Year: 1886

page_text: We, IVAR AXEL FERDINAND BANG, of 83 Rue de La Passy, Paris, France
Chemist and MARIE CHARLES ALFRED RUFFIN, of 18 Avenue d'Antin, Paris,
France, do hereby declare the nature of this invention to be as follows:-
In the specification to Patent No. 10870 of 1884 was described a process for the
purification of the phlegms whereby the totality of alcohol of good flavour was
obtained. As the process there described is open to certain objections on the
ground of. the slowness of the process as also the possible danger resulting from
the use of inflammable hydrocarbon, the present improvements have for their
object to obviate these objections. In the specification to the said Patent it has
been stated that there are employed, for disinfecting or deodorising the pblegins,
bydrocarbons that distil off at low temperatures and that these are by preference
obtained from the volatile products of petroleum, commonly called essence of
petroleum, the hydrocarbon employed by preference being that which boils at
between 40° and 50° C.
In order to satisfy the requirements of insurance companies, we have, in con-
sequence of further experiments, been led to adopt heavy hydrocarbons that do not
boil below 100° C. This oil, which is generally termed mineral lubricating oil,
offers no risk of burning and, as it does not evaporate in the open air, it has the
advantage of not requiring hermetically closed recipients so that the improved
process can be applied without danger in hot climates. This hydrocarbon is
already indicated in the specification to the said former Patent, as it belongs to the
fatty series, but it is to be understood that we can use, no matter what kind of
hydrocarbon of the aromatic series which fulfils the same conditions provided it be
of a liquid nature.
We have described in the former specification a method for disinfecting or
deodorising the hydrocarbon which has served for purifying the phlegms, by means
of sulphuric acid. This method caused an expenditure of acid which we have
found means of obviating. For this purpose, having found that if the hydrocarbon
has a great affinity for the oils contained in the aqueous alcohol or phlegm, it loses
this quality in contact with alcohol of a higher percentage, which, on the other
hand, is essentially absorbent of these oils, we have substituted in the washing

page_text: .
vessels ordinary alcohol for sulphuric acid. The purification of the hydrocarbon is
80 complete that it requires a very small quantity of alcohol which is readily
regained by partial distillation. By cur. improved process therefore we have
obviated all danger from fire as also the expense attendant on the use of
sulphuric acid.
In the said former specification it was stated that bydrocarbon was injected at
the bottom of a column filled with phlegms which hydrocarbon, by virtue of its
small specific gravity, rose to the surface while dissolving, and carrying with it all
the impurities contained in the alcohol. This hydrocarbon afterwards passed into
washing vessels in which it was purified and was then again injected into the
phlegms by means of a pump. This process had the inconvenience of being very
slow, because the alcohol, being only brought into contact with a small quantity of
hydrocarbon, it was necessary to repeat the washing frequently in order to obtain
perfect purification. To remedy this we have modified the apparatus as will now
be described.
•
In the first apparatus which requires the greatest room, the phlegms are passed
into the hydrocarbon which reduces the operation to simple filtration, the principle
remaining always the same viz. the removal of the bad flavour by the repeated
contact of the phlegms and hydrocarbon. For this purpose there are employed a
series of vessels, the bottom of one being connected with the top of the next
following one, so that the liquid which has passed in a downward direction through
the one will enter at the top of the next following one in order to pass through
the same in a downward direction also, and so on. These vessels are filled with
hydrocarbon and they also, by preference, are partly filled at their middle either
with sponge or with diaphragms having openings alternately on opposite sides, in
order to ensure perfect contact of the phlegms with the hydrocarbon as they are
made to pass through the vessels, being introduced into the first one from a raised
tank. It will be understood that the more impure the phlegms are, the greater
will be the number of vessels required in order to repeat the purifying operation a
sufficient number of times, until the alcohol passes in a perfectly pure state from
the last of the vessels. As it is essential to maintain the hydrocarbon of the last
vessel in a perfect state of purity, it is advisable to provide each vessel with a
sample cock in order to ascertain from time to time the degree of saturation of the
hydrocarbon so as to change it, if necessary.
For renewing the hydrocarbons, the passage of the phlegms through the vessels
is stopped by the closing of the supply and discharge cocks and a communication
is established between the last vessel of the series and a second tank containing
hydrocarbon, so that a supply of hydrocarbon is now introduced into the purifying
vessels in the contrary direction to that in which the alcohol flows, so that, by this
means, the hydrocarbon in the vessels, which is saturated with the impurities, is
driven out through a cock on the first vessel of the series in proportion as the fresh
charge of hydrocarbon enters. By this means, either the contents of the whole of
the vessels may be changed at one time or only a portion thereof. The hydro-
carbon is purified in the washing vessels either by means of sulphuric acid or by
means of alcohol as aboved described.
Another modification of the apparatus, which is employed by preference, on
account of its simplicity and the small space occupied by it, consists of a single
vertical column of some height which varies according to the quantity and quality
of the phlegms to be operated upon. This column is provided with either porous
material or with separate diaphragms in a similar manner to. 'the vessels above
described. Its lower end is made to communicate with a reservoir filled with
hydrocarbon situated at a level somewhat above the top of the column, the hydro-
carbon being admitted at a level some distance above the bottom. The top of the
column is made to communicate with a reservoir charged. with phlegms to be
purified and discharge pipes are provided at the top and bottom of the column.
The lower part of the column having been filled with water up to the level of
the inlet pipe for hydrocarbon, the latter is allowed to flow in until the column is

