Improvements in the Distillation of Solid and Liquid Matters.
Year: 1899

page_text: Date of Application, 15th June 1800
Complete Specification Left, 13th Mar., 1900-Accepted, 12th May, 1900
Complete Specification Left, 13th Mar., 1900-Accepted, 12th May, 1900
PROVISIONAL SPECIFICATION.
Improvements in the Distillation of Solid and Liquid Matters.
I, MOSES WALSSBELN, of No. 9, Great Wulf Street, St. Petersburg, in the
Empire of Russia, Technologist, do hereby declare the nature of this invention
to be as follows: :-
This invention relates to a process of distillation applicable to the simple,
fractional or dry (destructive) distillation of any solid, as well as liquid matters.
It would be superfluous to describe all the different details of its application
to the various matters which may be treated by this process; it will be sufficient
to explain the course of the operation:-
(a) for treating wood, as an example of dry distillation generally;
(b) for treating naphtha, as an example of the distillation of liquids.
These examples serve to prove, that the operation is substantially identical
in the two cases and to demonstrate the advantage of this process in all its
various applications for purposes of distillation.
Before explaining the details of the dry distillation of wood, it may be men-
tioned that the attempts to conduct this process by means of hot gases devoid
of free oxygen (or by means of superheated steam) whose heat when such gases
are led into direct contact with the matters to be distilled, serves as agent for
the operation, have given very advantageous results. But since distillation by
means of hot gases (carbonic oxide, carbonic acid, generator gas, water gas, etc.,)
notwithstanding all its advantages, has not only failed to generally supplant
the older methods but has not even been adopted in practice, it is by reason of
certain serious inconveniences inherent to this system as, for example excessive
dilution of the products, the necessity of utilizing the exhaust gases, and so on.
In fact, when the dry distillation of wood (or other organic matters) is per-
formed in a medium of hot gases devoid of free oxygen the heat of such gases
serving as the distilling agent the products of distillation are mixed with con-
densed water vapours always contained in the gases so that the product becomes
more or less diluted. This necessitates an enlargement of dimensions of the
plant, of the receivers, and of the apparatus for treating the matters, occasioning
a considerable waste of products and increased expense for fuel for the final
treatment of the products; moreover the condensation of aqueous vapors con-
tained in the hot gases necessitates more voluminous cooling apparatus, such
vapours in their condensation giving up a considerable quantity of latent heat.
In certain cases, as for instance in working with generator gas. the products
of distillation are contaminated with resin contained in this gas, which may be
disadvantageous. Finally, in many cases, as in the distillation of small waste
matters (saw-dust, spent tan, dye-wood waste, or the like) when wood is dear
and coal cheap, as in industrial centres, it will be always more advantageous
to forego this method because the hot gases of coal contain sulphur which causes
rapid wear of the apparatus. The inconvenience of the hot gas process as here-

page_text: tofore proposed for this purpose, consists, moreover, in the fact that such gases
require to be utilized after being exhausted, otherwise the cost of fuel would
be considerably increased as will be readily seen when the fact that these gases,
such as carbonic oxide, generator gas, water gas, etc., are nothing less than
products of incomplete combustion of fuel, is taken into consideration. On the
other hand the utilization of these gases increases the structural cost of the
plant and the complication of the apparatus whilst the amount of gases to be
utilized may considerably exceed that which can be used as fuel.
It is obvious from the foregoing that the method of dry distillation of wood
or other organic matters in a medium of hot gases supplied from without not-
withstanding its material advantages (increase of efficiency, economy of time,
simplicity of the operation, etc.,), is nevertheless very imperfect owing to the
presence in such gases of deleterious constituents (aqueous vapours, resin,
sulphur, etc.,). It may of course, be possible to eliminate all these deleterious
matters but, apart from the cost of the plant, this operation may entail a con-
siderable loss of heat because the purification of the gases would involve their
cooling and subsequent re-heating to the temperature required for distillation.
Whatever modifications may be introduced into the process of dry distillation
of wood or other organic matters, the solid products (charcoal, coke, etc.,) and
the liquid products (tar-water, ammoniacal water, resins, etc.,) will always con-
tain gases which remain uncondensed in the cooling apparatus.
The method forming the subject of the present invention consists in the
utilization of such uncondensable gases free from aqueous vapours and from
resin (as well as from sulphur when none is contained in the matters under-
going distillation) and obtained in comparatively small quantities, as an agent
or medium in which to effect the dry distillation of organic or other matters.
