Year: 1897

page_text: Date of Application, 6th May, 1897
Complete Specification Left, 5th Feb., 1898-Accepted, 6th May, 1898
A communication from abroad by Messrs. KNOLL & Co. of Ludwigshafen a/ Rh.,
Germany, Chemical Manufacturers.
I, WILLIAM LLOYD WISE, of 46 Lincoln's Inn Fields, in the County of London,
Consulting Engineer and Chartered Patent Agent, do hereby declare the nature of
this invention to be as follows:-
If a solution of albumen or a compound of albumen be mixed with ichthyolsulpho-
acid, a precipitate is produced consisting of a compound of ichthyol with the said
albumen or compound thereof. The compound thus formed by being heated to a
comparatively high temperature or by treatment with certain solvents, can be caused
to entirely lose the extremely unpleasant smell and taste possessed by ichthyol. It is
also found that by this treatment such compounds are rendered only slightly subject
to the digestive action of the stomach and are therefore only dissolved very slowly
in the intestines without interfering in any way with the digestive organs.
The following shows by way of example one method of carrying out the invention:-
10 kilogs. of albumen are dissolved in 30 litres of water, and to the solution thus
formed there is gradually added with energetic stirring a solution of 6 kilogs. of
ichthyolsulphoacid (or a corresponding quantity of an ichthyolsulphoacid salt with an
addition of a stronger acid) in 50 litres of water. The resultant precipitate, after
being pressed and dried, is powdered and then heated say for about 24 hours at a
temperature of from about 100° C. to 150° C., preferably at about 125° C.
The desired result of rendering the preparation free from taste or smell and with
difficulty affected by the digestive action of the stomach may also be obtained by
treatment with alcohol or acids instead of by the application of heat. Serum albumen,
peptone or casein are examples of substances other than ordinary albumen that may,
be precipitated with ichthyol as described.
46, Lincoln's Inn Fields, London, W.C., Chartered Patent Agent.
COMPLETE SPECIFICATION.
Manufacture of Compounds of Ichthyol.
A communication from abroad by Messrs. KNOLL & Co., of Ludwigshafen a/ Rb.,
Germany, Chemical Manufacturers.
I, WILLIAM LLOYD WISE, of 46, Lincoln's Inn Fields, in the County of London,
Consulting Engineer and Chartered Patent Agent, 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 :-
If a solution of albumen or a compound of albumen be mixed with a solution of

page_text: ichthyol-sulpho-acid, or with a solution of ichthyol, the ammoniacal salt of ichthyol-
sulpho-acid, a precipitate is produced containing all the constituents of the ichthyol.
If the mixture be made with ichthyol instead of the acid, a stronger acid must be
added.
The precipitate thus formed contains besides the sulphoacids and sulphones, which
have entered into chemical combination with the albumen, also small traces of an
ethereal oil, which are the cause of the offensive odour and taste in ichthyol. In
spite of many attempts, it has heretofore been found impossible to remove this
offensively smelling oil from ichthyol without completely altering the latter.
According to this invention, however, this oil may be easily removed from the
ichthyol compounds, without materially altering the ichthyol in the compounds, by
heating them as hereinafter set forth, or by treating them with certain solvents.
If the dried and powdered ichthyol compounds be heated for a period of several
hours up to about from 100 to 150° C., the ethereal oil will gradually be volatilized
and be removed by conducting a warm current of air over the heated compounds.
In this process of removing the oil, the active constituents of the ichthyol (sulpho-
acids and sulphones) will not be decomposed. The result of this process will be an
odourless and nearly, tasteless preparation which is perfectly fit for use, for therapeutic
purposes.
Instead of removing the ethereal oil by heating, it may be removed by solvents
such as benzol, ligroin, chloroform or alcohol, for example ethylic alcohol. These
solvents will easily extract from the ichthyol compounds mainly the oil, which is but
mechanically mixed or enclosed in the compounds, and also a small part of the
sulphones and sulpho-acids, thus freeing the preparation from offensive odour and
taste whilst leaving the therapeutically important constituents of the ichthyol
unaltered in the compounds. With this method of extraction no separation of the
sulphones from the sulphoacids will take place.
By continuing the systematic treatment for a prolonged period with solvents, the
entire bulk of sulphones could be gradually extracted with a part of the sulphoacids,
the combination of the sulphones with the albumen being less permanent than that
of the sulphoacids with the albumen. This however is to be avoided in carrying out
this invention.
By using alcohol as a solvent or by the method of heating the ichthyol-albumen-
compounds the latter are at the same time rendered incapable of being. digested by
the juices of the stomach, so that they pass the stomach without causing any
injury to the latter and are gradually dissolved and absorbed by the intestines
only.
Casein and peptone are examples of albumen substances other than ordinary
albumen that may be precipitated in combination with ichthyol as above described.
The described method of making the ichthyol compounds odourless and almost
tasteless without decomposing the ichthyol itself may in the same way, be employed
to render other non-fluid ichthyol precipitates odourless and almost tasteless.
The following shows by way of example one method of carrying out the
invention:-
(1) Ten kilogramines of albumen are dissolved in sixty litres of water and to the
solution thus formed ten kilogrammes of ichthyol (ammonium-sulpho-ichthyolicum)
are added. To this mixture a solution of 900 grainines, of concentrated sulphuric
acid and ten litres of water are gradually added with constant stirring. The
precipitate thus obtained after the liquid has been pressed off, is dried and powdered
and in order to remove the offensive odour and taste is then heated for about 24
hours at about 120° C.; instead of heating the compound it may be treated with a
solvent. When using alcohol for this purpose 10 kgs. of the powder are stirred for
about half an hour with double the quantity of alcohol; the latter is then filtered off
and the product washed with alcohol in order to perfectly remove the adhering
alcoholic solution of the strongly smelling and tasting constituents of ichthyol; after
which the product is dried and powdered.
(2) 10 kilogrammes of albumen are dissolved in 30 litres of water, and to the

page_text: solution thus formed there is gradually added with energetic stirring a solution of
6 kilogs. of ichthyolsulphoacid in 50 litres of water. The resultant precipitate,
after being pressed and dried, is powdered and treated with a solvent as herein before
described or heated for about 24 hours at a temperature of from about 100° C., to
150° C., preferably at about 125° C.
Having now particularly described and ascertained the nature of the said
invention and in what manner the same is to be performed I declare that what
I claim is
1. The manufacture of ichthyol-albumen compounds by precipitating a solution
of albumen by ichthyol and a stronger acid, or by free ichthyol-sulphoacid, as set
forth.
2. Converting the ichthyol compounds prepared according to the preceding claim,
or other non-fluid ichthyol precipitates, into nearly odourless and tasteless
preparations, by heating the compounds for a prolonged period, or by treating them
with a solvent such as alcohol, as set forth.
3. The manufacture of the herein described nearly odourless and tasteless ichthyol
compounds as set forth.
Dated this 5th day of February 1808
W. LLOYD WISE,
46, Lincoln's Inn Fields, London, W.C., Chartered Patent Agent.