page_text: filled, the water introduced at bottom having for its object to prevent the hydro-
carbon from escaping through the lower discharge pipe. The communication
between the top of the column and the reservoir of phlegms is now opened, and
the latter, by virtue of their greater specific gravity, now descend through the
column, driving out the water at the bottom and passing away through the lower
discharge pipe perfectly purified. The porous material, which may be carried on
perforated diaphragms arranged at distances apart in the column, serves to sub-
divide the liquids so as to bring them into intimate contact with each other as the
phlegmis pass through. The apparatus is made to act continuously, the phlegins
being discharged continuously through the lower discharge pipe as they descend
through the column of hydrocarbon, which at the same time rises up through the
vessel and passes off through the upper discharge pipe. The advantage of this
arrangement of apparatus, in addition to the economy which is effected in its
installation, is that the phlegms are continuously in contact with the pure bydro-
carbon which is always renewed, so that the process of purification is effected
much more rapidly.

page_text: We, IVAR AXEL FERDINAND BANG of 83 Rue de La Passy, Paris, France
Chemist and MARIE CHARLES ALFRED RUFFIN, of 18 Avenue d'Antin, Paris
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:-
In the Specification to Patent No. 10870 of 1884 was described a process for the
purification of phlegms whereby the totality of alcohol of good flavour was obtained.
As the process there described is open to certain objections on the ground of the
slowness of the process as also the possible danger resulting from the use of
inflammable hydrocarbon, the present improvements have for their object to
obviate these objections. In the specification to the said Patent it has been stated
that there are employed, for disinfecting or deodorising the phlegms, hydrocarbons
that distil off at low temperatures and that these are by preference obtained from
the volatile products of petroleum, commonly called essence of petroleum, the
hydrocarbon employed by preference being that which boils at between 40°
and 50° C.
In order to satisfy the requirements of insurance companies, we have, in conse-
quence of. further experiments, been led to adopt heavy hydrocarbons that do not
boil below 100° C. This oil, which is generally termed mineral lubricating oil,
offers no risk of burning and, as it does not evaporate in the open air, it has the
advantage of not requiring hermetically closed recipients so that the improved
process can be applied without danger in hot climates. This hydrocarbon is
already indicated in the specification to the said former Patent, as it belongs to
the fatty series, but it is to be understood that we can use, no matter what kind
of hydrocarbon of the aromatic series which fulfils the same conditions provided it
be of a liquid nature.
We have described in the former specification a method for disinfecting or
deodorising the hydrocarbon which has served for purifying the phlegms, by means
of sulphuric acid. This method caused an expenditure of acid which we have
found means of obviating. For this purpose, having found that if the hydrocarbon
has a great affinity for the oils contained in the aqueous alcohol or phlegm, it loses
this quality in contact with alcohol of a higher percentage, which on the other
hand is essentially absorbent of these oils, we have substituted in the washing
vessels ordinary alcohol for sulphuric acid. The purification of the hydrocarbon is
so complete that it requires a very small quantity of alcohol which is readily
regained by partial distillation. By our improved process therefore we have
obviated all danger from fire, as also the expense attendant on the use of sulphuric
acid.
In the said former specification it was stated that hydrocarbon was injected at
the bottom of a column filled with phlegms which hydrocarbon, by virtue of its

