Improvements in the Treatment of Oleic Acid.
Year: 1897

page_text: PROVISIONAL SPECIFICATION.
Improvements in the Treatment of Oleic Acid.
I, JULES DAVID, of No. 7, Rue Laffitte, Paris, France, Analytical Chemist, do hereby
declare the nature of this invention to be as follows:-
My invention relates to a process for transforming oleic acid into various white
solid bodies which can be employed alone or in admixture with ordinary stearine for
manufacturing stearine and candles.
For this purpose monohydrated sulphuric acid mixed with 5 per cent. of Nordhausen
acid is added drop by drop to dry oleic acid, cooled to about zero C, while agitated.
The quantity of acid added has to be from 40 to 50 per cent. of the weight of the oil
according to its purity or richness in solid matter. During the mixture the
temperature should never exceed 20° C, and therefore the vessel in which the mixture
is made, is provided with a jacket for circulation of cold water.
The mixture, after being kept 12 hours at rest, is run into a quantity of cold water
3 times the weight of the oleic acid treated, and the whole is stirred so that the paste
becomes separated, the temperature being kept under 30° C. The mixture, being
then left at rest for about 2 hours, becomes divided into two separate layers, the lower
layer being water mingled with about half the acid originally added; the acidulated
water can be applied for decomposing lime soap and for acid washing. The upper
layer is oleic acid partly converted into solid products.
After running off the acidulated water, fresh water, about 1 times the weight of
the acidulated water, is poured upon the layer containing the oleic acid, the whole is
thoroughly mixed and then left at rest in the cold for 24 hours. At the end of this
time the liquid has distributed through it fine crystals in great abundance, which are
separated by filtration and thoroughly washed. They are melted in boiling water
and produce a white slightly yellowish mass, melting at about 48° C, which being
distilled gives a white product, that can be made into candles in the usual way, or
can be used in the manufacture of stearine as will presently be explained.
This first product, which may be termed a, amounts to about 20 per cent. of the
weight of the oleic acid treated, consequently there remains about 80 per cent.
in the brown liquid filtered off the crystals.
80
This liquid is boiled in a vessel with a steam coil, taking care that there is no
reduction of volume, from time to time cold water being added to keep up the level.
After boiling for about 1 hour, the liquid separates into two layers, the lower layer
being water with the rest of the sulphuric acid, and the upper layer being the
cent. of oleic acid partly converted into hard material. After resting an hour,
the acidulated water is run off and cold water is added, the whole being boiled for a
short time to get rid of all traces of sulphuric acid. The oily matter, being run
into cooled moulds, crystallises in hard sandy crystals soiled with blackish impure
liquid. When they are purified they melt at 65° C and are quite white. These
per

page_text: crystals being cold pressed in bags, the black oil runs off and there remains in the
bags only a hard brittle mass still a little yellow, but easily purified as in the ordinary
stearine manufacture. This product which may be termed ẞ, amounts to 30 to
35 per cent. of the weight of the oil treated, so that the two products a and B
together amount to 50 to 55 per cent. of the oleic acid.
These products can be applied practically in various ways. Preferably 6 parts
of a are mixed with 9 parts of ẞ and with 60 parts of the matter which flows from
the hot pressing of fatty acids, tallow, or palm oil saponified or distilled. This
mixture is boiled in water heated by steam coil, and, after 12 hours rest, is run into
moulds and pressed both cold and hot. The stearine obtained is white and hard, and
behaves exactly as that obtained in the usual way.
The black oil pressed out from the crystals ẞ is distilled by superheated steam, the
distilled product being oleine, almost white, containing still a considerable proportion
of white solid, which is separated by pressing and amounts to about 25 per cent. of
the black oil.
By the processes described I obtain from tallow which melts at 44° the following
results. Instead of 50 per cent. stearine, 44 per cent. oleine, and 10 per cent.
glycerine obtained by the usual processes, I obtain 72 to 75 per cent. stearine,
21 to 18 per cent. oleine, and 10 per cent. glycerine. If I operate with a mixture of
tallow and palm oil, instead of 60 per cent. stearine, 30 per cent. oleine, and
7 per cent. glycerine, I obtain 75 to 80 per cent. stearine, 14 to 9 per cent. oleine and
7 per cent. glycerine.
It is to be noted that for separating the products a and B, I use no costly or
dangerous solvents such as ether, alcohol, petroleum, carbon bisulphide, etc., only
employ cold, water, heat, and pressure, all practical and ready means of operating.
Dated this 11th day of February 1897.
ABEL & IMRAY,
Agents for the Applicant.
I, JULES DAVID, of No. 7 Rue Laffitte, Paris, France, Analytical 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:-
My invention relates to a process for transforming oleic acid into various white
solid bodies which can be employed alone or in admixture with ordinary stearine for
manufacturing stearine and candles.
For this purpose by means of suitable apparatus such as that shewn in section in
the accompanying drawing, monohydrated sulphuric acid mixed with 5 per cent. of
Nordhausen acid is added drop by drop to dry oleic acid contained in a lead lined
vessel A and cooled to about zero C while agitated by a revolving agitator B. The
quantity of acid added has to be from 40 to 50 per cent. of the weight of the oil
according to its purity or richness in solid matter. During the mixture the
temperature should never exceed 20° C, and therefore the vessel A in which the
mixture is made is provided with a jacket for circulation of cold water.
The mixture after being left 12 hours at rest is by opening cocks a run into a lead
lined vessel D containing a quantity of cold water 3 times the weight of the oleic
acid treated, and the whole is stirred by wooden rakes so that the paste becomes
separated, the temperature being kept always under 30° C. The mixture being then

