New or Improved Method of Distilling Products by Means of Steam, and Classifying or Separating them according to their Respec- tive Points of Vaporization, and Apparatus therefor.
Year: 1889

page_text: Date of Application, 6th July, 1889
Complete Specification Left, 8th Apr., 1890-Accepted, 10th May, 1890
PROVISIONAL SPECIFICATION.
New or Improved Method of Distilling Products by Means of Steam,
and Classifying or Separating them according to their Respec-
tive Points of Vaporization, and Apparatus therefor.
A communication from abroad by NAUM NOTKIN, of Moscow, Russia, Chemist, and
PAUL MARIX, of Paris, France, Proprietor.
I, WILLIAM PHILLIPS THOMPSON F.C.S., M.I.M.E., of the Agency for Foreign
Patent Solicitors, 6, Lord Street, Liverpool, and 6, Bank Street, Manchester, both
in the County of Lancaster, and 323, High Holborn in the County of Middlesex, Civil
Engineer, do hereby declare the nature of this invention to be as follows:
:-
It has been found, from experiments, that to obtain, on an economical scale, a.
thorough distillation and continuous classification of products by means of steam, it.
is essential on the one hand, that the steam should only act indirectly on the
substance, while this latter is at a degree of temperature below that of its point of
vaporisation, that the direct action of the steam, by mixing with the substance,
should only be commenced gradually by introducing small quantities at a time, in
order to produce exclusively vaporisation and the force required to carry off the
vapour produced, and finally that the action of the steam should not be prolonged on
those parts of the substance which resist distillation at the temperature which it
can develop; on the other hand, it is also essential that the respective temperatures
of the substance and of the steam should be well regulated, so that the distilled.
products will be regularly and methodically separated according to the temperatures.
of their points of vaporisation.
The object of the present invention is to effect, on an industrial scale a realisation
of these essential conditions, and also to obtain a process of continuous distillation
and a classification of the products by means of steam, as hereinafter described.
To attain the objects above mentioned, the substance to be distilled is first
heated in a supply vat by means of a serpentine steam pipe passing alternately and
repeatedly from the vat to the superheated, and vice versa, so as to bring the substance:
repeatedly in contact with the steam during the superheating of the latter and thus
to regulate the respective temperatures of the steam and of the substance. The
substance is thus brought to a temperature very nearly equal to that of the point of
vaporisation of the most volatile components contained therein. During this process.
of heating, the steam acts indirectly, that is to say, without mixing with the substance.
It is well to utilise the heat lost in the furnace of the superheater, by making the
products of combustion pass across the masonry surrounding the supply vats.
The substance thus heated is only then introduced, in small quantities at a time,
into a special receptacle, named a distiller, and is there submitted to the direct actions
of the steam from the superheater, the temperature of which has been regulated by,
its successive and repeated passages into the supply vat, as above described. By
properly regulating the temperature of this mixture, only the most volatile com-
ponents are vaporised, these being the components that are to be extracted in the first.
place.
The automatic method of regulating the respective temperatures of the substance..
and of the steam by means of their reciprocal and indirect action before being inter-
mixed, is one of the characteristic points by means of which this invention has been
realised. Furthermore, the distillation in a receptacle distinct from that in which the..
substance was heated to the temperature corresponding to its points of vaporisation,..
is one of the most important points of the invention.
The vaporisedi products, are separated from those which do not distil at the

page_text: temperature of the mixture, either by means of pulverisation, or by a process of
steam clearing on small quantities at a time.
In the first case, the following substances are introduced continuously into a
pulveriser which opens out into a receptacle provided with a swan's neck, namely, on
the one hand, the substance to be distilled which is already heated to the proper
temperature as above shown, and on the other hand, the steam (the temperature of
which has been regulated as above mentioned, and coming finally from the super-
heater) so that the first components to be separated off are vaporised by admixture,
without, however, the elements of a higher point of vaporisation, being vaporised.
