Improvements relating to the separation of Fusel or Ethereal Oil from Substances Containing the same.
Year: 1887

page_text: Date of Application, 10th June, 1887
Complete Left, 10th Mar., 1888
Complete Accepted, 13th Apr., 1888
Improvements relating to the separation of Fusel or Ethereal
Oil from Substances Containing the same.
We, Dr. ISIDOR TRAUBE, and Dr. GUIDO BODLÄNDER, both of Hanover, in the
Empire of Germany, do hereby declare the nature of this invention to be as
follows:-
Our invention relates to the separation of fusel and ethereal oils from aqueous
ethyl alcohol or methyl alcohol.
If mixtures of methyl alcohol and ethyl alcohol and water, in which ethereal oils or
fusel oils are contained, are nearly saturated with certain salts such as sodium carbonate
ammonium sulphate or the like, or, if the aqueous alcohol containing the extraneous
admixtures above named is introduced into concentrated aqueous solutions of the
said substances, a separation of the entire liquid into two well-defined strata takes
place at certain degrees of concentration and temperature.
Upon examination it will be found that the upper stratum of liquid contains nearly
all the admixture of ethereal or fusel oils that were present in the alcoholic liquids.
Upon the above mentioned observation is based the process which forms the subject
of the present application.
In our improved process the aqueous alcoholic liquid to be freed from its admixture
or impurities is put into a vessel in which the separation of the two strata can be
conveniently effected the said liquid is then nearly saturated with sodium carbonate
or ammonium sulphate either by introducing the salts in a solid state into the solution
containing spirits of wine, or, preferably, by mixing the raw spirit with a more or
concentrated aqueous solution of the salts till a separation of the two strata commences,
this separation may if desired be accelerated by heating the solution.
If the upper stratum becomes too large it contains, besides the substances to be
separated, a comparatively large quantity of ethyl alcohol or methyl alcohol. By
gradually adding suitable quantities of water, or by cooling or heating, the volume of
the upper stratum can be so regulated that it contains all the admixtures but only
little ethyl alcohol or methyl alcohol.

page_text: In order to arrive at the most favourable results, the treatment is preferably such
that from 30 to 40 kilogrammes of anhydrous sodium carbonate or of ammonium
sulphate, are dissolved in 1 hectolitre of water. To this solution is added a temper-
ature of from 20 to 40 degrees Centigrade, 50 litres of raw spirit (of about 80 per
cent.) or of raw methyl alcohol. At the aforesaid temperatures two strata of liquid
will be formed, the upper of which can, desired, be readily decreased or augmented
by slightly heating or cooling the liquid or by adding water or salt.
Exactly the same proportions of weight, degrees of concentration and temperature
are used if, instead of introducing the raw alcohol into the aqueous solution of the
sodium carbonate or ammonium sulphate, the solid substance or the saturated aqueous
solution thereof is introduced into the diluted or into the raw spirit.
The two strata of liquid are separated in a suitable manner, or a further separation
is caused in the lower stratum, if necessary, by further adding small quantities of the
solid substances, or by slightly increasing the temperature, in which case any traces
of fusel oil or ethereal oils that may have been present in the lower stratum will be
caused to combine with the upper stratum.
The ethyl alcohol or methyl alcohol is then separated from the upper stratum
according to the above process. These strata are treated with concentrated aqueous
solutions of carbonate of sodium or sulphate of ammonium by means of which highly
concentrated solutions of fusel oil or ethereal oils can be obtained. These solutions
can be further treated according to any known method for the purpose of extracting
the said substances.
From the lower strata, which consist of mixtures of pure ethyl alcohol or methyl
alcohol and water, a separation of the alcohol from the solution of the salt is effected
by distillation in any simple apparatus.
The distillate contains pure alcohol free from fusel oil whilst the aqueous solutions
which remain during the distillation of the said salts can always be used again.
In the solutions for producing two strata and in which spirits of wine form one
of the elements thereof, besides the sodium carbonate and ammonium sulphate the
said solution contains a large number of other salts and bases such as potassium
carbonate potassium hydroxide, and sodium hydroxide, sodium sulphate, sodium
phosphate, magnesium sulphate and zinc sulphate, and the alums. These substances
as well as their mixtures can also be used instead of the sodium carbonate and
ammonium sulphate, the same proportions of weight and temperature relatively to
the anhydrous salt, being adhered as with the sodium carbonate and ammonium
sulphate.
The character of the present invention is based upon the more mechanical separation
of two strata, whilst a chemical action of the said substances does not takes place at
least upon the fusel oil.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London,
Agents for the Applicants.

