A New or Improved Process and Apparatus for the Distillation and Rectification of Alcohols.
Year: 1890

page_text: SOME LEIE SPECIFICATION.
[Communicated from abroad by FLORE HAECK, of No. 68, Avenue d'Auderghem,
Brussels, in the Kingdom of Belgium, Widow.]
A New or Improved Process and Apparatus for the Distillation and
Rectification of Alcohols.
I WILLIAM THOMAS WHITEMAN of No. 7 Staple Inn in the County of Middlesex
Patent Agent 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 consists in the new process hereinafter described for the distillation
and rectification of alcohols of every origin and the new or improved apparatus
also hereinafter described for carrying out the said process.
The said process consists in a series of operations the objects of which are as
follows:-
1. The separation from the must or raw wort of the matters which are in suspension
therein.
2. The extraction from the must or raw wort of the matters called "bad head
flavours" (aldehydes ordinary ether acetic ether) and." bad tail flavours" (propylic
alcohol butylic alcohol amylic alcohol).
3. The extraction from the must or wort from which the bad head and tail flavours
have been eliminated of ethylic alcohol concentrated to a very high degree and in
certain cases brandies of great aromatic richness.
4. The elimination from the concentrated ethylic alcohol and from the brandies
arising from the preceding operations of the poisonous gases contained therein.
In order that the invention may be properly understood each of the four successive
operations and the apparatus used for carrying them out are hereinafter separately
described with reference to the accompanying Drawings.
Figure 1 of the said Drawings is a vertical section of the receiver in which the
must or the raw wort is placed and of the filters by which the first operation is
effected.
Figure 1 is a sectional plan of one of the filters the section being taken on the
line LL Figure 1.
Figure 2 is an elevation (partly in vertical section) of the distillation apparatus for
the extraction of the bad head and tail flavours.
Figure 3 is an elevation (partly in vertical section) of the apparatus for the production
of the ethylic alcohol.
Figure 4 is an elevation (partly in vertical section) of the apparatus for the
elimination of the poisonous gases.
FILTERS.
Referring to Figure 1 of the Drawings A is a cylindrical vessel which receives the
must or the raw wort to be treated which is introduced through the aperture a. It is
provided with an agitator B furnished with paddles P for mixing the must or wort.
A tube N shows the level of the must or wort in the said vessel A. C is a pipe
provided with a tap R through which the must or wort flows into the upper filter.
Although I have only shown two filters a larger number may be used if deemed
necessary.
The said filters consist of a pocket or bag of conical form 6 ellipsoidal at the top
and round at the bottom and made of the stuff called by the French "Molleton "or
of any other suitable textile fabric lined on the inside with a filtering layer formed of
paper pulp 6' adhering to the said stuff. In order to prevent the pocket or bag b
from getting out of shape it may be surrounded by a cage formed of bars arranged at

page_text: some distance apart (not shown on the drawing). The bottom of the bag b is attached
to a perforated disc c which forms the cover of a lower chamber d at the bottom of the
filter. The upper edge of the said bag bis also attached to the bottom e of an upper
chamber or reservoir f. Access of atmospheric air to the interior of the bag bis
provided for by means of a pipe g. A movable lid closes the chamber f. The said
chamber f communicates with the lower chamber d by means of a pipe k. i is a case
which surrounds the filter on all sides. This case is furnished with apertures which
admit of access to the interior thereof for renewing the bag b. m is an overflow pipe
which connects the chamber f with a reservoir `n. 7 is a pipe which connects the
bottom of the case of one filter with the upper chamber f¹ of the filter placed
immediately beneath. o is a pipe analogous to the pipe 7 which connects the bottom
of the case of the last filter or lower filter with a reservoir g destined to receive the
filtered or clarified alcoholic must or wort. The apparatus works as follows:
The raw alcoholic wort or the must which is to be operated upon must first of all
be freed from the substances which can be eliminated by filtration.
It is first of all introduced through the aperture a into the receiver A and if its
alcoholic strength is above 30 per cent. it is reduced to 30 per cent. by an addition of
water in order to set at liberty in a state of suspension the substances which are but
little or not at all dissolved in a weak mixture of water and alcohol.
-894
The agitator B is then operated in order to produce a homogeneous mixture after
which the tap R of the pipe C is opened through which the raw wort or must passés
into the upper chamber of the upper filter D whence it is conducted by the pipes k
into the lower chamber or compartment d of the filter.
