Improvements in and in Connection with Distilling Apparatus.
Year: 1886

page_text: COMPLETE SPECIFICATION.
Improvements in and in Connection with Distilling Apparatus.
We, THOMAS TRAIN MATHIESON, of 9 Croxteth Road, Liverpool, in the County
of Lancaster, Chemical Manufacturer and JOSEF HAWLICZEK, of 40 Bentley Road,
Liverpool, aforesaid Chemist do hereby declare the nature of the Invention for
IMPROVEMENTS IN AND IN CONNECTION WITH DISTILLING APPARATUS and in what
manner the same is to be performed, to be particularly described and ascertained
in and by the following statement :-
Our Invention relates to certain improvements hereinafter particularly set forth
in and in connection with apparatus for distilling volatile liquids and gases, the
apparatus being what is known as a Distilling Column, and the following is a full
clear and exact description of our Invention sufficient to enable any person skilled
in the art to which it belongs, or with which it is most nearly connected to make,
use, and put the same into practical operation, reference being had to the annexed
sheet of Drawings which make a part of this Specification and to the letters and
figures of reference marked thereon, like letters and figures of reference being used
to denote like parts throughout the figures of the Drawings.
The object of our present Invention is to so construct distilling columns as to
increase their efficiency, simplify their construction and afford a means for cleaning
certain parts of the apparatus during work, without losing the volatile gases.
Our said Invention consists of several parts to be hereinafter described, the
several parts appertaining more, or less to each other and all contributing to the
complete system of working which is carried on in the apparatus.
DESCRIPTION OF THE DRAWINGS.
Figure 1 is a vertical section of a distilling column and parts constructed according

page_text: Figure 7 is an enlarged plan of one of the side concave shelves of the upper
vessel shown at Figure 1.
Figure 8 is an enlarged plan of one of the distributors of the lower vessel shown
at Figure 1.
Figure 9 is a section through X X Figure 8.
In the carrying out of our Invention we use the following parts which are
common to distilling columns of this type and our Invention does not consist in
these parts broadly but consists in their particular arrangement and in the particular
construction and arrangement of the details. A designates a vessel in which the
liquid and gases to be distilled are first treated and in which the freer volatile
gases, or vapours are given off. This vessel A is is superposed (and connected by
ducts or pipes hereinafter described) on the vessels B B into which the liquor to be
distilled is led from the vessel A and in which decomposition takes place, freeing
the more fixed gases, or vapours, which pass from the vessels B into the vessel A.
The vessel A as in apparatus of this type is divided into compartments A¹ by
diaphragms C and is provided with distributing shelves D and D₁ the particular
construction and arrangement of which forms one of the features of our Invention,
which we will now describe.-It is highly desirable in distilling columns of this
type to so retard and at the same time distribute and expose the liquor flowing
through the vessel A that the free vapours and gases may be entirely given off
from the liquor as it passes through the vessel A and before it enters into the
decomposers B B. With this object we construct the distributors D D¹ in the form
of concave shelves having serrated edges and being perforated near the edges with
small holes. We place as many of these shelves as convenient in the compart-
ments A¹. In the Drawings we have shown four of these shelves in the central
compartments A¹ and three shelves in the lower compartment and one shelf in the
upper compartment. The vessel A is preferably cylindrical and the shelves D are
formed as in Figures 5 and 6 and extend laterally across the centre of the vessel A.
The shelves D' are formed as shown in Figure 7 and extend laterally across the
sides of the vessel A and intermediately to the shelves D. The top of the vessel A
is provided with a pipe F for the supply of liquor to be distilled. This pipe F-has
branch G, the underside of the horizontal arm of which is perforated as shown
at Figures 2 and 3 and is internal to the vessel A. and extends across the vessel A
just over and in line with the upper shelf D. The lower compartment of the
vessel A is provided with a pipe or duct H surmounted by a distributor of the form
shown at Figures 8 and 9. This pipe H is connected by a branch Hand a valve J
to each of the vessels B. The vessel A is also provided with side pipes K and
valves K¹ which communicate between the vessels A and B. As usual in distilling
columns of this type the vessels B are divided into compartments B' by diaphragms L.
Each compartment B¹ is in communication through trapped central pipes M and by
alternated dip pipes N which pipes M and N are provided in the diaphragms L the
upper portions of the pipes N projecting above the diaphragms L. Each of the
pipes M is provided with a distributor I of the form shown at Figures 8 and 9.
The particular construction and arrangement of which forms another of the
features of our Invention. The distributor I consists of a covered rose the under-
side of which is provided with tapered slots i the function of which is hereafter
described. The distributor 1 in the bottom compartment B¹ of each vessel B is
provided with a steam pipe P. The upper compartment of each vessel B is provided
with an opening Q and the lower compartment of each vessel B is provided with
an opening R. Each of the compartments B¹ is provided with a manhole and door
for removing the deposits and cleaning the compartments.
a
The beforegoing being a description of the apparatus, or distilling column, we
will now describe its operation.
Amongst the numerous distilling purposes to which the apparatus herein
described. is applicable, is that of the distillation of ammonia especially for the
recovery of ammonia from the liquor resulting by the ammonia soda process.