The accompanying drawing shews diagrammatically the general arrangement
of the plant employed for this purpose. A is the apparatus (regenerator or
recuperator) in which the uncondensable products of distillation are heated;
B is a conduit (pipe or channel) conveying the heated gases to the retorts C;
1) is a receiving conduit (pipe or channel) conveying the product of distillation
and the gases to the condenser E F is the receiver; K à conduit leading the
uncondensable gases already cooled and free from water, to the fan L: M is a
gas vessel which may be a gas-holder in a plant of considerable size; N is a con-
duit conveying the surplus gas to the fire-box of the apparatus A or to a motor,
to lighting burners or the like.
The course of the operation is as follows:-The apparatus A is heated and
the dampers connecting the main conduit B to the retort C, as well as the
dampers connecting the retorts to the receiving conduit D, are opened. The
fan L is then started, thus producing a circulation of gases in a closed circuit,
that is to say the gases heated in the apparatus A are lead through the conduit B
into the retorts C where they give up their heat to the matters to be treated:
then, charged with the products of distillation, they are conveyed through the
conduit D to the cooling apparatus E where the liquefied products fall into the
receiver and the uncondensable products are conveyed by the fan L into the gas-
holder M whence they are partly led through the conduit Q into the fire-box
and partly returned through the conduit N into the heating apparatus A and
so on.
It is obvious from the foregoing that the hereinbefore described method of
distillation is equally applicable in the case when the distillation in a medium
of hot gases supplied from without (generator gas, water gas, etc.,) may be com-
pletely unavailable for any reason as, for instance, in the case of gas-works,
where the principal product, that is lighting gas, being mixed with foreign
gaseous matters would be spoiled, or of coking furnaces for producing ordinary
or metallurgical coke, where the bulk of the gases obtained during the process
is always greater than the quantity capable of being utilized as fuel for such
furnaces.

page_text: I will now explain the operation in the distillation of naphtha as an example
of fractional distillation.
Whatever modifications may be introduced into the naphtha-distilling pro-
cess, the products of distillation always contain gases uncondensable in the
cooling apparatus. Such gases or vapours emanating from the cooling apparatus
are conveyed into a special furnace where they are heated to the required
degree and then led into an alembic or still containing naphtha to be distilled
to which the gases give up their heat and then, enriched by the naphtha-
vapours, are conveyed into the cooling apparatus where the gaseous products are
condensed and the uncondensable products are conveyed partly to the heating
furnace and the surplus to the apparatus where they can be utilized, as for
instance fire-boxes, heating or lighting burners, or the like. The gases led
into the heating furnace are again conveyed into the still and so on, the course
of the operation being in short, analogous to that of the dry distillation of
wood. The hot gases entering the still not only heat the matters to be dis-
tilled (naphtha, its derivatives, resins, or the like) but at the same time agitates
and mixes the liquid for which purpose superheated steam is ordinarily used.
To produce the required circulation of the gases they are generally exhausted
from the still (but they may be also forced in when necessary) so that a certain
vacuum is produced in the still which accelerates and improves the distillation.
As by this process the external heating of the still is completely avoided,
since the heat required for the distillation is communicated by direct contact
of the hot gases with the matters undergoing distillation, the following advan-
tages are attained: -
(1) The masonry of the still, which impedes the supervision and maintenance
of the apparatus is dispensed with;
(2) The still is not exposed to burning and to the destructive action of the
flame:
(3) The projection of the liquid, caused by ebullition, is avoided :
(4) A fire-dangers are obviated:
(5) In case of an obstruction in the cooling apparatus, as for instance by
paraffine, an explosion cannot take place, since the current of gases to the still
will be intercepted and the temperature in the still will fall:
(6) The stoppage of the neighbouring stills installed in the same room, in the
event of one of them being cooled down, is avoided whilst in existing plants all
the furnaces are ordinarily extinguished in such a case:
(7) The distillation is considerably accelerated because the requisite heat is
transmitted to the distilled liquid directly and quickly, without danger of
decomposing the products;
(8) The possibility of fractionating the products within narrower limits than
by the existing methods, since the heat required for the distillation being trans-
mitted by direct contact, can be easily controlled to the desired degree.
Should the distilled solid or liquid matter yield uncondensable gases in
insufficient quantity, suitable admixtures of gases supplied from without may
be made. At the commencement of the distillation of very thick liquids they
may be heated by any suitable means, to diminish the resistance to the current
of gas.
When a newly-installed plant is started, or one which has been out of
work for a long time and of which the conduits are filled with air, the latter
can be displaced and removed by means of a gas supplied from without, or a
small quantity of fuel, such as charcoal, may be charged into one of the retorts,
then fired up and the retort closed while the fan is started, so that after the
circulation has made several cycles through the conduits and apparatus all the
paces will be filled with a mixture of neutral gases.
Dated this 15th day of June 1800.
A. M. & WM. ('LARK,
Chartered Patent Agents, 53, Chancery Lane, London.