From there it rises through the holes in the disc c and passes into the filtering bag
which it gradually fills. The liquid part of the must or wort filters through the paper
pulp and the stuff 6 of the bag and flows into the case of the filter while the
substances which were in suspension in the wort are retained in the bag in consequence
of the tenuity, of the filtering material.
1441
From the upper filter D the filtered must or wort flows through the pipe into the
upper compartment 1 of the second filter D¹ whence it passes through the pipe k¹ into
the chamber d and thence into the bag to undergo a second filtration. If more than
two filters are used the same operation is repeated with each of them.
On leaving the last filter the clarified must or wort is conducted through a pipe o
into the reservoir q.
If in consequence of the accumulation of the substances retained by the paper
pulp of one of the filters the latter should become choked and should no longer
act, the must or wort accumulated in the chambers for f¹ would flow through the
pipe m or m² into a reservoir n whence it can be withdrawn to be poured again into
the receiver A.
111
"When the filtering bag is thus choked it is removed from the filter in order to be
replaced by another one and it may be rendered fit for reuse by being washed in hot
water.
!
**
\*477
DISTILLING APPARATUS FOR THE ELIMINATION OF THE SUBSTANCES OALLED BAD
HEAD AND TAIL FLAVOURS.
J
This apparatus represented in Figure 2 consists of a boiler I which communicates
by pipe R furnished with a tap running out into the bottom of the boiler I
with a steam generator not shown in the drawing and the top of which ends in a
conduit pipe which runs into the bottom of a distilling column I, formed of
superimposed cylindrical sections. This column. L is enclosed in a chamber K which
communicates by a pipe P provided with a tap P¹ with a cold water reservoir Qand.
by a pipe R provided with a tap R¹ with the steam generator. The lower sections
of the column L are separated' from each other by discs d pierced with large
apertures provided with tubes M which are a little higher than the vertical overflow
tubes e placed close to the walls of the column L. The tubes M are covered with
caps m.

page_text: The upper sections p of the column L are not separated by discs like the lower
sections but each of the lower sections land of the upper sections p is traversed by
two series of pipes N arranged crosswise in the sections. The interior of these
pipes N are open at both ends to the chamber K which is in free communication with
the latter. The chamber K is likewise provided with an overflow pipe T the upper
end of which is almost level with the summit of the column. This pipe T ends in a
collector U provided with a thermometer and a discharge tap. The chamber K is
likewise provided at the bottom with a let off tap k. The bottom of the column L
communicates by means of a pipe W with a receiver V which is connected at the top
and at the bottom with a second identical receiver V₁ which likewise communicates
by a pipe X furnished with a tap with the boiler I. By means of a pipe Z provided
with a tap z the receiver V communicates at top with the bottom of a collector =
furnished with a discharge tap z. Y is a pipe provided with a tap y' which connects
the boiler I with the bottom of the reservoir 7 shown in Figure 1. The top of the
distilling column L communicates by means of a pipe S with a refrigerating
condenser A enclosed in a chamber or case f provided with a lid fi through which the
pipe S passes a¹ is a cylinder with a conical bottom in which is placed a second
cylinder a² of the same form the conical bottom of which is closed but the top of
which opens into the case f. The space comprised between the two cylinders is
completely closed except at the top at the place where the pipe S runs out and at the
bottom where it ends in a pipe c' d' of zigzag shape and preferably with a flat bottom
the lower extremity of which pipe runs out into a collector e provided with a
discharge tap. A considerable swelling all round the upper part of the interior
cylinder a² at the part to which the pipe S is connected facilitates the distribution of
the vapours around the interior cylinder a in the space between the two cylinders.
The chamber or case f and the cylinder a² are filled with water or some other
refrigerating liquid intended to produce the condensation of the vapours coming out
of the pipe S.
This apparatus acts as follows:-
By opening the tap y₁ of the pipe y communication is opened between the
reservoir (Figure 1) containing the filtered must or wort and the boiler I. The
said boiler is charged with filtered must or wort and the tap y' is then closed.
The tap P of the pipe P which comes from the cold water reservoir Q and runs
into the chamber K is then opened. Similarly the tap is opened on the pipe R
coming from the steam generator combining the heating action of the steam with the
refrigerating action of the water from the reservoir Q so as to raise and maintain the
water which has just filled the chamber K and the pipes N to a temperature of
22 degrees to 24 degrees Centigrade.
