Improved Process for the Preparation of Permanent Emulsions Soluble in Water of Aromatic Hydrocarbons and Etherial Oils and Pharmaceutical Products.
Year: 1899

page_text: Date of Application, 19th June, 1809
Complete Specification Left, 13th Mar., 1900-Accepted, 13th June, 1900
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Complete Specification Left, 13th Mar., 1900-Accepted, 13th June, 1900
PROVISIONAL SPECIFICATION.
Improved Process for the Preparation of Permanent Emulsions
Soluble in Water of Aromatic Hydrocarbons and Etherial Oils
and Pharmaceutical Products.
I, FRIEDRICH BOLEG, of Esslingen a/N, in the Kingdom of Wurtemberg.
Germany, Chemist, do hereby declare the nature of this invention to be as
follows:
As set forth in the Specification of my process for making pure, mineral,
resinous and tar oils soluble in water for which I am applying for Letters Patent
No. 12349 dated June 13th 1899, these oils can be used as a basis for making
aromatic hydro-carbons and essential oils and the like pharmaceutical prepara-
tions (medicaments) which are soluble in water, better and more economically
than soluble or emulsified oils hitherto employed which were made by means of
fatty acids or fatty acid soaps as the fatty acids contained in these oils must
operate injuriously in both cases and make a proper action almost impossible.
On the other hand it is known and proved that nothing is so suitable as the
pure neutral mineral and resin oils for combining with aromatic hydro-carbons
essential oils and certain drugs and to make the same into soluble products
intense and lasting. Even five per cent. solutions thereof in water diffuse a
much stronger odour than the pure undiluted products, and retain their qualities
for months in the open air and even after previously heating for ten hours at a
temperature of 40° to 65° Celsius and can consequently be used in manifold ways
with great advantage and considerable saving over the pure products.
The manufacture of aromatic hydro-carbons, essential oils and the like phar-
maceutical preparations soluble in water or easily and strongly emulsifying is
as follows:-
The
The hydrocarbon to be treated is placed in the so-called oxidisation apparatus
which is closed in this case and connected with a condenser. Here the substance
is treated at a temperature produced by steam heat of 50° Celsius slowly rising
to 70° for about half an hour with finely divided compressed air; at the same
time 2 to 5% of caustic soda lye of 20° Beaume is added almost drop by drop,
and besides that to replace the condensed water about 2% of hot water.
temperature and the addition of lye must always vary a little according as an
essence or an oil is treated. The slightly alkaline essences or oils so treated
are then (after it has been ascertained that they have become perfectly clear
again after a slight turbidity at the beginning) according to the nature and
quality of the essences or oils concerned, mixed with from 30 to 50% of the
aforesaid pure mineral and resin oil mixture soluble in water, by means of a
further supply of compressed air at a temperature of 50° to 70° Celsius for about
ten minutes. The mixture is treated immediately and directly without access
of air in a distilling apparatus under pressure, and is then exposed for half an
hour to an hour by means of steam heat to a pressure of a half to one atmosphere.
The length of time and amount of the pressure here also depends entirely on
the kind and quality of the essences and oils concerned.

page_text: The essence or oil soluble in water is now ready but is preferably allowed to
remain to cool completely in the apparatus or in a special cooling vessel to avoid
turbidity and is then drawn off into vessels.
For making aromatic hydrocarbons, and essential oils soluble according to the
above described method the following compounds are especially proposed :-
Raw and rectified Nitro-benzene, Oil of Cloves, both common and free from
Eugenol, Oil of Camphor, Oil of Patchouli, Lavender, Citron, Cucumber,
Geranium, Heliotrope, Hyacinth, Menthol, Turpene, Neroli, Bromalia, Eucalyp-
tus, Chlorophyll, Safrol, Thymol and many others.
Of these soluble oils nitro-benzol (crude) common oil of cloves and also
camphor and lavender oils are used for disinfecting purposes, all the remainder
of those mentioned being employed in the manufacture of soap and for perfumery
purposes with great advantage, and considerable saving of expense.
