Improvements in Distilling and Rectifying Alcohol or other Liquids, and in Apparatus employed therein.
Year: 1891

page_text: Date of Application, 14th Aug., 1891
Complete Specification Left, 13th May, 1892-Accepted, 9th July,
1892
PROVISIONAL SPECIFICATION.
Improvements in Distilling and Rectifying Alcohol or other Liquids,
and in Apparatus employed therein.
I, ODILON PERRIER of 23 Boulevard de Strasbourg, Paris, France, Engineer,
do hereby declare the nature of this invention to be as follows:-
The continuous rectification of alcoholic vapors which enter a distilling apparatus
uninterruptedly so as to pass through the various parts thereof requires the classifi-
cation of these vapors, that is to say they must be divided or fractioned at fixed
points or stages. As this classification is only obtained owing to the differences of
temperature which exist at the various points of condensation the classification is
only possible by the vapors being submitted to successive and perfectly defined
lowerings of temperature, each analyzer being assigned an invariable line of
of demarcation in its degree of heat. This problem is completely solved by the
employment of condensers at constant temperatures, condensers in which the baths
for effecting the condensation of the vapors remain at an invariable maximum
temperature, never being able to rise above the fixed degree rigorously determined
beforehand for each of them, and this notwithstanding any variations in intensity,
composition and heat of the currents of vapor submitted to their action in the
course of the operations.
In order to complete the action of these dephlegmators of high degree which
separately would remain powerless to give purified fractional products it is
necessary to annex to each condenser and analyzer acting by direct contact and
exclusively supplied by the products retrograded from the condenser which
corresponds with it.
Fractioning stages are thus formed comprising a condenser at constant temperature
and an analyzer of direct contact or rectifier.
By thus establishing fractioning stages at progressively decreasing temperatures
there are obtained in the continuous work invariable falls of temperature which
automatically classify the fractioned products according to their nature and in their
order of volatility.
A simple and certain way of obtaining these constant temperature baths is to
employ liquids which separately or mixed together have for their boiling point the
precise degree which it is desired to communicate to the condensing baths; the
invariability of this boiling degree thus ensures the invariability of the maximum
temperature of the baths.
I give the above example only to indicate how readily a distiller can form his
baths and vary their degree at will; it is not, however, the nature of the baths nor
the mode of regulating them which primarily forms the subject of this invention
but the employment of condensers at invariable maximum temperatures without
limiting the invention to any particular means for ensuring this invariability of
maximum temperature in each of them.
For analyzers intended to complete the work of the condensers the ordinary plates
can be employed and the constant temperature condensers be arranged above the
columns ordinarily used, but simpler and more energetic means can be adopted
which are hereinafter described in the explanation of the apparatus, arrangements,
however, to which the present invention is not limited.
Proceeding on the principles rigorously observed in exact analyses which require
the division in the molecular state of the products to be analyzed I cause the vapors
to pass through apparatus filled with beads (perles) the perfectly regular dimensions
of which limit in their turn by the regularity of their interstices the spaces simul-
taneously occupied by the fluids to be analyzed.

page_text: 1
This breaking up of the fluids in contact and at determined and invariable
temperatures gives very exact and rapid analyses which dispense with the use of
high columns.
These molecular analyzers on account of their small dimensions have the further
advantage that they can be utilized as condensers. It suffices to jacket them so
that they can be surrounded by baths of constant temperature and be thus formed
into condenser-analyzers which by utilizing the outer walls of the analyzers avoid
useless and costly, height.
It therefore only remains to interpose these analyzers between a very restricted
number of plates in which vapors and condensed liquids interchange or identify
their temperatures up to convergence of degree without any external cooling, and a
prompt and complete analysis under the best conditions is effected.
The apparatus for carrying out the distillation on the principles above set forth
comprises:
1. An exhausting boiler or heater in which the wine, fermented must, or wash
maintained in a thin layer comes in contact with obstructions that cause it to
circulate in contact with the heating device which completely deprives it of all
trace of alcohol before passing into the atmosphere.
2. Distilling plates in which the alcholic distillation is effected owing to the
multiplied and direct contact of the wash with the vapors from the boiler.
3. Rectifying plates through which the vapors become enriched by multiplied
and direct contact with the retrograded liquids from which they remove their more
volatile constituents.