page_text: small specific gravity, rose to the surface while dissolving, and carrying with it all
the impurities contained in the alcohol. This hydrocarbon afterwards passed into
washing vessels in which it was purified and was then again injected into the
phlegms by means of a pump. This process had the inconvenience of being very
slow, because the alcohol, being only brought into contact with a small quantity of
hydrocarbon, it was necessary to repeat the washing frequently in order to obtain
perfect purification. To remedy this, we have modified the apparatus as will now
be described referring to the accompanying drawings.
In the first apparatus which requires the greatest room, the phlegms are passed
into the hydrocarbon which reduces the operation to simple filtration, the principle
remaining always the same viz, the removal of the bad flavour by the repeated
contact of the phlegms and hydrocarbon. For this purpose as shewn in section in
Fig. 1 there are employed a series of vessels V VI V, the bottom of one being
connected with the top of the next following one, so that the liquid which has
passed in a downward direction through the one will enter at the top of the next
following one in order to pass through the same in a downward direction also, and
so on. These vessels which are filled with hydrocarbon may have deflecting
diaphragms p like those described in the previous specification, but they are partly
filled at their middle with pieces of sponge q or other porous material, in order to
ensure perfect contact of the phlegms with the hydrocarbon as they are made to
pass through the vessels. They are introduced into the first vessel V from a raised
tank A by a pipe L provided with a stop cock B and they pass from vessel to
vessel till they issue-from the last V2 on opening the cock E being then pure and
ready for rectification. It will be understood that the more impure the phlegms
are, the greater will be the number or height of vessels required in order to repeat
the purifying operation a sufficient number of times, until the alcohol passes in a
perfectly pure state from the last of the vessels. As it is essential to maintain the
hydrocarbon of the last vessel in a perfect state of purity, it is advisable to provide
each vessel with a sampling cock D in order to ascertain, from time to time, the
degree of saturation of the hydrocarbon so as to change it if necessary.
For renewing the hydrocarbons the passage of the phlegms through the vessels is
stopped by the closing of the supply and discharge cocks B and E and, by opening
a cock F, a communication is established between the last vessel V of the series
and a second tank G containing hydrocarbon, so that, on opening a cock C, &
supply of hydrocarbon is introduced into the purifying vessels in the contrary
direction to that in which the alcohol flows, so that, by this means, the hydrocarbon
in the vessels, which is saturated with the impurities, is driven out through the
cock C on the first vessel in proportion as the fresh charge of hydrocarbon enters.
By this means, either the contents of the whole of the vessels may be changed at
one time or only a portion thereof. The hydrocarbon is purified in the washing
vessels either by means of sulphuric acid or by means of alcohol as aboved described.
A modification of the apparatus shewn in Fig. 2 which is employed by preference,
on account of its simplicity and the small space occupied by it, consists of a single
vertical column X of some height which varies according to the quantity and
quality of the phlegms to be operated upon. This column is provided with
deflecting diaphragms or preferably with porous material separated by diaphragms.
The lower end of X communicates with a reservoir G of hydrocarbon situated at a
level somewhat above the top of the column, the hydrocarbon being admitted
into X at a level oo some distance above the bottom. The top of the column
communicates by a pipe L with a reservoir A charged with phlegms to be purified,
and discharge pipes C and E are provided at the top and bottom of the column.
At the lower part of the column there is an external pipe K making communications
at different levels. The lower part of the column having been filled with water up
to o o, the cock F is opened and hydrocarbon flows in until there is overflow at C.
The water introduced at bottom prevents the hydrocarbon from escaping through
the discharge pipe E. The cock B is now opened, and the phlegms from A by
virtue of their greater specific gravity, now descend through the column, driving

page_text: out the water at the bottom and passing away through E perfectly purified. The
porous material, which may be carried on perforated diaphragms arranged at
distances apart in the column, serves to subdivide the liquids so as to bring
them into intimate and repeated contact with each other.
The advantage of this arrangement of apparatus, in addition to the economy.
which is effected in its installation, is that the phlegms are continuously in contact
with the pure hydrocarbon which is always renewed, so that the process of puri-
fication is effected much more rapidly.
.
In order to promote disappearance of the aldehyde contained in the phlegms, a
little alkali, preferably soda, may be intimately mixed with them before washing,
and if after washing they are found to be too alkaline, they should be neutralised
before rectifying.
Having now particularly described and ascertained the nature of our said
invention and in what manner the same is to be performed we declare that what
we claim is
1. Purifying alcoholic phlegms by means of heavy hydrocarbon oils of the
aromatic series which have a boiling point not below 100° C.
2. Purifying by means of strong alcohol, hydrocarbons that have been used for
purifying alcoholic phlegms.
3. For purifying alcoholic phlegms the use of apparatus substantially as described
with reference to Fig. 1, this apparatus consisting of a series of vessels communi-
cating with each other and with reservoirs, and arranged to operate as herein set
forth.
4. The use of the modified apparatus, substantially as described with reference
to Fig. 2, wherein a vertical column divided into compartments by perforated
diaphragms is substituted for the series of separate vessels.
1000