THE MANUFACTURE OF A NEW OR IMPROVED COLOURING MATTER
Year: 1868

page_text: LETTERS PATENT to Anton Leykauf, of Nuremberg, in the Kingdom
of Bavaria, Chemist, for the Invention of "THE MANUFACTURE OF A
NEW OR IMPROVED COLOURING MATTER."
Sealed the 7th May 1869, and dated the 20th November 1868.
PROVISIONAL SPECIFICATION left by the said Anton Leykauf at the
Office of the Commissioners of Patents, with his Petition, on the
20th November 1868.
I, ANTON LEYKAUF, of Nuremberg, in the Kingdom of Bavaria,
Chemist, do hereby declare the nature of the said Invention for "THE
MANUFACTURE OF A NEW OR IMPROVED COLOURING MATTER," to be as follows:-
I manufacture a new or improved colouring matter by employing
manganese or its compounds, and ammonia or its salts or compounds,
together with phosphoric acid or phosphorus, or compounds of the
same.
The process may be performed as follows:-I take pure manganese
or the cheap residuary compounds of manganese from the preparation of
chlorine, and mix it with phosphoric acid; I heat it till liquefied.

page_text: After cooling the manganese is precipitated by ammonia or carbonate of
ammonia, and is poured with the liquid flowing from the coarser
undecomposed manganese ore into another vessel in which the mixture
is steamed or evaporated. Iron or an oxide or other compound of iron
may be added for certain shades.
If my process be properly performed the mass decomposes with water,
gas is emitted, an acid solution results, and the colour remains separated
in great fineness as a compound of oxide of manganese, (and of oxides of
iron, if a compound of iron has been added,) ammonia water, and
phosphoric acid.
Like results may be obtained from other compounds of manganese,
iron, ammonia, and phosphoric acid, as well as directly from phosphorus,
and ammonia, with or without nitric acid, and likewise from
a solution of burnt bones in hydrochloric acid and digested with sulphate
of ammonia.
manganese,
Various shades may be obtained by decomposing bones by sulphuric
acid, and mixing with manganese and heating the whole mass or
the phosphate of lime which is separated. Ammonia can be added at
once, or the mass can be washed and ammonia added to the salt when
steamed or evaporated. In this process the lime whether contained
therein as gypsum or as phosphate of lime is only an impurity.
In one mode of carrying out the process I decompose calcined bones
by sulphuric acid, and use throughout the operation a lye of phosphate
of lime. I saturate the lime with an excess of ammonia, filter the
solution, and steam or evaporate. The phosphate of ammonia is heated
to a high temperature, and when the water and the excess of ammonia
are driven off I gradually add manganese and raise the temperature.
When saturation takes place no more manganese is added. The wash
waters may be evaporated and the phosphate again utilized with
manganese with or without ammonia.
The analysis of the colour will sometimes present the following
approximate proportions:-

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent,
filed by the said Anton Leykauf in the Great Seal l'atent Office
on the 20th May 1869.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, ANTON
LEYKAUF, of Nuremberg, in the Kingdom of Bavaria, Chemist, send
greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her
Letters Patent, bearing date the Twentieth day of November, in the year
of our Lord One thousand eight hundred and sixty-eight, in the thirty-
second year of Her reign, did, for Herself, Her heirs and successors, give
and grant unto me, the said Anton Leykauf, Her special licence that
I, the said Anton Leykauf, my executors, administrators, and assigns, or
such others as I, the said Anton Leykauf, 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 vend, within the
United Kingdom of Great Britain and Ireland, the Channel Islands, and
Isle of Mau, an Invention for "THE MANUFACTURE OF A NEW OR IMPROVED
COLOURING MATTER," upon the condition (amongst others) that I, the
said Anton Leykauf, 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
Invention, and in what manner the same was to be performed,
and cause the same to, bc 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 Anton Leykauf, do hereby declare
the nature of the said Invention, and in what manner the same is
to be performed, to be particularly described and ascertained in and
by the following statement thereof, that is to say :-
I manufacture a new or improved colouring matter by employing
manganese or its compounds, and ammonia or its salts or compounds,
together with phosphoric acid or its compounds.
The process is best practically performed as follows:-I take pure
manganese or the cheap residuary compounds of manganese from the

page_text: preparation of entorine, and mix it with pыоspпoric acid; 1 neat it tur
liquefied. After cooling the manganese is precipitated by ammonia or
carbonate of ammonia, and is poured with the liquid flowing from the
coarser undecomposed manganese ore into another vessel in which the
mixture is evaporated. Iron or an oxide or other compound of iron
herein-after explained may be added for certain shades.
If my process be properly performed the mass decomposes with
water, gas is emitted, an acid solution results, and the colour remains
separated in great fineness as a compound of oxide of manganese, (and
of oxide of iron if oxide of iron has been added,) ammonia water, and
phosphoric acid.
Like results may be obtained from other compounds of manganese,
iron, ammonia, and phosphoric acid, as well as directly from phosphorous,
manganese, and ammonia, with or without nitric acid, and likewise
from a solution of burnt bones in hydrochloric acid, and digested
with sulphate of ammonia, substantially as herein-after described.
Various shades may be obtained by decomposing bones by sulphuric
acid and mixing with manganese and heating the whole mass, or the
phosphate of lime which is separated; ammonia can be added at once,
or the mass can be washed and ammonia added to the salt when
evaporated. In this process the lime whether contained therein as
gypsum or as phosphate of lime is only an impurity.
In one mode of carrying out the process I decompose calcined bones
by sulphuric acid, and use throughout the operation a lye of phosphate
of lime, I saturate the Eme with an excess of ammonia, filter the
solution, and evaporate. The phosphate of ammonia is heated to a high
temperature, and when the water and excess of ammonia are driven off
I gradually add manganese, and raise the temperature. When saturation
has taken place no more manganese is added. The wash waters may be
evaporated and the phosphate again utilized with manganese, with or
without ammonia.
To explain the mode of carrying the process into practical effect I
describe it more particularly as follows:-I premise that it is well.
known that manganese with phosphoric acid heated almost to redness
gives a bright violet product, which in water turns to a red color. But

