Improvements in and relating to the Manufacture of Alcohol and in Apparatus therefor.
Year: 1891

page_text: Date of Application, 7th Feb., 1891-Accepted, 25th Apr., 1891
COMPLETE SPECIFICATION.
[Communicated from abroad by GASTON GUIGNARD and ANDRÉ HÉDOUIN,
both of 95, Boulevard, Beaumarchais, Paris, in the Republic of France,
Chemists.]
Improvements in and relating to the Manufacture of Alcohol and in
Apparatus therefor.
I, HENRY HARRIS LAKE, of the firm of Haseltine, Lake & Co., Patent Agents,
45, 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 the manufacture of alcohol, and to apparatus
therefor.
In the various processes of manufacturing alcohol which have heretofore been
employed the fermentation of the juice is effected in presence of air and therefore
in presence of all the germs contained therein.
Now if the impurities which are contained in the alcohol thus manufactured, are
examined from a chemical point of view, which impurities are eventually to be
removed by means of one of the numerous processes devised for this purpose so as
to obtain pure alcohol, it will be ascertained that these impurities arise either from
the germs contained in the air, or from the germs contained in the impure yeast
employed, or from the germs contained in the juice itself.
In fact the impurities whose destruction or transformation becomes necessary for
effecting the purification of the alcohol consist of aldehydes; superior homologous
alcohol of ethyl alcohol ethers; and bases.
Now the communicators have observed that the aldehydes arise from the
oxidation of the alcohol during the fermentation, by the acetic ferment which is in
the juice.
The superior alcohol is produced by the life of the butyric ferment which
decomposes the sugar glycerine and the like into butyric acid, butyl alcohol, carbonic
acid and hydrogen; and by the purely chemical action of nascent hydrogen which.
when acting upon the glucose, yields mannite and the series of monoatomic alcohol
from B-hexyl-alcohol.
The organic acids which contain the juice gives rise to odorous ethers more
especially when acidified wine is distilled with a mineral acid.
The albuminoid substances of the juice and even those contained in the cells of
yeast which are already dead, yield on becoming hydrated, acids; ammonia and
amidated acids.
All the impurities which I have enumerated arise and have a fatal effect when
alcohol is manufactured by the known processes; and when such alcohol is to be
purified it is necessary to have recourse to more or less expensive means for
destroying and transforming them.
The improved process to which the aforesaid invention relates has for its object
to obviate the production of the impurities herein before referred to from the com-
mencement of the manufacture of alcohol. Hence it will be understood that if
this object is realized my process must ensure a much greater production and an
important economy because I manufacture directly pure alcohol.
For preventing the production of the said impurities which arise as above stated
from the presence of the ferments contained either in the air or in the juice or in
the impure yeast I propose to prevent any of these deleterious ferments entering into
the material under treatment from the beginning to the end of the manufacture.
My process of manufacture is therefore based upon the following principles, that

page_text: is to say the sterilization of the wort; the aeration of the wort by sterilized air;
the fermentation of the wort protected from non-sterilized air, and under the action
of pure yeast obtained by the previous culture of a determined or selected cell ;
the regulation of a temperature which is nearly uniform during the fermentation
the filtration of the wine after fermentation in filters constructed so that the juice
and yeast which they contain will remain protected from the air and any germ
foreign to the yeast furthermore the neutralization or slight alkalization of
the fermented juice, the distillation of the neutral slightly alkaline juice; and the
distillation upon an acid salt.
By effecting the fermentation of the sterilized juice under protection from the
air and under the action of a pure yeast I obviate the oxidizing action of the acetic
ferment and consequently the destruction of part of the alcohol formed. I also
prevent the formation of superior alcohol produced either by the life of the butyric
ferment or by the nascent hydrogen acting upon the glucose, and caused by the
butyric ferment. I also prevent the original acidity of the juice from increasing
materially.
Butyric and acetic ferments not being present I obviate the transformation of
the sugar into butyric acid by the first and the transformation of part of the alcohol
into aldehyde and into acetic acid by the second.
Accordingly I obviate these two causes of the production of acids, and therefore
the production of ethers.
There remains however one cause depending upon the life of the yeast. The
albuminoid substances in the juice or as above-stated even those contained in the
cells of yeast which are already dead yield acids, ammonia, and amidated acids on
becoming hydrated.
When the acids are once formed whatever may be their source, they will produce
ethers, especially when the acidified wine is distilled with a mineral acid.
For obviating this etherifications and for destroying the ethers already formed
I distil the neutral or very slightly alkaline wine in my process.
But as the products of an ammoniacal nature which arise, like the acids, from the
decomposition of albuminoid substance in yeast or that contained in the juice may
proceed to the distillation, I distil a second time upon an acid salt capable of
forming with these substances a stable double salt. For this purpose use can be
made of an acid salt or a salt such as aluminium sulphate.
By my process I therefore obviate during the fermentation the formation of
aldehydes amylic butyric and other alcohols; and part of the acids.
;
We obviate the production of ethers (acetates ethyl butyrates and the like)
during the distillation of the wine by distilling this alkalized wine. For retaining
the ammoniacal products a second distillation of the alcohol obtained by the first
distillation is if necessary performed upon an acid salt such as potassium or sodium
tartrate or upon aluminium sulphate.
In the accompanying drawing I have shown how my said invention may be
conveniently and advantageously carried into practice.
The sterilization can be effected by any suitable means. I preferably sterilize
Use can
by superheating as being one of the simplest and most convenient modes.
also be made of filtration upon porous partitions. The sterilization by superheating
is performed by heating the juice for about twenty minutes at 125 degrees
Centigrade. The heating is effected through the medium of a movable coil A in
which steam is caused to circulate. This coil is provided in a vessel B wherein it
is adapted to turn upon its axis in order to serve as a stirrer for maintaining a
uniform temperature in all the parts of the vessel. For this purpose it extends
through a stuffing box at the upper part of the vessel and a tight joint is formed
at the lower part of the same. The aforesaid vessel B containing the coil is closed
and operates as a juice-pump.
The sterilized juices are caused to pass to a bent pipe or coil C placed in an open
vessel D wherein cold water circulates in the opposite direction to that of the
movement of the juice the latter being thus cooled to about 20 degrees Centigrade.

