Improvements in Processes and Apparatuses for Distillation.
Year: 1894

page_text: Date of Application, 22nd Oct., 1894-Accepted, 2nd Mar., 1895
COMPLETE SPECIFICATION.
Improvements in Processes and Apparatuses for Distillation.
I, ODILON PERRIER, of 30 Quai de Béthune, Paris, in the Republic of France,
Engineer, 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 has for its object improvements which I have made in apparatuses
designed to realise industrially my process of distillation and rectification of all
volatile products such as those described in my English Patent No. 13729 of 1891,
and resins fatty acids, acetic acid, and the like.
In this Patent I have specified the application of an ordinary vertical plate
column A as the distilling apparatus. This vertical column suits very well when
only clear liquids have to be distilled but when muddy liquids more or less thick
have to be treated the distillation effected in the column separates the more fluid
elements and it results that the matter in suspension becomes more and more
concentrated and form deposits which obstruct the apparatus and cause a stoppage
in the course of the distillation.
To remove these inconveniences I replace the vertical plate column by one or more
horizontal or inclined cylinders divided into several parts in their length by
partitions cut away to form overflows. In each cylinder rotates a shaft provided
with perforated helicoidal palettes.
In this Patent I have also described and shown a distilling apparatus formed by
the combination of vertical analysers with condensers of uniform and constant
temperature for the purpose of obtaining the fractional separation of volatile
products exactly identical to themselves by establishing at fixed stages determined
in advance an invariable control of the temperature of the current of vapours in
course of distillation and in the composition and the degree of rectification of the
vapours of this current. I have described for this purpose bead analysers
surrounded by baths of constant temperature and I have also mentioned columns
of plates of any shape surrounded by baths of constant temperature which also
give good results.
I would point out that the object of the analysers is to complete the work of
analysis of the vapours by ridding them of the less volatile products which con-
densation is unable to precipitate from the gaseous mass, and it is for this purpose
that I interpose the dissolvant property which liquids exert on gaseous elements to
neutralise this gaseous diffusion by exposing as much as possible the fluids in a
state of subdivision approaching the molecular condition.
The exchange of calories which also takes place between the condensed liquids
and the vapours is so rapid that the analysis of the vapours is effected without
resource to high temperatures which leads me to prefer horizontal analysers to
vertical analysers. Horizontal analysers enable me to suppress the high rectifying
columns hitherto used.
For this purpose I arrange either, as shown in Fig. 4, a conduit divided into
two superposed parts and in which the lower compartment is filled with beads
whilst the condenser liquid is poured into the upper compartment; or as shown in
Fig. 3 a single horizontal conduit filled with beads and provided at the upper part
with a multi-tubular body g in which is placed the condenser liquid.
The condenser liquids g h &c. enclosed in the series of analysers G H &c. have
temperatures progressively decreasing in such manner that the vapours to le

page_text: fractionally separated passing through the bead compartments G H &c. of this
series of analysers undergo progressive and fixed decreases in temperature which
effect the condensation of the least volatile products and progressive analysis in
their passage on contact with the liquids which moisten the beads.
In these horizontal analysers, the vapours to be separated lose their ascending
speed and their displacement is only effected by the effort of the resulting fluid,
so that the beads produce therein a molecular separation still more complete than
by the vertical columns and their contact with the liquids is still better insured.
In order that the series of horizontal analysers may occupy a moderate length I
divide them into parts which I superpose and I thus obtain the industrial analyser E
shown, Fig. 1.
The complete system of apparatuses enabling me to realise commercially the
distillation, fractional separation and rectification of fermented wort or wine which
I will take as example is represented diagramatically on the annexed drawing.
Fig. 1 shows in elevation the entire system the various apparatuses being
represented in vertical and longitudinal section.
Fig. 2 shows to a larger scale in longitudinal and transverse section a part of
the horizontal distilling column.
The distilling apparatus which allows me to obtain the most economical produc-
tion of the vapours together with their maximum output, whether clear or thick
liquids be dealt with is formed of a horizontal or inclined cylinder divided into
several parts BC by overflow partitions ; this cylinder is traversed lengthwise by
a rotating shaft o carrying perforated palettes & c. This shaft o being actuated by
a continuous rotating movement, the helicoidal perforated palettes c raise the
liquid exposing it in thin layers which flow over the said palettes with the heating
vapours entering by the tube 1 into the cylinder B. These vapours remove the
most volatile products contained in the liquid to be distilled without carrying over
any liquid or over elevation of temperature or pressure. The liquid to be distilled
enters by the tube 26 and its agitation by the palettes & maintains the thick matters
in suspension whilst these helicoidal palettes 6 carry them backwards and forwards
from one compartment to the other. The solid matter is thus rejected in a
continuous manner and the cylinder is always charged with liquid clearer than that
which enters it. Deposits are suppressed.