The vapors then arrive at their first fractioning stage and enter the first
analyzing group comprising :-
:-
4. A molecular analyzer surmounted, or preferably surrounded by a constant
temperature condenser.
To the invariable maximum temperature of the constant temperature condenser
.corresponds a minimum limit in the lowering of temperature which the vapors can
undergo. This minimum limit is regulated so as to effect the dehydration of the
vapors, but the head products, the alcohol, and the products of intermediate
volatilization, tail products, remain under tension of vapors and escape from it in
order to undergo the ulterior analyses after having equalized or identified their
temperature with that of their condensed products without any external cooling in
plates above the condenser-analyzer.
5. The vapors then arrive at their second fractioning stage. They enter the
second analyzing group comprising the same parts, analyzer and condenser, which
submit them to similar analyses under the influence of a lower temperature which
the constant temperature condenser defines.
The vapors first meet the condensed products in the second analyzing group,
equalize or identify their temperature with them up to convergence of degree, taking
from them their more volatile products (alcohol) substituting for 'these and 'in
exchange for the heat given up their less volatile products. The retrograde current
thus rectified undergoes a final boiling by a beating device in the last plate and is
then withdrawn from the apparatus, cooled in a refrigerator and collected as
tail product.
The vapors on the other hand continuing to rise undergo molecular analysis at
the temperature fixed by the minimum temperature condenser regulated so as to
maintain under tension the alcoliol and. the head products, but sufficiently low
to arrest and retrograde any product less volatile than alcohol.
6. These last vapors are in their turn separated in a third analyzing, group which
being composed of the same parts causes them to undergo a similar analysis, but
under the influence of a less temperature, which arrests the alcohol the analysis
and extraction are effected while the more volatile head products maintained under
tension effect their condensation in the refrigerator.
7. The refrigerator containing three coils corresponding respectively with, the
three condensed products and a test coil.

page_text: 8 and 9. Two refrigerators one cooling with water and the other with the wine
or wash for condensing the vapors given off by the constant temperature baths, the
condensations being at once returned to their original baths.
Safety tubes allow non-condensable gases to become disengaged from the baths
at the commencement of the operation, so that any loss of vapor in the course of
the distillation is avoided.
10. A float valve keeps the level of the wine or wash constant in the
refrigerator and regulates, with the height of fall of the wine, its introduction into
the apparatus.
11. A heater heated by the vinasse or residue receives the wine or wash from
the refrigerator the wine circulates in a coil immersed in the boiling residue
which raises and regulates the temperature at which it is introduced into the
distilling plates.
12. A pressure regulator composed of two concentric cylinders one of which
acts as a float, is supplied by the residue in the boiler. The internal pressure
causes the residue to rise in the outer cylinder and lifts the float, and this
actuates the lever of the valve that introduces the heating vapors, no stuffing boxes
being required.
The regulator also allows of modifying at will the internal pressure of the
apparatus by modifying the weight of the float by degrees as sensible and as varied
as may be desired.
13. Finally, and especially where the distiller has to treat wines or liquors of
variable alcoholic richness, I employ a temperature regulator which enables the
apparatus in all cases to ensure with their constant maximum output the certain
and complete exhaustion of the vinasses or residues without the distiller having to
trouble himself about variations in strength which the wines or liquors submitted
to distillation may have. The vapors in passing through the jacket of the
temperature regulator communicate their heat to the interior medium which may
be water or other more or less volatile liquid. This is affected by all the variations
of temperature of the surrounding vapors and the dilatation of the liquid added to
the temperature of the vapors which it gives off immediately acts in the one
direction or the other upon the lever of the valve through which the wine enters.
The transmission can be effected either by the variations in weight of the liquid
displaced or by its pressure on a yielding diaphragm.
The apparatus above described can be variously modified to suit particular
circumstances. For the fractioning of products which are very little volatile there
should be a first condensing analyzer either after the distilling plates or before.
When it is desired to concentrate the vinasses it is best to direct the retrograde
liquor to a second boiler having rectifying plates.
The invention is not limited to the distillation of alcohol; it can be applied to
other products obtained by distillation.
1001
J. C. MEWBURN,
55 & 56, Chancery Lane, London, Patent Agent.
COMPLETE SPECIFICATION.
Improvements in Distilling and Rectifying Alcohol or other Liquids,
and in Apparatus employed therein.
