Improvements in Treating Mineral, Resin, and Tar Oils, and in the Preparation of Products therefrom.
Year: 1899

page_text: Date of Application, 13th June, 1899
Complete Specification Left, 13th Mar., 1900-Accepted, 14th Apr., 1900
PROVISIONAL SPECIFICATION.
Improvements in Treating Mineral, Resin, and Tar Oils, and in the
Preparation of Products therefrom.
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:
It is well known that pure neutral hydro-carbons, namely, the different mineral,
resinous, and tar oils, could not be saponified clearly without the addition of a
considerable amount of saponified fatty acids (especially olein) or of prepared
fatty acid soaps (riz. linseed oil potash soap) and the additions of alcohol and
ammonia. Nor could they be converted into clear liquid soaps (equal in appear-
ance to the oils employeil), or to convert the said oils into permanent emulsions
easily soluble in water. The soluble oils produced by means of fatty acids in
their employment by no means realize expectations in practice, and these acids
have been found to be unsuitable and imperfect for lubricating, boring, cutting
and polishing purposes, as also for producing remedial or pharmaceutical soluble
preparations, because on one hand the metallic surfaces are oxidised and attacked
thereby and especially rust is formed in the pores of the metal, whilst on the
other hand the fatty acids contained in the oils, in soluble medicaments made
with them must act disadvantageously in most cases, and therefore make it
impossible for the medicaments to act properly.
In order to prepare pure neutral hydrocarbons such as the various mineral and
resinous oils, and also tar oils which shall be soluble in water and easily emulsif.-
able, the following process has been devised:-
The mineral oil to be prepared is put into a washing trough with a certain
per centage of crude (but anhydrous) light-coloured resin oil. The per centage
may vary according to the specific weight of the mineral oil treated from about
fifteen per cent. to twenty five per cent.. and is there treated with direct steam
at about five atmospheres pressure which is distributed in equal finely divided
portions throughout the oil. The mixture is boiled at not more than 100° to
105° Celsius at highest; then from five to seven per cent. of caustic soda lye
of 40° Beaumé is added according to the specific gravity of the mineral oil, and
the more or less admixture of resin oil (say five, six, or up to seven per cent.)
The mixture is maintained for twenty to thirty minutes in a boiling state and
treated until the oil is seen to clearly separate from the soap lye.
After allowing the whole to stand from half to three quarters of an hour, the
clear oil is drawn off which takes with it two and a half to three per cent. of excess
lye clearly saponified, over the underlying resin oil soap solution
to an oxidising apparatus where the oil is treated with very finely
divided compressed air for two hours at a temperature of 60° to 80° Celsius and
afterwards for another hour at 80° to 110° Celsius for the purpose of supplying
oxygen to the oil and causing its further saponification; the slowly evaporating
water of the lye must be continuously added almost drop by drop during the
course of the process. This oxydising process can also be attained by means

page_text: of oxygen fluid (ozone). Immediately after this oxydising process is finished,
the oil is aspirated or blown directly into a pressure still and there treated with
an addition of three per cent. alcohol (preferably methylated spirit) two to
three per cent. strong ammonia solution and preferably one per cent. of gelatine
dissolved in water for half an hour to an hour under a pressure of one to one and
a half atmospheres at different temperatures, until the originally turbid mass of
oil and soap existing at the beginning of the process again becomes quite clear.
The oil is now finished, but must only be drawn off after cooling in order to
prevent the oils becoming turbid again.
It is to be noted that the addition of methylated spirit and ammonia and also
of the gelatine solution is not absolutely necessary to the process, and is only
recommended in particular cases so that the oils may dissolve rather more easily
in the water and emulsify more easily and make the respective solutions per-
manent.
In the same way, that is, by using resin oil (instead of fatty acid soaps) tar
oils soluble in water may also be manufactured.
The mineral and resin oils soluble in water or mixtures of the two kinds of oil
may be employed with great advantage for the following purposes:
1. For lubricating, boring, cutting and polishing purposes.
2. For greasing wool before spinning.
3. For treating cloth in textile industries.
4. For colouring and glazing bricks and building stones.
-
5. For producing aromatic hydrocarbons soluble in water and the like essential
oils for disinfecting, soap-manufacture, and perfumery purposes as well as
6. For manufacturing soluble medicinal and pharmaceutical preparations of
various kinds.
The process of manufacturing the products mentioned in paragraphs 5 and 6.
forms the subject of a special Application for Letters Patent, dated June 13th
1899 No. 12348.
The tar oils, soluble in water, are principally employed for disinfecting, and
preserving wood, and also for colouring and glazing bricks or tiles and so
forth.
Improvements in Treating Mineral, Resin, and Tar Oils, and in the
Preparation of Products therefrom.
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: ---
It is well known that pure neutral hydro-carbons, namely, the different mineral,
resinous, and tar oils, could not he saponified clearly without the addition of a
considerable amount of saponified fatty acids (especially olein) or of prepared
fatty acid soaps (riz. linseed oil potash soap) and the addition of alcohol and
ammonia. Nor could they be converted into clear liquid soaps (equal in appear-
ance to the oils employed), nor converted into permanent emulsions
easily soluble in water. The soluble oils produced by means of fatty acids in
their employment by no means realize expectations in practice, and these acids

