDOR TRAUBE, of Hanover, in the Empire of Germany, Dr. of Philosophy do
hereby declare the nature of this invention to be as follows:-
This invention relates to processes of and apparatus for separating mixtures of ethyl
alcohol and water from fusel oil and other impurities contained in spirit.
Mixtures of ethyl alcohol and water can be separated from their impurities by the
formation ef two strata of liquid, in the upper of which the impurities are for the most
part contained, the aforesaid formation being, caused by the salts and bases, such as
sodium carbonate, potassium carbonate, potassium hydroxide and sodium hydroxide,
sodium phosphate, sodium sulphate, ammonium sulphate, magnesium sulphate, or zinc
sulphate, or potassium alum or ammonium alum, which are used in the treatment of
pure and impure ethyl alcohol with an aqueous solution.
Extensive experiments have shown that the success of such a process is dependent
on the selection of the concentrations and temperatures to be used therein, and on the
number of strata produced and the special mode of in which the same is carried into
effect.
As far as the separation of aqueous ethyl alcohol and fusel oil is concerned, the
employment of the following temperatures and concentrations have proved suitable for
the above mentioned salts and bases, especially for potash. The aqueous solution of
salt as specially suitable has been found the solution of potash (potassium carbonate)
having a specific weight of 1. 2 or more at about 15 degrees is heated to from 40 to
78 degrees centigrade, and raw spirit containing about 80 per cent. of alcohol is added
until an upper stratum of liquid of about to of the total volume is formed. If
raw spirit of other degrees of concentration is to be employed, the solution of salt has
such a specific weight that the relative proportions of alcohol, salt and water remain
approximately the same, as follows from the use of the above stated proportions. In
this manner the largest quantity of the impurities which were contained in the raw
spirit employed is obtained in the upper stratum so that the lower stratum contains a
very much purer spirit which is however not yet quite pure.
In order to effect the complete purification it is necessary to repeatedly cause a
formation of strata in this lower stratum obtained in the described manner.
It is however advisable to cause these formations of strata not only by adding solid
substances alone or by increasing the temperature, but by adding after every removal
of the upper stratum, besides the aforesaid solid substances, also water and alcohol in
such proportions as these three components are contained in the upper stratum, in
order that the concentration of the lower stratum shall not change in an inconvenient
manner that especially the quantity of alcohol contained in the latter stratum shall not
become too small for the distillation.
As the upper strata obtained in such a manner gradually become purer and purer,
these strata, according to the said invention, are used in the order of their purity for
the subsequent distillations for the production of fresh strata in lieu of the above-
mentioned addition of salt, water and alcohol.
Accordingly in the first instance the operation is effected by adding in the
preparation for the first distillation, after the removal of the first upper impure
stratum obtained from the raw spirit by means of the solution of salt, pure spirit,
water and salt in approximately such quantities and such proportions as these con-
stituents were contained in the removed stratum. By repeating such an addition
and removing the upper strata formed, a series of strata of gradually increasing

page_text: purity are obtained which can be kept separated from each other and used in the
preparations for the next distillations for producing fresh strata, the second stratum
obtained in the preceding distillation being preferably used for the production of
first stratum in the following distillation, the third stratum obtained in the first
distillation, for the production of the second stratum in the following distillation and
so on.
By carrying out this process the upper strata gradually become richer in dissolved
impurities. The first strata obtained in each case are specially impure and are removed
for the purpose of further utilization or purification. For the production of the last
strata spirit and a solution of potash is used in the above stated proportions.
It may be observed that the solution of salt to be employed is preferably a solution
of potash of the specific weight above stated but an aqueous solution of the above-
mentioned salts or bases of approximately the same specific weight can also be used.
In carrying out this process the several successive separations and the distillation of
the solution of spirit which is sufficiently purified and contains salt can be effected in
the same receptacle, or the several successive separations can be effected in one
receptacle and the distillation in a separate distilling vessel, or the several
separations can be carried out in different receptacles, the distillation of the solution of
spirit which is sufficiently purified taking place either in these receptacles or in separate
distilling apparatus.
