Manufacture of Sulphocyanides from Nitrites, Bisulphide of Carbon, and Sulphuretted Hydrogen.
Year: 1895

page_text: Date of Application, 8th June, 1895
Complete Specification Left, 25th Feb., 1896-Accepted, 28th Mar., 1896
[Communicated from abroad by the Firm of GOERLICH AND WICHMANN, of No. 32
Ferdinandstrasse, Hamburg, in the German Empire, Merchants.]
Manufacture of Sulphocyanides from Nitrites, Bisulphide of Carbon,
and Sulphuretted Hydrogen.
I, OLIVER IMRAY, of No. 28 Southampton Buildings, Chancery Lane, in the
County of London, Chartered Patent Agent, do hereby declare the nature of this
invention to be as follows:-
Schlagdenhaufen stated in the year 1856 that nitrites, when heated with
bisulphide of carbon in a closed pipe to 160° are decomposed, with the result that
sulphocyanide, carbonic acid and sulphuretted hydrogen are formed. In repeating
these experiments I have found that the reaction under the conditions described
is very complicated, that a notable portion of the bisulphide of carbon is burned to
sulphuric acid and carbonic acid and that much nitrogen is lost, presumably as
elementary nitrogen or as protoxyde of nitrogen, so that this process cannot be
advantageously applied to the manufacture, on a large scale, of sulphocyanide
salts.
I found on the other hand that a very smooth reaction takes place if one
molecule of nitrite such as potassium nitrite, and one molecule of bisulphide of
carbon are heated with two molecules of sulphuretted hydrogen to about 150° C.
in a closed vessel..
The final result of the decomposition disregarding intermediate phases, may be
expressed by the equation, if potassium nitrite is used:-
ANU +
The sulphocyanide and sulphur are obtained in nearly their theoretical quantities.
The sulphur separates in crystalline crusts. In carrying out the process the
ingredients should be heated in the required proportions in a closed vessel
provided with an agitator, up to about 150° C. until the reduction of pressure
shewn by a gauge indicates the completion of the reaction. It is expedient to
apply the nitrite in the form of an aqueous solution. The sulphuretted hydrogen
may be forced into the vessel or it may first be absorbed by the nitrite solution.
It is of advantage to use a slight excess of sulphuretted hydrogen in order to
ensure complete decomposition of the nitrite.
If pure ingredients are used, the resulting sulphocyanide is also nearly pure and
can be obtained from the solution without difficulty, the separation of the sulphur
being likewise very easy.
Dated this 8th dore of Tu1005
ABEL & IMRAY,
Agents for the Applicant.

page_text: Manufacture of Sulphocyanides from Nitrites, Bisulphide of Carbon,
and Sulphuretted Hydrogen.
,I OLIVER IMRAY, of No. 28 Southampton Buildings, Chancery Lane, in the
County of London, Chartered Patent Agent 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 :-
Schlagdenhaufen stated in the year 1856 that nitrites, when heated with
bisulphide of carbon in a closed pipe to 160° are decomposed, with the result that
sulphocyanide, carbonic acid and sulphuretted hydrogen are formed. In repeating
these experiments my foreign correspondents have found that the reaction under the
conditions described is very complicated, that a notable portion of the bisulphide
of carbon is burned to sulphuric acid and carbonic acid and that much nitrogen
is lost, presumably as elementary nitrogen or as protoxyde of nitrogen, so that this
process cannot be advantageously applied to the manufacture, on a large scale, of
sulphocyanide salts.
They found on the other hand that a very smooth reaction takes place if one
molecule of nitrite such as potassium nitrite, and one molecule of bisulphide of
carbon are heated with two molecules of sulphuretted hydrogen to about from
120° to 150° C. in a closed vessel.
The final result of the decomposition disregarding intermediate phases, may be
expressed by the equation, if potassium nitrite is used:-
KNO + CS + 2 HS = KSON + S + 2 HO.
The sulphocyanide and sulphur are obtained in nearly their theoretical quantities.
The sulphur separates in the fused state becoming crystalline crusts when cool.
In carrying out the process the ingredients should be heated in the required
proportions in a closed vessel provided with an agitator, up to about 120° C. until
the reduction of pressure shewn by a gauge indicates the completion of the reaction.
It is expedient to apply the nitrite in the form of an aqueous solution. The
sulphuretted hydrogen may be forced into the vessel or it may first be absorbed
by the nitrite solution.
It is of advantage to use a slight excess of sulphuretted hydrogen in order to
ensure complete decomposition of the nitrite.
If pure ingredients are used, the resulting sulphocyanide is also nearly pure and
can be obtained from the solution without difficulty, the separation of the sulphur
being likewise very easy.
Having now particularly described and ascertained the nature of this invention
and in what manner the same is to be performed, I declare that what I
claim is :-
The herein described manufacture of sulphocyanides by heating together under
agitation in a closed vessel a nitrite such as potassium nitrite, bisulphide of carbon
and sulphuretted hydrogen.
Dated this 95th day of Feb 1806.
ABEL & IMRAY,
Agents for the Applicant.