page_text: on the
The ammonia liquor from the well known ammonia soda process contains the
ammonia in a free, or volatile state, and combined as a now volatile salt of
ammonia, thus making it necessary to divide the distillation! into two different
stages, which operation can be carried out in the distilling column herein described.
The first part of the operation (the distilling or freeing of the ammonia liquor
from the volatile ammonia) is performed in the superposed vessel A. For this
purpose the ammonia liquor to be distilled is supplied through the pipe
top of the vessel A the liquor passes through the perforated branch G of the pipe F
and is thus distributed in the form of a spray, or rain onto the whole length of
the shelf D, the liquor being collected on the shelf D falls in finely divided streams
onto the top diaphragm C, it then passes through the slotted opening in the
diaphragm C and falls onto the next shelf D. From this centre shelf D the liquor
is distributed in numerous finely divided streams in two parts which fall into the
side shelves D from thence partially onto the next central shelf D while the.
smaller part of the liquor falls direct onto the diaphragm C while the liquor from
the central shelf D is falling over both sides onto the diaphragm C and so on, the
liquor having thus been distributed and collected numerous times in the vessel A
from the bottom of which it finally passes through the pipes K into the vessels B
where the second stage of operation (the decomposition and distillation of the non
volatile ammonia salt) is carried out.
By the above method of distributing, a very large surface of liquor is exposed to
the upward current of steam, thus giving a more perfect distillation of the volatile
ammonia.
The liquor freed from the volatile ammonia passes from the vessel A through the
pipes K into the vessels, or decomposers B. In these vessels the decomposition of
the non-volatile ammonia salt, or salts is effected by the addition of milk of lime
which is supplied through the pipes Q into the top compartments of the vessels B
overflowing through the pipes N to each compartment B¹ next below, leaving a
trapped portion of the liquor on each diaphragm L. The steam enters through the
pipes P into the lowest compartments B₁ of the vessels B passing through the
tapered slots i of the rose distributor I. The object of tapering the slots i is to
ensure uniform diffusion, and mixing of the steam through the trapped liquor.
The steam passing through the trapped liquor in the lowest compartments B' of
the vessels B ascends through the central pipes M to the compartment next above
and so on through the series, passing through the trapped liquor on its way and
finally entering the vessel A through the pipe H carrying with it the freed ammonia
which finally is led off by the outlet a at the top of the vessel A. The liquor
entering the lowest compartment B¹ of the vessels B being free from ammonia is
continuously discharged through the outlets R.
When either vessel B requires cleaning the same may be carried on without
stoppage of the other by closing valves J and K.
The liquor remaining in the isolated vessel B can, before cleaning be entirely
freed from ammonia by allowing the steam to pass through, the ammonia escaping.
with the steam through the outlet O may be recovered as convenient.
By this means a great loss of ammonia is avoided.
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:
First. Distributing the liquor passing through distilling columns in finely
divided streams over a number of concave shelves D D arranged in duplex, or
multiple series, the shelves of each series being so arranged as to catch the liquor
from the other series substantially as and for the purposes set forth.
..
Second. The use in connection with distilling apparatus of concave shelves D
constructed as described and shown in reference to Figures 5 and 6 of the Drawings
hereto annexed.

page_text: :. Third. The use in connection with distilling apparatus of concave shelves D1
constructed as described and shown in reference to Figure 7 of the Drawings hereto
annexed.
Fourth. The use in connection with distilling apparatus of rose distributors I
constructed as described and shown in reference to Figures 8 and of the Drawings
hereto annexed.
Fifth. Constructing and arranging distilling apparatus as herein described with
reference to the Drawings.
Sixth. In apparatus of the type herein described the vessels A and B thereof
arranged and connected by ducts and valves substantially as and for the purposes
set forth.
Seventh. The combination of the vessel A, ducts such as H¹ valves such as J
vessels B and ducts and valves such as K K operating as described substantially as
and for the purposes set forth.
Dated this 19th day of May 1886.
THOMAS TRAIN MATHIESON.
JOSEF HAWLICZEK.
By Cheesbrough & Royston, Agents.