An Improved Process for the Complete Purification of Perfumes in the Manufacture of which Sulphuret of Carbon has been Used.
Year: 1886

page_text: Date of Application, 1st May, 1886.
Complete Left, 1st Feb., 1887.
Complete Accepted, 1st Mar., 1887
Repune OF STATIC]
An Improved Process for the Complete Purification of Perfumes in
the Manufacture of which Sulphuret of Carbon has been Used.
I, EDMUND EDWARDS, of the firm of Edwards and Co., Patent Agents and
Engineers, of 35 Southampton Buildings, Chancery Lane, in the County of Middlesex
do hereby declare the nature of this invention to be as follows:-
In the ordinary process of obtaining perfumes from flowers or other substances by
means of sulphuret of carbon, it is found difficult to eliminate the whole of the latter,
and the present invention has for its object an improved process for the complete and
absolute decomposition and removal of the last traces of sulphuret, of carbon from the
perfumes.
For this purpose pure and neutral alcohol is used (preferably of 80 to 95 degrees
Gay-Lussac) the perfume obtained in the usual way by sulphuret of carbon being first
concentrated to dryness and the sulphuret of carbon removed by means of a current of
pure hydrogen gas.
The product is then transferred to a hermetically closed vessel, pure alcohol being
added in quantity which may be varied more or less but always so as to maintain the
perfumed product, even when cold, in a pasty or semifluid state. The proper propor-
tion will depend upon the greater or less proportion of waxy matters which the
perfumed product contains, and the consequent consistency of the latter. The vessel
having been hermetically closed, it is submitted to a temperature sufficient to bring its
contents to a state of complete fluidity, taking care not to heat it to such a point as to
render the alcoholic vapour explosive, and it is briskly agitated by any convenient
means until the perfumed product and the liquid alcohol are thoroughly mixed. By
the action of the alcohol upon the sulphuret of carbon the real perfume in the mixture
is unaffected and undergoes no decomposition, whilst the sulphuret of carbon is imme-
diately attacked and completely decomposed, in evidence of which sulphureited

page_text: hydrogen gas escapes when the vessel is opened. In order to get rid of the
sulphuretted hydrogen, a current of pure warm hydrogen gas is then passed through
the liquid product, and in order to eliminate the last traces metallic silver in a state of
impalpable powder is introduced into the mixture of alcohol and perfumed material.
The vessel is then reclosed and again agitated, any remaining sulphuretted hydrogen
combining with the silver and forming a sulphuret which is separated with the other
residues and from which the silver can be recovered.
The perfumed material being then entirely freed first from the sulphuret of carbon
and afterwards from the sulphuretted hydrogen, retains only the alcohol used as a
re-agent as described, but by reason of the chemical reactions to which it has been
submitted the atomic composition of this alcohol has been greatly modified, and it is
necessary to separate it from the perfume, which is done by very slow distillation at a
low temperature until it is completely evaporated.
The remaining perfumed material then gives out a scent the fineness and sweetness
of which recall absolutely the real scent of the flowers or plants from which it has
been extracted, and it only remains to remove the greasy and waxy matters and the
silver pure or sulphuretted, or any other remaining inert substances, which may he
effected in the ordinary well known way by the use of fatty bodies and paraffine as
agents for the extraction of the perfume; it being sufficient in order to effect the
separation of the waxy or fatty matters, and the pure silver or sulphuret of silver,
which accompany the real perfume, to dissolve the entire mass in alcohol which collects
the whole of the real perfume by successive washings, and then to separate the foreign
matters by submitting the solution to refrigeration at a low temperature.
The true perfume remains in the form of a more or less concentrated solution in
alcohol, which may be brought to any desired degree of concentration by slow
evaporation.
From the residues any silver or sulphuret of silver may be recovered in the usual way.
The employment of a current of pure hydrogen gas as described above, is for the
purpose of hastening the elimination of any small particles of free sulphuret of carbon
mechanically detained in the perfumed material, but it need not necessarily be
employed, a larger proportion of alcohol as a reagent and of metallic silver being used
instead to remove the greater quantity of sulphuret of carbon which would in such case
be present in the perfumed material.
Though metallic silver in a fine state of division is preferable for use as above
described, Iron, Copper, or Lead, in impalpable powder may be used in its place.
By the improved process, perfumes are obtained absolutely pure and of exquisite
freshness and delicacy, every trace of sulphuret of carbon being removed, which has
never been the case with perfumes manufactured in the ordinary way.
EDWARDS & Co.,
Agents for the Applicant.

