Improvements in the Manufacture of Ethyl Mercaptane.
Year: 1889

page_text: Date of Application, 16th Apr., 1889
Complete Specification Left, 17th Feb., 1890-Accepted, 22nd Mar., 1890
PROVISIONAL SPECIFICATION.
Improvements in the Manufacture of Ethyl Mercaptane.
I, OSCAR JULIAN STEINHART, Doctor of Philosophy of 15 Bolton Gardens West,
South Kensington in the County of Middlesex, do hereby declare the nature
of my said invention for "IMPROVEMENTS IN THE MANUFACTURE OF ETHYL
MERCAPTANE" to be as follows :-
The object of this invention is to prepare chemically pure Ethyl-Mercaptane
(Ethyl-Hydrosulphide) from commercial methylated spirits, so as to render this
mercaptane available for the production of other fine chemicals, more especially of
Sulphonal (Diethyl-sulphion-diethyl-methane).
Heretofore Mercaptane was only prepared from strong pure alcohol; according to
the present invention however, I proceed as follows:
I take one part by weight of ordinary commercial methylated spirits and mix
therewith two parts of concentrated sulphuric acid and gently heat the mixture
(preferably on a waterbath) for one hour. The mixture is then slowly poured into
about three times its bulk of cold water and carefully neutralized with carbonate of
potassium sodium or the like.
The neutralized solution is next evaporated and thus the greater part of the alkaline
sulphate as well as resinous matter due to the impurities in the wood spirit are
eliminated.
The remaining solution is mixed with a strong solution of hydrosulphide of
potassium.
The mixture thus obtained, if heated produces both Ethyl and Methyl Mercaptane.
It is distilled, preferably over a waterbath. The bulk of the Methyl compound,
owing to its low boiling point, escapes, whilst the Ethyl Mercaptane is condensed
and collected.
The resulting Ethyl, Mercaptane is still contaminated with a Methyl Mercaptane
and other impurities and from these it is freed by careful fractional distillation.
Doted this
day of Aneil 1880
BERNHARD DUKES,
226, High Holborn, London, W.C., Agent for the Applicant.
COMPLETE SPECIFICATION.
Improvements in the Manufacture of Ethyl Mercaptane.
I, OSCAR JULIAN STEINHART Doctor of Philosophy, of 15 Bolton Gardens West,
South Kensington in the County of Middlesex 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 this invention is to prepare chemically pure Ethyl-Mercaptan
us to render this
(Ethyl-hydrosulphide) from commercial methylated spirits so
mercaptan available for the production of other fine chemicals especially of sulfonal
(Diethyl sulfon diethyl methance).
Heretofore ethyl mercaptan was only prepared from strong pure alcohol, according
to the present invention however I proceed as follows:
I take one part by weight of ordinary methylated spirits and mix therewith two
parts of concentrated sulphuric acid and gently heat the mixture (preferably over a
water bath) for one hour. The mixture is then slowly poured into about three times
its bulk of cold water and carefully neutralised with carbonate of potassium sodium
or the like.

page_text: The neutralized solution (impure sulfo-vinate of potash) is next evaporated and thus
the greater part of the alkaline sulphate as well as resinous matter due to the
impurities in the wood spirit are eliminated.
The solution now remaining is mixed with a strong aqueous solution of hydra sulfide
"of potassium.
Instead of beginning by making the impure sulfo-vinate of potash for the preparation
of the ethyl mercaptan, I may begin by making an impure ethyl chloride.. In this
case I saturate the methylated with hydrochloric acid.
The resulting gaseous ethyl chloride contaminated with methyl chloride on further
treatment with alcoholic solution of sulf-hydrate of potash also be made to yield
impure mercaptan.
The product obtained by either of the means above described, if heated produces
both ethyl and methyl mercaptan.
It is distilled, preferably over a waterbath. The bulk of the Methyl-compound
owing to its low boiling point, escapes whilst the ethyl-mercaptan is condensed and
collected.
The resulting ethyl-mercaptan is still contaminated with some methyl-mercaptan
and other impurities and from these it is freed by careful fractional distillation.
Having now. particularly described and ascertained the nature of the said inven-
tion and in what manner the same is to be performed I declare that what: I
claim is
The manufacture of pure ethyl mercaptan from commercial methylated spirits by
transforming the methylated spirit into either sulfo-vinate of potash or into 'ethyl-
chloride treating the same with hydrosulfide of potassium (in aqueous or alcoholic
solution) heating the resultant liquid and finally distilling the same, all as set
forth.
Dthis 10th
Lanno.. 1000
BERNHARD DUKES,
226, High Holborn, London, W.C., Agent for the Applicant.