IMPROVEMENTS: IN THE PREPARATION OF SUPERPHOSPHATE OF LIME AND IN THE MANUFACTURE OF NITROGENIZED MANURES.
Year: 1874

page_text: LETTERS PATENT to Rudolf Giebermann, of No. 70, Lower Thames,
Street, in the City of London, for the Invention of "IMPROVEMENTS:
IN THE PREPARATION OF SUPERPHOSPHATE OF LIME AND IN THE MANUFACTURE
OF NITROGENIZED MANURES.".
Sealed the 15th January 1875, and dated the 21st July 1874.
PROVISIONAL SPECIFICATION left by the said Rudolf Giebermann.
at the Office of the Commissioners of Patents, with his Petition,
on the 21st July 1874.
I, RUDOLF GIEBERMANN, of No. 70, Lower Thames Street, in the
City of London, do hereby declare the nature of the said Invention for
"IMPROVEMENTS IN THE PREPARATION OF SUPERPHOSPHATE OF LIME AND IN THE
MANUFACTURE OF NITROGENIZED MANURES," to be as follows:-
The object of the Invention is to produce from phosphorites,
coprolites, and in general from substances which contain, besides
phosphate of lime, silicates, fluorides, iron, and alumina compounds a

page_text: dry superphosphate of lime, in which the phosphoric acid which has been
made soluble in water remains in that state by adding sulphuric acid
quickly in form of rain or shower, and keeping the batch agitated or
stirred after this time with such rapidity as to prevent as much as
possible the mass from heating.
The process is carried out in the following manner :-A quantity of
fine ground phosphorite, coprolite, or other matter referred to is spread
on a floor, and is poured over by sulphuric acid, which is first to be
diluted to, say, 36° Beaumé, and in quantity that only 7/10th to 10th of
the content of lime of the phosphate of lime is saturated. After pouring
the acid on the mineral the mass is be kept continually agitated or
stirred, so as to keep it in motion after the acid is rained down on it.
This I effect by means of the following apparatus:-The dilute sulphuric
acid is supplied to a hollow central axis, from the lower part of which
radiate arms, also hollow, and perforated with numerous small holes by
which the dilute acid is freely distributed on the mass; and these arms
are also provided with projections acting as stirrers, so that in the rotary
motion imparted to the central axis the agitation of the mass and the
distribution of the dilute acid are effected. I do not however confine
myself to the use of such apparatus.. By these means the mass is pre-
vented from agglutinating or sticking together, and its heating is
avoided. I get a thin mixture which I spread on any suitable place
only, say about 4 inches high, and stir up from time to time. After,
say, a quarter of an hour it must be turned again, and cooled very
quickly by a draught from any suitable blast engine. At this time the
superphosphate is already pretty dry; and easy to be powdered; but it
may also be put in heaps after it has become quite cold, when it gets
after some days so dry that it can easily be sifted or be powdered by a
disintegrator, or I leave the whole mass in the mixing machine, and
operate on it there by a blast engine.
..
The principal thing is quick cooling after the mixing, and by this
method I get easily, say, 12 to 13 per cent. of soluble phosphoric acid
with a total content of, say; 14 to 15 per cent. of phosphoric acid out of
phosphates of, say, 55 per cent. of phosphate of lime, and, say, 15 pér
cent. of soluble phosphoric acid out of phosphates of, say, 65 per cent.
The soluble phosphoric acid obtained will not be diminished in the
superphosphates thus prepared.
:

page_text: If I desire to prepare nitrogenized superphosphates I add together
with the sulphuric acid a concentrated solution of horn, hair, hoof,
leather, wool, or other animal refuse, and proceed in the same way as
described above. By this I get a manure containing the nitrogen in a
condition readily assimilable by vegetation.
SPECIFICATION in pursuance of the conditions of the Letters Patent,
filed by the said Rudolf Giebermann in the Great Seal Patent
Office on the 21st January 1875.
+
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, RUDOLF
GIEBERMANN, of No. 70, Lower Thamas Street, in the City of London,
send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Twenty-first day of July, in the year of
our Lord One thousand eight hundred and seventy-four, in the thirty-
eighth year of Her reign, did, for Herself, Her heirs and successors,
give and grant unto me, the said Rudolf Giebermann, Her special
license that I, the said Rudolf Giebermann, my executors, admini-
strators, and assigns, or such others as I, the said Rudolf Giebermann,
my executors, administrators, and assigns, should at any time agree with,
and no others, from time to time and at all times thereafter during the
term therein. expressed, should and lawfully might make, use, exercise,
and yend, within the United Kingdom of Great Britain and Ireland, the
Channel Islands, and Isle of Man, an Invention for "IMPROVEMENTS
IN THE PREPARATION OF SUPERPHOSPHATE OF LIME AND IN THE MANUFACTURE OF
NITROGENIZED MANURES," upon the condition (amongst others) that I, the
said Rudolf Giebermann, my executors or administrators, by an instru-
ment in writing under my, or their, or one of their hands and seals,
should particularly describe and ascertain the nature of the said In-
vention, and in what manner the same was to be performed, and
cause the same to be filed in the Great Seal Patent Office within
six calendar months next and immediately after the date of the said
Letters Patent.
.
NOW KNOW YE, that I, the said Rudolf Giebermann, do hereby
declare the nature of the said Invention, and in what manner the same

