IMPROVEMENTS IN THE CONSTRUCTION OF APPARATUS FOR DISTILLING AND CONCENTRATING OF AMMONIA-WATERS AND AMMONIA-CONTAINING LIQUORS
Year: 1879

page_text: LETTERS PATENT to Dr. Hermann Grüneberg, of Cologne, in the German
Empire, for the Invention of "IMPROVEMENTS IN THE CONSTRUCTION OF
APPARATUS FOR DISTILLING AND CONCENTRATING OF AMMONIA-WATERS AND
AMMONIA-CONTAINING LIQUORS."
Sealed the 12th March 1880, and dated the 11th December 1879.
PROVISIONAL SPECIFICATION left by the said Dr. Hermann Grüneberg at
the Office of the Commissioners of Patents on the 11th December 1879.
*IMPROVEMENTS
Dr. HERMANN GRÜNEBERG, of Cologne, in the German Empire.
IN THE CONSTRUCTION OF APPARATUS FOR DISTILLING AND CONCENTRATING OF
AMMONIA-WATERS AND AMMONIA-CONTAINING LIQUORS."
This Invention relates to the construction and arrangement of apparatus for the
distillation of ammoniacal liquids, so as to obtain therefrom ammonia in more or
less concentrated aqueous solution or salts of ammonia. For this purpose a still is
employed constructed and arranged as follows:-A vertical cylindrical distilling
boiler heated by flues surrounding it has within it a vertical central tube, the bottom
of which extending some distance below the bottom of the boiler beyond the
heating zone thereof is closed, and the upper end of which reaching nearly to the
top of the boiler is open to the upper part thereof. Above the distilling boiler is a
vessel supplied with and containing milk of lime, and above this vessel is a hollow
column divided by borizontal partitions into a number of compartments communi-
cating with each other by pipes, and containing distributing partitions for the
purpose hereinafter explained. From the top of the boiler extend pipes which enter
the lime vessel at its top, and extend down within it nearly to its bottom,
terminating in ends perforated with numerous small holes. By these pipes the
vapours generated in the distilling boiler are conveyed into the lime vessel, and
they bubble or rise in subdivided streams through the milk of lime therein, agitating
it; from the lime vessel the vapours pass through the successive compartments of
the column above. These compartments are supplied by a pipe at the top with the
ammoniacal liquid to be distilled, which descends through the successive compart-
ments of the column, while the vapours as above described are ascending through

page_text: them, the distributing partitions causing intimate mixture of the two fluids. Thus
the vapours become gradually cooled as they ascend, while the liquid becomes
gradually warmed as it descends. Such volatile ammonia as the liquid contains is
thus liberated and rises to the upper part of the column, whence it passes away by
a discharge pipe, whilst the condensible portions of the ascending vapours, such as
the vapour of water, become condensed and flow downwards mixed with the
descending liquid. Near the top of the column the condensation is so complete that
scarcely any condensible portions pass off by the discharge pipe. From the bottom
of the column the liquid which still contains the ammonia salts that are not volatile
flows by a pipe into the lime vessel, and in mixing with the lime these salts become
decomposed, producing volatile ammonia. A portion of this is liberated and passes
with the vapours into the column, and thence by the discharge pipe; the rest along
with the rest of the liquid descending from the column, descends by a central
overflow pipe from the upper part of the lime vessel to the bottom of the boiler
tube, which is below the heating zone, and thence it rises through a sieve or screen
into the boiler tube in which the line subsides. The liquid overflows the upper
edge of the boiler tube into the space of the boiler annularly surrounding the tube,
and in this space, while being partly evaporated, it descends flowing continuously
out by a pipe at the bottom of the boiler, fresh liquid to be operated on being
continuously supplied to the column as above described. In its descent to the
bottom of the boiler the liquid parts with the last portions of its volatile ingredients,
which with the other vapours generated in the boiler rise through the lime vessel
and column as above set forth. As the lime vessol is not subjected to the heat of
the boiler fire there is no burning of the lime therein, and in like manner the boiler
tube being protected froin the direct action of the fire the lime in it is not burned,
so that in neither case does the lime injure the metal. By the described
arrangement of apparatus the process is conducted in a continuous manner, the
liquid continuously supplied at the top becoming gradually warmed as it descends,
and having the ammonia liberated from it with little or no mixture of vapour. The
ammonia discharged at the top of the column can be applied in various ways and in
various apparatus for the production of more or less concentrated aqueous solutions
or ammoniacal salts. For the production of concentrated aqueous solution, or for
concentrating a weak solution, the ammonia discharged froin the column with a
mixture of aqueous vapour is led through a worin or other cooler into a vessel
arranged so as to constitute a hydraulic valve, the overflow of this vessel being
concentrated aqueous solution of ammonia. It is of advantage to extend the discharge
pipe from the column vertically upwards and surround it with cold water, so that
a considerable portion of the aqueous vapour that accompanies the ammonia may
become condensed and flow back into the column. For effecting the cooling, the
liquid to be treated may be employed, being for that purpose fed into a closed cooling
vessel at its bottom and discharged at its top, being thus somewhat heated on its
way to the column. For the production of an aminoniacal salt, such as ammonium
sulphate, the discharge from the column is led into a vessel containing sulpuric acid.