page_text: and phosphorous and their compounds for the production of a Deautiful
violet colouring matter, which will be fixed or permanent in water and
acids, is I believe quite new.
My colouring matter is manufactured as. above stated, by employing
manganese or its compounds, and ammonia or its salts or compounds,
together with phosphoric acid or its compounds.
In carrying this Invention into effect the mode in which I prefer to
proceed is as follows:-I take pure manganese or the cheap residuary
compounds of manganese from the preparation of chlorine, and mix it
with phosphoric acid. I heat the mixture in clay or iron vessels till an
uniform liquefaction of the violet product is obtained. After cooling the
manganese is precipitated by ammonia or carbonate of ammonia and is
poured with the liquid flowing from the coarser undecomposed
manganese ore into another vessel in which the mixture is evaporated,
and when the ebullition of the less fusible and violet mass has ceased
then sometimes at this stage more phosphoric acid or manganese may
be added, or the temperature may be raised or the heating prolonged
according to the behaviour and tint of the product and the experience
of the operator. If, for instance, too little phosphoric acid is present a
liquefaction of the mass very favorable to the production of the violet
requires too high a temperature, in which case by the driving out of
ammonia at the parts most exposed to the heat, a compound like a white
glass Mn, P results on reduction. In the presence of too much
phosphoric acid, on the contrary, the mass melts easily, and dissolves in
water if the heat is not sufficient, or gives a more glassy red product,
which turns white on being subjected to a stronger heat. By using iron
or various oxides of iron with ammonia phosphoric acid and manganese
and treating as above described various shades can be produced. Instead
of the oxide of iron other equivalent compounds of iron may be used
to produce shades of the above product from violet to blue.
If my process be properly performed the mass decomposes with
water, gas being emitted and an acid red solution results, and the colour
remains behind separated in great purity as a compound of oxide of
manganese, and of oxide or compound of iron also if a compound of iron
has been added, ammonia water, and phosphoric acid.

page_text: ITUM
Mn, O, PO,+H, NO Mn O HOPO,,
a compound hitherto unknown to chemistry, yet agrecing with the
fundamental scientific laws of that science.
Like results may be obtained from other compounds of manganese
iron, ammonia, and phosphoric acid, as well as directly from phosphorous,
manganese, and ammonia (with or without nitric acid), and likewise from
a solution of burnt bones in hydrochloric acid, digested with sulphate
of ammonia.
Various shades may be obtained by decomposing bones by sulphuric
acid and mixing the product with manganese and heating the whole mass;
or the acid phosphate of lime which is separated. Either ammonia can
immediately be added at once, or the mass can be washed and ammonia
added to the compound when evaporated, but by this process a colour is
always produced strongly mixed with gypsum and phosphate of lime.
But while ammonia is present as a constituent of the dye in this process
the lime whether contained therein as gypsum or as phosphate of lime
is only an impurity.
I' may particularly describe one mode which I find suitable for the
preparation of the colouring matter. I use throughout the decomposition
of the burnt bones by sulphuric acid a lye of acid phosphate of lime,
saturate the lime with an access of ammonia, filter off the solution, and
evaporate the same.
The phosphate of ammonia so prepared is subjected to prolonged heat
(to a high temperature) in a clay vessel up to 150° Celsius, say 302°
Fahrenheit, and when the water and excess of ammonia are driven off
I gradually add pure manganese and raise the temperature to 180°
Celsius, say. 356° Fahr. or if the manganese is very hard to 240°
Celsius, say 464° Fahr. I carefully notice when ebullition takes
°

page_text: place, and then and for the first time intermit the putting in of
the manganese, that is to say, no more manganese is added when the
manganese remains undissolved in the violet mass. This takes place
according as the manganese is more or less soluble, when from to of
the salt solution is carried in. The colouring matter is ready so soon as
the inflation or ebullition of the mass has ceased and it can then also
be immediately washed and further used or worked without being injured
in tint. The wash waters may be evaporated and the phosphate again
utilized with manganese, and it can be made appropriate for this purpose
with or without ammonia.
The proportions I find suitable are the following:-I take 100 parts
calcined bones, and 75 parts sulphuric acid at 66° Baumé. This mixture
I saturate with ammonia and evaporate it, I heat the compound to 120°
Celsius, say 248° Fahrenheit, so that the superfluous water is driven off.
To 2 parts of this compound I add 1 part manganese gradually. This
mixture is liquefied or brought to a molten condition by heat at 250°
or 270° Celsius, say 482° to 518° Fahrenheit, and thus the colouring
matter is obtained.
Having now described the nature of the said Invention and in what
manner the same may be performed, I declare that I claim, the manu-
facture of a new or improved colouring matter by employing manganese
or its compounds, and phosphoric acid or its compounds, together with
ammonia or its salts or compounds, substantially as described, and with
or without iron or its oxides, or equivalent compounds, as described.
In witness whereof, I, the said Anton Leykauf, have hereunto
set my hand and seal, this Fifteenth day of May, in the year
of our Lord One thousand eight hundred and sixty-nine.
Witness,
JOHANNES ZELTNER.
ANTON LEYKAUF. (L.S.)