The Manufacture of Organic Persulphates.
Year: 1899

page_text: Date of Application, 19th Dec., 1899-Accepted, 17th Feb., 1900
COMPLETE SPECIFICATION.
The Manufacture of Organic Persulphates.
I, BENJAMIN JOSEPH BARNARD MILLS, of 23, Southampton Buildings, in the
County of London, Patent Agent, do hereby declare the nature of this invention
(a communication to me from Auguste Lumière, and Louis Lumière Manufac-
turers of Photographic Materials, both of 21, Rue Saint-Victor, Lyon-Monplaisir,
France), and in what manner the same is to be performed to be particularly
described and ascertained in and by the following statement:-
Hitherto no organic persulphate has been prepared and the direct means con-
sisting of electrolysing solutions of organic sulphates have not given satisfactory
results, as this method causes a very profound oxidation which reaches the organic
molecule itself.
The communicators have succeeded in preparing persulphates of organic bases
by the following processes.
1st. By treating sulphates of organic bases by the persulphate of barium.
2nd. By treating a persulphate and by preference the persulphate of barium or
of calcium with sulphuric acid in such manner as to put the persulphuric acid at
liberty and by adding to this acid the organic base. The temperatures herein-
after mentioned are all of the Centigrade scale.
EXAMPLES.
A. In order to prepare the persulphate of cocaine 7 parts of sulphuric acid are
added to 35 parts of cocaine so as to form the sulphate of cocaine by adding
the smallest possible quantity of water. Also 30 parts of persulphate of barium are
dissolved in the smallest possible quantity of water.
The two solutions being mixed, the liquid becomes a mass; it is heated very
lightly in a water bath to about 50° to redissolve the pasty product which is
formed; it is then filtered to eliminate the sulphate of barium. The fihered
liquid cooled in ice water, allows the persulphate of cocaine to deposit which is
then dried and high dried at a low temperature (30° to 40°).
B. 25 parts of sulphuric acid are added to 100 parts of persulphate of barium
dissolved in 250 parts of water, this addition is made very slowly to avoid rise
of temperature, 50 parts of sparteine are then introduced into the solution of
persulphuric acid thus obtained; this base is dissolved slowly and, when the
solution is complete it is filtered to eliminate the sulphate of barium, the liquid
being maintained at about 40° to 50° during the filtration. By cooling the
filtered liquid, the persulphate of sparteine crystallizes.
The communicators have thus been able to prepare most of the persulphates
of organic bases which do not oxidize too, easily, such are:-
The persulphate of pyridine which crystallizes into thin plates soluble in water;
at 150, 100 parts of water dissolve 285 parts of it, this body like all the following
decomposes easily when it is heated, its solution takes place with ebullition; it
liberates the iodine from the iodide of potassium.
The persulphate of quinoline, small white crystals, soluble to 4.4 per cent. in
water at 15°.

page_text: The persulphate of quinine, soluble to 0.1 per cent. in water at 15°.
The persulphate of cocaine soluble to 5.7 per cent at 15°.
The persulphate of sparteine soluble to 14.5 per cent. at 15°. etc. etc.
All these products can be employed in industry as antiseptics and anti-fer-
menting agents.
Having now particularly described and ascertained the nature of the said
invention and in what manner the same is to be performed, I declare that what
I claim is:-
The processes described for the manufacture of persulphates of organic bases,
which processes rest on the following reactions. 1st. On the double decom-
position of mineral persulphates and particularly of the persulphates of barium
or of calcium by the sulphates of organic bases.
2nd. On the treatment of organic bases by persulphuric acid obtained in solution
by means of a mineral persulphate and more particularly the persulphate of
barium and sulphuric acid.
Dated this 10th day of Decembar 1900
HARRIS & MILLS,
23, Southampton Buildings, London, W.C., Agents.