An Improved Manufacture of an Antiseptic Disinfectant.
Year: 1896

page_text: Date of Application, 20th Jan., 1896
Complete Specification Left, 28th Aug., 1896-Accepted, 10th Oct.. 1896
PROVISIONAL SPECIFICATION.
An Improved Manufacture of an Antiseptic Disinfectant.
A communication from FRANZ FRITZSCHE & COMPANY, Chemical. Works,
Hamburg, Empire of Germany.
I, ALFRED JULIUS BOULT of 323 High Holborn, County of Middlesex,
Chartered Patent Agent do hereby declare the nature of this invention to be as
follows:-
The present invention has for its object a process for preparing from oxychinolin
When it is
a solid antiseptic and disinfecting substance soluble in water.
attempted to prepare an antiseptic from oxychinolin by means of inorganic acids,
for instance sulphuric acid, the resulting substance is always too acid and too
corrosive as for instance the well known sulphate of oxychinolin C,H,.N.OH.H,SO
+ 2 H2O, or we get hygroscopic and smearing substances of which it is impossible
to prepare either powder or pastilles.
We have found now that out of pyrosulphate of potassium (K,S,O,), dissolved
in alcohol, it is possible to prepare a disinfecting substance, soluble in water, which
substance is remarkable for possessing a consistency which is not too firm and for
the facility with which it can be made into pastilles. The substance has no smell,
is neither irritating nor poisonous, but nevertheless has much greater power for
killing microbes than carbolic acid. The process for manufacturing this new
antiseptic and disinfecting substance is as follows:
We dissolve two molecules of o-oxychinolin in about five or six times that weight
of boiling alcohol, and add gradually, under constant mixing, the proportion of
qne molecule of pulverised, pyrosulphate of potassium and boil the whole during 10
or 12 hours on a back-flow cooling apparatus. When cooled, the contents of the
vessel form a tender crystal pulp, which can be easily pumped out, dried, pulverised
and compressed. For instance: 29 kg. oxychinolin are dissolved in 120 kg. alcohol
and to this is added gradually whilst a mixing arrangement keeps mixing the
contents of the boiler, under continual heating 25 kg. of finely pulverised
pyrosulphate of potassium.
After this all the contents of the boiler are boiled on the backflow cooling
apparatus till the end of the process. After 10 hours reaction the transformation
is complete; then follows the cooling and the product is extracted by removing the
alcohol by centrifugal force or by filtration. The dried mass is then pulverized or
2(CHEN.On) + =
The product arrived at in this way dissolves in water in any proportion nearly
instantaneously, and this water solution has a remarkable capacity for dissolving
phenols, as for instance cresol, and resorein and of giving clear solutions of them,
however weak they be.
It must be remarked that there have been already attempts to produce a water-
soluble antiseptic by the-reaction of sulphuric acid on the oxy.chinulin. But it is
uncommonly difficult to crystallize the product, and when the water is evaporated,
there remains a smeary mass, which consists of acid sulphate and of free oxychinolin

page_text: and which cannot be brought into the market as pastilles. The present process
differs from the old one in that pyrosulphate of potassium is used instead of
sulphuric acid and it is treated in a solution of alcohol. This new way of treating
it gives another product in the end, which, unlike the above mentioned can be
easily converted into pastilles or pulverized; further, the process is simpler, as it
consists only of one operation and there is no necessity for using sulphuric acid.
It ought also to be mentioned that the new substance cannot be obtained simply
by treatment of oxychinolin by kaliumpyrosulphate, but that it is absolutely
necessary to effect this treatment in alcohol. The inventors explain this fact by
great affinity of alcohol for water; that affinity seems to prevent in the present
case the formation of a hydrate and causes on the contrary formation of an
anhydrite which has the previously mentioned microbe-destroying qualities, forms
a crystalline powder and can be pressed directly into the shape of pastilles.
Dated this 20th day of January 1896.
BOULT & WADE,
Agents for the Applicant.
A communication from FRANZ FRITZSCHE & COMPANY, Chemical Works,
Hamburg, Empire of Germany.
I, ALFRED JULIUS BOULT formerly of 323 High Holborn, now of 111 Hatton
Garden, in the County of Middlesex, 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:-
This invention has for its object a process for preparing from oxychiuolin a
solid antiseptic and disinfecting substance soluble in water. When it is attempted
to prepare an antiseptic from oxychinolin by means of inorganic acids, for instance
sulphuric acid, the resulting substance. is always too acid and too corrosive, as for
instance the well known sulphate of oxychinolin C,H,N.OH.H,SO, + 2 H₂O, or
we get hygroscopic and smearing substances of which it is impossible to prepare
either powder or pastilles.
My foreign correspondent has found now that out of pyrosulphate of potassium
(K,S,O,), dissolved in alcohol, and oxychinolin it is possible to prepare a
disinfecting substance, soluble in water, which substance is remarkable for
possessing a consistency which is not too firm, and for the facility with which it
can be made into pastilles. The substance has no smell, is neither irritating nor
poisonous, but nevertheless has much greater power for killing microbes than
carbolic acid. The process for manufacturing this new antiseptic and disinfecting
substance is as follows:-
Two molecules of o-oxychinolin are dissolved in about five or six times that
weight of boiling alcohol, then add gradually, under constant mixing, the proportion
of one molecule of pulverised, pyrosulphate of potassium and boil the whole
during 10 or 12 hours on a back-flow cooling apparatus. When cooled, the
contents of the vessel form a tender crystal pulp which can be easily pumped out,
dried; pulverised and compressed, for instance :-
29 kg. oxychinolin are dissolved in 10 kg. alcohol and to this is added gradually
whilst a mixing arrangement keeps mixing the contents of the boiler, under
continual heating 25 kg. of finely pulverised pyrosulphate of potassium.
After this all the contents of the boiler are boiled on the backflow cooling
apparatus till the end of the process. After 10 hours reaction the transformation

page_text: is complete; then follows the cooling and the product is extracted by removing the
alcohol by centrifugal force or by filtration.
The chemical reaction is probably as follows.
UN TUTUW
2 (C,H,N.OH) + K,S,O, = 2 (C,H¸N.OSO,K) + H₂O.
The product arrived at in this way dissolves in water in any proportion nearly
instantaneously, and this water solution has a remarkable capacity of dissolving
phenols, as for instance cresol, and resorcin and of giving clear solutions of them,
however, weak they be.
The present process differs from those formerly in use by pyrosulphate of
potassium, instead of sulphuric acid, being brought to act upon oxychinolin and
by the process taking place in alcohol. This new way of treating it gives
another product in the end, which, being a crystalline anhydric powder can be
easily converted into pastilles, further, the process is simpler, as it consists only
of one operation and there is no necessity for using sulphuric acid.
Having now particularly described and ascertained the nature of this inven-
tion as communicated to me by my foreign correspondent and in what manner the
same is to be performed, I declare that what I claim is :-
1. A process for manufacturing an antiseptic disinfectant soluble in water con-
sisting in the treatment, of oxychinolin with pyrosulphate of potassium in alcohol
substantially as described.
2. A process for manufacturing an antiseptic disinfectant soluble in water
consisting in boiling two molecules o-oxychinolin in alcohol with one molecule
pyrosulphate of potassium or sodium delivering the product from the alcohol and
drying or pressing it, substantially as described.
3. The antiseptic disinfectant herein before described.
1000
BOULT & WADE,
Agents for the Applicant.