The union with the acid developes considerable heat, whereby the water present is
vaporized, and such gases as were mixed with the ammonia are driven off. These
vapours and gases being offensive should be discharged through the fire or into the
chimney of the boiler. On their way thereto they are conducted through a cooler
through which the ammoniacal liquor to operated on passes on its way to the
column, receiving considerable heat, whereby the, fuel for distillation is largely
economised.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent filed
by the said Dr. Hermann Grüneberg in the Great Seal Patent Office on the
7th April 1880.
Dr. HERMANN GRÜNEBERG, of Cologne, in the German Empire. "IMPROVEMENTS
IN THE CONSTRUCTION OF APPARATUS FOR DISTILLING AND CONCENTRATING OF
AMMONIA-WATERS AND AMMONIA CONTAINING LIQUORS."
This Invention relates to the construction and arrangement of apparatus for the
distillation of ammoniacal liquids, so as to obtain therefrom ammonia in a more or
less concentrated aqueous solution or salts of ammonia. For this purpose I arrange
a still as I will describe, referring to the accompanying Drawings. Fig. 1 shews an
external elevation of the still, and Fig. 2 shews principally a vertical section of the
still with certain adjuncts hereafter referred to. A is the still-boiler heated by the
products of combustion from a fire place q carried in flues round the boiler. Within
the boiler is a tube a open at the top to the vapour space in the boiler, and extending
down below the bottom of the boiler, where it has a cover with a blow off cock r
and a perforated screen d. Above the boiler is a vessel C which is charged with
milk of lime, and above this vessel is a column B, such as is often employed in spirit
stills, divided by horizontal partitions into numerous compartments communicating
with each other by pipes. From the upper part of the lime vessel C a pipe c, b,
open at both ends extends down to nearly the bottom of the boiler tube a, its
mouth being under the screen d. Pipes f, f, lead from the top of the boiler A into
the, lime vessel C, and open with numerous perforations near the bottom thereof.
A pipe supplies the upper part of the column B with the liquid to be distilled
which flows down the successive compartments of the column, while the vapours
and gases generated in the boiler A after passing through the lime vessel C rise
through the succesive compartments of the column B. Thus the descending liquid
becomes gradually heated as it descends, and has more less of its gaseous ingredients
liberated, whilst the ascending vapours become condensed and mix with the
descending liquid; and the uncondensed gases that were mingled with the vapours
join those liberated from the liquid, and pass away with them by the pipe k. The
liquid from the column B enters the lime vessel C and mixes with its contents,
which are kept in agitation by the passage through them of the vapours from the
pipes The ammonia salts in the liquid become decomposed by the action of
the lime, ammonia being liberated, part of which in gaseous form ascends the
column B. From the lime vessel C liquid still containing ammonia passes by the
overflow pipe c, b, to the bottom of the boiler tube a, which is removed from the
direct action of the fire, so that there is no danger of the lime which is mixed with
the liquid becoming burnt, or of the material of the tube becoming injured by heat,
and in like manner the lime vessel C and its contents are protected from overheating.
