New or Improved Apparatus for Separating Solid or Fluid Substances Dissolved in Alcohol, Ether, or Chloroform without Evaporation of the Solvent.
Year: 1892

page_text: COMPLETE SPECIFICATION.
New or Improved Apparatus for Separating Solid or Fluid
Substances Dissolved in Alcohol, Ether, or Chloroform without
Evaporation of the Solvent.
I, CARL WEITENKAMPF, Gentleman, of 15 Flieder Strasse, Berlin in the
Empire of Germany, 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 :-
This invention relates to apparatus by means of which in the case of solid or
fluid substances dissolved in achohol ether or chloroform the said substances may
be separated without evaporation of the solvent for the purpose of purifying
same or obtaining the dissolved products.
The mode of working of my apparatus is based upon the application of great
coldness to the solution during treatment in my said apparatus; the solution is
saturated under pressure with carbonic acid and the solution, thus treated is
carried over filter layers which retain the separated substances so that the pure
solvent runs off. The object of the apparatus according to my present invention
is to exclude effects of differing pressure and temperature as otherwise the
success of my present invention would be spoiled or at least be prejudiced.
A vertical sectional view of the apparatus according to my present invention
is shown on the hereunto annexed drawing.
I do not wish however to be confined to the precise details there shown as
modifications may possibly become necessary without deviating or departing from.
the substance of this invention.
I also wish to remark that the Specification of the Patent numbered to
immediately precede the number of this Patent may advantageously be read in
conjunction with this Specification..
In the case of the apparatus illustrated as an example the individual reservoirs
vessels or chambers of same are arranged one over the other because in this
way the gravity of the fluid to be driven through the entire apparatus under
pressure is made useful.
The apparatus consists of a vessel or reservoir a of suitable shape which is
advantageously provided with a conical shaped bottom a¹ and with a sieve a'
above the latter.
This reservoir a is tightly closed by a lid as through which is passed the feeding
cock or plug a and is enveloped within a larger reservoir bwhich is likewise
closed at its top by a lid or cover.. Any suitable cooling mixture (such as ice
with salt etc.) is placed in the space between the reservoirs a, and b in order to
thoroughly cool the solution intended for treatment in reservoir a.
In order to prevent any influence from the warmth of the outside air etc. the
reservoir 6 is surrounded at a proper distance by another and outer case c which
is packed with any suitable non-conductors of heat such, as infusoria earth ashes
sawdust etc.
As shown a worm d'is provided in the reservoir a and similarly a worm e in the
cooling mixture of reservoir 6 the object of which is to cool the solution intended
for treatment to about 20° to 25° C.
These worms d and e are (as shown in the drawing) attached or connected
to a vessel or holder A containing liquid carbonic acid and their other ends
respectively are connected with pipes d¹ and e in such. a way that by means of
these pipes joining each other the carbonic acid which has very considerably
cooled the solution in the reservoir a can be conveyed to a cistern (not shown in the
drawing) or can be drawn off by a pump for the purpose of being repeatedly used
over and over again.