Before leaving the pulveriser, the substance and the steam come in contact and
become intimately intermixed as they pass out in a state of perfect separation, the
exchange of heat is effected, and the products vaporisable at this temperature escape
with the steam through the swan's neck of the receptacle, and pass into the con-
denser, while the undistilled products are deposited of their own accord in the
receptacle. They are extracted from this receptacle by a tube or syphon in a con-
tinuous or intermittent manner to be passed into a second apparatus to supply a
second pulveriser working similarly to the former, in which the steam taken from the
superheater, (after having been regulated in the second supply vat in like manner
as was shown for the first) acts at a higher temperature, suitable for vaporising the
products which are distilled at a temperature immediately above that of the products
separated in the first operation.
It has been above shown that the distilled vapours are passed into the condenser,
but in order more completely to regulate the temperature of the steam and of the
substance by their reciprocal action in the supply vat, while at the same time
recuperating some of the heat contained in the said vapours, it is well to let these
latter pass across the supply vat before entering the condenser, this is another
essential point contributing to the proper working and the regularity of distillation
and classification, besides affording an appreciable economy of fuel.
Although any system of pulverisation may be employed, one type is here described
for purposes of illustration."
A hemispherical cup is divided into two equal parts by a diametrical diaphragm,
perpendicular to the circumference of the edge of the hemisphere. On each side of
and touching this diaphragm, small orifices are made in the hemispherical cup, said
orifices being inclined so that those on one side of the diaphragm converge towards
those on the other. This pulveriser receives the substance to be distilled in one of
these compartments, and in the other, the steam.
The pulverising apparatus opens into a closed receptacle with a swan's neck, and
is placed with the diaphragm horizontal, the steam entering the lower compartment
escapes through the small oblique orifices communicating therewith, and before it
escapes, meets the substance which, under the slight pressure due to the level of
the supply vat, escapes through the orifices formed above the diaphragm. This
meeting of the steam and of the substance, in a state of complete division, produces
a perfect intermixing, and the steam is present under conditions more favourable
for producing its effect. The separation of the distilled products takes place
immediately, since the vaporised particles rise with the steam into the swan's neck,
while the rest is at once deposited. The steam has not therefore to exercise any
force uselessly on the parts that are not susceptible of vaporisation by the same. This
is an effective advantage, conducing to a considerable saving of steain.
Where pulverisation is used for distilling, in order to produce a closer admixture
of the steam and the substance, a rotary paddle mixer or other device for stirring the
mixture, as it leaves the pulveriser, is, if necessary, employed.
The right is also claimed to pass the substance with steam, through several suc-
cessive distinct pulverisers for vaporising products of the same degree of vaporisation.
In this case the steam will have the samo temperature in the several pulverisers
combined in the vaporisation of each separate product.
By the use of multiple pulverisers, those parts can be vaporised that may have

page_text: escaped the action of the first pulveriser, although the temperature of vaporisation
may be the same as that for which the first pulveriser is ordained.
It was stated, at the commencement of this specification, that the products which
had not distilled vapours, either under a process of pulverisation or of steam clearing
could be separated out; the process of pulverisation having been described, the
following is that of steam clearing: :-
With the latter system of distillation, nothing is changed in the supply vats as
concerns the automatic regulating of the temperatures of the substance and of the
steam. The general working of the operation remains the same, clearers have merely
been substituted for pulverisers.
In order to effect distillation by a process of clearing, it is sufficient to introduce
the substance coming from a supply vat into a small receptacle supplied with a steam
clearer. But this primitive arrangement can not be recommended, because it does
not allow of those parts of the substance being separated out in a continuous and
exact manner, which do not distil at the given temperature of the steam.
In fact
the parts of the substance that have already been treated are mixed in the receptacle
with the fresh substance, which is continually flowing in from the supply vat, and it
is then impossible to separate the exhausted parts without taking out the fresh with
them. Thus, in the case of distillation by a process of clearing, the multiple clearing
operation hereinafter described is found to be the only one capable of satisfying the
object sought by this new process of distillation.
In order to obtain a multiple and methodical mixing of the steam in the substance,
this latter is introduced from the supply vat into a receptacle or alembic of any shape,
but divided by a system of inner partitions into several compartments, all communi-
cating with each other through their steam chambers, which open into the single
swan's neck of the alembic, with this object the separating partitions do not reach
quite to the top of the apparatus. A clearer opens into each compartment, intro-
ducing steam, the temperature of which has been regulated by its repeated passage
across the supply vat, this steam must, however, finally come from the superheater
in order to receive from thence, a suitable temperature before entering the clearing
apparatus.