The receptacles which serve for the separations, in order to enable the upper stratum
to be more easily and completely removed are preferably made of an upwardly tapering
shape at their upper part and are provided with a heating device (heating pipe,
heating coil) with an admission pipe for the spirit or solution of salt, which extends to
the bottom and is suitably perforated or provided with branches at its lower end for
the purpose of effecting a thorough mixing, with a mixing device for the thorough
mixing of the spirit with the solution of salt, furthermore with sight-holes for observing
the formation of strata, and also with devices (such as a bent-pipe float adapted to turn
upon its horizontal branch) for removing the upper strata. When a single receptacle
is employed for the several separations it is preferable to keep the removed upper
strata in separate receptacles in order to use them for the several separations in the
preparation of fresh quantities of spirit for the next distillation.
If the separations are to be carried out in different receptacles, any desired number
of the latter can be combined to constitute one system. At the beginning of the
operation all the cocks or valves are closed and the receptacles are partially filled with
a hot solution of salt.. By opening a cock in the admission pipe the quantity of raw
spirit necessary for the formation of strata is conducted into one of the receptacles,
whereupon the said cock is closed again.
After the raw spirit has been properly mixed with the solution of salt, and after the
formation of strata has taken place, the upper stratum is removed by means of a dis-
charge pipe which is preferably arranged to turn in such a manner that the outlet
orifice can be at a higher or lower level according to the level of the liquid, and after
opening a cock in the discharge pipe it is conducted through the latter to a receptacle
in which the strata which have first been removed and are therefore specially impure
can be collected. After closing the cock in the said discharge pipe the necessary
quantity of the solution of spirit and salt is introduced through the medium of the
above mentioned admission pipe by opening the cock in the latter for causing the
formation of the second stratum in the first receptacle, after which the said cock is
closed again. When the necessary mixing has been effected and after the strata
have been formed, the aforesaid second upper stratum after opening the respective
cocks is introduced through an admission pipe into the second receptacle. The said
cocks are now closed and another cock is opened in order to admit into the second
receptacle through admission pipes the quantity of raw spirit necessary for producing
the first stratum.
After closing the last mentioned cock and after the thorough mixing and the
formation of strata, the first stratum, as described with reference to the first receptacle
is 'conveyed on opening the respective cock, through the medium of a bent pipe, which

page_text: is suitably arranged so that it can be turned and other pipes into the basin designed
for collecting the first and therefore very impure strata. The said cock is then closed.
Another cock is now opened, and after adding the necessary spirit and the necessary
solution of salt in the first receptacle, the third stratum is produced as described with
reference to the second. This third stratum, like the second stratum previously, is
now introduced into the second receptacle for the production of the second strata.
This second stratum, produced in the second receptacle, in the same manner as the
second stratum produced in the first receptacle was employed for producing the
first stratum in the second receptacle, is conducted to the third receptacle for
the production of the first stratum, where, as was the case in the second receptacle, the
first formation of strata takes place after introducing the necessary raw spirit. Also in
this receptacle, as in all the others, the first stratum is conducted through the outlet
pipe to the vessel for the first impure strata.
This operation is continued in this manner until the lower stratum in the first
receptacle has been sufficiently purified, whereupon this receptacle, after the removal
of the upper stratum, is cut out of the system so that its contents are let out in order
to pass to the distilling apparatus.
If four formations of strata were necessary, the said first receptacle is cast out of
the system as soon as the fifth receptacle, as the last, is set in operation. Into the
second receptacle must then be admitted pure spirit and a solution of potash in the
same manner as the first receptacle has received it before. The first apparatus can
again be included in the system to work in this cyclical process, in which it is set in
operation as the last apparatus.
The pipes leading to the distilling apparatus and their branches can be dispensed
with if the above described discharge pipe has a branch which can be closed and which
leads to the receptacle for the first upper strata.
The upper strata can be removed by any suitable means, such as jet-apparatus
(monte-jus,) or by producing pressure in the receptacle to be emptied, or a vacuum in
the receptacle which is to be filled.
It is moreover advisable to provide the apparatus with suitable devices for cleaning
the pipes and receptacles.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, Agents for the Applicant.
