Improvements in the Manufacture of Vanillin.
Year: 1894

page_text: Date of Application, 15th Dec., 1894
Complete Specification Left, 14th Sept., 1895-Accepted, 14th Dec., 1895
Improvements in the Manufacture of Vanillin.
We MARIUS OTTO and ALBERT VERLEY both of 8 Passage Goudron, Paris in
the Republic of France, Chemists do hereby declare the nature of our invention
to be as follows:-
The object of our invention is to obtain vanillin in a cheap and expeditious manner
by synthesis.
To effect this object we oxydize a solution of iso-eugenate of soda (or other
convenient base) and treat the resulting product with an acid and separate the
vanillin so produced.
This oxydation may be effected by electrolysing an alkaline solution of
iso-eugenate of soda either cold or warm preferably at the temperature of an
ordinary water bath. This electrolysis may be conveniently effected by placing the
solution of iso-eugenate of soda in a vessel standing in a water bath and connected
with a vessel containing a solution of soda, by a U shaped tube which passes
through the sides of the respective vessels at a convenient height above the bottoms
of the vessels. Electrodes, preferably of platinum, are placed in the vessels and
connected to the respective poles of a source of electricity, the electrode in the
vessel containing the solution of iso-eugenate of soda being at the bottom and
connected by an insulated wire so that the current may pass through the whole
mass of the fluid and oxydize the iso-eugenate of soda. By this arrangement the
oxydation is effected without any substantial mixing of the two liquids.
When the oxydation is judged to be complete the solution is treated with an acid
which sets free the vanillin. It can be purified with bisulphite of soda and by
repeated crystallization as may be found requisite.
Dated this 15th day of December 1894.
JOHNSONS & WILLCOX,
47 Lincoln's Inn Fields, London, W.C., Agents.
COMPLETE SPECIFICATION.
Improvements in the Manufacture of Vanillin.
We, MARIUS OTTO and ALBERT VERLEY, both of 8 Passage Gourdon, Paris,
in the Republic of France, Chemists, 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:-
The object of our invention is to obtain vanillin in a cheap and expeditious
manner by synthesis.
To effect this object we oxydize a solution of iso-eugenate of soda, (or other
convenient base), and treat the resulting product with an acid, and separate the
vanillin so produced.
This oxydation is effected by electrolysing an alkaline solution of iso-eugenate
of soda, either cold, or warm, preferably at the temperature of an ordinary water
bath. This electrolysis may be conveniently effected by placing the solution of
T

page_text: iso-eugenate of soda in a vessel standing in a water bath, and connected with a vessel
containing a solution of soda, by a U shaped tube which passes through the sides of
the respective vessels at a convenient height above the bottoms of the vessels. The
isoeugenate of soda may be in solution in about Que third of soda at 30° Baumé
so that it liquifies at a temperature of about 50° Centigrade. The soda solution
in the other vessel may be of a density of say 36° Baumé. Electrodes, preferably
of platinum, are placed in the vessels and connected to the respective poles of
a source of electricity the electrode in the vessel containing the solution of
iso-eugenate of soda being at the bottom and connected by an insulated wire so
that the current may pass through the whole mass of the fluid and oxydize the
iso-eugenate of soda. By this arrangement the oxydation is effected without any
substantial mixing of the two liquids.
A suitable current is one of about 6 to 8 volts and say about 10 ampères for an
apparatus of 2-litres capacity.
=;
When the oxydation is judged to be complete the solution is removed and treated
with an acid which sets free the vanillin. For this purpose a solution of oxalic acid
or sulphuric acid may be used. It can be purified with bisulphite of soda and by
repeated crystallization as may be found requisite.
Having now particularly described and ascertained the nature of our inven-
tion and in what manner the same is to be performed, we declare that what we
claim is :-
1. The manufacture of vanillin by oxydizing a solution of iso-eugenate of soda
or other base by electrolysis and then treating by means of an acid.
Dated this 14th day of September 1895.
· JOHNSONS & WILLCOX,
47 Lincoln's Inn Fields, London, W.C., Agents for the Applicants.