The substance, on the other hand, comes from the supply vat in the first compart-
ment of the alembic, then carried through tubes to the bottom of the compartment,
and coming out over the separating partition a little below the surface level passes
into the second compartment, and thence in like manner into the third, and so on.
In these successive passages, it is the heavier parts that pass from the one co-
partment to the other, since the tubes of communication reach to the bottom of the
said compartments; this point must be noted, in order to understand what follows.
The substance in the first compartment is subjected to a first treatment with steam
by clearing, the most volatile parts are vaporised and carried off through the swan's
neck, the heavier parts fall to the bottom and pass into the second compartment where
they are subjected to a second treatment with steam identical with the first. The
effect of this second clearing is to vaporise the products volatile at the temperature at
which the steam acts, and which may have escaped from the action of the first
operation, the substance may then, if necessary, be treated a third time before being
taken out of the alembic by means of a syphon, in order to be placed in a second
distilling apparatus, or in a second supply reservoir where the distillation is continued
in like manner at progressively increasing temperatures, as has been above shown, in
order to obtain a rational and methodical classification of the distilled products
arranged according to their respective points of vaporisation.
It is thus seen that, by the action of steam alone on the substance, the latter is
distilled, and the distilled products separated: first, indirectly, by causing the steam
to circulate from the superheater to the supply apparatus in a continuous and repeated
manner, and vice versa, in order to place a larger number of surfaces in contact, and
to raise the substance to a temperature nearly equal to the point of vaporisation of
the most volatile products contained; then, directly, when the steam has reached the

page_text: necessary temperature for the production of the calorific force required to vaporise
the volatile products which are to be distilled first, and to carry away the vapours
formed, the mixing of the steam and the substance taking place in a distilling
apparatus distinct from the supply vat and fed by the latter, so as to act upon small
quantities at a time, either by means of simple or multiple pulverisations, or by simple
or multiple clearing operations, the distilled parts being separated immediately from
the undistilled parts, so that the steam will have to exert the least possible amount of
energy on inert parts. The distilled parts may be carried across the supply vat in
order that a part of their beat may be given over to it before passing into the con-
denser, and the undistilled parts are collected continuously and treated in like manner
as above shown, for the fresh substance, so that the products volatile at a temperature
immediately above the first are extracted, and so on, until the substance is completely
exhausted.
Dated this 5th day of July 1980
WM. P. THOMPSON & Co.,
Agents for the Applicant.
COMPLETE SPECIFICATION.
New or Improved Method of Distilling Products by Means of Steam,
and Classifying or Separating them according to their Respec-
tive Points of Vaporization, and Apparatus therefor.
A communication from abroad by NAUM NOTKIN, of Moscow, Russia, Chemist, and
PAUL MARIX, of Paris, France, Proprietor.
I, WILLIAM PHILLIPS THOMPSON, F.C.S., M.I.M.E., of the Agency for Foreign
Patent Solicitors, 6, Lord Street, Liverpool, and 6, Bank Street, Manchester, both in
the County of Lancaster and 323, High Holborn, in the County of Middlesex, Civil
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 :-
We have found, from experiments that to obtain on an economical scale, a thorough
distillation and continuous classification of products by means of steam, it is essential
on the one hand, that the steam should only act indirecly on the substance, while this
latter is at a degree of temperature below that of its point of vaporisation, that the
direct action of the steam, by mixing with the substance, should only be commenced
gradually by introducing small quantities at a time, in order to produce exclusively
vaporisation and the force required to carry off the vapour produced, and finally that
the action of the steam should not be prolonged on those parts of the substance which
resists distillation at the temperature which it can develop; on the other hand it is
also essential that the respective temperatures of the substance and of the steam shouki
be well regulated, so that the distilled products will he regularly and methodically
separated according to the temperatures of their points of vaporisation.
The object of the present invention is to effect on an industrial scale, a realisation
of these essential conditions and also to obtain a process of continuous distillation and
a classification of the products by means of steam, as hereinafter described.
To realize the conditions just explained we first beat the substance to be distilled in
a supply vat by means of a coil containing super-heated steam. We then bring the
substance to a degree near the one which corresponds to the point of vaporisation of
the most volatile parts contained therein. In this heating the steam acts in an indirect
way viz. without mixing with the substance.