COMPLETE SPECIFICATION.
Improvements relating to the Separation of Mixtures of Ethyl,
Alcohol, and Water from Fusel Oil and other Impurities, and to
Apparatus therefor.
I, ISIDOR TRAUBE, of No. 9 Göthe Strasse, in the City of Hannover, Germany,
Doctor of Philosophy, 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 :-
This invention relates to processes of and apparatus for separating mixtures of
ethyl alcohol and water from fusel oil and other impurities contained in spirit.
Mixtures of ethyl alcohol and water can be separated from their impurities by the
formation of two strata of liquid, in the upper of which the impurities are for the
most part contained, the aforesaid formation being caused by the salts and bases, such
as sodium carbonate, potassium carbonate, potassium hydroxide and sodium hydroxide,
sodium phosphate, sodium sulphate, ammonium sulphate, magnesium sulphate or zinc
sulphate, or potassium alum or ammonium alum, which are used in the treatment of
pure and impure ethyl alcohol with an aqueous solution.
Extensive experiments have shown that the success of such a process is dependent on
the selection of the concentrations and temperatures to be used therein, and on the
number of strata produced and the special mode of in which the same is carried into
effect

page_text: As far as the separation of aqueous ethyl alcohol. and fusel oil is concerned, the
employment of the following temperatures and concentrations have proved suitable for
the above mentioned salts and bases, especially for potash. The aqueous solution of
salt as specially suitable has been found the solution of potash (potassium carbonate),
having a specific weight of 1. 2, or more, at about 15 degrees, which is heated to from
40 to 78 degrees Centigrade, and raw spirit containing about 80% of alcohol is added
until an upper stratum of liquid of about to g of the total volume is formed. If
raw spirit of other degrees of concentration is to be employed, the solution of salt
has such a specific weight that the relative proportions of alcohol, salt and water
remain approximately the same, as follows from the use of the above stated pro-
portions. In this manner the largest quantity of the impurities which were contained
in the raw spirit employed is obtained in the upper stratum so that the lower stratum
contains a very much purer spirit which is, however, not yet quite pure.
In order to effect the complete purification it is necessary to repeatedly cause a
formation of strata in this lower stratum obtained in the described manner.
It is, however, advisable to. cause these formations of strata not only by adding
solid substances alone or by increasing the temperature, but by adding, after every
removal of the upper stratum, besides the aforesaid solid substances, also water and
alcohol in such proportions as these three components are contained in the upper
stratum, in order that the concentration of the lower stratum shall not change in an
inconvenient manner that especially the quantity of alcohol contained in the latter
stratum shall not become too small for the distillation.
As the upper strata obtained in such a manner gradually become purer and purer,
these strata, according to the said invention, are used in the order of their purity, for
the subsequent distillations for the production of fresh strata in lieu of the above
mentioned addition of salt, water and alcohol.
Accordingly in the first instance the operation is effecied by adding in the pre-
paration for the first distillation, after the removal of the first upper impure stratum
obtained from the raw spirit by means of the solution of salt, pure spirit, water and
salt in approximately such quantities and such proportions as these constituents were
contained in the removed stratum. By repeating such an addition and removing the
upper strata formed, a series of strata of gradually increasing purity are obtained,
which can be kept separated from each other and used in the preparations for the next
distillations for producing fresh strata, the second stratum obtained in the preceding
distillation being preferably used for the production of first stratum in the following
distillation, the third stratum obtained in the first distillation, for the production of
the second stratum in the following distillation and so on.
By carrying out this process the upper strata gradually become richer in dissolved
impurities. The first strata obtained in each case are specially impure and are removed
for the purpose of further utilization or purification. For the production of the last
strata spirit and a solution of potash is used in the above stated proportions.
It may be observed that the solution of salt to be employed preferably a
solution. of potash of the specific weight above stated, but an aqueous solution of
the above mentioned salts or bases of approximately the same specific weight can also
be used.