The tap R is also opened on the pipe R running from the generator to the
boiler 1 and the filtered must or wort therein is raised to and maintained at a
temperature of 22 degrees to 25 degrees Centigrade.
At this temperature the aldehydes which constitute one of the bad flavour head
matters to be extracted from the must or wort and the evaporating temperature of
which is 22 degrees Centigrade evaporate rise out of the boiler through the conduit
pipe J and pass into the column L where they rise from section to section passing
through the apertures M of the discs d. During their ascent these vapours pass
round the pipes N and concentrate while separating themselves from the substances
brought with them the boiling points of which are above 24 degrees Centigrade that
being the temperature of the water which surrounds the column L and fills the
pipes N.
On reaching the top of the column L the vapours of the aldehydes escape through
the pipe S which conveys them to the refrigerating condenser A between the two
cylinders a' a'. The said vapours pass round the cylinder a' in' consequence of the
swelling and they descend in a thin layer in the zig-zag pipe e d¹ which directs
them in a liquid state to the collector e¹ where the liquid accumulatės.
As to the substances (the boiling points of which are above 24 degrees Centigrade)
which have become separated from the aldehyde vapours in the column Lin

page_text: consequence of their condensation in contact with the pipes N they deposit themselves
upon the discs d and descend again through the pipes e to the bottom of the column L
whence they flow through the pipe W into the receiver V.
As soon as it is perceived that no more aldehydes are coming into the collector e¹
.the temperature of the water in the chamber V and in the pipes N is raised by means
of the steam pipe R in the generator to about 53 degrees to 56 degrees Centigrade and
the temperature of the must or wort in the boiler I is also raised to about 53 degrees
to 56 degrees Centigrade. At that temperature the ordinary ether contained in the
must or wort evaporates its boiling point being 53 degrees Centigrade and its vapours
follow the same course as the aldehyde vapours leaving in the column L those matters
of which the boiling points are above 56 degrees Centigrade. These matters descend
again from the column L through the pipes e e e and are directed by the pipe W to
the receiver V as in the previous case.
The vapours of ordinary ether pass from the column L into the refrigerator A
where they are condensed and can be collected upon leaving the collector e¹.
When the last traces of ordinary ether have been collected upon leaving the
.collector e the water in the chamber K and the must or wort in the boiler I are
raised to and maintained at a temperature of 73 degrees to 76 degrees Centigrade.
At this temperature the acetic ether evaporates; its vapours rise in the column L
while ridding themselves of the matters of which the boiling points are above
76 degrees Centigrade. Thence they pass into the refrigerator A and can be collected
as in the previous operations in a liquid state in the collector e' while the matters
which they have left in the column L are directed to the receiver V by the pipe W.
When the last portions of acetic ether have come out of the refrigerator A the
temperature of the must or wort in the boiler I is on the one hand raised to 85 degrees
Centigrade and on the other hand the temperature of the water in the chamber K
of the pipes N is reduced to about 50 degrees Centigrade and the distillation is
continued.
The propylic butylic and amylic alcohols are only feebly dissolved in an alcoholic
phlegm containing 30 per cent. of alcohol the density of which phlegm is about
0.967 per cent. of alcohol while that of propylic alcohol is 0.800 that of butylic
alcohol 0.810 and that of amylic alcohol 0.815. The result is that the natural
tendency of these bad flavour tail alcohols is to rise to the surface of the must or
wort in the boiler I and there to form a thin layer. The distillation vapours of the
aldehydes of the ordinary ether and of the acetic ether as also the vapours produced
by the heating of the must or wort to 85 degrees Centigrade must necessarily traverse
this layer in order to reach the column L. In traversing it these vapours mechanically
carry away with them successive portions and deposit thein in the first section or
sections of the column L.
