Ix- PROVEMENTS IN THE MANUFACTURE OF HYDROCYANATE OF AMMONIA, AND OF ALKALINE AND EARTHY CYANIDES
Year: 1863

page_text: LETTERS PATENT to William Clark, of.53, Chancery Lane, in the County
of Middlesex, Engineer and Patent Agent, for the Invention of " Ix-
PROVEMENTS IN THE MANUFACTURE OF HYDROCYANATE OF AMMONIA, AND OF
ALKALINE AND EARTHY CYANIDES." A communication from abroad by
Louis Joseph Frédéric Margueritte, of 29, Boulevart St. Martin, Paris,
Chemist.
Sealed the 1,6th October, 1863, and dated the 30th, April 1863..
PROVISIONAL SPECIFICATION left by the said William Clark at the
Office of the Commissioners of Patents, with his Petition, on tlie
30th April 1863.
I, WILLIAM CLARK, of 53, Chancery Lane, in the County of Middlesex,
Engineer and Patent Agent, do hereby declare the nature of the said Inven-
tion for: "IMPROVEMENTS IN THE MANUFACTURE OF HYDROCYANATE OF AMMONIA,
AND OF ALKALINE AND EARTHY CYANIDES," to be as follows:-
The production of cyanides by the passage of ammoniacal gas. over a mixture
of charcoal and alkaline carbonate, heated to redness, has hitherto presented
great difficulties in a commercial point of view, and bas produced but in-
complete.results. The preparation of cyanogen, or rather of cyanhydrate
(hydrocyanate) of ammonia, which in a laboratory appears simple and easy,
becomes almost impracticable when acting on large quantities in apparatus of
considerable dimensions, both in consequence of the imperfect contact of the
ammonia with the heated charcoal, and from the unequal and at some points
excessively high temperature, which decomposes the ammoniacal gas at a pure

page_text: loss. After carefully studying this reaction, I have found that the nature of
the charcoal employed has a great influence on the quantity of cyanhydrate
obtained, thus the production becomes much easier and more considerable
according to whether coke, graphite, charcoal, either slightly or highly
calcined, or, lastly, soot or lampblack be employed. The two latter species
of charcoal, from their extreme subdivision and the low temperature at which
they are produced, present physical and chemical conditions which singularly
facilitates the combination of the carbon with the azote of the ammonia, or,
in other words, the production of cyanogen; lampblack especially is a substance
which furnishes the best results. But it will be understood that its practical
application presents inconveniences inherent from its light weight, its bulk,
and high price.
This Invention relates to a method of producing the carbon in, & nascent
state, and furnishing it to the ammonia during the operation itself..
The following is the method of operation :-A retort of small diameter is
first filled with fragments of brick, porcelain, gravel, and other separating
substances, or preferably charcoal previously. pounded, and calcined; at the
mouth of this retort is a point not acted on by the heat, and on the ammoniacal
gas reaching said point, a jet of napthaline is introduced, which becomes
vaporized, mixes with the volatile alkali, and with it simultaneously traverses
the fragments heated to redness, that is, at a temperature at which the
napthaline decomposes and deposits its carbon. Under these conditions it will
be understood that the intimate mixing of the napthaline vapours with the
ammoniacal gas constitutes, so to speak, an atomic mixture of the carbon and
azote, which in reacting forms cyanogen. In this manner the production will a
be considerable, and an abundant quantity of cyanhydrate of ammonia may be
collected in the retort. The cyanhydrate of amnionia is received in a lye of
potash or caustic soda, which frees the ammonia and produces an alkaline
cyanide; this solution of alkaline cyanide is boiled with iron filings, in order
to form ferrocyanide, and then evaporated until crystallization takes place.
Instead of napthaline I may employ other carburetted hydrogens, such as
light or heavy oils of tar, schist, or petroleum, éssence of turpentine, oil of
naptha, or others. I however give the preference to napthaline, it being a
substance which may be easily purified of all oxygenated-matters; the presence
of which would be injurious to the formation of cyanogen, às. if it is indis-
pensable to dry the ammoniacal gas in a complete manner; it is no- less
important to remove in the reaction any thing, such as water for instance,
which might burn the carbon of the cyanogen, an eminently combustible
matter.

page_text: The apparatus used may be of various kinds, for example, I introduce the
ammoniacal gas into a vessel containing napthaline kept constantly in
ebullition, and so produce a perfect mixture of the two vapours before entering
the retort, where the reaction is effected..
The chief features of the present Invention are, 1st, the reaction at a red
heat of ammoniacal gas on soot or lampblack, or preferably carburetted
hydrogens, or other matters producing at a high temperature carbon in a
nascent state.
2ndly, the production of cyanhydrate of ammonia, and its transformation
into cyanide with a base of lime, potash, soda, or of metallic oxide.
Srdly, the simultaneous passage of the ammonia, carburetted hydrogen,
or napthaline over a mixture of charcoal and alkaline carbonate heated to
redness.
Lastly, the method of producing the carbon necessary for the formation of
the cyanogen in a nascent state in intimate mixture with the ammoniac by the
decomposition of a hydrocarburet or other matter capable of producing
carburetted vapours.
SPECIFICATION in pursuance of the conditions of the Letters Patent, filed
by the said William Clark in the Great Seal Patent Office on the
26th October 1863.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, WILLIAM
CLARK, of 53, Chancery Lane, in the County of Middlesex, Engineer and
Patent Agent, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Thirtieth day of April, in the year of our Lord
One thousand eight hundred and sixty-three, in the twenty-sixth year
of Her reign, did, for Herself, Her heirs and successors, give and grant.
unto me, the said William Clark, Her special licence, that I, the said
William Clark, my executors, administrators, and assigns, or such others
as I, the said William Clark, 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 Man, an Invention for
“IMPROVEMENTS. IN THE MANUFACTURE OF HYDROCYANATE OF AMMONIA, AND OF
ALKALINE AND EARTHY CYANIDES," a communication to me from-abroad by Louis