page_text: t
is to be performed, to be particularly described and ascertained in and
by the following statement thereof, that is to say :-
The object of this Invention is to produce from phosphorites,
coprolites, and in general from substances which contain besides
phosphate of lime silicates, flourides, iron, and alumina compounds a
dry superphosphate of lime, in which the phosphoric acid which has
been made soluble in water remains in that state by adding sulphuric
acid quickly in the form of rain or shower or finely divided streams, and
keeping the batch agitated or stirred after this time with such rapidity
as to prevent as much as possible the mass from heating.
The object may be variously effected, but a process I adopt is as
follows: A quantity of finely ground phosphorite, coprolité, or other
matter referred to is in a divided state poured upon by sulphuric acid;
which is first to be diluted to, say, 36° Baumé, and in quantity that
only to ths of the content of lime of the phosphate of lime is
saturated. After pouring or intermixture of the acid with the mineral,
cach in a divided state, the mass is kept agitated or stirred, so as to
kept it in motion..
ths
Figure 1 shows by longitudinal section, and Figure 2 by transverse
section apparatus which I find to answer well in carrying out my
Invention.
The finely ground phosphorite, coprolite, or other matter referred to
in a finely divided state is placed in a trough or hopper a, from which
it is allowed to escape in a continuous stream capable of being regulated
through the longitudinal opening 6 formed between the lower edges of
the two sides a¹, a², of the hopper a. One of these sides a¹ is fixed, but
the other a² is at its lower part a³ moveable to admit of the width of the
mouth or opening between them at 6 being varied. A convenient method
of regulating the width of this opening is adopted by me is to connect
the lower part a³ of the side a² to one end of chains indicated by the
dotted lines c, the opposite ends of which are connected to pulleys or a
roller d worked by a winch handle, or by other suitable means.
The dilute sulphuric acid is supplied from a suitable reservoir to pipes
or tubes e, e, perforated variously in the direction of their length for the
passage therefrom in numerous streams or jets of the dilute acid to meet
and act upon the stream of powdered matters falling through the opening.

page_text: r
from the hopper a. The saturated matters thence in falling become
acted upon by a series of stirrers f¹, f, arranged diagonally around the
axis f, and which are affixed to that axis so as to revolve with it.
Rapid rotary motion is given to the axis f from a steam engine, or other.
motive power. The box or case g, acting as a receiver for the matters
whilst being operated upon by the stirrers f¹; is provided with an outlet h,
by which the accumulated matters may be removed therefrom as desired.
By these means the mass is prevented from agglutinating or sticking
together, and its heating is avoided. I now obtain a thin mixture
which I spread on any suitable place, say about 4 inches high, and
which I stir up from time to time. After, say, a quarter of an hour it
should be turned again and cooled very quickly by any suitable draught.
When the superphosphate has become tolerably dry, and easy to be
powdered it may then when cold be put in heaps. It then gets after
some days so dry that it can be easily sifted or be powdered by a disin-
tegrator, or I leave the whole mass in the mixing machine, and operate
on it there by a suitable blast.
B
It is very desirable to obtain quick cooling after the mixing, and by
the means stated I readily obtain, say, 12 to 13 per cent. of soluble
phosphoric acid with a total content of, say, 14 to 15 per cent. of
phosphoric acid out of phosphates of, say, 55 per cent. of phosphate of
lime and, say, 15 per cent. of soluble phosphoric acid out of phosphates
of, say, 65 per cent. The soluble phosphoric acid obtained will not bo
diminished in the superphosphates thus prepared.
•
If I desire to prepare nitrogenized superphosphates I, after the
operation described for mixing the sulphuric acid with the other
matters, each in divided streams, then add thereto a concentrated
solution of horn, hair, hoof, leather, wool, or other animal refuse. By
these means I obtain a manure containing the nitrogen in a condition
readily assimilable by vegetation; and when using apparatus such as
described in relation to Figures 1 and 2, I introduce such nitrogenized
matters to the other matters in the chamber g through the passage i.
Having thus described my Invention and means which I adopt in
carrying the same into effect, I would have it understood that I do not
confine myself to the precise details herein referred to, as the same may be
varied without departing from the peculiar character of the Invention;
but what I do claim is, the improvements in the preparation of super-

page_text: phosphate of lime by the combination of the sulphuric acid with the
other matters, each in a divided state, and the manufacture of nitro-
genized manures in manner substantially as described.
In witness whereof, I, the said Rudolf Giebermann, have here-
unto set my hand and seal, this Twentieth day of January, in 5
the year of. our Lord One thousand eight hundred and seventy-
.. five.