I, ODILON PERRIER of 23 Boulevard de Strasbourg, Paris, France, Engineer,
do hereby declare the nature of this invention and in what manner the same is
io be performed, to be particularly described and ascertained in and by the
following statement:-
The continuous rectification of alcoholic vapors which enter a distilling apparatus
uninterruptedly, so as to pass through the various parts thereof requires the classi-
fication of these vapors, that is to say, they must be divided or fractioned at fixed

page_text: points or stages. As with volatile products this classification is only obtained
owing to the differences of temperature which exist between the various points of
condensation of the different gaseous elements composing the mixture; the
classification is only possible by the vapors being submitted to successive and
perfectly defined lowerings of temperature each analyzer being assigned an
invariable line of deinarcation in its degree of heat. This problem is completely
solved by the novel application to the distilling apparatus of condensers having a
uniform and constant temperature in each of them condensers in which the baths
for effecting the condensation of the alcoholic vapors remain at an invariable
uniform temperature which is strictly assigned to them, notwithstanding that the
continual afflux of the alcoholic vapors at a degree of heat which is always higher
tends to raise the temperature of the bath and notwithstanding that these alcoholic
vapors present in their flow variations in intensity, composition and heat which
tend to very differently affect the condenser baths in the course of one operation.
A simple and certain way of obtaining these uniform and constant temperature
baths is to employ liquids which separately or mixed together have for their
boiling point the precise degree which it is desired to assign to the condensing
baths the invariability of the boiling degree thus ensures the invariability of the
maximum temperature of the baths.
:
This fixity in the boiling degree naturally implies constancy in the composition
of the condenser liquids that is to say that the vapors given off during the
boiling should be immediately condensed in independent refrigerators and
reintegrated in their respective baths as soon as they have been restored to the
liquid state.
Stagnant condenser liquids are in a manner obtained which have no other
renewal than that which results from the slight return of their condensed vapors
which come back to their point of departure immediately after having given off to
the refrigerator their latent heat of condensation. The slight liquid current
reintegrated in the mass of the boiling bath becomes dispersed therein and
immediately identifies or equalizes its temperature with that of the bath without at
all affecting the latter, it then becomes charged with caloric given up by the
alcoholic vapors submitted to its action, takes up the latent heat necessary for its
vaporization, and being converted into vapor it again carries to the refrigerator
this excess caloric the loss of which restores it to the liquid state and permits it to
return to the charge. It is a transfer of caloric by way of latent heat, and uniform
temperature in each condenser is ensured and complete. This constancy of degree,
this uniformity of temperature keeps the alcoholic vapors automatically free from
the irregularities of all existing condensers in which recourse is had to currents of
cold or irregularly warmed liquids and the intensity of which varies every moment.
Now in any condenser in which homothermy does not exist there cannot be those
constant separations which cause invariable lowerings of temperature.
The action of these uniform and invariable temperature condensers is completed
in my apparatus by direct contact analyzers in which the vapors remain exclusively
exposed to the products condensed by the corresponding analyzer.
I can employ ordinary plates as analyzers and arrange the condensers either
above or around the columns but I can also adopt simpler means which I explain
in the description of the apparatus.
Proceeding on the principles rigorously observed in exact analyses, 1 expose in
the state of extreme division the fluids submitted to the analysis and with this view
I cause the vapors to pass through apparatus filled with beads (perles) the regular
dimensions of which limit in their turn by the regularity of their insterstices the
spaces simultaneously occupied by the finids to be analyzed.
This breaking up of the fluids in contact, the temperature of which is absolutely
determined and invariable, gives very exact and rapid analyses which dispense
with the use of high columns.
These molecular analyzers on account of their small dimensions and the simplicity
of their construction have the further advantage that they can be utilized as

page_text: condensers. It suffices to jacket them so that they can be surrounded by baths of
constant temperature and be thus formed into condenser-analyzers thereby avoiding
useless and costly height in the apparatus.
Therefore, by arranging analyzer groups each comprising a constant temperature
condenser and a direct contact analyzer or rectifier and by assigning or allotting
to the condensers progressively decreasing temperatures the alcoholic vapors in
traversing these analyzer groups undergo in their turn lowerings of temperature
which are equally determined and constant and effect their fractioning, that is to
say, the classification of the volatile products according to their order of
volatility.
.
The new method or process of fractioning or of effecting classification will be
more fully understood by the following more detailed explanation and by the
annexed drawing which represents an apparatus for carrying out the same.