page_text: have been found to be unsuitable and imperfect for lubricating, boring, cutting
and polishing purposes, as also for producing remedial or pharmaceutical soluble
preparations, because on one hand the metallic surfaces are oxidised and attacked
thereby and especially rust is formed in the pores of the metal, whilst on the
other hand the fatty acids contained in the oils, in soluble modicaments made
with them must act disadvantageously in most cases, and therefore make it
impossible for the medicaments to act properly.
In order to prepare pure neutral hydrocarbons such as the various mineral and
resinous oils, and also tar oils, mixtures of mineral and resin oils, and of tar and
resin oils or resin oils alone, without the addition of other oils, which are soluble
in water and easily emulsifiable, the following process has been devised: -
The mineral oil to be prepared is put into a washing trough with a certain
per centage of crude (but anhydrous) light-coloured resin oil. The per centage
may vary according to the specific weight of the mineral oil treated from about
fifteen per cent. to twenty five per cent., and is there treated with direct steam
at about five atmospheres pressure which is distributed in equal finely divided
portions throughout the oil. The mixture is boiled at not more than 100° to
105° Celsius at highest; then from five to seven per cent. of caustic soda lye
of 40° Beaumé is added according to the specific gravity of the mineral oil, and
the more or less admixture of resin oil (say five, six, or up to seven per cent.)
The mixture is maintained for twenty to thirty minutes in a boiling state and
treated until the oil is seen to clearly separate from the soap lye. Refined resin
oils cannot be used as they do not take up more lye.
to
oil
After allowing the whole to stand from half to three quarters of an hour, the
clear oil is drawn off which takes with it two and a half to three per cent, of excess
saponified,
lye clearly
solution
the underlying resin
over
soap
is treated with very finely
an oxidising apparatus where the oil
divided compressed air for two hours at a temperature of 60° to 80° Celsius and
afterwards for another hour at 80° to 110° Celsius for the purpose of supplying
oxygen to the oil and causing its further saponification; the slowly evaporating
water of the lye must be continuously added almost drop by drop during the
course of the process. This oxydising process can also be attained by means
of oxygen fluid (ozone). Immediately after this oxydising process is finished,
the oil is aspirated or blown directly into a pressure still and there treated with
an addition of three per cent. alcohol (preferably methylated spirit) two to
three per cent. strong ammonia solution and preferably one per cent. of gelatine
dissolved in water for half an hour to an hour under a pressure of one to one and
a half atmospheres at different temperatures until the originally turbid mass of
oil and soap existing at the beginning of the process again becomes quite clear
and easily soluble. The oil is now finished, but must only be drawn off after
cooling in order to prevent the oils. becoming turbid again.
It is to be noted that the addition of methylated spirit and ammonia and also
of the gelatine solution is not absolutely necessary to this process, as it is in
others, and is only recommended in particular cases so that the oils may dissolve
rather more easily in the water and emulsify more easily and make the respective
solutions permanent.
In the same way, that is, by using resin oil (instead of fatty acid soaps) tar
oils soluble in water may also be manufactured.
In order to obtain these products with the required degree of permanency all
the three processes must be carried out in their order, as if only one of them
be employed the object desired is only partially attained. The soluble and emulsifi-
able oils and oil mixtures thus obtained can now be easily mixed with any
quantity of water and are specially applicable for the purposes mentioned below
if further treated with 50% to 75% of distilled water (ordinary water can also
be used) for a quarter to half an hour in the distilling or oxydation apparatus,
when clear, in parts a trifle opalescent but invariably permanent oil and water
solutions of great value and universal applicability are obtained.

page_text: The mineral and resin oils soluble in water or mixtures of the two kinds of oil
may be employed with great advantage for the following purposes:-
1. For lubricating, boring, cutting and polishing purposes.
2. For greasing wool before spinning.
3. For treating cloth in textile industries.
4. For colouring and glazing bricks and building stones.
5. For producing aromatic hydrocarbons soluble in water and the like essential
oils for disinfecting, soap-manufacture, and perfumery purposes as well as
6. For manufacturing soluble medicinal and pharmaceutical preparations of
various kinds.
The process of manufacturing the products mentioned in paragraphs 5 and 6,
is described in my Patent Application No: 12348 of 1899.
The tar oils, soluble in water, are principally employed for disinfecting, and
preserving wood, and also for colouring and glazing bricks or tiles and so
fortlí.
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
Process for preparing permanent emulsifiable mineral, resin and tar oils casily
soluble in water or soluble mixtures of mineral oil and resin oil, and of tar oil
and resin oil, or soluble resin oil without any admixture of other oils, also of clear
watery solutions of mineral and resin oils, characterized by first washing and
treating the oils with direct steam and excess of caustic soda bye, then subjecting
the oil mixtures after the resinous soap lye has been separated to an oxydation
process by introducing oxygen in the form of compressed air or ozone, and finally
subjecting them to more or less prolonged treatment under pressure with or
without the addition of chemicals and distilled water, substantially as set forth.
Dated the 13th day of March 1900.
W. P. THOMPSON & Co..
Of London, Liverpool, Manchester and Birmingham.