It is well to utilise the heat lost in the furnace of the superheater by making the
products of combustion pass across the masonry surrounding the supply vats.
The substance thus heated is only then introduced, in small quantities at a time,
into a special receptacle, named a distiller, and is there submitted to the direct action
of the steam from the superheater, taken from various points on the circuit of the
superheater in such a way as to obtain from a single superheater steam at various

page_text: temperatures as desirable. By properly regulating the temperature of this mixture
of steam and substance only the most volatile components are vaporised these being
the components that are to be extracted in the first place.
The distillation in a receptacle distinct from that in which the substance was heated
to the temperature corresponding to its point of varporisation, is one of the most
important points of the invention.
The vaporised products are separated from those which do not distil at the tempera-
ture of the mixture, either by means of pulverisation or by a process of steam clearing
on small quantities of substance at a time.
In the first case, the following substances are introduced continuously into a
pulveriser which opens out into a receptacle provided with a swan's neck, namely, on
the one hand, the substance to be distilled which is already heated to the proper
temperature as above shown, and on the other hand the steam so that the first com-
ponents to be separated off are vaporised by admixture, without however the elements
of a higher point of vaporisation being vaporised.
On leaving the pulveriser the substance and the steam come in contact and become
intimately intermixed as they pass out in a state of perfect separation, the exchange
of heat is effected, and the products vaporisable at this temperature escape with
the steam through the swan's neck of the receptacle and pass into the condenser,
while the undistilled products are deposited of their own accord in the receptacle.
They are extracted from this receptacle by a tube or syphon in a continuous or
intermittent manner to be passed into a second apparatus to supply a second
pulveriser working similarly to the former, in which the steam taken from the super-
heater acts at a higher temperature suitable for vaporising the products which are
distilling at a temperature inmediately above that of the products separated in the
first operation.
It has been above shown that the distilled vapours are passed into the condenser
but in order to recuperate some of the heat contained in the said vapours, it is well
to let these latter pass across the supply vat before entering the condenser this is
another essential point contributing to the proper working and the regularity of
distillation and classification, besides affording an appreciable economy of fuel.
Although any system of pulverisation may be employed one type is here described
for purposes of illustration.
A hemispherical cup is divided into two equal parts by a diametrical diaphragm,
perpendicular to the circumference of the edge of the hemisphere. On each side of
and touching this diaghragm small orifices are made in the hemispherical cup,' said
orifices being inclined so that those on one side of the diaphragm converge towards
these on the other. This pulveriser receives the substance to be distilled in one of
these compartments and in the other the steam.
The pulverising apparatus opens into a closed receptacle with a swan's neck, and is
placed with the diaphragm horizontal, the steam entering the lower compartment
escapes through the small oblique orifices communicating therewith and before.it
escapes, meets the substance which under the slight pressure due to the level of the
supply vat, escapes through the orifices formed above the diaphragm. This meeting
of the steam and of the substance, in a state of complete division, produces a perfect
intermixing and the steam is present under conditions more favourable for producing
its effect. The separation of the distilled products takes place immediately since the
vaporised particles rise with the steam into the swan's neck, while the rest is at once
deposited. The steam has not therefore to exercise any force uselessly on the parts
that are not susceptible of vaporisation by the same. This is an effective advantage,
conducing to a considerable saving of steam.
Where pulverisation is used for distilling, in order to produce a closer admixture
of the steam and the substance a rotary paddle mixer or other device for stirring the
mixture, as it leaves the pulveriser is if necessary employed.
The right is also claimed to pass the substance with steam through several
successive distinct pulverisers for vaporising products of the same degree of vaporisa-

page_text: .
tion. In this case the steam will have the same temperature in the several pulverisers
combined in the vaporisation of each separate product.
By the use of multiple pulverisers those parts can be vaporised that may have
escaped the action of the first pulveriser although the temperature of vaporisation
may be the same as that for which the first pulveriser is ordained.
It was stated at the commencement of this specification that the products which
had not distilled vapours either under a pulverisation or of steam clearing could be
separated out; the process of pulverisation having been described the following is
that of steam clearing ;-
With the latter system of distillation nothing is changed in the supply vats. The
general working of the operation remains the same, clearers have merely been sub-
stituted for pulverisers.