In this drawing A is a boiler or heater in which the wine, fermented must, or
wash is deprived of all trace of alcohol and which furnishes the steam necessary for
the distillation. This boiler is shown as heated by a steam coil a.
BB are distilling plates in which the alcoholic distillation is effected owing to
the multiplied and direct contact of the wash with the vapors from the boiler A.
CC are rectifying plates in which the vapors become enriched by multiplied
and direct contact with the liquids retrograded by the analyzers or by a chauffe-
vin (or warming apparatus) when such is employed as hereinafter mentioned.
F and Gare the first analyzer group composed of the molecular analyzer F
surrounded by its condenser G. The condenser G is shown in the drawings as
supplied by the liquid retrograded by the condensations effected in the superposed
analyzer K surrounded by a constant temperature bath L; the condenser liquid
is therefore of a temperature intermediate between that of the bath L and that of
the vapors arriving by the tube but as this temperature of the condenser bath
need not be strictly exact as it can vary between 81° and 85° centigrade I can
attain the same results by a chauffe-vin. Whether the condensation be effected by
the one or the other of the means indicated the products condensed in the
analyzer Fare separated from the apparatus and conducted by the outlet pipe 1
to a boiler H surmounted by an analyzer group I, 1', J, in which the classification
of the retrograded products is effected clear of the current of vapor from the
boiler. The boiler H. communicates to the liquid retrograded by the pipe an
increase of temperature which carries it to ebullition. The constant temperature
bath Jeffects the condensation of the less volatile aqueous products which fall
constantly into the boilers whence they are discharged by the overflow pipe 2
which leads them to the distilling plates B. The tail products condensed in their
turn although more volatile tend also to fall into the boilers but the high
temperature of the vapors which they meet in the lower stages drives them higher;
they therefore collect in the upper stage I. Having reached this second part of
the analyzer they meet only a vapor become lukewarm by the suppression of the
aqueous products; on the other hand the outlet pipe 3 removes from these same
vapors all cause of supersaturation; they flow out at 3 and are collected after
cooling in R.
With regard to the alcoholic vapors which are still more volatile they are main-
tained under gaseous tension because of the temperature being too high to effect
their condensation, kept up in this analyzer by the constant temperature bath J ;
they escape in the state of vapor by the pipe 4, their condensation is effected in
the condenser V and they are returned by the pipe 5 to the general body of liquid
and undergo more precise analyses.
The alcoholic vapors after having traversed the first analyzer group F G are
therefore partially dehydrated and deprived of the less volatile impurities. They
then enter the molecular analyzer K surrounded with its constant temperature
bath L. To the uniform and invariable temperature which exists in L corresponds
a minimum limit to the lowering of temperature which the vapors can undergo and
this fall of temperature is regulated so that only the alcohol and the still more

page_text: volatile head products can be maintained at vapor tension as any product less
volatile than alcohol is condensed and retrograded.
The alcoholic vapors this deprived of their less volatile ingredients undergo
in X a final washing in their-condensed products and their temperature becomes
the same as that of the condensed products without any active external refrigera-
tion and this is in order to put into play the coefficient of solubility of the alcohol
in the liquid state upon the amylic and other products which might have been
drawn into the gaseous current by, natural tension or gaseous solution.
The vapors now comprising only alcohol and products more volatile than alcohol
then enter the last analyzer group M N. Under the influence of the degree of
heat maintained in the analyzer M by the constant temperature bath N the alcohol
becomes condensed while the more volatile head products remain under gaseous
tension, are discharged at the upper part and after having, equalized their
temperature in the washer X they are condensed and cooled in the refrigerator R,
to which they are conducted by the pipe 6.
With regard to the condensed alcohol it is drawn off by the overflow pipe g and
conducted to the refrigerator R where it is collected after cooling.
A heating device Q is shown below this analyzer group. It is to volatilize at
the beginning of the operation the head products which become condensed on
coming in contact with the beads and the cold walls.
As regards the washers X X they are represented as composed of perforated
plates on which the vapors bubble in contact with the liquids condensed by the
cold of the outer walls, but the washers may consist of simple molecular analyzers
like those above described.
The refrigerator R contains 3 coils corresponding respectively with the 3 con-
densed and fractioned products from the pipes 3, 6 and 9.
