Apparatus Employed therein.
Year: 1885

page_text: Apparatus Employed therein.
I ALFRED GEORGE BROOKES of the firm of Wa Brookes & Son of 55 & 56
Chancery Lane in the County of Middlesex Patent Agent do hereby declare the
nature of my invention for IMPROVEMENTS IN THE DISTILLATION OF GLYCERINE
AND IN MEANS OR APPARATUS EMPLOYED THEREIN communicated to me from
abroad by Rudolph Giebermann of 56 M-nomonee Street Chicago, County of Cook
and State of Illinois one of the United States of America Manufacturing Chemist
to be as follows:-
This invention relates to au apparatus for Distilling Glycerine and it consists in
certain peculiarities of the construction and arrangement of the same whereby the
product is rendered of better quality, and the glycerine water saved.
In carrying out my invention I employ a steam superheating furnace provided
with a grate and having a steam supply pipe coiled over the tire pot.
Over this furnace is placed an air tight still for holding the crude glycerine, and
into which is projected the perforated end of the steam pipe which is also provided
with a hydrometer. The upper part of the still is connected by a pipe with the
condenser consisting of a number of vertical pipes connected in pairs at their upper
ends by return binds, and having their lower ends opening into the vacuum pans.
Each of these pans is provided with a glass gauge and suitable pipes for drawing
off the distilled product.
The opposite end of the condenser is by a suitable pipe connected to a cooling
and condensing cylinder within which is arranged a second cylinder and the former
is provided with an outlet pipe connecting it with a suitable receptacle or reservoir
while the inner cylinder is provided with a water supply pipe having a nozzle and
an exbaust pipe. The outer cylinder is also connected to a pipe leading to a
vacuum pump located at any convenient point, and being of any of the usual and
well known forms.

page_text: Distillation in vacuo, has been in use for many years and has been tried with
glycerine, but many experiments have proved that it is impossible to produce a
bighly concentrated article of uniform quality in the apparatus which has been
used.
Another disadvantage was that the glycerine water received in the condenser
was a total loss, as it was not of sufficient quantity to keep the vacuum pump
sealed and therefore a very large amount of water had to be added to it, which
rendered it impossible to again use it.
By my invention means are afforded for overcoming these difficulties, and to
produce a perfectly concentrated glycerine of a uniform quality, and also to save
the water of condensation, which contains a considerable quantity of glycerine,
which may be extracted by redistillation.
The operation is carried out as follows:
The crude glycerine is placed in the still and the fire started, as soon as this is
fairly going, steam is turned on the superheater and the vacuum pump, and water
admitted to the surface condenser and also the pipe leading to the vacuum pump
through the nozzle projected therein.
The water soon condenses in the receivers or pans but disappears again as they
become leated.
In about half an hour the glycerine will commence to distil over, which can be
tested from time to time at the gauges.
The first few pounds condensing in the pan are not perfectly pure, and are drawn
off into a small receiver.
From this time however, the glycerine received in the pan will be found to be
perfectly pure and concentrated, and amount to about 80 per cent of the charge of
the still.
The product received in the second pan does not possess such a high degree of
purity as that in the first mentioned, but is odorless, and is a very good article for
nitroglycerine purposes, but it may be drawn off and re-distilled thus giving an
exceedingly brilliant quality.
The steam with its remnant of glycerine which passes into the condenser is by
contact with the constantly cooled inner cylinder thereof fully condensed and this
glycerine water is drawn off into another receptacle and from this it may be again
tran-ferred to the still and redistilled.
The receivers must be of sufficient size to hold the whole charge of the still, and
this enables me to operate without interruption, and produces an article of uniform
density.
This is an important feature, as the density of the distilled article always
changes with the pressure and temperature of the steam in the apparatus.
Great economy in fuel is also obtained by placing the still directly over the
superheating furnace, as in that case the fire for one purpose serves equally well
for the other at the same time.