The ascent of these propylic butylic and amylic alcohols towards the summit of the
column L is prevented by the temperature of the water in the chamber K and the
pipes N which never exceeds 76 degrees Centigrade in the operations previously
described. They are therefore condensed upon contact with these pipes N and they
descend again to the bottom of the column L and as the projection of the conduit
pipe J prevents them from returning to the boiler they flow through the pipe W into
the receiver V which communicates at top and bottom with the receiver V₁. The
.latter is connected at the bottom with the boiler I so that when the specific density of
the liquid in the boiler I increases that of the liquids in the receivers V and Vi
increases in the same proportion. For this reason the bad tail flavours (propylic
butylic and amylic alcohols) which by reason of their lower density have formed a
floating layer in the boiler I and which have been mechanically conveyed into the
column L form upon leaving the latter a floating layer at the top of the liquid in the
receivers V and VI and cannot for that reason return to the boiler I. They pass from
the receiver V through the pipe Z into the collector where they may be collected.
When the sample drawn from the tap ¹ no longer shows the presence of bad
flavour tail alcohols it may be concluded that the latter have been entirely extracted
from the must or wort in the boiler.

page_text: APPARATUS FOR THE PRODUCTION OF CONCENTRATED ETHYLIC ALCOHOL.
This apparatus shown in Figure 3 of the accompanying Drawings has considerable
analogy with the distilling apparatus represented in Figure 2 which has just been
described. It consists of a boiler I connected with the boiler I of Figure 2 by a
pipe. The boiler l' communicates with the steam generator by a pipe R furnished
with a tap R running out into the bottom of the boiler I¹. A conduit pipe J' at the
top of the boiler communicates between the latter and the column L' which is
similar to the column L of the apparatus in Figure 2 but of larger dimensions.
The reason why the column L is larger than the column L is that the quantities of
concentrated ethylic alcohol (and brandy) to be produced by the column Lare much
greater than the quantities of bad flavour head and tail alcohols which have to be
separated from the must or wort by the column L.
The column L' is enclosed in a chamber K¹ connected with the steam generator by
a pipe G provided with a tap G₁ and with the cold water reservoir Q by a pipe Pi
provided with a tap P. The top of the column L' communicates by a pipe S¹ with
a refrigerating condenser A similar to the one in the apparatus of Figure 2 but of
larger dimensions. dare the discs which separate the lower sections of the
column L. Mare apertures in the disc d' provided with tubes and caps m¹. N¹ are
pipes which traverse each of the sections of the column L'. W₁ is a pipe which
conveys to the receiver V2 the liquids which descend from the column L' through the
pipes e. The receiver V2 is connected at the bottom with the boiler I by a pipe X'.
I is the discharge tap of the boiler. I. k is the discharge tap of the chamber K
and T is an overflow pipe running from the top of the chamber K¹ to a collector U'
furnished with a tap U and a thermometer which shows the temperature of the water
in the chamber K'.
a
The refrigerating condenser A' is arranged like A of the distilling apparatus
Figure 2. It is formed of a chamber or case f' containing the refrigerating liquid
and provided with a lid f³ through which passes the pipe S' which is connected with
swelling formed round the top of the cylinder at which is placed inside the
cylinder a in such a way as to leave between them a free space for the passage of the
vapours. The conical bottom of the outer cylinder a³ ends in a zig-zag pipe c d like
that of the refrigerator A in Figure 2. The pipe d² runs into a collector e furnished
with a discharge tape and an areometer which is not shown in the drawing to indicate
the degree of the alcohols and brandies collected in the collector e².
This apparatus works as follows.
As soon as the last parts of the bad flavour tail alcohols have been separated from
the wort of the boiler 1 Figure 2 the tap y¹ of the pipe X is opened and the contents
of the boiler I (Figure 2) are passed into the boiler 1. Cold water from the
reservoir is introduced into the chamber K' through the pipe V and by the aid of
the steam pipe G coming from the generator the temperature of the water in the
chamber K is raised to and maintained at 78 degrees Centigrade which is the boiling
point of absolute alcohol.
By means of the steam pipe R² the temperature of the phlegm in the boiler I
is similarly raised to and maintained at between 85 degrees and 88 degrees
Centigrade.
In consequence of the temperature (78 degrees Centigrade) of the water in the
chamber K and in the pipes N the vapours of the ethylic alcohol are the only
vapours which are not condensed in the column L¹. They rise in it from section to
section and concentrate progressively by their separation from the water and such of
the other constituents of the phlegm as have boiling points above 78 degrees
Centigrade.
The water and the said other constituents are condensed upon contact with the
pipes N and descend again in a liquid state to the bottom of the column L' whence
they pass through the pipe W to the receiver V2 and return to the boiler I¹.
