IMPROVEMENTS IN THE MANUFACTURE OF BICHLORIDE OF CARBON AND CHLORIDE OF SULPHUR
Year: 1865

page_text: LETTERS PATENT to Richard Ransford, of Huron Lodge, West Brompton,
in the. County of Middlesex, for the Invention of "IMPROVEMENTS IN THE
MANUFACTURE OF BICHLORIDE OF CARBON AND CHLORIDE OF SULPHUR."
Sealed the 12th June 1866, and dated the 15th December 1865.
PROVISIONAL SPECIFICATION left by the said Richard Ransford at
the Office of the Commissioners of Patents, with his Petition, on the
15th December 1865.
I, RICHARD RANSFORD, of Huron Lodge, West Brompton, in the County
of Middlesex, do hereby declare the nature of the said Invention for "Im-
PROVEMENTS IN THE MANUFACTURE OF BICHLORIDE OF CARBON AND CHLORIDE OF
SULPHUR," to be as follows:-
This Invention has for its object improvements in the manufacture of
bichloride of carbon and chloride of sulphur. For this purpose I take
bisulphide of carbon and mix therewith a metallic chloride or chlorine
compound; afterwards I treat the mixture with chlorine until the bisulphide
of carbon is decomposed. Bichloride of carbon and chloride of sulphur are
amongst the products obtained, the action being probably that the metallic

page_text: chloride or chlorine compound continually hands chlorine over to the carbon
and sulphur of the bisulphide of carbon. I prefer to employ the anhydrous
terchloride of antimony, but sesquichloride of iron and terchloride of arsenic
and other compounds also succeed well. I find that a mixture of 20 parts by
weight of bisulphide of carbon to one part of the terchloride of antimony
works well. The bichloride of carbon and chloride of sulphur can be
separated from the other products and from each other by well-known means.
By this process I am enabled to make bichloride of carbon much more readily
and cheaply than heretofore, so that it becomes available as an anæsthetic and
also as a solvent, and in many cases its use has great advantages; chloride
of sulphur also is a substance of well-known commercial value.
SPECIFICATION in pursuance of the conditions of the Letters Patent, filed
by the said Richard Ransford in the Great Seal Patent Office on the
14th June 1866.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, RICHARD
RANSFORD, of Huron Lodge, West Brompton, in the County of Middlesex,
send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Fifteenth day of December, in the year of our
Lord One thousand eight hundred and sixty-five, 'in 'the twenty-ninth year of
Her reign, did, for Herself, Her heirs and successors, give and grant unto me,
the said Richard Ransford, Her special licence that I, the said Richard
Ransford my executors, administrators, and assigns, or such others as I, the
said Richard Ränsford, 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 imight make,
use, exercise, and vend, within the United Kingdom of Great Britain and
Ireland, the Channel Islands, and Isle of Man, an Invention for "IMPROVE-
MENTS IN THE MANUFACTURE OF BICHLORIDE OF CARBON AND CHLORIDE OF
SULPHUR," upon the condition (amongst others) that I, the said Richard
Ransford, my executors or administrators, by an instrument in writing
under my, or their, or one of their hands and seals, 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.

page_text: NOW KNOW YE, that I, the said Richard Ransford, do hereby declare
the nature of the said Invention, and in what manner the same is to be
performed to be particularly described and ascertained in and by the
following statement thereof, that is to say!
This Invention has for its object improvements in the manufacture of
bichloride of carbon and chloride, of sulphur. For this purpose I take
bisulphide of carbon and mix therewith a metallic chloride or chlorine com-
pound; afterwards I treat the mixture with chlorine until the bisulphide of
carbon is decomposed. Bichloride of carbon and chloride of sulphur are
amongst the products obtained; the action being probably that the metallic
chloride or chlorine compound continually hands chlorine over to the carbon-
and sulphur of the bisulphide of carbon. I prefer to employ the anhydrous
terchloride of antimony, but sesquichloride of iron and terchloride of arsenic
and other compounds also succeed well. The bichloride of carbon and
chloride of sulphur can be separated from the other products and from
each other by well-known means. By this process I am enabled to make
bichloride of carbon much more readily and cheaply than heretofore, so that
it becomes available as an anesthetic and also as a solvent, and in many
cases its use has great advantages; chloride of sulphur also is a substance
of well-known commercial value,
And in order that my spid Invention may be most fully understood and
readily carried into effect, I will proceed to describe the method in which I
prefer to conduct the process I take bisulphide of carbon and place it in
vessel of earthenware capable of holding at least four times the quantity.
5 I add to it one-twentieth part of its weight of solid terchloride of antimony,
and warm it to about 100° Fahrenheit, I then pass into the mixture dry
chlorine, which it will absorb rapidly; the conducting pipe should dip down
into the liquid, and as it is liable to become choked it is advisable to use two
such pipes, and to make them of large diameter; then when one pipe.
becomes choked the other can be employed. After a time the obstruction
in the first pipe will be dissolved away by the mixture, so that it will be
again ready for use. During the process the temperature should not be allowed
to rise to the boiling point of the mixture, or, as is preferable, an efficient
condensing apparatus may be connected with the vessel in which the vapours
5 produced are condensed and allowed to run back into the converting vessel,
The current of chlorine is continued until the precipitate which at first is formed
and immediately re-dissolved becomes permanent; the admission of chlorine
may then be stopped and the mixture transferred to an earthenware retort.
for distillation. In connection with the retort are two condensers; the first is