page_text: Joseph Frédéric Margueritte, of 29, Boulevart St. Martin, Paris, Chemist,
upon the condition (amongst others) that I, the said William Clark, my
executors or administrators, by an instrument 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 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 William Clark, do hereby declare
the nature of the said Invention, and in what manner the same is to be per-
formed, to be particularly described and ascertained in and by the following
statement (that is to say):-
The production of cyanides by the passage of ammoniacal gas over à
mixture of charcoal and alkaline carbonate heated to redness has hitherto
presented great difficulties in a commercial point of view, and has produced
but incomplete results. The preparation of hydrocyanate of ammonia, which
in a laboratory appears simple and easy, becomes almost impracticable when
acting on large quantities in apparatus of considerable dimensions, both in
consequence of the imperfect contact of the ammonia with the heated charcoal
and from the unequal and at some points excessively high temperature, which
decomposes the ammoniacal gas in pure waste. . After carefully studying this
reaction, I have found that the nature of the carbon employed has a great
influence on the quantity of hydrocyanate obtained; thus the production
becomes much easier and more considerable according to whether coke,
graphite, charcoal, either slightly or bighly calcined, or, lastly, soot or lamp-
black be employed. The two latter species of carbon, from their extreme
subdivision and. the low temperature at which they are produced, present
physical and chemical conditions which singularly facilitates the combination
of the carbon with the azote of the ammonia, or, in other words, the pro-
duction of cyanogen. Lampblack especially is a substance which furnishes
the best results. But it will be understood that its practical application
presents difficulties which are inherent from its light weight, its bulk, and
high price.
This Invention relates to a method of producing the carbon in a nascent
state and in combination with the ammonia during the operation itself.
The following is the method of operation:-A retort of small diameter is
first filled with fragments of porcelain, gravel, or other separating substances,
or preferably charcoal previously pounded and calcined; at the mouth of this
retort is a point not acted on by the heat; and on the admission of the

page_text: ammoniacal gas-a jet of napthaline is introduced, which becoming vaporized,
mixes with the volatile alkali, and with it simultaneously traverses the
fragments heated to redness, that is, at a temperature at which the napthaline
decomposes, and deposits its carbon. Under these conditions it will be under-
stood that the intimate mixing of the napthaline vapours with the ammoniacal
gas constitutes, so to speak, an atomic mixture of the carbon and azote, which
in reacting forms cyanogen; in this manner the production will be considerable,
and an abundant quantity of hydrocyanate of ammonia may be collected in the
retort. The hydrocyanate of ammonia is received in a lye of potash or caustic
soda, which frees the ammonia and produces an alkaline cyanide; this solution
of alkaline cyanide is boiled with iron filings, in order to form ferrocyanide,
and then evaporated until crystallization takes place.
Instead of napthalinė I may employ other carburetted hydrogens, such as
light or heavy oils of tar, schist, or petroleum, essence of turpentine, oil of
naptha, or others. I, however, give the preference to napthaline, it being a
substance which may be easily purified of all oxygenated matters, the presence
of which would be injurious. to the formation of cyanogen, as if-it is indis-
pensable to dry the ammoniacal gas in a complete manner, it is no less
important to remove in the reaction any oxygenated compounds, such as water,
for instance, that might burn the carbon of the cyanogen, which is an eminently
combustible matter.
less
The apparatus used may be of various kinds, for example, I may introduce
the ammoniacal gas into a vessel containing napthaline, kept constantly in
ebullition, and so produce a perfect mixture of the two vapours before entering
the retort where the reaction is effected.
Having described the nature of this Invention, and the manner of per-
forming the same, I declare that what I claim as the Invention to be
protected by the herein-before in part recited Letters Patent, is,-
First, the reaction at a red heat of ammoniacal gas on soot or lamp-.
black, or preferably carburetted hydrogens, or other matters producing at a
high temperature carbon in a nascent state.
Secondly, I claim the production of hydrocyanate of ammonia, and its
transformation into cyanide, with a base of lime, potash, soda, or of metallic
oxide.
Thirdly, I claim the simultaneous passage of the ammonia, carburetted
hydrogen, or napthaline, over a mixture of charcoal and alkaline carbonato
-heated-to-redness, as described...
Lastly, I claim the method of producing the carbon necessary for the
formation of the cyanogen in-a-nascent state-and-in-intimate mixture with the

page_text: ammonia by the decomposition of a hydrocarburet or other matter capable of
producing carburetted vapours...
In witness whereof, I, the, said William Clark, have hereunto set my
hand and seal, this Twenty-sixth day of October, in the year of our Lord
One thousand eight hundred and sixty-three.
Witness,
⚫
W. G. E. SwINNOCK,
58; Chancery Lane,
London.
W. CLARK. (L.B.)