The partitions (Fig. 2) are pierced in the centre with an opening u² allowing
the passage of a rotating shaft o. This opening is cut away at the lower part to
a line uu forming an overflow to allow the liquid to flow from one compartment
to the other, in the direction of the arrow a, the horizontal overflow u ul limits
the level of the liquid in each compartment of the cylinder. The overflows u¹ u¹
have progressively decreasing levels from one compartment to another in the
direction of the arrow a.
The shaft o turns in the direction shown by the arrow Fig. 2 it causes the
helicoidal perforated palettes b to continuously urge the liquid towards the outlet 30
and to displace longitudinally towards this outlet the thick matters held in
suspension in the liquid by the movement of the palettes ; these matters then
accumulate against the partitions u and are thrown from one compartment to
another. The more liquid parts escape from the propelling action of the palettes
by passing through their perforations and maintain the level constant in each
compartment.
As the overflows u₁ u have decreasing levels it results that the liquid as it
approaches the outlet 30 is exposed in a smaller and smaller volume to the action
of a mass of heating vapour entering by the tube 1 becoming larger in volume and
higher in temperature. Furthermore these differences of level prevent any return
of the liquid and any mixture between liquids unequally treated.
In the compartments C into which enter only clear liquids returned by the
analysers and washers I J the belicoidal palettes may be replaced by perforated
discs.
In order to rotate the shaft o I make the toothed wheel o' engage in a pinion m¹
J. i

page_text: keyed on the shaft m of a hydraulic motor M which rotates under the pressure of
the water of condensation arriving by the tube a aud falling in the buckets of this
motor M. The movement of the palettes b and c is thus protected from any outside
cause of stoppage.
The analysers are formed of receptacles E composed of superposed rectangular
or other chambers horizontal or more or less inclined in which are alternately in
one the vapours to be fractioned and rectified, in the other, condenser liquids. The
chambers through which the vapours pass are formed with corrugations and are
filled with beads in porcelain or other refractory material which reduce the current
of vapours to a state of extreme subdivision. The vapours circulate horizontally
in each chamber around the beads and pass through the interstices left between
them. During this circulation of the vapours as the beads touch the surface of
the chamber which is in contact with the condenser liquid the vapours partially
condense in contact with these beads and the condensed liquid flows in a thin layer
over the circumference of the beads moistens them and establishes an intimate
molecular contact between the vapours and their condensed liquids which completes
the rectification of the vapours by submitting them to an analyser at the same
temperature as that at which they are treated.
To obtain in each analyser a single and automatically invariable temperature I
effect the condensation by means of condensing liquids brought to their boiling
point.
I introduce into the condensing surface chambers condensing liquids the boiling
points of which correspond with the exact temperatures which I wish to obtain for
each analyser taking care to establish boiling temperatures progressively decreasing
from one analyser to the next starting from the heating apparatus.
As soon as the current of distilled vapours coming from the cylinder B C
through the tube 4 passes through the various analysers F G H KL their
respective condensing liquids f g h klare progressively and automatically
brought to the boiling point and the degree of temperature is thenceforth maintained
invariable in cach analyser during the continuance of the distillation whatever
may be the variations produced in the intensity of the current of distilled
vapours.
To give the apparatus a uniform and invariable output I arrange at the outlet
of the distilling cylinder B C an apparatus D through which the vapours pass and
in which a temperature meter enables the introduction of the liquids to be distilled
into the column B through the tube 25 to be automatically regulated.
This feed regulator is composed of a receptacle D containing either some bulbs d
or a tubular arrangement in which is isolated a more or less volatile liquid as for
example water or alcoholised water; this fluid is then exposed over a large surface
to contact with the vapours being distilled and which enter by the tube 3 and pass
through the receptacle D.