In carrying out this process the several successive separations and the distillation
of the solution of spirit which is sufficiently purified and contains salt can be
effected in the same receptacle, or the several successive separations can be effected in
one receptacle and the distillation in a separate distilling vessel, or the several
separations can be carried out in different receptacles, the distillation of the solution
of spirit. which is sufficiently purified taking place either in these receptacles or in
separate distilling apparatus.
t
The receptacles, which serve for the separations, in order to enable the upper
stratum to be more easily and completely removed, are preferably made of an upwardly
tapering shape at their upper part and are provided with a heating device (heating
pipe, heating coil), with an admission pipe for the spirit or solution of salt which
extends to the bottom and is suitably perforated or provided with branches at its

page_text: lower end for the purpose of effecting a thorough mixing, with a mixing device for
the thorough mixing of the spirit with the solution of salt, furthermore with sight
holes for observing the formation of strata, and also with devices, (such as a bent
pipe float adapted to turn upon its horizontal branch), for removing the upper
strata.
When a single receptacle is employed for the several separations it is preferable to
keep the removed upper strata in separate receptacles in order to use them for the
several separations in the preparation of fresh quantities of spirit for the next
distillation. If the separations are to be carried out in different receptacles, any
desired number of the latter can be combined to constitute one system, such for
instance as represented in the accompanying drawing in which A', A etc. represent
the separating receptacles. At the beginning of the operation all the cocks or valves
are closed and the receptacles are partially filled with a hot solution of salt. By
opening the cock in the admission pipe B the quantity of raw spirit necessary for
the formation of strata is conducted into the receptacle A' whereupon the said cock b¹
is closed again.
After the raw spirit has been properly mixed with the solution of salt, and after
the formation of strata has taken place, the upper stratum is removed by means of
a discharge pipe which is preferably arranged to turn in such a manner that the
outlet orifice can be at a higher or lower level according to the level of the liquid,
and after opening the cock e in the discharge pipe E it is conducted through the
pipe E to a receptacle in which the strata which have first been removed and are
therefore specially impure can be collected. After closing the cock el in the said
discharge pipe the necessary quantity of the solution of spirit and salt is introduced
through the medium of the above mentioned admission pipe B by opening the cock b¹
in the latter for causing the formation of the second stratum in the first receptacle,
after which the said cock-b' is closed again. When the necessary mixing has been
effected and after the strata have been formed, the aforesaid second upper stratum,
after opening the respective cocks c¹, d², is introduced through admission pipes C, C1, C
into the second receptacle A2. The said cocks c', d are now closed and another
cock bis opened in order to admit into the second receptacle A* through admission
pipes B B, the quantity of raw spirit necessary for producing the first stratum..
After closing the last mentioned cock 2 and after the thorough mixing and the
formation of strata, the first stratum, as described with reference to the first
receptacle A', is conveyed on opening the respective cock e through the medium of a
bent pipe
(2, which is suitably arranged so that it can bo turned, and through the
pipes E, E into the basin designed for collecting the first and therefore very impure
strata. The said cock e² is then closed. Another cock is now opened, and after
adding the necessary spirit and the necessary solution of salt in the first receptacle A¹
the third stratum is produced as described with reference to the second. This third
stratum, like the second stratum previously, is now introduced into the second
receptacle A² for the production of the second strata. This second stratum, produced
in the second receptacle A² in the saine manner as the second stratum produced in the
first receptacle A' was employed for producing the first stratum in the second
receptacle A² is conducted to the third receptacle A³, for the production of the first
stratum, where, as was the case in the second receptacle A, the first formation. of
strata takes place after introducing the necessary raw spirit. Also in this receptacle
as in all the others the first stratum is conducted through the outlet pipe E to the
vessel for the first impure strata.
This operation is continued in this manner until the lower stratum in. the first
receptacle A has been sufficiently purified, whereupon this receptacle, after the
removal of the upper stratum, is cut out of the system so that its contents are
let out by means of the cock fand discharge pipe F in order to pass to the distilling
apparatus.
If four formations of strata were necessary. the said first receptacle A' is cast out
of the system as soon as the fifth receptacle A* as the last is set in operation. Into
the second receptacle A² must then be admitted pure spirit and a solution of potash in

page_text: n
the same manner as the nrst receptacle Ahas received it before. The first app
can again be included in the system to work in this cyclical process in which it is
set in operation as the last apparatus.
