Improvements in and Apparatus for Treating or Purifying, Rectifying, Ageing, Deodorizing, and Decolourizing Alcoholio and other Liquids or Liquefied Matter.
Year: 1896

page_text: Date of Application, 29th Dec., 1896-Accepted, 27th. Mar., 1897
Improvements in and Apparatus for Treating or Purifying,
Rectifying, Ageing, Deodorizing, and Decolourizing Alcoholio
and other Liquids or Liquefied Matter.
I, JAMES YATE JOHNSON of 47 Lincoln's Inn Fields, in the County of London
Gentleman, do hereby declare the nature of this invention (which has been com-.
municated to me from abroad by The Electric Rectifying and Refining Company,
a Company organized under the laws of the State of New Jersey, United States
of America, having an office at 552 Federal Street Camden New Jersey aforesaid
and doing business in Philadelphia Pennsylvania) and in what manner the same is
to be performed to be particularly described and ascertained in and by the following
statement :-
This invention has for its object to provide an improved process of treating or
purifying rectifying ageing deodorizing and decolourizing alcoholic and other
liquids or liquified matter and in apparatus for carrying out the said process.
The principal objects of this invention are to effect the purification, rectification
and ageing of ordinary alcoholic liquids and the like and the decolourizing and-"
deodorizing of methylated spirits, (I will refer to the matter to be treated generally
as the liquid) by treatment with ozone in such a way as to effect the desired result.
in the most efficient and speedy as well as in the simplest manner, and also to.
provide a simple and effective apparatus for carrying out the process, in which the
parts are arranged so as to cause the ozone gas to act upon the liquid in the most
direct and effective way.
The process consists essentially in subjecting the liquid to the action of ozone-
gas in vacuo and in the details of the said process, as hereinafter more particularly;
described and the novel features of the apparatus for carrying out the said process;.
are hereinafter particularly described with reference to the accompanying:
drawings.
According to this invention the liquid to be treated is introduced into a vessel
connected with an air exhauster or vacuum pump for the purpose of exhausting the
air therefrom. After the air has been sufficiently exhausted to establish a suitable
vacuum, the connection with the air exhauster or vacuum pump is closed and the
vessel is then put in communication with the ozone supply. The degree of vacuum
to be maintained in the treating vessel may be varied, the general rule being that
the nearer a perfect vacuum is approached the more rapid will be the treatment.
A sufficient quantity of the ozone gas is then admitted to the vessel containing the
liquid, the said gas permeating the liquid and thoroughly and intimately mixing
with every portion of the same, the ozone readily and completely filling the spaces
previously occupied by the air.
In the treatment of liquids in this manner the ozone by oxidation converts the
more carbonized alcohols and compound ethers into other ethers and acids, and I
give the following as illustrating the particular change that takes place in alcoholic
liquid or other impurities when subjected as aforesaid to the action of the ozone.
As fusel oil found in 'spirits contains amyl alcohols (C,H,OH), propyl alcohols
(C,H,,OH), butyl alcohols (C.H, OH), and oenanthol aldehyde (CH,COH), the
oxidation by the ozone, causes the amyl alcohol to be converted into isovaleric
acid (CHO), the butyl alcohol into butyric acid (CHO), and oenanthol
aldehyde into oenanthylic acid (C,HO,), while some of the essential oils are
:

page_text: entirely destroyed, and this conversion of the alcohols into the corresponding acids
and destruction of the essential oils imparts to the spirits the boquet and mellowness
hitherto imparted by time, while the action upon wood alcohol effects the complete
decolourization and deodorization of the same.
In order to increase the efficiency of the process, it is preferred to employ means
for regulating the temperature of the liquid, while undergoing the treatment.
In the apparatus according to this invention there is preferably employed a spiral
coil pipe situated within the vessel containing the liquid to be treated, through
which coil, a fluid such as steam, air or water may be passed for regulating the
temperature of the liquid and, although the ozone may be derived from any suitable
source, it is found that the most economically and efficiently obtained ozone for the
treatment is that obtained by subjecting oxygen gas to refrigeration and then
passing the cooled gas through an ozone generator in which fine sprays, or streams,
of cooling water or other fluid are caused to cool the gas, thereby decreasing its
temperature, and simultaneously subjecting the gas to the, influence of an electrical
brush discharge, thus converting the oxygen into ozone of great strength. The
ozone thus generated may be led directly into the vessel containing the liquid under
treatment, or, if desired, it may be led to a reservoir kept sufficiently cool by
suitable means, and thence withdrawn as needed for the treatment.
I will now describe the preferred form of apparatus for carrying out the process,
as shewn in the accompanying drawings, in which,.
Figure 1 is a side elevation of the complete apparatus, partly in section.
Figure 2 is a detail sectional view of the ozone generator.
Figure 3 is a side elevation of a modified form of moveable carrier for the liquid
treating vessels..
Figure 4 is a plan of the carrier shewn in Figure 1.
Figure 5 is a detail side view, (partly in section,) of the improved liquid treating
vessel.
The same reference characters indicate the same or.corresponding parts in all the
figures.
Referring first to Figure 1, A is a tank or reservoir for the oxygen gas which is
derived from any suitable source. This tauk or reservoir A is connected by pipe a
to the ozone generator C, and interposed between the ozone generator and the tank
or reservoir A is a refrigerating or cooling tank B, through which the pipe a
passes on its way to the generator C, a portion of the pipe a being preferably
spirally coiled and being surrounded by a refrigerating liquid, or cooling medium,
for example, ammonium nitrate and water.
Instead of passing the oxygen gas through a cooling medium, the said gas may
be compressed to, say 150 atmospheres, and, by rapid expansion of the compressed
gas into either the ozone generator or the supply chamber for the same, the
temperature of the said oxygen will be decreased to a sufficient degree.
The ozone generator C consists essentially of a casing of dielectric
material
(say glass) c preferably in the form of a tube or pipe, (which may for example be
about 36 inches long and 5 inches in diameter,) closed at each end by caps which
are provided, respectively, with two apertures and cc (see Figure 2)."
Within this outer glass casing c is another casing or. box b, preferably of metal
and centrally supported therein and of such smaller diameter than the outer casing,
as to form a space between the two, and within the inner casing is a spraying
device consisting, in the example shewn of a perforated metal tube d closed at one
end and open at the other end which latter end passes through the perforation.
in the cap. at one end and is connected with a supply of cooling fluid such as air
or water, which may be admitted and out off as desired by means of the valve 65.
Connected to the inner casing b, preferably at one end, is a discharge pipe e
leading to an ejector E which may be used when desired for the purpose of
withdrawing any surplus fluid that may interfere with the spraying of the cooling
fluid within the said casing b.
Communicating with the interior of the glass tube cis a pipe secured in the

page_text: perforation. and leading to a T-coupling D, and forming one branch of the said
coupling, the other branch g being connected to a suitable vacuum or air pump G.
This coupling has a main stem connected to the admission pipes of the liquid
treating vessels H, and the said coupling is supported by suitable standards or
supports a sufficient distance from the floor to permit the stem to be readily
connected with the liquid treating vessels H, successively brought into position for
the treatment of the liquid.
The said vessels H are preferably carried upon a movable carrier or platform J
mounted on rollers i so that the several vessels, after being supplied with the liquid
for treatment, may be readily moved into position for connection with the
T-coupling D.
These moveable carriers or platforms. may be circular and mounted upon a
central axis, as shewn in Figures 1 and 4,; or they may be replaced by trucks, or
cars, running upon tracks, as shewn in Figure 3.
Referring again to the construction of the ozone generator, it will be seen that
the outer surfaces of the metal casing b and of the glass casing c are coated with a
layer or covering t of a material suitable for inducing an electric brush-discharge,
such as powdered carbon, lead dust, or other equivalent material, to each of which
casings are respectively connected the terminals of the secondary coil of a step-up
transformer supplied with a suitable current of electricity, preferably an alternating
current. The negative terminal is connected to the outer surface of the inner
casing, and the positive terminal is connected to the outer surface of the glass
casing. When the electric current is turned on a brush discharge is induced
between the inner walls of the glass casing, and the outer walls of the inner casing.
The oxygen gas enters the glass casing through the pipe a, and passes through
the annular space surrounding the inner casing, in which it is subjected to the
action of the brush-discharge, during which action cold water, or other suitable
cooling fluid, is caused to enter the perforated pipe or tube & being under
pressure the said air or water is forced through the perforations in the said pipe or
tube a, in fine streams, which strike the inner side of the metal casing b and any
surplus fluid that might interfere with the spraying action may be withdrawn from
the inner casing by means of the ejector E.
By refrigerating the oxygen, as herein before described, and by subjecting it to
the cooling action of the sprays of water or cold air in the casing b (the walls of
which separate the water or air from direct contact with the oxygen) ozone of a
very high degree of strength can be economically and rapidly produced, and for
this reason it is preferred to use in the present process the particular construction
of generator described,
The vessels for holding the liquid to be treated are preferably of a special
construction shewn in Figure 5, in which the said vessel consists of a glazed inetal
cylinder H, of a capacity of, say 100 gallons more or less, as the circumstances
may require. To the body of the said vessel is secured a top or cover L, provided
with a two-way valved inlet connected with the vacuum or air-exhauster and
gas supply through the stem, and through which inlet the liquid to be treated
may be introduced by way of the passages. This cover L is secured to the body
of the vessel by means of an air-tight joint consisting of projecting fanges bolted
together, between which flanges is interposed a lead gasket
m, or other suitable
packing material
A glass gauge n is connected to the sides of the vessel communicating with the
interior at the top and bottom, for the purpose of indicating the level of the liquid
in the vessel, and in this glass gauge is placed a thermometer o so that the
temperature of the liquid can be noted.
Within the vessel, preferably at the bottom, is a fluid conveyor, in the form of
a coil pipe p, placed so as to be covered by the liquid and having a valved' inlet p',
and a valved outlet p, the said inlet being connected with a suitable source of
refrigerating medium or heating medium, such as water, steam or air, for example,
whereby either of these media can be passed through the coil pipe p in order to