page_text: Through the lid of reservoir 6 and through a tight joint in the top of a there
runs a pipe which is attached to or connected with a carbonic acid vessel or
holder B and the open end of which leads through the sieve a' of reservoir a close
to the funnel-shaped bottom a' of same.
The pipe is provided with a stop cock or valve 1 in order to be able to stop
the passage of the carbonic acid to the reservoir a after the solution in the reservoir
has been saturated and shunt the supply of carbonic acid as hereinafter described.
A pipe g is also fixed to the funnel-shaped floor a¹ of reservoir a which is likewise
provided with a stop cock 2 and is connected with pipe by a branch pipe h. This
branch pipe has a meter (manometer) 3 and a stop cock 4.
The pipe 9 passes through the lid of the first filtering contrivance which consists
of a holder which holds the filtering mass (kept between the sieves i' and ').
The latter advantageously consists of charcoal lying upon a layer of wadding
of wool, wool fibres, asbestos or other suitable material preventing particles of
charcoal from being forced through owing to the prevailing pressure. Also this
first filtering chamber i is surrounded by a holder'; containing a cold mixture and this
holder is again surrounded by an outside holder k enclosing any suitable heat
protecting (i.e. non-conducting) material in approximately the same way as the
reservoir a is surrounded.
The filtering appliance i is connected with another filtering contrivance by a
shut off pipe which latter filtering device is arranged similarly to the previously
mentioned filtering contrivance ijk. The parts of the apparatus which receive the
cooling mixtures can be connected with each other so that it is only necessary to
cool the mixture of the receiving holder. Thus increase of temperature during
filtering is prevented.
From the last filtering body the pure solution cleansed by the filtering material
and released from the separated extractive matters is conveyed through a shut off
delivery pipe m to the closed receiver n to which a pipe o is fixed leading to the
carbonic acid pump in order to convey the carbonic acid taken from the pure
solution into the circuit again to be used afresh.
For this purpose a branch pipe p with a stop cock or stop contrivance is fixed to
pipe m in order to be able to carry off at once by a pump the gaseous carbonic acid
which has become free in the drawing off.
The holder n has a cock n¹ to draw off the entirely pure solvent.
The working of the apparatus is effected as follows:-
After filling the reservoir a and cooling its contents to a temperature of about
20° to 25° C. carbonic acid with a pressure of 3 to 4 atmospheres is allowed to pass
from the holder B to and through the solution by means of the pipe f. By this
means the solution is saturated with carbonic acid and the dissolved substances are
separated whereas the pressure of the carbonic acid which collects above the
solution in the closed reservoir a presses the contents of the reservoir into and
through the filtering vessels. After the reservoir a is emptied the cock 1 can be
closed and the constant pressure of holder B is passed through the pipe / upon the
solution in the filtering chambers. In this way the cooling vessel a is shut out so
that the reservoir a can be again filled and cooled before the solution is drawn off..
By this arrangement it is possible to carry on a continuous working for which
purpose if desired several cooling vessels such as a can be used for the same group
of filtering chambers.
h
The employment of carbonic acid for cooling purposes is not absolutely necessary
as if desired the requisite degree of cold may be obtained in any other suitable
manner.
Having now particularly described and ascertained the nature of my said inven-
tion and in what manner the same is to be performed I declare that what I
claim is :-
1. An apparatus for separating solid or fluid substances dissolved in alcohol
ether or chloroform without evaporation of the solvent consisting of the socionvair s

page_text: provided with cooling case b and protecting case c and capable of being made
particularly cold by worms such as d'e which reservoir is connected with the filtering
chambers and also to the carbonic acid holder by a pipe f substantially as and for
the purposes herein before set forth.
2. The apparatus claimed in Claim 1 in combination and in connection with one
or more filtering vessels connected between themselves each consisting of a closed
holder which holds the filtering material arranged between sieves and is kept at a
or surrounding
constant temperature by a cooling and heat protecting case
substantially as and for the purposes hereinbefore set forth.
3. The apparatus claimed in Claims 1 and 2 in combination and acting in
conjunction with means for returning the carbonic acid from the worms de and
from the delivery pipe m and the holder n to the carbonic acid reservoir for the
purpose of being again used over and over again for cooling or saturating the
solutions intended to be purified substantially as and for the purposes hereinbefore
set forth.
4. The combination with apparatus such as hereinbefore described of the
connection pipe with stop cock therein and a shut off branch pipe / so as to shut
off the cooling holder a after being emptied and to permit the refilling thereof with
fresh solution so as to prepare and cool same without interfering with the filtering
operation substantially as and for the purposes hereinbefore set forth.
Dated this 10th day of December 1892.
TONGUE & BIRKBECK,
34, Southampton Buildings, Chancery Lane, London, W.C.,
Agents for the Applicant.