From the bottom of the tube a the liquid rises in the tube and overflows its top
edge into the body of the boiler, where it is heated, and the gases and vapours
evolved from it rise by the pipes ff, to the lime vessel as already described. From
the bottom of the boiler A liquid from which the ammonia has been expelled
overflows by the pipe into a deep vessel I, the contents of which operate as a
hydraulic seal, and the overflow from this vessel is led by a pipe n to a drain or
elsewhere. Thus while the distilling apparatus is continuously supplied with
ammoniacal liquid or solution by the pipe l, there is a continuous overflow by the
pipe n of liquid from which the ammonia has been liberated, and a continuous
discharge of ammonia and vapour by the pipe k. The ammonia thus discharged
may be applied in various ways for the production of more or less concentrated
solutions or salts of ammonia. For producing concentrated aqueous solution
I employ the arrangement shewn in Fig. 1. The mixture of ammonia and aqueous
vapour issuing from the column B passes through a cooling pipe O, and thence to a

page_text: coil in the vessel D, wherein it becomes condensed to the condition of liquid ammonia. "
This flows down to a vessel E, the uncondensed gas or vapour passing into a
vessel H the contents of which form a bydraulic seal, and being there absorbed or
condensed, or issuing thence by a pipe p. The vessel D is closed, and the coil in it
is cooled by the raw ammonia-liquid which is supplied from the reservoir F by the
funnel pipe z. This raw liquid warmned by the coil passes from D by the pipe to the
column B. The cooling pipe O serves as a regulator of the concentration. The more
cold water is supplied to its casing by the pipe r the greater is the condensation of
the aqueous vapour in the pipe O, and the water of condensation flowing back into
the column B, the more concentrated is the residual fluid which passes to the coil
in D. Thus the degree of concentration of the product of liquid ammonia may be
regulated as desired. G is the vessel for supplying the milk of lime, which is
admitted as required to the lime vessel C by the funnel pipe e. For producing
ammonium sulphate I employ the adjuncts to the still shewn in Fig. 2. The
mixture of ammonia and vapour passes by the pipe k, and alternately by k¹ and k¹¹,
to the vessels K¹, K", containing sulphuric acid. Considerable heat is envolved by
the union of the ammonia and the acid so as to vaporise the excess of water
combined with the acid. The vapour thus generated, with a portion of that which
accompanied the ammonia, and various offensive gases passes away by the large
pipe u. I utilise the heat of these products to give preliminary heat to the gas
liquor that is to be distilled by leading them into a vessel E containing a coil or
set of tubes through which the gas liquor supplied by the pipe a passes before
entering the column of the still, to which it is conducted by the pipe l. The
uncondensed gases and vapours are led from the vessel E by a pipe v to the
fireplace q, where the offensive gases are consumed. The vessel L receives ammonium
sulphate from the vessels K¹, K". It has a perforated bottom through which the
lye drops into the receptacle M below it.
Having thus described the nature of my said Invention, and in what manner the
same is to be performed, I claim in respect of apparatus for distilling and
concentrating ammoniacal liquids,-
First. The arrangement of the lime vessel C between the still boiler A. and
the column B and of its connections therewith, so that liquid from the column
becomes mixed with the milk of lime in the vessel, which is kept in agitation by the
products of distillation from the boiler, substantially as herein described.
Second. In the production of liquid ammonia, the use for partial condensation of
the ammoniacal vapours issuing from the still of the cooling tube O within a vessel
supplied with cold water in quantity adjusted to suit the concentration desired in
the product, substantially as herein described.
Third. Utilizing the heat of the gases and vapours evolved in producing
ammonium sulphate for the preliminary heating of the ammoniacal liquor that is to
be distilled, substantially as herein described.
In witness whereof, I, the said Dr. Hermann Grüneberg, have hereunto set my
hand and seal, this Seventh day of April, in the year of our Lord One
thousand eight hundred and eighty.