IMPROVEMENTS IN THE TREATMENT OF SODA WASTE AND SULPHURETS
Year: 1861

page_text: LETTERS PATENT to John Louis Jullion, Chemist, Tynemouth, Northumber-
land, for the Invention of "IMPROVEMENTS IN THE TREATMENT OF SODA
WASTE AND SULPHURETS."
Sealed the 23rd July 1861, and dated the 9th February 1861.
PROVISIONAL SPECIFICATION left by the said John Louis Jullion at
the Office of the Commissioners of Patents, with his Petition, on the
9th February 1861.
I, JOHN LOUIS JULLION, Chemist, Tynemouth, Northumberland, do hereby
declare the nature of the said Invention for "IMPROVEMENTS IN THE TREAT-
MENT OF SODA WASTE AND SULPHURETS," to be as follows:-
My Invention relates to the treatment of soda waste or sulphuret of
calcium, and other sulphurets of a like character, in order to produce useful
products therefrom, and I propose to boil or otherwise heat the sulphurets
with powdered magnesia limestone, or a silicate of magnesia, in order that the
sulphur may combine with the magnesium to form a soluble compound, and
thus render it available for its ordinary uses.
5
SPECIFICATION in pursuance of the conditions of the Letters Patent, filed
by the said John Louis Jullion in the Great Seal Patent Office on the
9th August 1861.

page_text: WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Ninth day of February, in the year of our Lord
One thousand eight hundred and sixty-one, in the twenty-fourth year of Her
reign, did, for Herself, Her heirs and successors, give and grant unto
me, the said John Louis Jullion, Her special license that I, the said John
Louis Jullion, my executors, administrators, and assigns, or such others
as I, the said John Louis Jullion, my executors, administrators, and assigns,
should at any time agree with, and no others, from time to time and at
all times thereafter during the term therein expressed, should and lawfully
might make, use, exercise, and vend, within the United Kingdom of Great
Britain and Ireland, the Channel Islands, and Isle of Man, an Invention
for "IMPROVEMENTS IN THE TREATMENT OF SODA WASTE AND SULPHURETS," upon
the condition (amongst others) that I, the said John Louis Jullion, by an
instrument in writing under my hand and seal, should particularly describe
and ascertain the nature of the said Invention, and in what manner the
same was to be performed, and cause the same to be filed in the Great Seal
Patent Office within six calendar months next and immediately after the
date of the said Letters Patent.
NOW KNOW YE, that I, the said John Louis Jullion, do hereby declare
the nature of my said Invention, and in what manner the same is to be
performed, to be particularly described and ascertained in and by the fol-
lowing statement (that is to say) :-
In carrying out my Invention of "Improvements in the Treatment of Soda
Waste and Sulphurets," I make use of two different methods of working,
whereby I am enabled to avail myself of either the sulphur alone that is con-
tained in the waste or both the sulphur and a base, at the same time pro-
ducing several secondary products that are marketable commodities. The
products I purpose to obtain by these means are, first, sulphuret of magnesium
or hyposulphite of magnesia, from which magnesium compounds may be
prepared; second, a salt of lime from which lime compound may be prepared;
third, a salt which, on combustion, yields sulphurous acid; fourth, precipitated
sulphur applicable to all purposes for which precipitated or sublimed sulphur
is used. Each of these products is a direct result of one or other of my two
processes for the treatment of soda waste and sulphurets.
In the first process, I take soda waste or gas lime (preferring the former),
and I reduce the substance to a fine state of division by a crushing or
grinding mill, or other suitable machinery, and having ascertained the per-
centage of sulphur therein contained, I place a given quantity of it in a vessel
with a considerable quantity of water, and then add an equivalent of carbonate

