Improvements relating to the Production of Iodized Sulpho-acids of Phenol, Cresol, and Thymol.
Year: 1887

page_text: Date of Application, 31st Oct., 1887
Complete Specification Left, 30th July, 1888
Complete Specification Accepted, 28th Sept., 1888
Improvements relating to the Production of Iodized Sulpho-acids of
Phenol, Cresol, and Thymol.
I, Doctor EUGEN OSTERMAYER, of 4 Weissfrauengasse, Erfurt, in the Empire of
Germany, Chemist and Manufacturer, do hereby declare the nature of this Invention to
be as follows
:-
This Invention relates to a process of preparing iodized sulpho-acids of phenol, cresol
and thymol.
If the known phenol sulpho-acids, or their salts, are treated with their equivalent
quantity of iodine, in the form of iodic acid and iodine, iodide of potassium and
iodine or chloride of iodine, iodide of potassium in a hydrochloric solution or with
salts of iodine in presence of oxidizing agents, preferably with a solution that is
obtained by dissolving iodide of potassium in water, hydrochloric acid and nitrite of
sodium, or by introducing chlorine into the iodine suspended in the water, a mixture
of several iodized sulpho-acids is precipitated after a short time, which acids can be
separated by a fractional crystallization.
The sulpho-acids of cresol and thymol behave in the same manner, they are however
more difficult to separate from each other.
The process which finds employment with the said compounds is as follows.
For example 16.5 kilogrammes of iodide of potassium are dissolved in 10 kilogrammes
of water and 52 kilogramines of hydrochloric acid are added, whereupon 7 kilogrammes
of nitrite of sodium are gradually introduced. The solution thus obtained is mixed with
a solution of 21 kilogrammes of sodium paraphenolsulpho-salt in 60 kilogrammes of
water. After a short time the precipitation of one iodine paraphenolsulpho-acid which
is slightly soluble in water commences, and this acid is separated by filtering. The
remaining liquid is evaporated at a gentle heat, whereupon the readily soluble iodine
para-phenol-sulpho-acid separates after the cooling. The raw acids are preferably
purified by converting them into their salts of baryta. The more readily soluble
acid crystallizes in hot water in the form of very beautiful, colourless columnar needles
the others that are readily soluble in colourless scales.

page_text: The iodine orthophenol-sulpho-acids are prepared in the same manner as the
para-compounds, also here a compound that is slightly soluble in water is precipitated
first, and one that is readily soluble remains in the original liquids from which it
separates after the evaporation and can be obtained pure by crystallization. The
slightly soluble acid crystallizes in small leaves or needles, the readily soluble acid, in
crystalline crusts.
Iodine-cresol-sulpho-acids, are obtained under similar circumstances one of which
crystallizes in bunch or tuft shaped colourless needles.
The iodine-thymolsulpho-acid, obtained in the same manner, is extremely soluble in
water, and crystallizes in alcohol in the form of small prisms. In an aqueous solution
it decomposes at a certain concentration on evaporation and is coloured blue,
partially reforming thymol, whereas tho potassium salt forms very durable colourless
needles.
Dated this 31st day of October 1887
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, W.C.,
Agents for the Applicant.

page_text: Improvements relating to the Production of Iodized Sulpho-acids of
Phenol, Cresol, and Thymol.
I, Dr. EUGEN OSTERMAYER, of 4 Weissfrauengasse, Erfurt, Germany, Chemist and
Manufacturer 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 :-
This invention relates to a process of preparing iodized sulpho-acids of phenol,
cresol and thymol and their salts.
If the known phenol sulpho-acids or their salts are treated with iodine in presence
of oxidizing agents, for example in the form of iodic acid and iodine, iodide of
potassium and fodine or iodine-chloride in an acid solution; or with iodine or iodine
salts, simultaneously using lixivial substances, i.e. substances suitable for neutralizing
acids, metallic oxides, in the simplest manner by dissolving iodide of potassium in
water, hydrochloric acid and nitrite of sodium, or by introducing chlorine into the
iodine suspended in water and mixing this solution which transmits iodine with the
predetermined quantity of the corresponding phenol, cresol or thymolsulpho-acid salts,
the acid salts of the corresponding sulpho-acids are precipitated in every case from the
acidified solution, the slightly soluble salts being the first. From the inother lyes are
obtained, after the evaporation, the readily soluble iodized sulpho-acids.
The process which is employed with the said compounds is as follows:
For example 165 kilogrammes of iodide of potassium are dissolved in 10 kilo-
grammes of water, and 52 kilogrammes of hydrochloric acid are added, whereupon
7 kilogrammes of nitrite of sodium are gradually introduced. The solution thus
prepared is mixed with a solution of 21 kilogrammes of paraphenolsulpho-acid potash
in 60 kilogrammes of water. After a short time the acid potassium salt of the iodized
paraphenolsulpho-acid commences to precipitate. By converting these raw products
into the slightly soluble salt of baryta and decomposing the latter with the exact
equivalent quantity of sulphuric acid the free iodized acid is obtained which crystallizes
in water in columnar needles. The acid potassium salt is slightly soluble in water and
crystallizes therein in columnar prisins. In the mother yes of the raw products
remains, after their evaporation, the readily soluble potassium salt of another iodized
phenolsulpho-acid which crystallizes in alcohol in colourless scales.
The iodine-ortho-phenolsulpho-acids are prepared in the same manner as the para-
compounds, in this case also a compound that is slightly soluble in water (acid
potassium salt of the iodized ortho-phenosulpho-acid) is precipitated first and a
compound that is readily soluble remains in the mother-lyes, from which it is pre-
cipitated after the evaporation. Both compounds are purified by crystallization. The
slightly soluble compound crystallizes in small colourless leaves or needles, and the
readily soluble compound in crystalline crusts.

page_text: Under the same conditions as above stated are prepared the iodine cresolsulpho-
acids, one of which crystallizes in bunch shaped colourless needles (acid potassium
salt).
The iodine thymolsulpho-acid which is produced in the same manner is very easily
soluble in water and crystallizes in alcohol in small prisms or needles. In an aqueous
solution it decomposes at a certain concentration during the evaporation, a blue colour
being produced and thymol being partially re-formed; whereas the potassium salt
forms very durable colourless needles.
Having now particularly described and ascertained the nature of my said inven-
tion, and in what manner the same is to be performed, I declare that what 1
claim is :-
:-
The production of iodine (ortho, para, meta) phenolsulpho-acids, iodine cresol-
sulpho-acids, iodine thymolsulpho-acids and their salts by treating the corresponding
sulpho-acids or their salts with iodine in the form of iodic acid and iodine, iodide of
potassium and iodine, or chloride of iodine, or with iodine suspended in water either
by the introduction of chlorine gas or by means of a solution of iodide of potassium,
hydro-chloric acid and nitrite of sodium, or with iodine and iodine salts in presence of
lixivial substances.
Dated this 20th to 1000