Improvements in and relating to Continuous Rectification and Distilling Apparatuses
Year: 1899

page_text: Date of Application, 14th Dec., 1899-Accepted. 14th Dec.. 1900
COMPLETE SPECIFICATION.
Improvements in and relating to Continuous Rectification and
Distilling Apparatuses,
I, CHARLES
CREPELLE-FONTAINE, Constructer, of La Madeleine-lez-Lille,
France, 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:-
My present invention relates to improvements in the continuous rectification
of alcohol for the purpose of separating it from ether, by means of a second
purification succeeding the rectification proper, and to certain improvements in
the construction and arrangement of the apparatus for carrying the improved
method of rectifying into practice and securing a regular and automatic working
of said apparatus.
In order that the invention may be readily understood and carried into practical
effect, reference is hereby made to the accompanying drawings, wherein
Fig. 1 is a vertical sectional view of the general arrangement of my
apparatus;
Fig. 2. is a vertical section of my improved test tube
The improved arrangement comprises a first purifier a, formed of a vertically
arranged hollow cylinder, the upper part a of which, is of somewhat smaller
diameter than the body of the purifier. Within said purifier are arranged suitable
horizontal pairs of plates a² ² a².
each one of which carries a short
vertical overflow tube at, whereby the material introduced, through the pipe a³,
into the upper part of the cylinder a may drop from pan to pan a², into the
bottom part of said cylinder. The reduced upper end a is also provided with
horizontally arranged pans or plates a, a6 and with over-flow tubes a, serving
The bottom of
the same purpose as the plates 2 and tubes at in the cylinder a.
the latter is provided with a perforated tube 8, extending through the wall of a
and serving to lead steam into the purifier a.
The apparatus b is termed "a reheater," because it serves to heat the phlegm
coming from the reservoir and prior to the introduction thereof into the first
purifier a.
The latter is connected, by means of the pipe as, to the reheater b, said pipe
extending from the upper part of the latter. Said reheater is formed of a tubu-
Jar apparatus, through which passes, upwardly, the phlegm flowing from a phlegm-
reservoir c, through the pipe 4, into the bottom part of the reheater b, whilst
hot water flows downwardly in said reheater, said hot water coming from the
bottom part of the rectifier (hereinafter described), through the pipe b into the
upper part of the reheater b, said water flowing off through the pipe 3.
When the phlegm is heated in the reheater b, it passes upwardly into the first
purifier a, within which it drops from pan to pan a², through the overflow
tubes a, whilst steam flows from the tube 8, upwardly, in an opposite direction;
this flow of steam may be controlled by means of any desired device (not shown).
The steam causes the ether vapours, more volatile than alcohol, to be volatilized,

page_text: which vapours will be concentrated within the upper part a¹ of the purifier a,
in the condenser d and the cooling apparatus e, the upper part a' of the purifier a
being connected, through the pipe a", to the upper part of the condenser d.
Ether vapours are only separated for the reason that the liquid under treatment
in the apparatus a is in a very impure state and contains about 5% of ether
with respect to the quantity of alcohol. About 4% of ether is separated in a.
Should alcohol or any other liquid (light oils) be volatilized in a, the same will
be liquefied in the condenser d and flow back through the pipe a into the
apparatus a a and drop from pan to pan upon the bottom of a, whilst ether is
liquefied in the coil and flows therefroni through the pipe e into the test
apparatus f
The condenser d is formed of a tubular apparatus similar to the reheater b,
and arranged within a cylindrical casing d¹ into the bottom part of which
discharges a pipe d², leading cold water into same, which is discharged therefrom,
through the pipe 3 at the top of the casing.
Under the condenser d, I arrange the cooling apparatus formed of a coiled
pipe e connected to the condenser d, by means of a pipe e, and the lower end
of which is connected with a pipe e², leading condensed ether into the test
apparatus f, hereinafter described.