The closed space d is shut off by a flexible diaphragm in such manner that
when the fluid contained therein becomes heated under the influence of the excess
of temperature transmitted thereto by the vapours in course of distillation the
tension of the vapours increases and more or less raises the diaphragm . By
the intermediation of the rigid rod and the lever arm q' these movements are
transmitted to the valve w¹ through which the liquid enters and the displacements
of which follow the variations of temperature which may take place in the vapours
on their passage through the receptacle D.
The distilled vapours thus enter by the tube 4 the analysers under a constant
volume due to the constant pressure maintained by the pressure regulator P. in the
cylinder B C. They enter therein furthermore with a constant composition due to
the invariable temperature maintained in the current of vapour by the feed
regulator D of the liquid to be distilled.
The apparatus comprises furthermore vertical plate colunins I J performing the
functions of washers, condensers ST containing coils in which circulate the vapours
emitted by the condensing liquids in the baths f g h kl; these vapours condense

page_text: therein before returning to their respective baths always kept boiling by the
vapours to be fractionally separated which circulate continuously in the
analysers F G H K L, a refrigerator R to cool the products separated and a float
pressure regulator P which regulates the entry of the heating vapour by opening
to a larger or smaller extent the cock p according to the greater or lesser pressure
of vapour resulting from the evaporation of the liquid to be distilled passing
through the cylinder B C.
In order to allow the operation of my apparatus as a whole to be better under-
stood will describe the progress of the liquids and vapours in the various parts
composing it.
Progress of fermented liquid or wine. The wine stored in the reservoir V is led
by the tube 24 into the condenser S in which it reaches a constant level regulated
by the float s. The wine leaving this condenser is conducted through the tube 25
into a second constant level heater U from which it flows into the cylinder B
through the tube 26. The wine is then submitted to the agitation and propulsion
of the perforated helicoidal palettes & which effect its overflow from one compartment
into the next until it reaches the outlet orifice 30.
It then enters the automatic purifier Z the level of which is constant and which
drives out the residual liquid or wine either into a heater or directly into the
atmosphere.
Progress of the vapours. The heating vapour enters the cylinder BC by the
tube 1 it is progressively enriched with the alcoholic vapours by its direct and
multiple contact with the liquids richer and richer in alcohol first the wine in the
compartments B and then the returned products which reach the parts C by the
tube 35.
The alcoholic vapours then escape from the cylinder C through the tube 3 pass
through the feed regulator D and communicate their heat to the liquid contained
in the bulbs d. The variations of temperature in this liquid modify the tension of
these vapours and the latter act with more or less intensity on the diaphragm
and in consequence on the inlet cock w' of the wine. This cock opens when the
temperature of the alcoholic vapours rises and closes when this temperature falls.
The alcoholic vapours leaving D through the tube 4 pass into the analyser F
(called amylic retainer) in which they give up the major portion of the amylic
products by reason of the constant temperature of the condensing liquid in the
bath which precipitates them from the gaseous current. The condensed liquid is
directed through the tube 37 either into a special retaining vessel in order to con-
centrate them separately or into an annexed analysing group N K L which allows
their immediate concentration to be effected.
In the latter case, the condensed liquid in F is directed by the tube 37 into the
boiler N where a coil n raises it to the boiling point. The vapours produced are
fractioned in the analysers Kk Ll. The most aqueous products condense in the
analyser K and fall again into the boiler N whence the overflow pipe 38 leads
them back into the cylinder C by the tube 35. The amylic and alcoholic products
reach the analyser L which condenses the amylic products and they are extracted
therefrom by the tube 39 and directed into one of the coils of the refrigerator R
where they are cooled. The more volatile alcohol cannot be condeused by the
condensing liquid 1; it escapes through the pipe 23 into the condenser S to return
by the tube 45 into the general circulation.
The alcoholic vapours which we have left in the analyser F penetrate by the
tube 5 into the analyser G where they undergo in their passage through the various
stages of this analyser a cooling due to the temperature of the condensing liquid
of which the boiling point determines exactly the class of alcoholic vapours
escaping therefrom. The vapours not condensed pass through the tube 7 into the
alcoholic washer I where refined and boiling alcohol spread over the plates of this
vertical column I expends. on these vapours its dissolvant property and retains the
last traces of the less volatile products which may be incorporated therein by
gaseous diffusion.

