Improvements relating to the Separation of Fats or Oils into Glycerine and Fatty Acids, and to Compounds for use therein.
Year: 1898

page_text: Date of Application, 25th Feb., 1898-Accepted, 30th Apr., 1898
[Communicated from abroad by ERNST TWITCHELL, of Cincinnati, Hamilton
County, State of Ohio, United States of America, Chemist.]
Improvements relating to the Separation of Fats or Oils into
Glycerine and Fatty Acids, and to Compounds for use therein.
I, HENRY HARRIS LAKE, of the firm of Haseltine, Lake & Co., Patent Agents,
45, Southampton Buildings, in the County of Middlesex, 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:-
The objects of my invention are first to separate these constituents without any
material discoloration and without any waste or destruction of either the fatty
acids or the glycerine.
Second to cheapen the process of carrying on the operation at the ordinary
temperature of boiling water, dispensing with costly apparatus, high temperatures,
and high pressures.
Third, to produce a new chemical compound adapted to be used in my process
of making glycerine.
By my process I separate the glycerine from the neutral fat or oils by boiling
with water in an open tank, the reaction being induced by a small quantity of a
reagent which I prefer to mix with the fat before adding the water. This reagent
is a compound acid-ether of a fatty acid with sulphuric acid, usually termed sulph-
fatty acid. There are a series of these compounds such as sulpho-stearic acid,
sulpho-palmetic acid, sulpho-oleic acid, etc., depending on the fat or oil employed
in their formation. This reagent is very simply prepared by treating oleic acid
of commerce with an excess of concentrated sulphuric acid preferably at a tempera-
ture near the boiling point of water. Then adding water and skimming off the
reagent. Any neutral oil treated in this manner will produce such a reagent, some
of course being more active than others. I add the water to wash out the excess
of sulphuric acid, to prevent the discoloration of the fats.
This sulpho-fatty acid is somewhat unstable, and readily decomposes and
separates into its component parts, and in preparing the same but a small per cent.
of the ingredients used are converted into the sulph-fatty acid, so that there is a
large per cent. of waste. I have discovered a new chemical compound adapted
to perform the same functions as the sulpho-fatty acid in my glycerine process,
which is stable in character under ordinary circumstances, can be more cheaply
prepared, and is not so liable to discoloration as the sulpho-fatty acid described. To
produce this compound I preferably mix a fatty acid, such as oleic acid of commerce,
with any member of the aromatic series such as benzol, phenol, naphthaline, etc.,
substantially in the proportion of their molecular weights, as that proportion gives
the most economical results, I then treat the mixture with sulphuric acid, allow it
to stand until the reaction has occurred and then I add water to wash out the
excess of sulphuric acid, and the resultant compound separates out and forms on
I have found
top of the acid as a clear oil, which can be readily removed for use.