page_text: kept at the temperature of boiling water or thereabouts, and the second is
cooled as far as it conveniently can be; in it the bichloride of carbon con-
denses, whilst in the first condenser the chloride of sulphur remains. The:
antimony compound left in the retort can be employed to work a fresh charge
of bisulphide of carbon, a small quantity of new terchloride of antimony being 5
added if necessary to compensate for loss. In order to purify the bichloride
of carbon, which will still contain some sulphur compounds, I put it into a
vessel fitted with a close cover and add to it enough milk of lime to make it
distinctly alkaline; this addition should be made slowly and from time to
time, so as to avoid the developement of excessive heat, and the whole should
be stirred up frequently. If arrangements are made to avoid loss of
bichloride of carbon by evaporation the milk of lime may be added. more
rapidly. After this alkaline treatment the whole is transferred to a still, which
conveniently may be heated over a sand bath until no more bichloride of
carbon comes over. This I again treat with lime or alkali and re-distil. The
bichloride of carbon will now usually be pure, but if not the alkaline treat--
ment and distillation should be repeated. The chloride of sulphur collected
in. the first receiver in the original distillation will usually be sufficiently pure-
for commercial purposes, but if not it can be distilled till pure. Although I
prefer, as above stated, to stop the admission of chlorine as soon as a precipitate
is produced, still if preferred the passage of the chlorine may be continued
until the production of the precipitate is complete, and then the antimony will
be brought into an insoluble form, and it may be separated by subsidence and.
decantation before the commencement of the distillation. The precipitate,
which is a chlorine compound of antimony, can be employed to work a fresh
charge of bisulphide of carbon. When working with sesquichloride of iron,
which in some respects is advantageous, I proceed as follows:-I-take a
vessel of cast iron, by préference of a cylindrical form, and several feet in
length; it should be mounted on horizontal axes, which are made hollow. This
vessel I fill loosely with coarse wrought-iron turnings, and then put in enough
bisulphide of carbon to fill it to the depth of about one-third of the radius or
less. I then admit chlorine through one of the hollow axes and sesquichloride
of iron is at once formed. The cylinder is slowly rotated, and its other hollow
axis should be connected with an efficient condenser to condense and return
to the cylinder any vapours which arise. From time to time I draw samples
by a cock provided for the purpose and test with the pentachloride of antimony;
as soon as this gives a precipitate the process is complete; the contents of the
vessel are then drawn off and distilled as before, and it will distil without
residue or nearly so; the method of purification will also remain unchanged.

page_text: In conducting this process it is desirable not to continue the passage of the
chlorine after the pentachloride of antimony gives a precipitate, otherwise a
higher and more volatile chloride of sulphur is produced in considerable
quantity, which is difficult to separate from the bichloride of carbon by distilla-
tion, and consequently it has to be destroyed by the alkaline process. Should
it at any time be desired to produce this more volatile chloride of sulphur, it
will be better to take the less volatile chloride of sulphur after the bichloride
of carbon has been distilled off, and to treat it again with iron turnings and
chlorine until it ceases to absorb; then by distillation the more volatile chloride
of sulphur formed is readily separated in a sufficiently pure state; it is, how-
ever, a substance for which at present there is no great demand.
In witness whereof, I, the said Richard Ransford, have hereunto set my
hand and seal, this Eighth day of May, in the year of our Lord One
thousand eight hundred and sixty-six.
RICHARD RANSFORD. (L.B.)