IMPROVEMENTS IN RECOVERING IODINE FROM PHOSPHATES OF LIME DURING THE MANUFACTURE OF SUPERPHOSPHATE OF ANTTY ADDADAMING MURD READ
Year: 1873

page_text: LETTERS PATENT to Louis Thiercelin, of Paris, France, Doctor of
Medicine, for the Invention of " IMPROVEMENTS IN RECOVERING IODINE
FROM PHOSPHATES OF LIME DURING THE MANUFACTURE OF SUPERPHOSPHATE OF
ANTTY ADDADAMING MURD READ"
Lin
Sealed the 20th October 1873, and dated the 25th April 1873.
PROVISIONAL SPECIFICATION left by the said Louis Thiercelin at
.
the Office of the Commissioners of Patents, with his Petition, on
the 25th April 1873.
I, LOUIS THIERCELIN, of Paris, France, Doctor of Medecine, do
hereby declare the nature of the said Invention for "IMPROVEMENTS IN
RECOVERING IODINE FROM PHOSPHATES OF LIME DURING THE MANUFACTURE OF
SUPERPHOSPHATE OF LIME, AND IN APPARATUS THEREFOB," to be as follows:-
The Invention relates to improvements in the manufacture of super-
phosphate lime, with the object of recovering the iodine contained in the
phosphates of lime to be acted upon, principally fossil phosphates, such
as coprolites or apatites. For this purpose, instead of, as was hitherto

page_text: done in the manufacture of superphosphate of lime, causing the sul-
phuric acid to act on the phosphate of lime in an open vessel, I do it in
a suitably closed one communicating with an air pump or other
exhausting apparatus for drawing the evolved vapours and iodine into a
condensing chamber, to the sides of which part of the iodine remains
adhering, whereas the remainder of the iodine passes into suitable
alkaline solutions, and combines with the alkali.
The iodine and its alkaline salts thus obtained may be further purified
by any suitable method, whereas the superphosphate of lime is made use
of for agricultural or other purposes..
In the annexed Drawing A represents a closed vessel of suitable
material for allowing the sulphuric acid to act on the phosphate of lime.
The vessel A is provided with funnels B and C, serving respectively for
introducing the phosphate and the acid into the vessel; D is an opening
provided with a sliding valve for allowing to withdraw the super-:
phosphate from the vessel A; E is a vertical shaft provided with blades e,
and to which shaft a suitable revolving motion may be imparted by any
suitable means, so as to cause the blades e to procure the proper mixing
of the materials contained in the vessel A, which latter communicates
with a condensing chamber G by means of a pipe F provided with a
valve f, and which chamber has a man-hole 9 for withdrawing from the
chamber the iodine which has condensed against the sides of this
latter.
The chamber G is further provided with a cock g¹ and a Welter or
safety tube g², and communicates by means of the tubes H, H', and H
with an air pump or other suitable exhausting apparatus, the tubes H
and H¹ dipping each into a suitable alkaline solution contained in the
Al Iand T1

page_text: WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Twenty-fifth day of April, in the year of our
Lord One thousand eight hundred and seventy-three, in the thirty-
seventh year of Her reign, did, for Herself, Her heirs and successors, give
and grant unto me, the said Louis Thiercelin, Her special licence that
I, the said Louis Thiercelin, my executors, administrators, and assigns,
or such others as I, the said Louis Thiercelin, my executors, adminis-
trators, or 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 RECOVERING
IODINE FROM PHOSPHATES OF LIME DURING THE MANUFACTURE OF SUPERPHOSPHATE
OF LIME, AND IN APPARATUS THEREFOR," upon the condition (amongst others)
that I, the said Louis Thiercelin, 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 Inven-
tion, 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 Louis Thiercelin, 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
following statement :-
The Invention relates to improvements in the manufacture of super-
phosphate of lime, with the object of recovering the iodine contained in
the phosphates of lime to be acted upon, principally fossil phosphates,
such as coprolites or apatites. For this purpose, instead of, as has been
done hitherto in the manufacture of superphosphate of lime, causing the
sulphuric acid to act on the phosphate of lime in open vessels, or in such
manner as to allow the evolved gases and iodine of escaping in the air,
and thus loosing this latter, I perform the operation in suitably closed
vessels, and by means of an air pump or other suitable exhausting
apparatus I cause the evolved vapours and iodine to be drawn into a
condensing chamber, to the inner sides of which parts of the iodine will
remain adhering, whereas the remainder passes into suitable alkaline
solutions, and combines with the alkali thereof.