The phlegm, from which a certain quantity (4%) of ether has thus been
extracted, flows from the bottom part of the purifier a, through the pipe a,
into the rectifier g.
The rectifier g is formed of a vertically arranged cylindrical casing, in which
I arrange suitable horizontal pairs of plates g¹, similar to the plates a² of the
rectifier a and also provided with overflow-tubes g². Extending into the bottom.
part of the rectifier is a perforated pipe g3 leading steam into the rectifier, the
steam pipe being provided with any suitable device for controlling the pressure
of steam. Above the rectifier 9 is another cylindrical casing g', the interior of
which is also provided with a plurality of horizontally arranged pans or plates g³,
95
each one of which carries an overflow tube The phlegm coming
from the bottom of the first purifier a, through the pipe a10, drops, from pan to
pan g', into the rectifier g, whilst steam passes upwardly from the tube g³, whereby
the remaining quantity of ether and alcohol is separated from the phlegm.
The vapours of alcohol and ether and also light oils flow upwardly into the
casing and are condensed and classified upon the several pans or plates ³.
The oils are condensed and remain upon the pans in the lower part of the
casing, and flow therefrom through the cock g' and pipe 8 into a special
cooling apparatus h, formed of a cylindrical casing, containing a coiled pipe h¹
and into which flows cold water, coming through a pipe h², extending to the
bottom of the casing, the water being afterwards discharged through another
pipe h, at the top of the casing. The coiled tube h¹ is provided with an out-
wardly extending branch h, carrying a suitable test-glass h5, provided with a
thermometer 6, for the purpose of making the usual assays and verifying the
state of the extracting operation. The coil ¹ terminates in a pipe 7, leading to
suitable oil-reservoirs (not shown).
The alcohol and ether vapours, flowing upwards from pan to pan g5 in the
casing g, pass through the pipe g into the condenser i, formed of cylindrical
casing and a plurality of internal vertical tubes, through which flow said vapours
and in which they are partially condensed, by the action of the cold water
flowing, through the pipe ', into the lower part of the condenser and upwards
around the internal tubes of same, said water being afterwards discharged
through the pipe at the top of the condenser. The liquefied vapours flow,
from the condenser i, again downwards, through the pipe into the casing g
where they drop from pan to pan and are separated from the pure alcohol and
ether vapors they contain, the water being finally collected at the bottom of
the rectifier g, whence it flows through the pipe into the reheater, as already
described,

page_text: A mixture of ether and alcoholic vapours, which have not been condensed and
liquefied in the condenser i, flows therefrom through the pipe into a second
purifier k, similar to the first purifier a (already described with reference to the
purification of phlegm) and also provided with pans ¹ and overflow tubes k³;
arranged at the bottom of said second purifier is a coiled steam pipe 3, whereby
the apparatus k is heated to cause the ether and alcohol vapours to flow upwardly
into a condenser 1, hereinafter described. This coil-pipe 3 receives steam through
the pipe, the condensation water flowing off through the pipe .
The ether and alcohol vapours flow from the second purifier k, upwardly,
through the pipe & into a tubular condenser 7, in the tubes of which the alcohol
is concentrated and separated fom the ether. The concentrated alcohol flows
downwardly through the pipe again into the apparatus k, wherein it flows
from pan to pan k upon the bottom, where said alcohol is heated by the coil ³ to
separate therefrom any remaining quantity of ether, the latter being then again
carried upwardly as already described.
The ether, which has not been liquefied in the condenser, 7 flows through a
pipe into a second condenser m, formed of a coiled tube, arranged within the
casing of the condenser and under the latter. Said casing is provided, at its
bottom part, with a pipe 2 leading cold water into the same, which is discharged
through the pipe 3, at the top of said casing.
The quantity of water, flowing through the pipe 2 into the condenser 1, is so
regulated that only a part of the ether vapours will be condensed in 1, whilst
the remaining ether vapours are condensed in the cooling coil m and pass there-
from into the test apparatus f¹ through the pipe m¹.