page_text: The coil has been previously sterilized by steam.
be coupled together.
Two similar refrigerators can
The above mentioned apparatus comprises a vessel D in which is arranged a pipe
beut upon itself alternately in a horizontal and in a vertical plane so as to provide
a large surface of contact with the cooling liquid.
Between the horizontal portions of the coil are arranged partitions alternately
to the right and left hand side of the vessel D containing the coil so as to cause
the cooling current to take a circuitous path and prolong its contact with the coal.
The hot pieces enter the coil at the upper part whilst the cold water or the cold
juices enter the vessel at the lower part below the first partition or baffle plate and
circulate therein around the coil. There are two currents, one hot and the other
cold, which pass in opposite directions, this being a necessary condition for a good
and effective operation.
From the above-mentioned coil the juices are conducted under protection from
the air to a closed filter, comprising a vessel E which is divided into two parts by
a filter cloth F. Steam is previously introduced in order to expel the air and after
the air has been forced out the cock R¹ for the escape of the air is closed, for some
time, the steam being left therein at a pressure of about 2 kilogrammes in this
vessel whereupon the cock R' for the introduction of the steam is closed, and a
cock R³ for the admission of the juice is opened. The condensation of the steam
causes the filtration of the juice through the cloth.
From the said filter the juice is caused to pass to an aerating vessel G filled with
sterilized air wherein it is charged with oxygen. Having entered the upper part
of this vessel through a rose, the juice descends upon a series of metallic
diaphragms H H H formed of perforated plates. These diaphragms are slightly
inclined from the centre to the circumference the inclination of two consecutive
diaphragms being in opposite directions. The aerating vessel communicates on the
one hand through a pipe I, with the general steam pipe and on the other hand
through a branch pipe K with the vessel containing sterilized air.
From the aerating vessel the juice flows to a fermenting vessel L which has been
previously sterilized. This vessel has a cover provided with an hydraulic joint for
the purpose of obviating the access of external air. In the centre of this cover is
pierced an opening through which extends a movable coil M similar to the one
arranged in the sterilizing vessel and in the interior of which either water or cold
juices circulate. At the lower part of the vessel is arranged a perforated pipe O
through which sterilized air or steam can be introduced the said pipe communicates
on the one hand through a pipe with the general steam pipe, and on the other hand
through a pipe P with the sterilized air apparatus.
The cover of the said vessel is provided with a series of copper tubes Q of small
diameter which are bent to a helical form and closed by means of a plug of
asbestos covered by another plug of cotton. It is also provided with two pipes
terminating in roses one pipe G being designed to conduct the wort, and the other T
the pure yeast prepared in a small vessel of similar construction.
The air sterilized at a pressure of 1 kilogramme per centimeter serves for the
dabbling. Steam may be introduced in case the temperature should be too low.
The carbonic acid gas produced during the fermentation escapes at the upper part
of the vessel through a pipe Q whose extremity placed in the ambient air is closed
by an asbestos plug covered by a plug of cotton as above stated or preferably by
being plunged into an antiseptic liquid.
The vessel U which consists of metal is sterilized before the juice is admitted
from the aurating vessel. It is strewn with a yeast cultivated with every necessary
precaution and carefully examined before the strewing to make certain of its
purity.
This yeast vessel is provided two cocks, one being arranged quite at its bottom
for completely emptying the vessel and another a little higher for discharging the
material only from part of the vessel, in order to keep leaven in the vessel and
render the preparation of the yeast continuous. This vessel U like the aforesaid