In order to effect distillation by a process of clearing it is sufficient to introduce
the substance coming from a supply vat into a small receptacle supplied with a steam
clearer. But this primitive arrangement can not be recommended because it does
not allow of those parts of the substance being separated out in a continuous and
exact manner, which do not distil at the given temperature of the steam. In fact
the parts of the substance that have already been treated are mixed in the receptacle
with the fresh substance which is continually flowing in from the supply vat and it is
then impossible to separate the exhausted parts without taking out the fresh with
them. Thus in the case of distillation by a process of clearing the multiple clearing
operation hereinafter described is found to be the only one capable of satisfying the
object sought by this new process of distillation.
In order to obtain a multiple and methodical mixing of the steam in the substance
this latter is introduced from the supply vat into a receptacle or alembic of any shape
but divided by a system of inner partitions into several compartments, all communi-
cating with each other through their steam chambers which open into the single
swan's neck of the alembic with this object the separating partitions do not reach
quite to the top of the apparatus. A clearer opens into each compartment intro-
ducing steam taken from the superheater at a point where its temperature is suitable
as above described.
The substance on the other hand comes from the supply vat in the first compart-
ment of the alembic then carried through tubes to the bottom of the compartment
and coming out over the separating partition a little below the surface level passes
into the second compartment and thence in like manner into the third and so on.
In these successive passages it is the heavier parts that pass from the one compart-
ment to the other since the tubes of communication reach to the bottom of the said
compartments; this point must be noted in order to understand what follows.
The substance in the first compartment is subjected to a first treatment with steam
by clearing, the most volatile parts are vaporised and carried off through the swan's
neck the heavier parts fall to the bottom and pass into the second compartment where
they are subjected to a second treatment with steam identical with the first. The
effect of this second clearing is to vaporise the products volatile at the temperature
at which the steam acts and which may have escaped from the action of the first
operation the substance way then if necessary be treated a third time before being
taken out of the alembic by means of a syphon, in order to be placed in a second
distilling apparatus, or in a second supply reservoir where the distillation is continued
in like manner at progressively increasing temperatures as has been above shown in
order to obtain a rational and methodical classification of the distilled products
arranged according to their respective points of vaporisation.
In one word it will be seen that it is intended to distil and fractionate the distilla-
tion by steam alone by making it act on the substances first indirectly, to bring it to
the degree of distillation. Then directly when the steam has reached the necessary
temperature for the production of the calorific effort required to vaporise the volatile
products which are to be distilled first, and to carry away the vapours formed, the
mixing of the steam and the substance taking place in a distilling apparatus distinct
from the supply vat and fed by the latter, so as to act upon small quantities at a time,

page_text: either by means of simple or multiple pulverisations, or by simple or multiple
clearing operations the distilled parts being separated immediately from the undistilled
parts so that the steam will have to exert the least possible amount of energy on
inert parts. The distilled parts may be carried across the supply vat in order that a
part of their heat may be given over to it before passing into the condenser and
the undistilled parts are collected continuously and treated in like manner as above
shown, for the fresh substance so that the products volatile at a temperature imme-
diately above the first are extracted and so on, until the substance is completely
exhausted.
If desired there may be applied a vacuum to the above process of distillation by
pulverisation by interposing between the stills and the condensers apparatus capable
of producing vacuum and especially "turbines" acting at the same time as aspirators
and as "deflegmateurs."
Having now particularly described and ascertained the nature of the said inven-
tion and in what manner the same is to be performed as communicated to me by my
foreign correspondents, I declare that what I claim is ;-
1. A process of continuous distillation and classification of distilled products by
means of steam used (a) indirectly-viz. (without mixing it) to carry those to a
temperature near the point of vaporisation of the more volatile parts, and then
(b) directly by acting successively on small parts at a time to produce distillation and
classification of the products that distil substantially as described above.
2. In the above process of continuous distillation and classification of products the
special manner or method whereby the steam acts by a direct way consisting in
mixing the steam and substance in stills separated from the supply vat and thus by
proceeding either by pulverisation (single or repeated) or by single or repeated steam
clearing and at temperatures conveniently increasing from one still to the other to
obtain the classification of the distillation substantially as described.
Dated this 2nd day of April 1890
WM. P. THOMPSON & Co.,
Agents for the Applicant.