page_text: Apparatus Employed therein.
I ALFRED GEORGE BROOKES of the firm of Wm Brookes & Son of 55 & 56
Chancery Lane in the County of Middlesex Patent Agent do hereby declare the
nature of my invention for IMPROVEMENTS IN THE DISTILLATION OF GLYCERINE
AND IN MEANS OR APPARATUS EMPLOYED THEREIN, 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 an apparatus for Distilling Glycerine and it consists in
certain peculiarities of the construction and arrangement of the same, whereby the
product is rendered of better quality, and the glycerine water saved, substantially
as will be hereinafter more fully described and claimed.
In order to enable others skilled in the art to which my invention appertains
to make and use the same, I will now proceed to describe its construction and
operation, referring to the accompanying drawing, which represents a vertical
section of my apparatus, in position for use.
A represents a steam superheating furnace, provided with the grate a, and
having the steam supply pipe B, coiled over the fire pot as shown at b. Over this
furnace is placed an air tight still C, for holding the crude glycerine, and into
which is projected the perforated end 61 of the steam pipe B, which is also provided
with a hydrometer, B', as shown.
The upper part of the still C, is connected by a pipe C, with the condenser D,
consisting of a number of vertical pipes d, connected in pairs at their upper ends
by return binds d', and having their lower ends opening into the vacuum pans E, E',
Each of these pans is provided with a glass gauge e e and suitable pipes el for
drawing off the distilled product.
The opposite end of the condenser is, by a pipe d' connected to a cooling and
condensing cylinder G, within which is arranged a second cylinder G¹ and the
former is provided with an outlet pipe g, connecting it with a suitable receptacle
or reservoir G2, while the inner cylinder is provided with a water supply pipe g',
having a nozzle g², and an exhaust pipe g³ as represented. The outer cylinder is
also connected to a pipe H, leading to a vacuum pump located at any convenient
point, and being of any of the usual and well known forms, it was not considered
necessary to illustrate it in this connection.
Distillation in vacuo, has been in use for many years and has been tried with
glycerine, but many experiments have proved that it is impossible to produce a
highly concentrated article of uniform quality in the apparatus which has been
used. Another disadvantage was that the glycerine water received in the con-
denser was a total loss, as it was not of sufficient quantity to keep the vacuum
pump sealed and therefore a very large amount of water had to be added to it,
which rendered it impossible to again use it.
By my invention means are afforded for overcoming these difficulties, and to
produce a perfectly concentrated glycerine of a uniform quality, and also to save
the water of condensation, which contains a considerable quantity of glycerine,
which may be extracted by redistillation.
The operation is carried out as follows
The crude glycerine is placed in the still C, and the fire started, as soon as this
is fairly going, steam is turned on the superheater and the vacuum pump, and

page_text: water admitted to the surface condenser G, G¹, and also the pipe H, through the
nozzle h projected therein. The water soon condenses in the receivers or pans E, E,
but disappears again as they become heated. In about half an hour the glycerine
will commence to distill over, which can be tested from time to time at the
gauges e, e. The first few pounds condensing in the pan E, are not perfectly pure,
and are drawn off into a small receiver i. From this time however, the glycerine
received in the pan E, will be found to be perfectly pure and concentrated, and
amount to about 80 per cent of the charge of the still. The product received in
the second pan E¹, does not possess such a high degree of purity as that in E, but
is odourless, and is a very good article for nitroglycerine purposes, but it may be
drawn off and redistilled thus giving an exceedingly brilliant quality. The steam
with its remnant of glycerine wich passes into the condenser G, is by contact with
the constantly cooled inner cylinder G¹, fully condensed and this glycerine water is
drawn off into the receptacle G³, and from this it may be again transferred to the
still and redistilled.
The receivers E, E', must be of sufficient size to hold the whole charge of the
still, and this enables me to operate without interruption, and produces an article
of uniform density. This is an important feature, as the density of the distilled
article always changes with the pressure and temperature of the steam in the
apparatus.
Great economy in fuel is also obtained by placing the still directly over the
super heating furnace, as in that case the fire for one purpose serves equally well
for the other at the same time.
Having now particularly described and ascertained the nature of my said
Invention, and in what manner the same is to be performed, I declare that what
I claim is
1. In an apparatus for distilling glycerine, a still or receptacle for containing the
charge, in combination with a furnace placed directly beneath the still, and a steam
pipe coiled over the fire box and connected to the still, substantially as shewn and
described.
2. In an apparatus for distilling glycerine, a condenser composed of several coils
of pipe, connected to the still and also to a vacuum pump, in combination with two
receivers or vacuum pans beneath the condenser coils, and connected therewith,
substantially as shewn and described.
3. In an apparatus for distilling glycerine, a steam condenser consisting of two
cylinders, one within the other, the outer of which is connected to the still, and
also to a vacuum pump, and the inner provided with an inlet pipe, and an outlet
pipe, whereby a constant stream of cold water can be passed through the inner
cylinder substantially as shewn and described.
4. In an apparatus for distilling glycerine, the furnace A, having the super-
heating steam coil b and still C, directly over it, the glycerine condenser D, and
the receivers E, E¹, connected thereto and provided with guages e and draw off
pipes e in combination with the surface condenser G, G¹, supply pipe gl and
outlet g and the pipe H, having the jet h, and leading to a vacuum pump, all
constructed and arranged to operate substantially as and for the purpose set forth.
Dated this 20th day of January 1886