In order to make pharmaceutical preparations (medicaments) soluble in water,
of different kinds for different purposes for outward as well as inward application
the process is as follows:-
Mineral oil (vaseline oil) soluble in water is put into the oxidation apparatus
and heated by means of steam heat according to the kind of medicament to
be treated, to a temperature of 40° to 60° Celsius and there is then added accord-
ing to requirements and the solubility of the particular medicament, 1 to 25% of
the medicament drop by drop under air pressure and the apparatus is allowed
to go on working until the mixture has become perfectly clear (usually ten to
fifteen minutes).
It is recommended that the mixture should be first cooled in a special cooling
basin before the bottles or vessels are filled with it. The preparations are then
ready.
For making easily prepared and permanent emulsions of pharmaceutical pre-
parations (medicaments) soluble in water the following medicaments are especi-
ally applicable:
Iodine, Creosote, Guiacol, Iodoform, Chloroform, Camphor, Ichthyol, Tur-
pentine, Salicylline, Codeine, Quinine, Ergotine, Creoline, Menthol, Pyoptanine,
Mercury, Potassic Iodide and so forth.
1
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Improved Process for the Preparation of Permanent Emulsions
Soluble in Water of Aromatic Hydrocarbons and Etherial Oils
and Pharmaceutical Products.
I, FRIEDRICH BOLEG, of Esslingen a/N, in the Kingdom of Wurtemberg,
Germany, Chemist, 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:—
As set forth in the process described in the Patent No. 12349 of 1899 for
making pure, mineral, resinous and tar oils soluble in water for which I
am about to apply for Letters Patent, these oils can be used as a basis for making
aromatic hydro-carbons and etherial oils and the like pharmaceutical preparations
(medicaments) which are soluble in water, better and more economically than
soluble or emulsified oils hitherto employed which were made by means of fatty

page_text: acids or fatty acid soaps as the fatty acids contained in these oils must operate
injuriously in both cases and make a proper action almost impossible. On
the other hand it is known and proved that nothing is so suitable as the pure
neutral mineral and resin oils for combining with aromatic hydro-carbons
etherial oils and certain drugs and to make the same into soluble products intense
and lasting. Even five per cent. solutions thereof in water diffuse a much
stronger odour than the pure undiluted products, and retain their qualities for
months in the open air and even after previously heating for ten hours at a
temperature of 40° to 65° Celsius and can consequently be used in manifold
ways with great advantage and considerable saving over the pure products.
The manufacture of aromatic hydro-carbons, etherial oils and the like pharma-
ceutical preparations soluble in water or easily and strongly emulsifying is as
follows-
The hydrocarbon to be treated is placed in the so-called oxidisation apparatus
which is closed in this case and connected with a condenser. Here the substance
is treated at a temperature (produced by steam heat) of 50° Celsius slowly rising
to 70° for about half an hour with compressed air introduced through a hose
provided with fine holes; at the same time 2 to 5% of caustic soda lye of 20°
Beaumé is added almost drop by drop, and besides that, to replace the condensed
water, about 2% of hot water. The temperature and the addition of lye must
always vary a little according as an essence or an oil is treated.
The employment of compressed air is expressly noted as without at the same
time a plentiful supply of oxygen in the alkaline hydrocarbons and oils, by.
means of any other method of stirring or mixing alone, no clear, strong, and
suitably alkaline reacting mixtures can be made thereof which are applicable
for manufacturing products which are emulsifiable or soluble in water. The
mixtures are obviously oxidised hereby somewhat if only partly. By intimately
mixing with ozone or liquid oxygen the same result can of course be obtained.
In special cases, as for instance in the preparation of lumarin thymol and the
like where the treatment with lye is unsuitable or not necessary on account of
their solubility or only a small percentage of addition is necessary in consequence
of their strong scent, this treatment can be omitted.