page_text: left at rest for about 2 hours, becomes divided into two separate layers, the lower
layer being water mingled with about half the acid originally added; this acidulated
water can be applied for decomposing lime soap and for acid washing. The upper
layer contains oleic acid partly converted into solid products.
After running off the acidulated water from D), fresh water about 1 times the
weight of the acidulated water is poured upon the layer containing the oleic acid,
the whole is thoroughly mixed and then left at rest in the cold for 24 hours. At the
end of this time the liquid has distributed through it fine crystals in great abundance,
which are separated by filtration either by a filter press or by cloth filters E and
thoroughly washed until the washing water is quite clear and limped. The white
product remaining on the filter is melted in boiling water producing a white slightly
yellowish mass melting at about 48° C which being distilled, gives a white product
that can be made into candles in the usual way, or can be used in the manufacture
of stearine as will presently be explained.
This first product which may be termed a amounts to about 20 per cent. of the
weight of the oleic acid treated consequently there remains about 80 per cent. in
the brown liquid filtered off the crystals.
This liquid is boiled in a vessel F with perforated steam coil G taking care that
there is no reduction of volume, from time to time cold water being added to keep up
the level. After boiling for about one hour the liquid separates into two layers, the
lower layer being water acidulated with the rest of the sulphuric acid originally used
and the upper layer being nearly the 80 per cent. of oleic acid partially converted into
hard material. After resting an hour the acidulated water is run off by the cock f
and cold water is added in the vessel F, the whole being boiled for a short time to get
rid of all traces of sulphuric acid. The oily matter being run into cooled moulds
crystallises in hard sandy crystals soiled with blackish impure liquid. When they are
purified they melt at 65° C and are quite white. These crystals being cold pressed
in bags, the black oil runs off and there remains in the bags only a hard brittle mass
still a little yellow, but easily purified as in the ordinary stearine manufacture. This
product which may be termed ẞ, amounts to 30 to 35 per cent. of the weight of the
oil treated, so that the two products a and ẞ together amount to 50 to 55 per cent. of
the oleic acid.
These products can be applied practically in various ways. Preferably 6 parts of a
are mixed with 9 parts of ẞ and with 60 parts of the matter which flows from the hot
pressing of fatty acids tallow or palm oil saponified or distilled. This mixture is
boiled in water heated by perforated steam coil, and after 12 hours rest is run into
moulds and pressed both cold and hot. The stearine obtained is white and hard, and
behaves exactly as that obtained in the usual way.
The black oil pressed out from the crystals ẞ is distilled by superheated steam, the
distilled product being oleine almost white, containing still a considerable proportion
of white solid, which is separated by pressing and amounts to about 25 per cent. of
the black oil.
By the processes described I obtain from tallow which melts at 44° the following
results. Instead of 50 per cent. stearine 44 per cent. oleine and 10 per cent. glycerine
obtained by the usual processes I obtain 72 to 75 per cent. stearine 21 to 18 per cent.
oleine and 10 per cent. glycerine. If I operate with a mixture of tallow and palm
oil, instead of the usual 60 per cent. stearine, 30 per cent. oleine and 7 per cent.
glycerine I obtain 75 to 80 per cent. stearine, 14 to 9 per cent. oleine and 7 per cent.
glycerine.
It is to be noted that for separating the products a and ẞ I use no costly or
dangerous solvents such as ether, alcohol, petroleum, carbon bisulphide &c. I only
employ cold, water, heat, and pressure, all practical and ready means of operating..
Having now particularly described and ascertained the nature of this invention
and in what manner the same is to be performed, I declare that what I
claim is :-
The treatment of bodies containing oleic acid for the production of two white

page_text: crystallised substances melting respectively at about 45° and 65° C; and forming by
their mixture stearine melting at about 54° C, substantially as described.
Dated this 22nd day of October 1897
ABEL & IMRAY,.
Agents for the Applicant.