page_text: Oil from Substances Containing the same.
We, Dr. ISIDOR TRAUBE and Dr. GUIDO BODLÄNDER, both of 6 Mehlstrasse,
Hanover, Prussia, in the Empire of Germany, 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 :-
Our invention relates to the separation of fusel and ethereal oils from aqueous
ethyl alcohol or methyl alcohol.
If mixtures of methyl alcohol and ethyl alcohol and water, in which ethereal oils
or fusel oils are contained, are nearly saturated with certain salts such as sodium
carbonate ammonium sulphate or the like, or, if the aqueous alcohol containing the
extraneous admixtures above named is introduced into concentrated aqueous solutions
of the said substances, a separation of the entire liquid into two well-defined strata
takes place at certain degrees of concentration and temperature. Upon examination
it will be found that the upper stratum of liquid contains nearly all the admixture of
ethereal or fusel oils that were present in the alcoholic liquids.
Upon the above mentioned observation is based the process which forms the
subject of the present application.
In our improved process the aqueous alcoholic liquid to be freed from its admixture
or impurities is put. into a vessel in which the separation of the two strata can be
conveniently effected; the said liquid is then nearly saturated with sodium carbonate
or ammonium sulphate, either by introducing the salts in a solid state into the solution
containing spirits of wine, or, preferably, by mixing the raw spirit with a more or
Jess concentrated aqueous solution of the salts till a separation of the two strata
commences, this separation may if desired be accelerated by heating the solution.
If the upper stratum becomes too large it contains, besides the substances to be
separated, a comparatively large quantity of ethyl alcohol or methyl alcohol. By
gradually adding suitable quantities of water, or by cooling or heating, the volume
of the upper stratum can be so regulated that it contains all the admixtures but only
little ethyl alcohol or methyl alcohol.
In order to arrive at the most favourable results the treatment is preferably such
that from 30 to 40 kilogrammes of anhydrous sodium carbonate, or of ammonium
sulphate, are dissolved in 1 hectolitre of water; to this solution is added at a tempe-
rature of from 20 to 40 degrees Centigrade, 50 litres of raw spirit (of about 80 per
cent.) or of raw methyl alcohol. At the aforesaid temperatures two strata of liquid
will be formed, the upper of which can if desired be readily decreased or augmented
by slightly heating or cooling the liquid or by adding water or salt.
Exactly the same proportions of weight, degrees of concentration and temperature
are used if, instead of introducing the raw alcohol into the aqueous solution of the
sodium carbonate or ammonium sulphate, the solid substance or the saturated
aqueous solution thereof is introduced into the diluted or into the raw spirit.

page_text: The two strata of liquid are separated in a suitable manner and the lower strata
is further separated into two strata if necessary, by further adding small quantities
of the solid substances, or by slightly increasing the temperature, in which case
the upper stratum contains any traces of fusel oil or ethereal oils that may have
been present.
The ethyl alcohol or methyl alcohol is then separated from the upper stratum
according to the above process. These strata are treated with concentrated aqueous
solutions of sodium carbonate or ammonium sulphate by means of which highly
concentrated solutions of fusel oil or ethereal oils can be obtained. These solutions
can be further treated according to any known method for the purpose of extracting
the said substances.
From the lower strata, which consists of mixtures of pure ethyl alcohol or methyl
alcohol and water, a separation of the alcohol from the solution of the salt is effected
by distillation in any simple apparatus.
The distillate contains pure alcohol free from fusel oil whilst the aqueous solutions,
which remain during the distillation, of the said salts can always be used again.
The property of producing two strata in liquids containing spirits of wine is
possessed besides by the sodium carbonate and ammonium sulphate, and by a large
number of other salts and bases, such as potassium carbonate, potassium hydroxide
and sodium hydroxide, sodium sulphate, sodium phosphate, magnesium sulphate and
zinc sulphate, and the alums. These substances as well as their mixtures can also be
used instead of the sodium carbonate and ammonium sulphate, the same proportions
of weight and temperature relatively to the anhydrous salt, being adhered to as with
the sodium carbonate and ammonium sulphate.
The character of the present invention is based upon the more mechanical separation
of two strata, whilst a chemical action of the said substances does not take place at
least upon the fusel oil.
Having now particularly described and ascertained the nature of our said inven-
tion and in what manner the same is to be performed, we wish it understood
that what we claim is
First. Process of separating the ethyl alcohol or methyl alcohol and water from
fusel oil and ethereal oils, consisting in adding to the respective mixtures aqueous
solutions of certain salts and bases, such as potassium carbonate and sodium carbonate,
potassium hydroxide and sodium hydroxide, sodium phosphate, sodium sulphate,
ammonium sulphate, magnesium sulphate, zinc sulphate, the alums, and the like,
thereby causing the formation of two strata of liquid, the upper of which contains
the admixtures, and the lower the purified alcohol.
Second. The extraction of pure alcohol on the one hand, ethereal oils and fusel oil
on the other hand, from the two liquids obtained as set forth in the first claim.
Dated 10th day of March 1888
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, W.C.,
Agents for the Applicants.