page_text: The iodine and its salts thus obtained may be further purified by any
suitable means, whereas the superphosphate formed in the first vessel is
withdrawn therefrom and made use of for agricultural or other suitable
purposes.
By the hitherto practised methods of manufacturing superphosphate
of lime in open vessels, the iodine evolved during the action of the sul-
phuric acid on the phosphate of lime is lost in the air, whereas by my
method of carrying on the manufacture in suitably closed vessels, all or
at least the greater part of the iodine contained in the phosphate of
lime acted upon is recovered, and the manufacture may be carried on in
a regular continuous manner. For this purpose I prefer making use of
an apparatus, the general arrangement of which is represented in longi-
tudinal sectional view in the here annexed Drawing, which apparatus
consists of a large cylindrical mixing vessel A, by preference of wood or
other suitable material, and in which are introduced the pulverized
phosphates to be acted upon, and the sulphuric acid of the required
strength and proportion. The vessel A is provided with two stoneware
funnels B and C, respectively, serving for introducing the phosphates
and the sulphuric acid, and at the bottom the vessel A is provided
with an opening D, which may be closed by a corresponding register or
door D' sliding between friction rollers d, and by which opening D the
superphosphate is to be withdrawn from the vessel A. E is a vertical
wooden arbor or shaft provided with suitable wooden arms or blades e,
which arbor at its lower end turns into a wooden pan e¹, whereas its
upper part passes through a corresponding opening in the cover or lid
A¹ of the vessel A, and is provided with proper gearing and pulleys for
receiving suitable revolving motion from any suitable prime mover, and
cause the arms e of suitably mixing the phosphate and sulphuric acid,
and thus transform the phosphate into superphosphate. The funnels B
& C are provided with plugs or other means for keeping the vessel A
as hermetically as possible closed after the introduction therein of the
phosphate and sulphuric acid. A pipo F, and valve or cock f, allows of
putting the vessel A in communication with a chamber G, in which part
of the iodine and of the vapours evolved in the vessel A are condensed,
the iodine remaining adhering against the inner sides of the chamber,
whereas the remainder of the vapours and iodine are drawn by means of
an air pump or other exhausting apparatus into a series of washing
vessels I, I', containing suitable alkaline solutions, the series being in
'

page_text: communication with the condensing chamber G by the dipping pipe g,
and with each other, and with the air pump or exhauster, respectively,
by the dipping pipe H and pipe H'.
".
-
The condensing chamber G I prefer to construct of brickwork lined
at the inside with stoneware, and the same is provided with a well-
closing wooden lid G₁, and a discharge pipe G³, and cock 2. The
vessels I, I', and the pipes and cocks should by preference be made of
stoneware or glass.
The manner of making use of the apparatus is as follows:-The vessels
I, I, having being provided with the required alkaline solutions and the
necessary quantity of finely pulverized phosphate, and diluted sulphuric
acid having been introduced in the chamber A respectively by means of
the funnels B and C, these latter and the sliding door D¹ are closed, after
which the revolving shaft E and the air pump or exhaustor are put in
operation, the latter producing a partial vacuum in the various vessels of
the apparatus which causes the iodine and vapors evolved in the
vessel A by the action of the sulphuric acid on the phosphate of lime
entering into the condensing chamber G, against the inner sides of which
the greater part of the iodine will deposit, whilst the remainder passes
into the washing vessels I, I', and combines with the alkali of the solu-
tions contained therein, from which combination the same may be
afterwards separated by chlorine or other means. The iodine having
thus been collected the motion of the exhaustor and of the mixing
apparatus is stopped, the superphosphate of the vessel A. taken out by
the opening D, after which this latter is closed again and the operation
may be repeated at once.
Having thus described and particularly ascertained the nature of my
Invention, and the manner in which the same is or may be put into
operation, I wish it to be understood that I do not intend to limit or
restrict myself to the precise details of the apparatus here-above described, '
as many variations may be made therefrom without departing from the
principles or main features of the same, neither to any particular size or
material of which the apparatus or its constituent parts may be con-
structed; but what I consider to be novel and original, and therefore
claim as the Invention secured to me by the herein-before in part
recited Letters Patent is,―
1ly. Recovering the iodine from phosphates of lime during the manu-

page_text: facture of superphosphate of lime, by causing the said manufacture to
take place in suitably closed vessels, and by the aid of a suitable vacuum.
2ly. The general arrangement of the here above described apparatus
for manufacturing superphosphate of lime in closed vessels, and by the
aid of a suitable vacuum, for the purpose of recovering the iodine con-
tained in the phosphate of lime to be acted upon.
In witness whereof, I, the said Louis Thiercelin, have hereunto set
my hand and seal, this Twenty-first day of October, in the year
of our Lord One thousand eight hundred and seventy-three.
Witness,
DREXFOUS.
L. THIERCELIN. (L.S.)