page_text: cool, or heat, the liquid in the vessel, according as it is desired to lower, or raise.
the temperature thereof, by which means the temperature of the liquid may be
maintained at any desired point, preferably at a low temperature.
From this description the mode of operating the apparatus and the manner of
carrying out the process according to this invention will be readily understood,
and may now be briefly summarized as follows:-
After the vessel is filled with the liquid, it is brought into position by means of
the rotatable platform, or the trucks, and connected with the main stem / of the
T-coupling D and there locked in position by suitable chocks, or otherwise, in
order to prevent movement of the platform and injury to the connections, while
the liquid is being treated. The gas valve being closed, connection with the air
pump is opened and air is then exhausted from the vessel by means of the pump G,
or other suitable air exhausting apparatus, the temperature of the liquid being
noted by the thermometer o in the glass gauge and the cooling, or heating, fluid
being circulated through the coil pipe p in order to regulate the temperature of
the liquid contained in the vessel.
The colder the liquid to be treated, the more readily is the vacuum formed
and the greater is the action of the gas in the conversion of the impurities such as
the ethers, acids and aldehydes into other ethers and acids, and the greater is the.
destruction of the essential oils.
After the air has been exhausted to the desired degree, the air pumpis stopped,
its connection closed, and the ozone gas connection is opened, admitting ozone gas
to the vessel, the said ozone having been generated preferably in the manner
bereinbefore described, and when the liquid has become sufficiently charged with.
the gas, the valves of all connections are then closed and the vessel is.disconnected
from the charging apparatus, the platform shifted or truck removed and another
vessel filled with liquid is moved into position for treatment:
In the term "rectifying" I include also that action which causes the deodoriza-
tion and decolorization of methylated alcohols.
Although the described apparatus for generating ozone gas constitutes the
preferred means of producing ozone gas for use in the process according to this
invention it is to be understood that ozone gas obtained in any other suitable
manner; may, if desired; be used in carrying out the process herein claimed."
Having now particularly described and ascertained the nature of this inveu-
tion and in what. manner the same is to be performed, I declare that what I
claim is
1. The treatment, or purifying, rectifying, ageing, deodorizing, and decolourizing
of alcoholic and other liquids, or liquified matter, by subjecting them in vacuo, to
the action of ozone gas, substantially as herein before explained.
2. The treatment, or purifying, rectifying, ageing, deodorizing and decolourizing
alcoholic and other liquids, or liquified matter by first removing the air therefrom
and afterwards intimately mixing ozone gas therewith, substantially as hereinbefore
described.
3. In apparatus for treating alcoholic and other liquids; or liquified matter, the
combination with an air-tight vessel for holding the liquid or liquified matter of a
fluid conveyor within the said vessel, means for connecting the said conveyor with
a supply of heating or cooling medium, an air exhausting device connected with
the said vessel, connections between the said vessel and a supply of ozone gas, and
means for connecting the vessel with the air exhausting device and the ozone
supply respectively, substantially as herein before described.
4. In apparatus for treating alcoholic and other liquids, or liquified matter, the
combination with a vessel for holding the liquid. or liquified matter and provided
with an inlet and mounted upon a movable platform or truck of an ozone supply
pipe, leading from a supply of ozone, and au air exhaust pipe leading from an air
exhausting device, the said pipes being supported in position to be connected with
the inlet of the vessel, and means for connecting by means of the said pipes the

page_text: said vessel with the air exhauster and the ozone supply substantially as, and for-
the purposes bereinbefore described.
5. The arrangement and combination of parts constituting the apparatus as a
whole, substantially as herein before.described and illustrated in the accompanying-
drawings.
Dated this 29th day of December 1896.
JOHNSONS & WILLCOX,
47 Lincoln's Inn Fields, London, W.C., Agents.