The purified and rectified alcohol flows from the bottom of the apparatus k
through the pipe into the upper part of a tubular cooling apparatus n, the
lower part of which is provided with a tube or pipe n¹ leading the cooled alcohol
to another test-apparatus f" hereinafter described. The casing of the cooling
apparatus is provided with a pipe n² leading cold water thereto, which is dis-
charged through the pipe into the condenser i, as already described.
The test-device may be termed a "flow-regulating" apparatus, throughout.
However the devices shewn in the drawings allow of testing the products, as in
the devices f, f, and f¹¹; the alcohol collected will be in a progressively purified
state, alcohol in a perfectly pure state being obtained at fi. The tube 18 may
be graduated in order to enable it to indicate the varying level of liquid in
the apparatus and therefore the quantity of liquid flowing into the latter.
In order to have a constant flow in the several test-apparatus, the arrangement
must be provided with (1) a regulator for regulating the pressure within the
purifying and rectifying apparatus, and therefore the quantity of steam admitted
into the same, and (2) regulators for regulating the quantity of water admitted
into the condensers.
The pressure regulator I employ for the rectifier g, comprises two reservoirs
1 and 2, arranged one above the other, at a distance corresponding to the normal
pressure to be obtained within the rectifier. Said reservoirs are connected by
means of a tube 3, extending to a short distance from the bottom of the reservoir
(1), from the top part of which extends a pipe 4 leading to the rectifier. This
The upper
reservoir is filled with water rising to the mouth of said pipe 4.
reservoir 2 contains a float 5 the stem 6 of which is pivotally connected with a
fulcrumed lever 7, suitably connected with a rod 8 adapted to actuate the valve
rod 9 of the steam pipe g3 as the float 5 is raised or lowered. The pressure pro-
duced within the rectifier being also produced upon the surface of the liquid
contained in the reservoir 1; when said pressures increases, the liquid in said
reservoir is forced through the tube 3, into the upper reservoir 2, whereby the
float 5 is raised and whereby the valve on the steam pipe g³ is closed. When the
pressure decreases within the rectifier, the float is lowered, whereby the steam
valve is again opened.

page_text: The first rectifier a is provided with a similar pressure-regulator, of which it
is not necessary to give further description.
My flow-regulating test-apparatus (f, f¹, f¹¹) comprises a glass reservoir 10
of any suitable form secured on a tubular support 11, provided with an inlet 12,
through which the liquid coming from the respective cooling coil or second
condenser (for instance e or m) enters the reservoir 10 and with an outlet 13,
through which the liquid flows off to suitable reservoirs (not shown). The
central tube 18 is provided with an opening 22, which may be controlled by
means of a sliding sleeve, or its equivalent 21. Said tube 18 is screwed into the
outlet nozzle 13, and the opening 22 serves as an outlet for the liquid flowing
through the nozzle 12 into the reservoir 10. The reservoir 10 contains a float 14
the stem 15 of which is pivotally connected with the water admission valve 16,
on the pipe leading water to the respective second condenser or cooling coil,
the connection being made in such a manner that said valve is opened when the
float is raised, which occurs when the flow of liquid increases in the reservoir 10.
When said valve is opened, more water is admitted into the first condensers
(for instance d or 1) and the condensation therein is increased, therefore less
vapour passes into the corresponding cooling coil (for instance e or m) and less
liquid (condensed in the latter) enters the reservoir 10. The float has a central
bore 17, into which extends the vertical tube 18 communicating with the out-
let 13. The reservoir 10 is surrounded at its bottom by a circular cup 19, into
which drops the liquid passing through the joint, between the reservoir and its
support, said liquid flowing through a tube 20 into the outlet 13. In the.
event of the glass reservoir being accidentally broken, the liquid will flow
directly into the outlet 13 through the tube 20 from the cup 19.
OPERATION.