page_text: the Manufacture of which Sulphuret of Carbon has been Used.
(A communication to me from abroad by ETIENNE ANTOINE VITEAU, Chemist, of
Paris, in the Republic of France.)
I, EDMUND EDWARDS, of the firm of Edwards and Co., Patent Agents and
Engineers, of 35, Southampton Buildings, Chancery Lane, 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, (that is to say) :-
-
In the ordinary process of obtaining perfumes from flowers or other substances by
means of sulphuret of carbon, it is found difficult to eliminate the whole of the latter,
and the present invention has for its object an improved process for the complete and
absolute decomposition and removal from perfumes of the last traces of sulphuret of
carbon used in their manufacture.
For this purpose pure and neutral alcohol is used (preferably of 80 to 95 degrees
Gay-Lussac), the perfume obtained in the usual way by sulphuret of carbon being first
concentrated to dryness and the sulphuret of carbon removed by means of a current of
pure hydrogen gas.
The product is then transferred to a hermetically closed vessel, pure alcohol being
added in quantity which may be varied more or less but always so as to maintain the
perfumed product, even when cold, in a pasty or semifluid state. The proper propor-
tion will depend upon the greater or less proportion of waxy matters which the
perfumed product contains, and the consequent consistency of the latter.
The vessel having been hermetically closed, it is submitted to a temperature
sufficient to bring its contents to a state of complete fluidity, taking care not to heat it
to such a point as to render the alcoholic vapour explosive, and it is briskly agitated
by any convenient means until the perfumed product and the liquid alcohol are
thoroughly mixed. By the re-action in the conditions described of the alcohol upon
the sulphuret of carbon the real perfume in the mixture is unaffected and undergoes no
decomposition, whilst the sulphuret of carbon is immediately attacked and completely
decomposed, in evidence of which sulphuretted hydrogen gas escapes when the vessel
is opened.
In order to get rid of the sulphuretted hydrogen, a current of pure warm hydrogen
gas is then passed through the liquid product, and in order to eliminate the last traces
metallic silver in a state of impalpable powder is introduced into the mixture of
alcohol and perfumed material.
The vessel is then reclosed and again agitated briskly, any remaining sulphuretted
hydrogen combining with the silver and forming a sulphuret which is separated with
the other residues and from which the silver can be recovered.

page_text: The perfumed material being then entirely freed (by this series of reactions and
processes) first from the sulphuret of carbon and afterwards from the sulphuretted
hydrogen, retains only the alcohol used as a re-agent as described, but by reason of
the chemical re-actions to which it has been submitted the atomic composition of this
alcohol has been greatly modified, and it is necessary to separate it from the perfume,
which is done by very slow distillation at a low temperature until it is completely
evaporated.
The remaining perfumed material then gives out a scent the fineness and sweetness
of which recall absolutely the real scent of the flowers or plants from which it has
been extracted, and it only remains to remove the greasy and waxy matters, and the
silver pure or sulphuretted, or any other remaining inert substances, which may be
effected in the ordinary well known way by the use of fatty bodies and paraffine as
agents for the extraction of the perfume; it being sufficient in order to effect the
separation of the waxy or fatty matters, and the pure silver or sulphuret of silver,
which accompany the real perfume, to dissolve the entire mass in alcoliol which collects
the whole of the real perfume by successive washings and then to separate the foreign
matters by submitting the solution to refrigeration at a low temperature.
The true perfume remains in the form of a more or less concentrated solution in
alcohol, which may be brought to any desired degree of concentration by slow
evaporation.
From the residues any metallic silver which they may contain may be recovered in
the usual way in a pure state or as a sulphuret.
The employment of a current of pure hydrogen gas as described above, is solely for
the purpose of hastening the elimination of any small particle of free and volatilizable
sulphuret of carbon, mechanically detained in the perfumed material, but it need not
necessarily be employed, a larger proportion of alcohol as a re-agent and of volatile
silver being used instead to remove the greater quantity of sulphuret of carbon which
would in such case be present in the perfumed material.
Though metallic silver in a fine state of division is preferable for use as above
described, Iron, Copper, or Lead, in impalpable powder may be used in its place.
By the improved process, perfumes are obtained absolutely pure and of exquisite
freshness and delicacy, every trace of sulphuret of carbon being removed, which has
never been the case with perfumes manufactured in the ordinary way.
Having now particularly described and ascertained the nature of my said Invention,
and in what manner the same is to be performed, I declare that what I claim is :-
1. In the purification of perfumes obtained by sulphuret of carbon the novel use of
metallic silver substantially in the manner and for the purpose described.
2. The method and processes substantially as described of obtaining perfectly pure
perfumes from which the whole of the sulphuret of carbon is removed.
EDWARDS & Co.,
Agents for the Patentee.