page_text: fermenting vessel, L contains a cold water coil ƒ for maintaining the temperature
constant and at the desired degree.
The pure yeast produced in the above mentioned vessel U is conducted with the
liquid by means of which it has been produced through a pipe T into the sterilized
fermenting vessel, and falls into the latter with its wort in a divided form. Then
the liquid to be fermented is caused to enter little by little through a pipe S in the
form of a shower.
When the vessel is full the fermentation is permitted to take place as soon as the
material is swollen the wine is conducted to a special filter V which enables the
yeast to be collected without exposure to the air.
This filter V comprises a cylinder closed at the top through the medium of a
plate which possesses an orifice for the introduction of the wine; a stuffing box Y
a stirrer, an air
at its centre through which passes a hollow shaft Y₁ carrying
cock Z; and another cock Z which communicates with the sterilized air vessel.
The aforesaid cylinder terminates at its lower part in a cone separated from the
body of the cylinder by a filter cloth W which carries at its centre a metallic part
serving as a support for the shaft of the stirrer. This part serves at the same time
for effecting the discharge from the upper compartment. It is closed by a slide
valve actuated by a shaft 2 which is placed in the interior of the hollow shaft Y¹
of the stirrer in such a manner that the slide valve can be operated from the outside.
The liquid leaves through the openings 5 provided in the conical portion of the said
metallic part.
The conical portion of the filter also comprises a stirrer. This is formed of a
hollow shaft 3 which carries strikers and is supported upon a solid shaft 4 fixed
upon the said metallic part 1. The hollow shaft 3 extends from the filter through
a stuffing-box and carries a pulley through the medium of which the necessary
rotary movement is imparted to it."
The juice which leaves the filter which we have above described passes to a
centralizing vessel W₁ and hence to the distilling column where it is neutralized or
alkalized.
The alcohol produced in this first distillation is subsequently distilled a second
time upon an acid salt, if there is any necessity for it.
The air used in the whole course of the manufacture must as hereinbefore stated
be sterilized. This sterilization is performed by its passage through an iron coil a
heated through the medium of a hearth. The heated air passes into a casing 6x
comprising baffling plates and containing sulphuric acid. Its passage through the
acid deprives the air of any germs which it may still contain.
From the said
casing leads a pipe c passing through a cotton filter b, behind which are branched
off the pipes communicating with the various vessels.
In order to sterilize the aerator the admission pipe R and the discharge pipe S
for the juice and also the admission pipe K for the sterilized air are closed whilst
pass
the coiled pipe d provided with a cotton plug is opened, and steam is caused to
into the aerating vessel. After all the air which this vessel contained has left it
the cock included in the said coiled tube is closed and the pressure is maintained at
2 or 2-5 kilogrammes in the vessel for from 10 to 15 minutes. At the end of this
time the steam admission pipe I is closed. The vessel now cools, and if the admission
pipe K for the sterilized air is opened the latter will enter and ultimately fill the
aerating vessel.
The fermenting vessel L is sterilized by causing water to boil therein through
the medium of the steam dabbling device N. When the steam has passed to the
outside and the boiling has been kept up for from 15 to 20 minutes the steam
admission pipe I connected with the said dabbling device is closed. This device
communicates at P with the sterilized air vessel and permits the passage of sterilized
air into the vessel which is ready to receive the wort.
I have stated that I employ pure yeast in the manufacture, and have described
the means for obtaining it. When the wine has filtered through the special
filter W and is of such a nature as to yield yeast it leaves upon the filter cloth the

page_text: yeast without any foreign substance I propose to bring this yeast which is a kind
of bye product obtained in our process into the market in the form of pure yeast.
For this purpose the pure yeast left upon the cloth of the said filter W is washed
two or three times with sterilized wort, then with sterilized and cold water, and
finally a certain quantity of very diluted sterilized wort is caused to pass into the
filter. The stirrer contained in the filter is set in motion, whereupon the slide
valve is opened. The yeast is conveyed in the form of a pulp into the lower conical
part, whence through special cocks it is put together with the wort in copper bottles
of special shape.
Having now particularly described and ascertained the nature of this 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 herein described process for the manufacture of pure alcohol which
consists in the employment of pure yeast made especially in a continuous manner
and by the aid of a cell previously selected and also in the sterilization of the wort
as well as of the air with which it is in contact, with the object of obviating the
presence of ferments and organized germs in the material under treatment, sub-
stantially as and for the purpose above specified.
Second. With the object of removing all traces of ether which may still be
produced after the fermentation, the distillation of the wine rendered neutral or
slightly alkaline and if necessary a second distillation of the wine upon an acid
salt
Third. The improved apparatus constructed combined and operating substantially
as hereinbefore described and represented in the drawing as and for the purpose
specified.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, W.C., Agents for the Applicant.