Assuming the flow of liquid to be increased by any cause, the opening 22 of
the central tube 18 not being sufficiently large for the exhaust of the liquid
under a pressure a, the liquid will rise in the reservoir 10, carrying with it, the
float 14, which opens the valve 16 through the agency of the rod 15, whereby an
increased quantity of water flows into the condenser (for instance d or 1) and
whereby more vapours are condensed in said condenser. Therefore, a smaller
quantity of vapours will pass into the corresponding cooling apparatus (for
instance e or m) and thence into the test apparatus.
a
con-
When the flow of liquid into the reservoir 10 is decreased, said liquid will be
lowered and also the float 14, which closes the valve 16, through the agency
of the rod 15, whereby less water is admitted into the condenser
(for instance d or 7) and
is
smaller quantity of vapours
densed within the latter. Therefore a greater quantity of vapours
will pass into the connected cooling apparatus (for instance e or m)
to be condensed therein and thence into the test apparatus, to restore the
latter to its normal state. In the case of the test apparatus f" connected to the
cooling apparatus n the operation is as follows: When the valve 16 is opened,
more water flows into the apparatus n and therefore through the pipe into the
condenser i, wherein more vapours are therefore condensed and brought back into
the apparatus g through the pipe . It will be understood that thereby a smaller
quantity of vapours pass through the pipe into the apparatus k and thence into
the apparatus n and fll as herein described.
Having now particularly described and ascertained the nature of my said
invention, and in what manner the same is to be performed, I declare that what
I claim is:.
1) The improved method of continuously rectifying alcohol, which consists
in submitting the phlegm coming from the rectifier proper, to a second purifi-
cation with retrogradation, to relieve it from ether, which has escaped the action
of the first purification, and in controlling the operation of the condensers and

page_text: cooling apparatus and of the purifier, by controlling the admission of water and
vapour into said apparatus, by means of a suitable flow-controller, substantially
as set forth.
2) The improved apparatus for the continuous rectification of alcohol, com-
prising a purifier provided with a cooling apparatus and a condenser; a rectifier
proper, provided with a condenser and a cooling apparatus, between which said
purifier is arranged and to which the same is connected; a phlegm purifier
provided with a condenser and a cooling apparatus and connected to the rectifier
proper, means for controlling the operation of the condensers and cooling
apparatus and of the rectified product and means for controlling the pressure
within the rectifier and the phlegm purifier, substantially as set forth.
3) The apparatus for continuous rectification comprising a purifier, provided
with a condenser and a cooling apparatus, a rectifier proper, provided with a
condenser and a cooling apparatus, between which said purifier is arranged and
to which the same is connected; a phlegm purifier provided with a condenser
and a cooling apparatus and connected to said rectifier; a suitable regulator for
controlling the admission of water into the condensers and cooling apparatus,
in order to control the operation of said apparatus and means for controlling the
pressure within the rectifier and the phlegm purifier, substantially as set forth.
4) The apparatus for the continuous rectification of alcohol, comprising a
purifier provided with a condensing and cooling apparatus; a rectifier proper,
provided with a condensing and cooling apparatus, between which said purifier
is arranged and to which the same is connected; a phlegm purifier, provided
with condensing and cooling apparatus and connected to the rectifier, means for
controlling the operation of the condensing and cooling apparatus, and a float
pressure controller, acting on the admission of steam into the rectifier and phlegm
purifier to control the pressure within said apparatus, substantially as set forth.
5) In the apparatus of the class set forth, the combination of a pressure
controller, comprising a receptacle divided into a lower and upper compartment
connected by means of a central tube, a suitable connection between the lower
compartment and the apparatus, the pressure of which is to be controlled, a float
in the upper compartment, a rod on said float and a lever operating the inlet cock
of the steam-pipe and connected to said rod, substantially as set forth.
Dated this 14th day of December 1899.
J. P. BAYLY,
18, Fulham Place, London, W., Agent for the Applicant.