U and V are two refrigerators the one cooling with water and the other with
the wine or wash, for condensing the vapors given off by the constant temperature
baths, the condensations being at once returned to their original baths.
vare safety tubes to allow non-condensable gases to become disengaged
from the baths at the commencement of the operation so that any loss of vapor in
the course of the distillation will be prevented and a constant pressure in the
interior of each condenser bath can be maintained.
A float valve S keeps the level of the wine or wash constant in the refrigerator V
and regulate the speed of the flow by maintaining the height of fall of the wine
constant.
A heater D heated by the vinasse or residue again raises the temperature of the
wine already heated in the refrigerator V by utilizing the lost heat of the vinasse
which continually enters the upper part of the vessel D traversed from top to
bottom by the wine in the coil d which leads to the distilling plates B B.
A regulatory serves to maintain a constant pressure of the vapors within the
apparatus. This regulator is composed of a cylinder y and a float Y, the cylinder
being in direct communication with the boiler A by the pipe 10. The pressure of
the vapors in the boiler A forces wine or wash through the pipe 10 into the
cylinder y and the height it attains in this cylinder depends upon the degree of
the said pressure. Any variation will correspondingly raise or lower the float Y
and thereby through the intermediation of the lever regulate the opening of the
valve z.which controls the supply of steam to the coil a.
Thus as the pressure
in the boiler tends to rise above or fall below the normal, the valve is acted
upon through the intermediation of the float Y and the extent of its opening
reduced or increased as the case may be.
.
The regulator also allows of modifying, at will the internal pressure of the
apparatus by modifying the weight of the float by degrees as small and as varied
as may be desired in the course of the operation.
Finally, and especially where the distiller has to treat wines or liquors of
variable alcoholic richness, it is convenient to be able to automatically vary the
inlet of wine into the apparatus. For this purpose I employ a temperature

page_text: regulator T which enables the apparatus in all cases to ensure with their constant
maximum output the certain and complete exhaustion of the vinasses or residues
without the distiller having to trouble himself about variations in strength which
the wines or liquors submitted to distillation may have. The vapors from the
boiler A pass by the tube into the jacket of the regulator T and thence to
the tube leading to the first analyzer group. The regulator T contains any
suitable liquid and this becomes more or less heated by the vapors according as
their temperature is more or less high. The consequent variations in the dilata-
tion of this liquid as well as the variations in tension of the vapors it gives off
immediately act in the one direction or the other upon the lever of the valve
through which the wine enters. The transmission can be effected either by the
variations in weight of the liquid displaced or as is shown in the drawing by its
pressure on a yielding diaphragm . The pressure regulator by maintaining
constant the internal tension of the alcoholic vapors imparts to them a speed of
flow which is equally constant the volume of the vapors introduced into the
analyzers is therefore always the saine.
The apparatus above described can be variously modified to suit particular
circumstances. For the fractioning of products which are very little volatile there
should be a first condenser-analyzer either after the distilling plates or preferably
before. adopt this last arrangement in the distillation of wines when it is
necessary to collect the very slightly volatile euanthic products.
The invention is not limited to the distillation of alcohol; it can be applied
to other products obtained by distillation such for example as methylenes,
petroleum, tars and essences.
Having now particularly described and ascertained the nature of my said inven-
tion and in what manner the same is to be performed declare that what I
claim is :-
1. In the distillation or rectification of alcohol or other liquids the employment
of condensers each of which has a uniform and constant temperature, substantially
as and for the purpose set forth.
2. In the distillation or rectification of alcohol or other liquids the employment
of condensers each of which has a uniform and constant temperature, such
temperature being maintained by using in each condenser a liquid, the boiling
point of which exactly coincides with the pressure it is desired to maintain in that
condenser, the vapors disengaged therefrom being separately condensed and
immediately returned so as to maintain the invariability of the composition of the
liquid, substantially as and for the purpose set forth.
3. In the distillation or rectification of alcohol or other liquids the employment
of a regulator actuated by the temperature of the vapors which are on their way
to the analyzers so as to automatically regulate the inflow of the wine or liquid
and maintain constant the richness of the vapors produced, substantially as set
forth.
4. Constructing apparatus substantially as hereinbefore described for distilling
or rectifying alcohol or other liquids.
Dated this 12th dov of New 1892
J. C. MEWBURN,
55 & 56, Chancery Lane, London, Chartered Patent Agent.