Improvements in Apparatus for Distillation.
Year: 1894

page_text: Date of Application, 15th Dec., 1894
Complete Specification Left, 16th Sept., 1895-Accepted, 2nd Nov., 1895
PROVISIONAL SPECIFICATION.
Improvements in Apparatus for Distillation.
1 MARIUS OTTO of 8 Passage Gourdon Paris in the Republic of France
Chemist do hereby declare the nature of this invention to be as follows:-
The object of this apparatus is to facilitate the separation of liquids by
distillation, and more especially such as have their boiling points at temperatures
not far distant from each other or as it is commonly termed fractional distillation.
I construct my apparatus by placing between the still or vessel in which the liquids
are boiled and the worm or other arrangement used for condensing the vapour of
the fluid or fluids to be separated, a series of elements of the type shown in the
accompanying drawing, Figure 2. Each such element is composed of a receiver,
preferably of a cylindro-conical form, provided with four tubes. The upper tubes
serve the one for the entry and the other for the exit of the vapours coming from
the still. The other two tubes are of smaller diameter, say about one-third of
that of the two tubes already mentioned and serve for the reflux of fluid condensed
in the series of elements. They enter the element at the bottom and at a point
just above the commencement of the conical portion respectively and the former
communicates with the element next above and the latter with the element next
below. The tube which brings the vapours to the element has its orifice at a
short distance below the orifice of the latter tube as shewn in the drawing.
In order to divide up the current of vapour brought by the tube and render
more effectual the cleansing action due to the bubbling through the fluid collected
in the element I put a cap on the end of this tube with perforations which may be
conveniently effected by clipping thereon two metallic plates of a U shape
arranged in the form of a cross.
The arrangement of the tubes as well as their function is easily seen from the
drawings. Of the two smaller tubes the one which enters at the bottom serves to
bring to the element the overflow of the liquid collected in the clement next above
it and the smaller tube to take the overflow of the element itself to the element
next below, so that there is a regular back flow of fluid which has been condensed
in the elements. The fluid serves to wash the vapour free from all liquids of
higher boiling point than those whose vapours are to be condensed. When
circumstances require it each of these smaller tubes is provided at its lower
part with a tap to enable the fluid to be emptied from the element. The
elements are all alike, excepting the first and the last so that they are independent
and interchangeable. The last element (counting from the still) usually carries a
thermometer, electrical or otherwise, with an indicator, so that the temperature in
that element can be accurately observed, and this being preserved constant ensures
that the vapour passing off to the condensing apparatus shall be of the proper
character.
Although I have described the element to be of a cylindro-conical shape its
form may be more or less modified without departing from the invention.
The apparatus for condensation of the vapour after it has passed through the
series of elements may be of any convenient form, such as the ordinary worm.
I prefer to place between it and the last clement. (but on the descending side)
beat economiser whereby the liquid to be boiled is subjected to a preliminary
warming by means of the waste heat of the vapours coming over from the
till

page_text: At the lower part of the condensing apparatus or between it and the vessel
which receives the products of distillation I prefer to place an automatic indicator
of the density of the fluid. The form of apparatus which I prefer to use for
this purpose is represented in Figures 3 and 4 and is essentially composed of a
vessel containing an interior cup into which the products of condensation pass and
which being open allows them to flow over, and thus, by being full maintains the
fluid at the constant level of its upper edge. In this liquid lies a float whose
movements are transmitted by means of a thread to an indicator whose graduations
thus shew the density of the products of distillation.
The general arrangement of the apparatus will be readily seen from the
accompanying drawings in which
Figure 1 shews the general arrangement of the whole apparatus.
Figure 2 is an enlarged view of a single element, and
Figures 3 and 4 are enlarged sections of the automatic indicator.
The elements should be arranged helicoidally each one being at a suitable
distance below the one next beyond it in the series counting from the still.
The working of the apparatus is based on the principle of methodically washing
the vapours that leave the still by means of the liquids condensed out of the
vapour by reason of their having a higher boiling point than that which is
possessed by the desired products of distillation. The heat of the still being
somewhat higher than the boiling point of these products it will give off vapours
containing liquids of a higher boiling point. These liquids will become condensed
in the elements and will gradually charge them with layers of liquid through which
the vapours will bubble on their passage to the condenser, and these vapours thus
become separated from all substances which have a higher boiling point than that
determined by the thermometer placed in the last element.
Dated this 15th day of December 1894.
JOHNSONS & WILLCOX,
47 Lincoln's Inn Fields, London, W.C., Agents.
Improvements in Apparatus for Distillation.
I, MARIUS OTTO of 8 Passage Gourdon Paris, in the Republic of France,
Chemist 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 :-
The object of this apparatus is to facilitate the separation of liquids by
distillation and more especially such as have their boiling points at temperatures
not far distant from each other, or as it is commonly termed, fractional distillation.
I will refer to the accompanying drawings in describing my invention.
Figure 1 showing in vertical section the general arrangement of an apparatus in
accordance with this invention.
Figure 2 shows one of the clements and its connections in section drawn to a
larger scale.
Figures 3 and 4 are vertical sections at right angles to each other of the
automatic indicator hereinafter described.
I construct my apparatus by placing between the still or vessel in which
the liquids are boiled, and the worm or other arrangement used for condensing
the vapour of the fluid or fluids to be separated, a series of elements
of the type shown in Figure 2. Each such element is composed of a
receiver B B B B to Bn, preferably of a cylindro-conical form, provided
with four tubes V₁ V¹¹³. The upper tubes V₁V serve, the one (V¹) for