The vapours of the ethylic alcohol reach the top of the column L' and pass through

page_text: the temperature of the must or wort to the degree required for obtaining the
successive evaporation of these various matters.
(c) In extracting from the filtered must or wort the matters called bad tail
flavours (propylic alcohol butylic alcohol and amylic alcohol) by preventing
their return to the boiler containing the must or wort after they have been
carried out of it by the vapours resulting from the heating of the said must
or wort.
(d) In extracting from the must or wort freed from the matters called had head.
and tail flavours ethylic alcohol concentrated to a high degree by raising the
temperature of the said must or wort to the degree required for obtaining
the evaporation of the ethylic alcohol and by ridding the vapours of the
ethylic alcohol from those matters of which the degree of evaporation is
higher.
(e) In extracting in certain cases from the phlegm which forms the residue of the
preceding operations brandies of great aromatic richness by continuing the
distillation of this phlegm by naked fire.
(f) In eliminating from the ethylic alcobol and the brandy produced by the two
last operations the poisonous gases which they contained by prolonged heating
in the water bath.
Secondly
t
For the purpose of separating from the raw must or wort the matters
herein held in suspension-the use of a series of superimposed filters in which that
part constituting the filter properly so called is formed of a stuff bag lined on the
nside with paper pulp substantially as hereinbefore described and illustrated in
Figure 1 of the accompanying Drawings.
Thirdly-For the extraction from the filtered must or wort of the matters called
bad head flavours (aldehydes ordinary ether and acetic ether) and the matters called
bad tail flavours (propylic acid butylic acid and amylic acid) the use in combination
with a boiler containing the filtered must or wort and connected with a steam
generator of the apparatus or parts of apparatus hereinafter referred to under
heads "a" """c?
(a) A distilling column enclosed in a water chamber which is connected with
a cold water reservoir and with the steam generator this column being
traversed by pipes communicating with the water chamber the lower part
of the said column being divided into compartments by discs having apertures
formed in them which permit of the ascent of the vapours passing from the
boiler and provided with pipes which permit of the descent of the matters
which separate themselves from the vapours by condensation in the
column.
(b) A refrigerating condenser apparatus communicating with the top of the
distilling column in which condenser the vapours passing from the said
column are condensed by passing first between two cylinders with conical
bases placed one within the other and thence into a zig-zag pipe which
conveys them to a collector.
(c) An arrangement for preventing the return to the boiler of the matters
called bad tail flavours which have been drawn into the column which
arrangement consists of a pipe running from the bottom of the column to
a pair of receivers communicating with each other at the top and at the
bottom and also communicating at the bottom with the boiler and at the
top with a collect or into which the matters called bad tail flavours pass and
in which the said matters collect the whole substantially as above described
and shown in Figure 2 of the accompanying Drawings.
Fourthly The use of apparatus constructed substantially as hereinbefore described
nd illustrated in Figure 3 of the accompanying Drawings for the extraction from
he must or wort which has been freed from the matters called bad head and tail
lavours of ethylic alcohol concentrated to a high degree and in certain cases of

page_text: brandy of great aromatic richness that is to say the use in combination with a boiler
connected with a steam generator and containing the must or wort to be operated
upon of a column surrounded by a water chamber and of a refrigerating condenser
with a collector for receiving the ethylic alcohol and the brandy and of a discharge
pipe for conveying the matters condensed in the column from the bottom of the said
column into a receiver connected with the boiler the said column and chamber and
condenser being of the same general construction as the column the chamber and the
refrigerating condenser referred to in the previous claim but of larger dimensions.
Fifthly The use for the purpose of eliminating the poisonous gases contained in the
ethylic alcohol and in the brandy produced by the preceding operation of an apparatus
consisting essentially of a vessel for containing the matters to be operated upon which
vessel is placed in a second vessel containing water and connected with the steam
generator the top of the inner vessel communicating by means of a pipe with a
refrigerating condenser substantially as hereinbefore described and illustrated in
Figure 4 of the accompanying Drawings.
:
Sixthly The use in combination with the filters referred to in the second claim of
the distilling apparatus referred to in the third claim and the apparatus for the
production of ethylic alcohol referred to in the fourth claim and the apparatus referred
to in the fifth claim for the purpose of eliminating the poisonous gases contained in
the etbylic alcohol and in the brandy produced by the preceding operations.
Dated this 29th day of April 1890.
.
W. T. WHITEMAN.