The slightly alkaline essences or oils so treated are then (after it has been
ascertained that they have become perfectly clear again after a slight turbidity at
the beginning (according to the nature and quality of the essences or oils concerned
mixed with from 30 to 50% of the aforesaid pure mineral and resin oil mixture
soluble in water, by means of a further supply of compressed air at a temperature
of 50° to 70° Celsius for about ten minutes. The mixture is treated immediately
and directly without access of air in a distilling apparatus under pressure, and
is then exposed for half an hour to an hour by means of steam heat to a pres-
sure of a half to one atmosphere. The length of time and amount of the pressure
here also depends entirely on the kind and quality of the essences and oils con-
cerned.
The essence or oils soluble in water is now ready but is preferably allowed to
remain to cool completely in the apparatus or in a special cooling vessel to avoid
turbidity and is then drawn off into vessels.
For making aromatic hydrocarbons, and etherial oils soluble according to the
above described method the following compounds are especially proposed:-
Raw and rectified Nitro-benzine, Oil of Cloves, both common and free from
Eugenol, Oil of Camphor, Oil of Patchouli, Lavender, Citron, Cucumber, Geranium,
Heliotrope, Hyacinth, Menthol, Turpene, Neroli, Bromalia, Eucalyptus, Chloro-
phyll, Safrol, Thymol and many others.
Of these soluble hydrocarbons and etherial oils nitro-benzol (crude) common oil
of cloves and also camphor and lavender oils are used for disinfecting purposes, all
the remainder of those mentioned being employed in the manufacture of soap and
for perfumery purposes with great advantage, and considerable saving of expense.
In order to make pharmaceutical preparations (medicaments) soluble in water,

page_text: such as iodine, creosote, guiacol, iodoform, chloroform, camphor, ichthyol, tur-
pentine, salicylline, quinine, codeine, ergotine, creoline, menthol, pyotanine, mercury
and potassic iodide, and so forth, the process is substantially the same as described
for aromatic hydrocarbons and etherial oils but with the soda lye treatment and
compressed air, apparatus omitted.
Mineral oil (vaseline oil) soluble in water is put into the oxidation apparatus
and heated by means of steam heat according to the kind of medicament to be
treated, to a temperature of 40° to 60° Celsius and there is then added according
to requirements and the solubility of the particular medicament, 1 to 25% of
the medicament drop by drop under air pressure and the apparatus is allowed
to go on working until the mixture has become perfectly clear (usually ten to
fifteen minutes). It is indispensable that the medicaments should be added
drop by drop, and that they should be intimately mixed if it is wished to
obtain clear, permanent preparations. These are only obtained with the soluble
mineral oil and resin oil mixture and the clear emulsions thereof, and not per-
manent preparations can be obtained by means of the emulsifying oils con-
taining fatty acids known hitherto but only those which speedily become de-
composed, and were therefore of little use.
It is recommended that the mixture should be first cooled in a special cooling
basin before the bottles or vessels are filled with it. The preparations are then
ready.
Having now particularly described and ascertained the nature of my said
invention and in what manner the same is to be performed I declare that what
I claim is: -
1. Process for preparing permanent emulsions soluble in water of aromatic
hydrocarbons and etherial oils and clear permanent solutions of these oils and
drugs by means of a preliminary treatment thereof with caustic soda lye and
compressed air (or ozone) in order to alkalize these preparations, by the addition
of a soluble mixture of mineral and resin oil; together with the further applica-
tion of compressed air at varying temperatures, and subsequently treatment of
the compounds in a distilling apparatus under slight pressure for a relatively
short period and final cooling, substantially as described.
2. A modification of the process claimed in Claim 1 in which the preliminary
treatment with soda lye and the subsequent treatment under pressure is omitted
for preparing permanent emulsions soluble in water and also clear hydrated
pharmaceutical preparations (medicines) of different kinds by intimately mixing
the respective drugs with a mixture of mineral oil (such as vaseline oil) and
resin oil soluble in water, or with suitably diluted clear mixtures of oil and
water thereof by means of compressed air at determined though sometimes varying
temperatures and subsequently carefully cooling the same substantially as
described.
Dated the 13th day of March 1000.
W. P. THOMPSON & Co.,
Of London, Liverpool, Manchester and Birmingham.