page_text: the entry, and the other (V*) for the exit of the vapours coming from the still.
The other two tubes are of smaller diameter (say about one-third of that of
the two tubes V1 V) and serve for the reflux of liquid condensed in the series of
elements. The last named two tubes enter the element the one (³) at the bottom
and the other (1) at a point just above the commencement of the conical lower
portion and the pipe o communicates with the element next above by joining the
pipe thereof and the pipe v communicates with the element next below by
joining the pipe thereof. The tube V¹ which brings the vapours to the element,
has its orifice at a short distance below the orifice of the latter tube v' as shown
in Figure 2.
In order to divide up the currents of vapour brought by the tube V₁ and render
more effectual the cleansing action due to the bubbling through the fluid collected.
in the element, I put a disperser on the end of this tube such for instance as a cap
with perforations, or two metallic plates m n of Ụ shape inay be clipped onto the
end of the tube so that they cross each other as shown in Figure 2.
The arrangement of the tubes as well as their function is easily seen from the
drawings. Of the two smaller tubes, the one which enters at the bottom, serves
to bring to the element the overflow of the liquid collected in the element next
above it and the other tube v¹ serves to take the overflow of the element to the.
element below so that there is through all the elements a regular back flow of
liquid which has been condensed in the elements. This liquid serves to wash the
vapour free from all liquids of higher boiling point, than those whose vapours are
to be condensed. When circumstances require it each of the tubes v² * is provided
at its lower part with a tap to enable the liquid to be emptied from the element.
The connections of the elements are all alike, excepting of course the first and.
the last, so that they are interchangeable. The last element (Bn) (counting from
the still) usually carries a thermometer T, electrical or otherwise, with an indicator,
so that the temperature in that element can be accurately observed and this.
temperature being preserved constant ensures that the vapour passing off to the
condensing apparatus shall be of the proper character.
Although I have described the elements as being of a cylindro-conical shape,
the form may be more or less modified without departing from the invention.
The apparatus for the condensation of the vapour after it has passed through the
series of elements may be of any convenient form, such as an ordinary condensing
worm. I prefer to place between it and the last element (but on the descending
side) a heat economiser, whereby the liquid to be boiled is subjected to a
preliminary warming by means of the waste heat of the vapours coming over from
the still.
C is the still provided with a gauge N'and A is the tank of liquid to be distilled
passing through the heat economizer R (provided with a gauge N²) and then by
the tube t¹ to the still C. The vapours from the elements pass from the last
element Bn through the coil in the economizer R and therethrough the condensing
worm S and by the pipes to the automatic indicator I and thence by the pipe &³
to the receptacle provided for them-shown in the drawing as a cask.
At the lower part of the condensing apparatus, or between it and the vessel which
receives the products of distillation I prefer to place an automatic indicator of the
density of the fluid. The form of apparatus which I prefer to use for this purpose
is represented in Figures 3 and 4. It is composed of a vessel E containing an
interior cup e into which the liquid products of condensation pass, which cup being
open at top allows them to flow over and thus by being always full maintains the
liquid at the constant level of its upper edge. In this liquid lies a float / whose
movements are transmitted by means of a cord f1 passing over a pulley f¹ to an
indicator finger i moving over a scale r whose graduations thus show the density of
the products of distillation. The finger i is shown as being actuated by a pinion ³
on its centre pin gearing with a pinion on the axis of the pulley f' but it may be
actuated in any other suitable way. The pipes where it enters the lower part of
the cup e is shown as being covered by a hoods. The elements B B B B to Bn

page_text: are preferably arranged helicoidally as shown in Figure 1 each one being at
a suitable distance below the one next beyond it in the series counting from the
still.
The working of the apparatus is based on the principle of methodically washing
the vapours that leave the still by means of the liquids condensed out of the vapour
by reason of their having a higher boiling point than that which is possessed by the
desired products of distillation. The heat of the still being somewhat higher than
the boiling point of these products, it will give off vapours containing liquids of a
higher boiling point. These liquids will become condensed in the elements and will
gradually charge them with layers of liquids through which the vapours will bubble
on their passage to the condensor, and these vapours thus become separated from
all substances which have a higher boiling point than that determined by the
thermometer placed in the last element.
Having now particularly described and ascertained the nature of my said inveu-
tion and in what manner the same is to be performed I declare that what I
claim is :-
1. In distilling apparatus the use of elements so arranged as to provide for the
methodical washing of the vapours from the still by means of the liquids of
higher boiling points condensed out of the vapours substantially as hereinbefore
described.
2. The combination with distillatory apparatus between the still and the
condenser of a series of elements provided with inlet and outlet tubes for vapours
from the still and return tabes for the reflux fluid condensed in the said elements
substantially as herein before described.
3. The combination with distillatory apparatus between the still and the
condenser of a series of elements provided with inlet and outlet tubes for vapours
from the still and return tubes for the reflux fluid condensed in the said clements
and a thermometer in connection with the element farthest from the still
substantially as hereinbefore described.
4. The combination with distillatory apparatus between the still and the
condenser of a series of elements provided with inlet and outlet tubes for vapours
from the still and return tubes for the reflux fluid condensed in the said elements
and a heat economizer between the condenser and the element furthest from the
still substantially as hereinbefore described.
5. In distillatory apparatus an automatic density indicator situated between the
condensing apparatus and the outlet for distilled products substantially as
herein before described.
6. The arrangement and combination of parts constituting distillatory apparatus
substantially as hereinbefore described and illustrated in the accompanying
drawings.
Dated this 16th day of September 1895.
JOHNSONS & WILLCOX,
47 Lincoln's Inn Fields, London, W.C., Agents.