page_text: The vapours thus purified from all products less volatile thau alcohol pass
through the tube 9 into the analyser H where the condensing liquid h maintains a
fairly low temperature (about 70% Centigrade) to condense the alcohol. This
temperature is too high to permit the aldehydes and other higher products to
condense therein so that these products escape by the tube 10 into the washer J on.
the plates of which they give up the alcohol carried by gaseous diffusion whilst
the vapours pass away through the tube 12 and are condensed in one of the coils:
of the refrigerator R.
The alcohol condensed in the analyser H flows through the tube 43 into one of
the coils of the refrigerator R where it is collected.
The vapours emitted by the condensing liquids forming the constant temperature
baths gk escape respectively through the tubes 17, 18 19. 20, 21 and are
condensed separately in the coils placed in the condensers ST, the condensed
liquids returning at once to their respective baths through the tubes 47, 48, 49, 50
and 51. A safety pipe connected with each of these coils serves for the discharge
of the air at the commencement of the distillation and then allows a column of
mercury to be interposed of invariable height which ensures the maintenance of
the constant pressure in the condensing baths f g h k land consequently the constancy
of the boiling point of the condensing liquid.
The retrograded alcoholic products coming from the analysers G and K and the
washer J return through the tubes 36, 38, 44 into the pipe 35 which leads them
again into the cylinder C.
The pressure regulator P automatically regulates the pressure of the vapours
within the apparatus. It allows the modification at will and by sharp or gradual
degrees of the amount of pressure by varying the weight of the hollow float P.
But as long as the weight remains the same the amount of pressure also remains
constant.
The refrigerating water contained in the reservoir A flows into the various.
apparatuses by the tubes a.
The apparatus above described may be varied in the construction and the number
of its parts according to the nature of the liquid to be distilled and as to whether it
is desired to extract a larger number of fractional products.
In the case where the above apparatus serves for the distillation and rectification
of alcohols:-The condensing bath of the analyser F is formed either of ethylic
alcohol alone or of alcohol to which a small quantity of methylene is added.
The condensing bath of the large analyser G which serves to fix the alcoholic
degree of the alcohol obtained, is formed by about half each of ethylic alcohol and
methylic alcohol.
The condensing bath H serving to separate the aldehydes and the ethylic alcohol
ethers is also formed of ethylic alcohol and methylic alcohol but the mixture.
contains a little more methylic alcohol.
The condensing baths K'and L are formed of a mixture of the same alcohols but
in proportions based on the boiling point which it is desired to obtain.
The baths enclosed in closed vessels are indecomposable by the most prolonged
boiling so that their boiling point remains constant.
Having now particularly described and ascertained the nature of my said inven-.
tion and in what manner the same is to be performed, 1 declare that what I
claim is :-
1. A process of distillation and of rectification applicable to all volatile products
in which the production of vapour is effected at a low temperature in one or several
horizontal or inclined cylinders divided over its length into compartments by
partitions the said partitions being cut away to form overflows having heights
progressively diminishing which maintain differences in level from one compartment
to the other for the purpose of exposing smaller and smaller volumes of liquid to.
contact with a mass of heating vapour larger and larger in bulk, and hotter; the
said cylinder is traversed lengthwise by a rotating shaft on which are fixed

page_text: helicoidal palettes preferably perforated which agitate the liquid and throw the
thick matters in suspension in the liquid from one compartment into the next to
avoid their forming a deposit, substantially as described and shown and for the
purposes specified.
2. A process of distillation effecting under continuous operation the automatic
fractional separation and rectification of all volatile products by forcing the distilled
vapours to traverse successive superposed horizontal analysers formed either of a
divided conduit in which the lower compartment is filled. with beads whilst the
liquid constituting the condensing bath is poured into the upper bath or of a single
horizontal or inclined tube filled with beads and provided at its upper part with a
multitubular body in which is the liquid constituting the condensing bath; these
arrangements being adapted so that the vapours to be fractionally distilled may be
exposed in each horizontal analyser to the. molecular and direct contact of the
products which are exclusively condensed by the condensing bath annexed to each
analyser whether it be composed of one or more stages substantially as described
and shown in Figures 1, 4 and 5 of the annexed drawing.
3. The parts as a whole constituting my apparatus for distilling, fractioning and
rectifying volatile liquids such as alcohols, petroleums, tars, resins, essences, fatty.
bodies, acetic acid etc., as described and shown in the annexed drawings and for the
purposes specified.
Dated this 22nd day of October 1894.
WHEATLEY & MACKENZIE,
40, Chancery Lane, London, W.C., Agents.