page_text: Improvements in the Distillation of Solid and Liquid Matters.
I, MOSES WAISSBEIN, of No. 9, Great Wulf Street, St. Petersburg, in the
Empire of Russia, Technologist, 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 relates to a process of distillation applicable to the simple,
fractional or dry (destructive) distillation of any solid, as well as liquid matters.
It would be superfluous to describe all the different details of its application
to the various matters which may be treated by this process; it will be sufficient
to explain the course of the operation:-
(a) for treating wood, as an example of dry distillation generally;
(b) for treating naphtha, as an example of the distillation of liquids.
These examples serve to prove, that the operation is substantially identical
in the two cases and to demonstrate the advantage of this process in all its
various applications for purposes of distillation.
Before explaining the details of the dry distillation of wood, it may be men-
tioned that the attempts to conduct this process by means of hot gases devoid
of free oxygen (or by means of superheated steam) whose heat when such gases
are led into direct contact with the matters to be distilled, serves as agent for
the operation, have given very advantageous results. But since distillation by
means of hot gases (carbonic oxide, carbonic acid, generator gas, water gas, etc.,)
notwithstanding all its advantages, has not only failed to generally supplant
the older methods but has not even been adopted in practice, it is by reason of
certain serious inconveniences inherent to this system as, for example excessive
dilution of the products, the necessity of utilizing the exhaust gases, and so on.
In fact, when the dry distillation of wood (or other organic matters) is per-
formed in a medium of hot gases devoid of free oxygen the heat of such gases
serving as the distilling agent the products of distillation are mixed with con-
densed water vapours always contained in the gases so that the product becomes
more or less diluted. This necessitates an enlargement of dimensions of the
plant, of the receivers, and of the apparatus for treating the matters, occasioning
a considerable waste of products and increased expense for fuel for the final
treatment of the products; moreover the condensation of aqueous vapors con-
tained in the hot gases necessitates more voluminous cooling apparatus, such
vapors in their condensation giving up a considerable quantity of latent heat.
In certain cases, as for instance in working with generator gas, the products
of distillation are contaminated with resin contained in this gas, which may be
disadvantageous. Finally, in many cases, as in the distillation of small waste
matters (saw-dust, spent tan, dye-wood waste, or the like) when wood is dear
and coal cheap, as in industrial centres, it will be always more advantageous
to forego this method because the hot gases of coal contain sulphur which causes
rapid wear of the apparatus. The inconvenience of the hot gas process as here-
tofore proposed for this purpose, consists, moreover, in the fact that such gases
require to be utilized after being exhausted, otherwise the cost of fuel would
be considerably increased as will be readily seen when the fact that these gases
such as carbonic oxide, generator gas, water gas, etc., are nothing less than
On the
products of incomplete combustion of fuel, is taken into consideration.
other hand the utilization of these gases increases the structural cost of the
plant and the complication of the apparatus, whilst the amount of gases to be
utilized may considerably exceed that which can be used as fuel.
It is obvious from the foregoing that the method of dry distillation of wood

page_text: or other organic matters in a medium of hot gases supplied from without not-
withstanding its material advantages (increase of efficiency, economy of time,
simplicity of the operation, etc.,) is nevertheless very imperfect owing to the
presence in such gases of deleterious constituents (aqueous vapours, resin,
sulphur, etc.). It may of course, be possible to eliminate all these deleterious
matters but, apart from the cost of the plant, this operation may entail a con-
siderable loss of heat because the purification of the gases would involve their
cooling and subsequent re-heating to the temperature required for distillation.
Whatever modifications may be introduced into the process of dry distillation
of wood or other organic matters, the solid products (charcoal, coke, etc.,) and
the liquid products (tar-water, ammoniacal water, resins, etc.,) will always con-
tain gases which remain uncondensed in the cooling apparatus.
The method forming the subject of the present invention consists in the
utilization of such uncondensable gases free from aqueous vapours and from
resin (as well as from sulphur when none is contained in the matters under-
going distillation) and obtained in comparatively small quantities, as an agent
or medium in which to effect the dry distillation of organic or other matters.
The drawing accompanying my Provisional Specification shews diagrammatic-
ally the general arrangement of the plant employed for this purpose. A is the
apparatus (regenerator or recuperator) in which the uncondensable products of
distillation are heated: B is a conduit (pipe or channel) conveying the heated
gases to the retorts C: D is a receiving conduit (pipe or channel) conveying the
product of distillation and the gases to the condenser E; F is the receiver; K a
conduit leading the uncondensable gases already cooled and free from water,
to the fan L; M is a gas vessel which may be a gas-holder in a plant of con-
siderable size; N is a conduit conveying the surplus gas to the apparatus A
for reheating and Q is a pipe leading to a motor, to burners or to the fire-box
of the apparatus A.
