Regenerating the Purifying Agent.
Year: 1887

page_text: Date of Application, 12th Apr., 1887
Complete Left, 13th Dec., 1887
Complete Accepted, 13th Jan., 1888
Regenerating the Purifying Agent.
We, IVAR AXEL FERDINAND BANG of Rue de la Passy, Paris, France, Chemist, and
MARIE CHARLES ALFRED RUFFIN of Avenue d'Antin, Paris, France, Chemist, do
hereby declare the nature of this invention to be as follows:-
In the specification No. 10870 of 1884 and No. 783 of 1886 were described means
of purifying crude spirit by the application of hydro-carbons capable of dissolving and
eliminating impurities such as fusel and other essential oils. This invention relates to
improvements in the process described in these specifications, and in the apparatus
employed for conducting it. The spirit to be treated is first rendered alkaline by the
addition of soda or potash, or it might be lime or other alkaline earth. Soda is pre-
ferred on account of its cheapness and solubility. When lime or other alkaline earth
is used the mixture has to be continuously agitated, but when soda or potash
is employed only occasional agitation is necessary. In applying the alkali, it is to be
mixed with the spirit in repeated small doses for 20, or 30 hours until at last the spirit
is found by testing to be decidedly alkaline. It is then charged into a vessel nearly
up to the level of an overflow pipe at the top, and a petroleum oil, as pure as possible
without taste or smell, and of such character that it does not boil under 100° C. is
pumped into the vessel through a perforated pipe near the bottom. The oil rising in
numerous small streams through the spirit, overflows at the top and descends through
a series of vessels to be regenerated. These vessels are first a filter which entraps solid
impurities, then a washer containing water which retains such spirit as the oil may
carry with it, next several successive vessels in which the oil is treated with sulphuric
acid, finally a vessel in which it is treated with solution of soda to neutralise such acid
as the oil may contain. Each of these vessels is arranged with a perforated floor on
which are placed fragments of flint, glass, or other substances not attacked by acid.
The oil enters under the perforated floor, and rises in subdivided streams through the
contents of the vessel, overflowing at the top by a pipe which leads it under the floor
of the next vessel in order. The regenerated oil from the last or soda vessel passes to
a pump by which it is forced back to the vessel containing the spirit, which by the

page_text: circulation of the oil during 20, or 30 hours becomes purified. During the operation,
at intervals of 2 or 3 hours a portion of the impure acid is withdrawn from the upper-
most of the vessels containing it, and a corresponding quantity is transferred from
each of these vessels to the next above it, a corresponding supply of fresh acid being
introduced into the lowest of the vessels. The preliminary alkalising of the spirit,
though not absolutely necessary is important as promoting elimination of aldehyde.
By the use of petroleum oil of a comparatively heavy character, not flashing under
140° C. risk of fire is avoided and as this oil is not volatile, all the vessels employed
may be open.

page_text: Regenerating the Purifying Agent.
We, IVAR AXEL FERDINAND BANG of Rue de la Passy, Paris, France, Chemist and
MARIE CHARLES ALFRED RUFFIN of Avenue d'Antin, Paris, 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:-
It has been proposed to purify crude spirit by the application of hydrocarbons
capable of dissolving and eliminating impurities such as fusel and other essential oils.
This Invention relates to an improved process and apparatus employed for conducting
it as will be described referring to the accompanying drawings. Fig. 1 represents a
longitudinal section and Fig. 2 a plan showing an arrangement of apparatus for
conducting the purifying process in the following manner.
The spirit to be treated is first rendered alkaline by the addition of soda or potash,
or it might be lime or other alkaline earth. Soda is preferred on account of its cheap-
ness and solubility. When lime or other alkaline earth is used, the mixture has to be
continuously agitated, but when soda or potash is employed only occasional agitation
is necessary. In applying the alkali it is to be mixed with the spirit in repeated small
doses for 20 to 30 hours until at last the spirit is found by testing to be decidedly
alkaline. It is then ready for purification and for this purpose the alkaline spirit is
run into a vessel A up to a level a little under that of the overflow pipe H.
A petroleum oil as pure as possible, without taste, or smell, and of such character
that it does not boil under 100° C. is now pumped into the vessel A through a per-
forated pipe T. The oil rises in numerous small streams through the spirit collects at
the top and overflows by the pipe H through the open stopcock G into the filter B
which has a partition B'. The oil descending on one side of the partition and ascending
on the other deposits in B some of the heavier impurities carried over by it. From B
the oil overflows to the next vessel C which it enters at the bottom from a perforated
pipe and through a perforated floor J. On this floor are laid a number of clean
fragments of flint, glass or other such like material and the vessel is charged with
water. The oil rising in fine streams subdivided by the solid fragments through the
water gives up to it such small quantity of spirit as may be carried over by it
from A. From the water vessel C the oil passes through a succession of vessels D
each of which is charged with sulphuric acid and with fragments of flint, glass or
substances of a like kind such as are not attacked by the acid. Practically it is found
that four of the sulphuric acid vessels D suffice for the complete regeneration of the
hydrocarbon, the acid taking up the essential oils which the hydrocarbon had eliminated
from the spirit. From the last of the vessels D the hydrocarbon passes to a vessel E
containing a solution of soda which neutralises such acid as the hydrocarbon may
contain.. Finally from E the regenerated hydrocarbon passes to a reservoir F from

page_text: which it is drawn by a pump P and sent by a pipe R back to A to pass again through
the spirit. This treatment continued from 20 to 30 hours effects purification of the
charge of spirit contained in A. During the operation at intervals of 2 or 3 hours a
portion of the impure sulphuric acid is withdrawn from the uppermost of the Vessels D
and a corresponding quantity is transferred from each of the vessels D to the next
above it a corresponding supply of fresh acid being introduced into the lowest of the
vessels D. The vessels D which contain sulphuric acid are preferably made of wood
lined with lead and provided with leaden pipes and their perforated branches S. The
perforated floors J not being exposed to oxidation may be of copper.
In the process above described the preliminary alkalising of the spirit though not
absolutely necessary is important as promoting the elimination of such aldehyde as the
spirit may contain. By the use of petroleum oil of a comparatively heavy character,
that does not flash under 140° C. risk of fire is avoided and owing to the oil not being
volatile all the vessels employed may be open as shown.
We make no general claim to the purification of crude spirit by hydrocarbons nor
to the regeneration of the hydrocarbons by sulphuric acid, operations of this kind
having been previously proposed and applied by us more or less experimentally
but having now particularly described and ascertained the nature of this Invention
and in what manner the same is to be performed we declare that what we claim is :-
1. The herein described process for purifying crude spirit by passing through it
heavy petroleum oil of the kind mentioned, and for regenerating the oil, so that the
process can be carried on continuously on a given quantity of spirit during the time
necessary for its purification.
2. The apparatus for purifying crude spirit and regenerating the hydrocarbon,
substantially as described and illustrated by the accompanying drawings.
Dated thin 12th day of December 1007
ABEL & IMRAY,
Agents for the Applicants.