page_text: of magnesia in the state of powdered magnesia limestone, and I boil the whole
together for half an hour.
By this process an interchange of elements or double decomposition takes
place, producing carbonate of lime and sulphuret of magnesium. In order to
separate these two compounds, the latter has to be made soluble in the water.
with which it is mixed; this is best effected by the addition of a second atom'
of sulphur, either in a free state or as a polysulphuret of an earthy base, after
which the lime may be separated by filtration. The liquid containing the
sulphuret of magnesium must be saturated with sulphurous acid in order to
form hyposulphite of magnesia from which to precipitate carbonate or bydrate,
or I at once boil it down and evaporate it to dryness, and burn it in ordinary
sulphur kilns, so that the excess of sulphur may form sulphurous acid, and the
residue be available to make Epsom salts or other magnesium compounds.
According to the second process, I oxidize the waste into a state known to
soda makers as "yellow liquor." This is effected by spreading the waste on.
an inclined surface, and exposing it fully to the action of air and moisture by
repeated turning over to expose the whole mass. Both oxygen and moisture
will be rapidly absorbed, and the greater part of the sulphur will run off as a
yellow fluid, which is a solution of a complex "sulphuretted hyposulphite of
lime. This is proved by the addition of a strong acid such as hydrochloric.
acid, giving off sulphurous acid and sulphuretted hydrogen gases at the same
time that sulphur is precipitated in an oily or soft state.
In order to bring this compound into use where a base is to be obtained, or
free sulphur is required, I saturate it in the first place with sulphurous acid;
this causes the precipitation of sulphur in an extremely minute state of
division well adapted to pharmaceutical purposes, or as a substitute for the
sublimed sulphur of commerce. This sulphur I separate by filtration, and
wash it with clean water, and dry it in a stove for use. The filtered liquid,.
which is a solution of hyposulphite of lime, is to be decomposed by boiling
with powdered magnesian limestone; this produces carbonate of limo and
hyposulphite of magnesia. The latter by the ordinary process yields both
carbonate and calcined magnesia, and by oxydation Epsom salts or sulphate of
Diagnesia.
:
When a lime salt is wanted I carefully filter the solution of byposulphite of
lime, and precipitate the lime as carbonate (such as sold under the name of
precipitated chalk) by a clear solution of carbonate of soda. Or, having
placed the solution of hyposulphite of lime in a close vessel, I decompose it
with an equivalent of bydrochloric acid, and collect the sulphur and sulphurous
acid given off, and I precipitate the lime with sulphuric acid in the form of

page_text: sulphate, such as sold to paper makers under the name of pearl hardening.
But when I desire to recover the sulphur only from the waste, I prefer con-
verting it into "yellow liquor;" this I boil down in a common evaporating
furnace, and when it is in a very concentrated state I stir in about three times
as much small or dust pyrites as the salt from the yellow liquor would weigh
if dried alone, and when the whole has attained a pasty consistence, it is to be
well stirred together, then raked out of the furnace and dried in a stove, after
which the cake is ready for burning in kilns, as practised with ordinary
pyrites.
The presence of dust or small pyrites is not necessary to the success of
producing a salt from soda waste that will burn and give off sulphurous acid,
because "yellow liquor" alone yields on evaporation a substance that burns
most freely; but I prefer to bind up such small or dust pyrites as a means of
utilizing them without in any degree hurting the sulphur-yielding quality of
the sulphuretted compound obtained from the waste.
Having now described my Invention of improvements in the treatment
of soda waste and sulphurets, and having explained the manner of carrying
the same into effect, I claim,-
Firstly, the processes herein set forth for the treatment of soda waste and
sulphurets.
- Secondly, the treatment of "yellow liquor" as herein described.
Thirdly, the treatment of small or dust pyrites with compounds obtained
from waste.
In witness whereof, I, the said John Louis Jullion, have hereunto set
my hand and seal, the Fifth day of August, in the year of our Lord
One thousand eight hundred and sixty-one.
Witness,
HENRY WATSON,
Nowcastle-on-Tyne.
JOHN LOUIS JULLION. (L.S.)