The course of the operation is as follows:-The apparatus A is heated and
the dampers connecting the main conduit B to the retort C, as well as the
dampers connecting the retorts to the receiving conduit D, are opened. The
fan is then started, thus producing a circulation of gases in a closed circuit,
that is to say the gases heated in the apparatus A are led through the conduit B
into the retorts (where they give up their heat to the matters to be treated;
then, charged with the products of distillation, they are conveyed through the
conduit 1 to the cooling apparatus E where the liquefied products fall into the
receiver and the uncondensable products are conveyed by the fan L into the gas-
holder M whence they are partly led off through the conduit Q and partly
returned through the conduit N into the heating apparatus A and so on.
It is obvious from the foregoing that the hereinbefore described method of
distillation is equally applicable in the case when the distillation in a medium
of hot gases supplied from without (generator gas, water gas, itc.,) may be com-
pletely unavailable for any reason as, for instance, in the case of gas-works.
where the principal product, that is lighting gas, being mixed with foreign
gaseous matters would be spoiled, or of coking furnaces for producing ordinary
or metallurgical coke, where the bulk of the gases obtained during the process
is always greater than the quantity capable of being utilized as fuel for such
furnaces.
I will now explain the operation in the distillation of naphtha as an example
of fractional distillation.
Whatever modifications may be introduced into the naphtha-distilling pro-
cess, the products of distillation always contain gases uncondensable in the
cooling apparatus. Such gases or vapours emanating from the cooling apparatus
are conveyed into a furnace where they are heated to the required
degree and then led into an alembic or still containing naphtha to be distilled
to which the gases give up their heat and then, enriched by the naphtha-
vapours, are conveyed into the cooling apparatus where the gaseous products are

page_text: condensed and the uncondensable products are conveyed partly to the heating
furnace and the surplus to the apparatus where they can be utilized, as for
instance fire-boxes, heating or lighting burners, or the like. The gases led
into the heating furnace are again conveyed into the still and so on, the course
of the operation being, in short, analogous to that of the dry distillation of
wood. The hot gases entering the still not only heat the matters to be dis-
tilled (naphtha, its derivatives, resins, or the like) but at the same time agitates
and mixes the liquid for which purpose superheated steam is ordinarily used.
To produce the required circulation of the gases they are generally exhausted
from the still (but they may be also forced in when necessary) so that a certain
vacuum is produced in the still which accelerates and improves the distillation.
As by this process the external heating of the still is completely avoided,
since the heat required for the distillation is communicated by direct contact
of the hot gases with the matters undergoing distillation, the following advan-
tages are attained:-
(1) The masonry of the still, which impedes the supervision and maintenance
of the apparatus is dispensed with;
(2) The still is not exposed to burning and to the destructive action of the
flame;
(3) The projection of the liquid, caused by ebullition, is avoided;
(4) All fire-dangers are obviated;
(5) In case of an obstruction in the cooling apparatus, as for instance by
paraffin, an explosion cannot take place, since the current of gases to the still
will be intercepted and the temperature in the still will fall;"
(6) The stoppage of the neighbouring stills installed in the same room, in the
event of one of them being cooled down, is avoided whilst in existing plants all
the furnaces are ordinarily extinguished in such a case;
(7) The distillation is considerably accelerated because the requisite heat is
transmitted to the distilled liquid directly and quickly, without danger of
decomposing the products;
(8) The possibility of fractionating the products within narrower limits than
by the existing methods, since the heat required for the distillation being trans-
mitted by direct contact, can be easily controlled to the desired degree.
Should the distilled solid or liquid matter yield uncondensable gases in
insufficient quantity, suitable admixtures of gases supplied from without may
be made. At the commencement of the distillation of very thick liquids they
may be heated by any suitable means to diminish the resistance to the current
of gas.
When a newly-installed plant is started, or one which has been out of
work for a long time and of which the conduits are filled with air, the latter
can be displaced and removed by means of a gas supplied from without, or a
small quantity of fuel, such as charcoal, may be charged into one of the retorts,
then fired up and the retort closed while the fan is started, so that after the
circulation has made several cycles through the conduits and apparatus all the
spaces will be filled with a mixture of neutral gases.
Having now particularly described and ascertained the nature of the said
invention and in what manner the same is to be performed, I declare that what
I claim is: :-
A new method of distillation of solid or liquid matters, characterized by the
fact that the operation is performed by means of the heat of uncondensable
gaseous products of the distillation itself, heated to the required temperature.
Dated this 12th day of March 1900.
A. M. & WM. CLARK,
Chartered Patent Agents, 53, Chancery Lane, London.