page_text: that this oil is a distinct chemical compound and believe it to be entirely new.
It is a double compound of the sulphonic radical with the fatty acid and the
aromatic body, and I have termed this new reagent, a sulpho-fatty-aromatic com-
pound. Of course there is a series of these compounds corresponding to the
members of the fatty acid series and of the 'aromatic series which are treated with
the sulphuric acid and which are united by the double reaction with the sulphonic
radical into a distinct class of chemical compounds.
This reagent besides being the equivalent of the sulphofatty acid used in my
process of preparing glycerine which I shall next describe, is capable of an extended
use in the arts, and produces better results than the sulpho-fatty acids in proportion
to its greater stability.
The following
and fatty acids....
the preferred form of separating the fats or oils into glycerine
Take an open tank, place in it a charge of melted fat or oil, add che per cent.
of the reagents above described, either the sulpho-fatty acid, or the sulpho-fatty-
aromatic compound, then mix the charge thoroughly, add fifty rer cent. of water
and boil the charge, preferably by the open steam process which supplies the
water lost by evaporation. The length of time of boiling depends somewhat upon
the amount of the reagent used.. When one per cent. is used the boiling should
be continued from 12 to 20 hours. When five per cent. is used, from 5 to 12 hours.
The objection to using a larger per cent. is simply one of cost, but it can be re
claimed and used over again, as hereafter explained.
After the boiling has been completed the glycerine and water are drawn from
the bottom of the tank..
" 1. 1
The reagent is also present in the liquid and is separated by precipitation. This
may be accomplished by the use of sulphuric acid or a metallic oxide or salt, such
as lime or alum. When sulphuric acid is used the reagent is precipitated from
the glycerine and water by lime. When lime is used it goes down with the reagent
leaving the glycerine water pure. The lime is then removed from the reagent
by a strong acid.
If the fat to be treated contains no free fatty acid it may be necessary to add
some in order to increase the solubility of the reagent in the fat.
The finished fatty acids are run off from the tank and are ready for use in soap
or candle factories. They may be of course refined by the ordinary process for
further uses.
There are many variations which may be used in carrying out this.. process.
More water may be used, but the smaller amount of water used the less evapora-
tion is required to reclaim the glycerine. After the first boiling I sometimes draw
off the water and add a second charge of water and then boil the charge for a few
hours, then draw off this liquid and use it as the first liquid for boiling of, a first
charge of tallow mixed with the reagent as first described.
It is not absolutely essential to boil the charge as the separation will take place
below the boiling point of water if the charge be well agitated. Of course this
operation can be carried on by boiling the charge under pressure, but it is objection-
able in that it adds to the cost without a corresponding benefit.
Another modification of my process would be to add the reagent direct to the
water and then thoroughly mix the melted tallow or oil with the water, but this
is not so quick as the first described method.
The above process is simple, cheap and effective. It can be carried on without
expensive apparatus as in the digester process. The reagent employed can be
chiefly reclaimed and used over and over again. A larger per cent. of the fatty
acids are obtained by this process, and they are purer and much less discolored
than by the ordinary acid process employed for the same purpose.
Also the glycerine is produced without material discoloration and no further
refining either of the glycerine or of the fatty acids is required, which alone is
a material saving over the older processes. No expensive machinery is necessary
the repairing of which is generally an item of considerable. expense.,, And, in

page_text: general my process is cheaper, simpler and more effective than any process to my
knowledge heretofore used.
Having now particularly described and ascertained the nature of my said
invention and in what manner the same is to be performed, as communicated to
me by my foreign correspondent, I declare that what I claim is:-
1. The process of separating fats or oils into glycerine and fatty acids, which
consists in mixing a reagent of the sulph-fatty acid series with fat and water, then
subjecting the charge to the action of heat, substantially as described.
2. The process of separating fats or oils into glycerine and fatty acids which
consists in mixing a reagent of the sulpho-fatty-aromatic acid series, with fat and
water, then subjecting the charge to the action of heat, substantially as described.
3. The process of separating fats or oils into glycerine and fatty acids, which
consists in mixing neutral fats or oils with a reagent of the sulpho-fatty acid series,
and water, then subjecting the charge to the action of heat until the substances
are separated, then drawing off the glycerine water and reclaiming the glycerine,
substantially as described.
4. The process of separating fats or oils into glycerine and fatty acids, which
consists, in mixing neutral fats or oils with a reagent of the sulpho-fatty-aromatic
series, then subjecting the charge to water and heating the mixture until the sub-
stances are separated, drawing off the glycerine water and reclaiming the glycerine,
substantially as described.
5. A sulpho-fatty-aromatic compound, substantially as described.
6. A chemical compound consisting of a molecular union of the sulphonic
radical with a member of the fatty acid series, and a member of the aromatic series,
substantially as described.
7. A chemical compound formed by a double reaction of sulphuric acid upon a
mixture of a fatty acid and a member of the aromatic series, substantially as
described.
8. The process of producing a sulph-fatty-aromatic compound which consists
in mixing a member of the fatty acid series with a member of the aromatic series,
and treating the mixture of sulphuric acid, substantially as described.
9. The process of separating fats into glycerine and fatty acids which consists
in mixing neutral fats or oils with a reagent of the sulpho-fatty acid series or of
the sulpho-fatty-aromatic series, with water, then subjecting the charge to the
action of heat until the substances are separated, then drawing off the glycerine
water and reclaiming the reagent from the glycerine water, substantially as
specified.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, W.C., Agents for the Applicant.