Improvements in the Production of Iodine and Iodine Compounds.
Year: 1888

page_text: Date of Application, 23rd June, 1883
Complete Specification Left, 20th Mar., 1889
Complete Specification Accepted, 20th Apr., 1889
PROVISIONAL SPECIFICATION.
Improvements in the Production of Iodine and Iodine Compounds.
We HIPPOLYTE SUILLIOT of 21 Rue St. Croix de la Bretonnerie and HIPPOLYTE
RAYNAUD of 5 Rue des Fètes, both of Paris, in the Republic of France,
Manufacturing Chemists, do hereby declare the nature of this Invention to be as
follows:-
:-
Previously to our invention iodine has been commercially produced either alone or
in compound with inorganic bases as for example with the metallic bases potassium
Sodium iron and copper. The object of our invention is to obtain organic compounds
containing iodine with a view principally to improve the processes for obtaining iodine
from kelp varec sea weed mother waters and residues containing iodine and from
other sources. By means of our invention we are enabled to produce iodine in the
state of so termed lodoform without loss of iodine so that we can obtain all or
nearly all of the iodine which a given quantity of an iodide is capable of
furnishing.
The process is founded upon two principal re-actions first the re-action of a
hypochlorite upon iodide of potassium or sodium from which results a hypoiodite
and secondly the re-action of the hypoiodite upon acetone from which results
iodoform
(C* H* O* + 3 KO, 10 = C HI³ + KO, C H³ 03 + 2 KO HO).
By way of example we will suppose that we are operating upon a cold solution containing
iodide of potassium or of sodium. To 1000 parts of such solution containing say
50 parts of potassium iodide we add 2 parts of Sodium hydrate and 6 parts of acetone
the latter being in excess. We agitate the mixture and add by slow degrees a weak
hypochlorite solution. Iodoform is thrown out as a curdy precipitate. The addition
of the hypochlorite solution is continued until the formation of the precipitate ceases.

page_text: At this time the supernatant liquor will contain only a small quantity of uncombined
hypochlorite and the excess of acetone the whole of the iodine having been thrown
down with the precipitate. The presence in the solution of many of the alkaline salts
even in like proportions will not interfere with the success of the operation. When
employing our process in the production of iodine from kelp varec and similar
sources we obtain directly iodoform from the liquors without interfering with the
production of potassium or other useful products and when operating with
mother waters containing iodine we precipitate the whole of the iodine in the
state of insoluble iodoform which can be readily separated washed and dried.
Iodine can be obtained from the iodoform by the employment of known processes.
Dated this 21st day of June 1888.
DUTTON & FULTON,
1, St. James Square, Manchester
Agents.

page_text: COMPLETE SPECIFICATION.
Improvements in the Production of Iodine and Iodine Compounds.
We HIPPOLYTE SUILLIOT of 21 Rue St. Croix de la Bretonnerie and HIPPOLYTE
RAYNAUD of 5 Rue des Fêtes, both of Paris in the Republic of France, Manufacturing
Chemists, 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 :-
Previously to our invention Iodine has been commercially produced either alone or
in combination with inorganic bases as for example with the metallic bases potassium
Sodium iron and copper. The object of our invention is to obtain organic compounds
containing Iodine with a view principally to improve the processes for obtaining
Iodine from kelp varec, sea weed, mother waters, and residues containing lodine and
from other sources. By means of our invention we produce compounds of Iodine
with organic bases or radicals without loss of Iodine so that we are enabled to obtain
all or nearly all of the iodine which a given quantity of an iodide or compound
containing Lodine is capable of furnishing.
The process is founded upon two principal re-actions namely. First the re-action
of a hypochlorite upon the iodide-say for example iodide of potassium or sodium-
from which results a hypoiodite
(CH O +3 KO. IO = C HI³ + KO, C* H³ 03 + 2 KO HO).
By way of example we will suppose that we are operating upon a cold solution
containing iodide of potassium or of sodium. To 1000 parts of such solution con-
taining say 50 parts of potassium iodide we add 2 parts of Sodium hydrate and 6 parts
We
of acetone the latter being in excess as compared with the amount of iodide.
agitate the mixture and add by slow degrees a weak hypochlorite solution and
Iodoform is thrown out as a curdy precipitate. The addition of the hypochlorite
solution is continued until the formation of the precipitate ceases. At this time the
supernatant liquor will contain only a small quantity of uncombined hypochlorite and
the excess of acetone the whole of the lodine having been thrown down in the
precipitate. The presence in the solution of many of the alkaline salts even in large
proportions will not interfere with the success of the operation but in this respect we
must make exception to the Alkaline Sulphides Sulphites and hypo-Sulphites and
other salts which are oxidisable by the Hypochlorites. When employing our process
in the production of Lodine from kelp varec and similar sources we obtain directly
lodoform from the liquors without interfering with the production of potassium or

page_text: other useful products the said Iodoform being more readily and economically
separated or recovered than when separated in the form of Iodine by ordinary
processes. When operating with mother waters containing lodine we precipitate the
whole of the Iodine in the state of insoluble Iodoform which can be readily separated
washed and dried. Iodine can be obtained from the lodoform by the employment of
known processes. In place of a Hypochlorite we may use any other salt or compound
which will produce a Hypoiodite in presence of an Iodide. The important feature in
our Invention is the re-action of a Hypochlorite upon an Alkaline lodide in the
presence of Acetone contained in an aqueous solution rendered alkaline by means of
Sodium or potassium hydrate or stated more broadly such important feature is
the re-action of any Hypochlorite or other compound capable of producing a
Hypoiodite upon an iodide of calcium, or of niagnesium zinc iron or other
inorganic base.
Having now particularly described and ascertained the nature of our said inven-
tion and in what manner the same is to be performed we declare that what we
claim is :-
(1). The production of the so termed Iodoform by the re-action of Hypochlorites
or other compounds capable of producing. Hypoiodites as aforesaid upon Iodides of
the indicated nature substantially as. herein set forth.
(2). The process for the production of Iodine compounds by re-acting with
Hypochlorite upon an alcalinised iodide solution in the presence of Acetone substantially
as set forth.
(3). The recovery of Iodine or Iodoform from solutions of the indicated nature by
adding thereto a small proportion of sodium hydrate and Acetone in equivalent excess
of the contained iodide and by slowly adding with agitation a hypochlorite solution
substantially as set forth.
(4). The treatment of mother waters and waters of lixiviation containing Iodine
with a Hypochlorite in presence of Acetone in order to recover the Iodine in association
with an inorganic base or radical as a precipitate.
Dated this 19th day of March 1889.
DUTTON & FULTON,
1, St. James Square, Manchester,
Agents.