The pipes E, E, E². Es leading to the distilling apparatus and their branches can
be dispensed with if the above described discharge pipe C has a branch.which can he
closed and which leads to the receptacle for the first upper strata.
The upper strata can be removed by any suitable means, such as jet apparatus
(monte-jus) or by producing pressure in the receptacle to be emptied, or a vacuum in
the receptacle which is to be filled.
It is moreover advisable to provide the apparatus with suitable devices for cleaning
the pipes and receptacles.
Instead of allowing only the upper layers or strata to pass one receptacle to the
other and allowing the lower strata to remain in the same receptacle, these said lower
strata can also he passed from one receptacle to the other in cyclical manner
simultaneously with the removal of the upper strata but in the reverse direction that
is to say, if the upper strata is abstracted from a vessel or receptacle and is caused to
pass into the receptacle standing to the right of the first mentioned receptacle to be
emptied the lower strata can be simultaneously drawn off and passed into the vessel
or receptacle standing next to the left of the first receptacle or the receptacle to be
emptied. In such cases the devices must be so arranged that the quantity of fluid
simultaneously passing or drawn off from the upper and lower layers or strata is in
correct proportion to the volume of the two said layers of strata.
My improved process can also be carried into effect by promoting the formation of
strata by means of one of the hydro-carbons between the first formation of strata and
the last such said formation. A hydro-carbon can also be added to the solution for
forming the first layers or strata..
Having now particularly described and ascertained the nature of my said inven-
tion, and in what manner the same is to be performed, I declare that what I
claim is
1. The separation of mixtures of ethyl alcohol and water froni fusel oil and other
impurities contained in spirit by employing an aqueous solution of salts or bases such
as potassium carbonate, sodium carbonate, sodium hydroxide, potassium hydroxide,
sodium phosphate, sodium sulphate, ammonium sulphate, magnesium sulphate or zinc
sulphate, or potassium alum, or ammonium alum, the process consisting therein that
raw spirit of about 80% of alcohol is added to a solution of one of the above named
salts or bases in water (of a specific gravity of 1. 2 and more at about 15° Centigrade)
at about 40° to 78° Centigrade, and for weaker or stronger spirits a corresponding
weaker or stronger solution of the aforesaid salts, until an upper stratum of fluid
has been formed, said upper stratum containing the greater part of the impurities
contained in the raw spirit and the lower stratum a considerably more pure spirit, so
that when the upper stratum is drawn off by the lower stratum or strata can, in order
to cause the repeated formation of strata, be treated either with upper strata which
are not too impure and are obtained in the manner given above or by the addition of
solid matter, water and alcohol in the same proportions as these three ingredients were
present in the above named stratum and as soon as strata has been thus formed,
drawing off the same in order that by repeatedly carrying out the process a perfect
purification of the treated matter may be attained, substantially as and for the purpose
set forth in the foregoing specification.
2. In the process characterised in the foregoing claim, the method of treatment
according to which the impure but continuously purer becoming, upper strata and
lastly perfectly purified spirit is so employed that a cyclical process for the
formation of strata is obtained, substantially as and for the purpose set forth.
3. An apparatus for carrying the aforenamed process into effect, consisting of a
series of receptacles A', A* etc. preferably tapered at the upper end and provided with
a pipe or tubular service for charging and discharging the fluids, said pipes or tubes
being so arranged that raw spirit is fed through the tubular service B into a

page_text: receptacle which has been previously charged with a saline solution, and as soon as
strata has been formed the same is led off by a pipe C for discharging or letting
off the upper stratum, said pipe C being in connection not only with the tubular
service E but also with a tubular service communicating with the other vessels of
the cyclical system in order that the succeeding purer upper strata can be led into
the said vessels in combination with a tubular service F communicating with the
lower part of the receptacles and by means of which the lower pure stratum of
fluid can be led off into a suitable vessel as soon as the purifying process is finished,
substantially as and for the purpose set forth in the foregoing specification.
Dated this 26th day of August 1889.
PHILIP M. JUSTICE,
Associate Agent.