IMPROVEMENTS IN OBTAINING SULPHURETTED HYDROGEN FROM SULPHIDE OF AMMONIUM
Year: 1885

page_text: Sulphide of Ammonium.
We EDWARD WILLIAM PARNELL of N° 28 Canning Street Liverpool in the
County of Lancaster Chemical Manufacturer and JAMES SIMPSON of N° 8A
Rumford Place, Liverpool in the county of Lancaster do hereby declare the nature
of the said invention for IMPROVEMENTS IN OBTAINING SULPHURETTED HYDROGEN
FROM SULPHIDE OF AMMONIUM to be as follows:-
When Leblanc alkali waste or other material containing sulphide of calcium is
treated with a solution of carbonate or sulphate of ammonia or chloride of
ammonium decomposition takes place, the acid or chlorine combining with the
calcium while the sulphur combines with the ammonia forming sulphide of
ammonium as described in British Patent 38185 and 193785. The object of our
invention is to treat sulphide of ammonium so as to liberate the sulphur it contains
in combination with hydrogen in a form available for the manufacture of sulphur
or its compounds and to leave the ammonia in the form of carbonate available for
employment in the ammonia alkali process or for the treatment of a further
quantity of sulphide of calcium or for other use in the arts.
In carrying our invention into practice we add super carbonated ammonia which
we will call sesquicarbonate of ammonia to the sulphide of ammonium and heat
the mixture to a moderate temperature say to boiling point in a closed vessel
which may be fitted with a steam coil or in lief of beat we subject the mixture to
the action of a partial vacuum. As a result of the employment of heat or action of a
vacuum a reaction takes place monocarbonate of ammonia being formed in solution
with evolution of sulphuretted hydrogen which latter after being washed in a
solution of ammonium sulphide or sulphydrate or in the sulphide or sulphydrate
of some other suitable base such as potash, soda, or calcium in order to arrest any
trace of carbonic acid and also washed in any suitable acid such as hydrochloric or
sulphuric to arrest any traces of ammonia is conducted to a gasometer or other
suitable receptacle for employment as required.
The monocarbonate of ammonia may be again converted into sesquicarbonate by
passing a current of carbonic acid through it (preferably in a tower such as that
employed in the manufacture of alkali by the aminonia process) and may be used
repeatedly or it may be passed into the absorbing plant of the ammonia alkali

page_text: process with chloride of sodium and carbonic acid in the well known manner for
the manufacture of alkali or it may be partly employed for any or each of these
purposes. In supercarbonating the mono-carbonate the escaping gases should be
washed in acid to arrest any traces of ammonia.
When the monocarbonate of ammonia which results from the treatment of
sulphide of ammonium with sesquicarbonate of ammonia is used for the treatment
of sulphide of calcium, the sesquicarbonate of ammonia employed for decomposing
the sulphide of ammonium may be very dilute and entirely in solution but when
the monocarbonate is required for the decomposition of chloride of sodium by the
ammonia-alkali process it is necessary that the sesquicarbonate should be in a
concentrated form under which condition it may become crystalline The crystals
however dissolve readily on coming in contact with the sulphide of ammonium.
We prefer in practice to arrest the supercarbonation prior to the formation of
crystals.

page_text: COMPLETE SPECIFICATION.
Improvements in Obtaining Sulphuretted Hydrogen from
Sulphide of Ammonium.
We EDWARD WILLIAM PARNELL of 28 Canning Street Liverpool in the County
of Lancaster Chemical Manufacturer and JAMES SIMPSON of No 8a Rumford
Place Liverpool in the County of Lancaster do hereby declare the nature of the
said invention for IMPROVEMENTS IN OBTAINING SULPHURETTED HYDROGEN FROM
SULPHIDE OF AMMONIUM and in what manner the same is to be performed, to
be particularly described and ascertained in and by the following statement :-
When Le Blanc Alkali Waste or other material containing sulphide of calcium
is treated with a solution of carbonate or sulphate of Ammonia or chloride of
Ammonium decomposition takes place the acid or chlorine combining with the
calcium while the sulphur combines with the Ammonia forming sulphide of
Ammonium as described in British Patents Nos 38185 and 193785. The object of
our invention is to treat sulphide of Ammonium so as to liberate the sulphur it
contains in combination with hydrogen in a form available for the manufacture of
sulphur or its compounds and to leave the ammonia in the form of carbonate
available for employment in the Ammonia Alkali process or for the treatment of a
further quantity of sulphide of calcium or for other use in the Arts.
In carrying our invention into practice we add supercarbonated Ammonia which
we will call sesquicarbonate of Ammonia to a solution of the sulphide of
Ammonium and heat the mixture to a moderate temperature say to boiling point
in a closed vessel which may be fitted with a steam coil or in lieu of heat we
subject the mixture to the action of a partial vacuum-As a result of the
employment of heat or action of a vacuum a reaction takes place mono-carbonate
of Ammonia being formed in solution with evolution of sulphuretted hydrogen
which latter is thoroughly cooled in a suitable condensing apparatus to arrest any
sulphide of Ammonium that may be carried over and after being washed in a
solution of ammonium sulphide or sulphydrate in order to arrest any traces of
carbonic acid and also washed in any suitable acid such as hydrochloric or sulphuric
to arrest any traces of ammonia is conducted to a gasometer or other suitable
receptacle for employment as required.
The mono-carbonate of Ammonia may be again converted into sesquicarbonate
by passing a current of carbonic acid through it (preferably in a tower such as
that employed in the manufacture of alkali by the ammonia process) and may be
used repeatedly or it may be passed into the absorbing plant of the Ammonia
Alkali process with Chloride of sodium and Carbonic Acid in the well known
manner for the manufacture of Alkali or it may be partly employed for any or
each of these purposes-In supercarbonating the mono-carbonate the escaping gases
should be washed in acid to arrest any traces of Ammonia.
When the mono carbonate of Ammonia which results from the treatment of
Sulphide of Ammonium with sesquicarbonate of Ammonia is used for the treatment
of sulphide of calcium the sesquicarbonate of Ammonia employed for decomposing
the sulphide of Ammonium may be very dilute say 5 per cent and entirely

page_text: in solution; but when the mono carbonate is required for the decomposition of
chloride of sodium by the Ammonia Alkali process it is necessary that the super
carbonate should be in a concentrated form, under which condition it may become
crystalline Bi carbonate being formed. The crystals however dissolve on coming in
contact with the sulphide of Ammonium. We prefer in practice to arrest the
super carbonation prior to the formation of crystals.
We find that 2 equivalents of sesquicarbonate of Ammonia to 1. equivalent of
sulphide of Ammonium are about the relative proportions in which the decom-
position of the sulphide and liberation of sulphuretted hydrogen can be efficiently
conducted but we prefer to have a slight excess of sesquicarbonate over these
proportions.
We wish it to be understood that in referring to solutions as consisting of
sulphide, mono carbonate, sesqui carbonate, or Bi-carbonate of Ammonia, we do not
mean that they consist exclusively of these salts or compounds but that the salt or
compound indicated predominates largely in such solution.
Having now particularly described and ascertained the nature of our said
invention and in what manner the same is to be performed We declare that what
we claim is
First. The above described method of obtaining sulphuretted hydrogen from
sulphide of ammonium consisting in treating a solution of sulphide of ammonium
with supercarbonated ammonia and heating the mixture or subjecting it to the
action of a partial vacuum in a closed vessel in the manner described.
Second. Supercarbonating the mono carbonate of Ammonia produced in the
preceding operation for repeated use in treating sulphide of Ammonium.
J. T. KING,
Per W. B. Johnson,
Agent.