IMPROVEMENTS IN THE TREATMENT OF CERTAIN RESIDUES IN ORDER TO OBTAIN FATTY ACIDS THEREFROM
Year: 1866

page_text: LETTERS PATENT to Robert Irvine, of Magdalen Bridge, in the County
of Mid Lothian, North Britain, Chemist, and Peter Brash, of Leith, in
the same County, Soap and Candle Manufacturer, for the Invention of
"IMPROVEMENTS IN THE TREATMENT OF CERTAIN RESIDUES IN ORDER TO
OBTAIN FATTY ACIDS THEREFROM."
Sealed the 18th January 1867, and dated the 19th July 1866.
PROVISIONAL SPECIFICATION left by the said Robert Irvine and Peter
Brash at the Office of the Commissioners of Patents, with their Petition,
on the 19th July 1866.
We, ROBERT IRVINE, of Magdalen Bridge, in the County of Mid Lothian,
North Britain, Chemist, and PETER BRASH, of Leith, in the same County,,
Soap and Candle Manufacturer, do hereby declare the nature of the said
Invention for "IMPROVEMENTS IN THE TREATMENT OF CERTAIN RESIDUES IN ORDER
TO OBTAIN FATTY ACIDS THEREFROM," to be as follows:-
This Invention consists in treating the material known as "cotton seed.
foots," or the residuum containing the impurities separated from the oil
expressed or extracted from cotton seed in its purification by means of alkalies
or alkaline earths, for the purpose of obtaining the fatty acids present therein
in a pure or nearly pure state. For this purpose we treat the cotton seed
foots with any of the acids known as sulphuric, nitric, bydrochloric, or.
phosphoric acids, either alone or with mixtures of the same.

page_text: In the first operation we have for our object the neutralization of the
alkali or alkaline earth which has been made use of to effect the purification
of the oil, and which is combined or mixed with the fats or fatty acids present,
as also colouring matters and resin. When sufficient acid has been employed
the alkali or alkaline earth present combines with the above-mentioned acids,
forming a salt or salts therewith, and the impure fatty acid matters rise to the
surface, forming a layer on the surface on account of their low density, and
the resulting alkaline or alkaline earthy salts either dissolve in the water or
sink to the bottom.
In order to carry out our Invention we employ a metallic pan, heated either
by means of fire or by steam, and after the acid solution and the foots have
been thoroughly incorporated and mixed in a heated state, the separation of
the salt or salts formed takes place, and the watery solution is drawn off by
means of a cock at the bottom of the pan. The crude fats or fatty acids
mixed with resins and coloring matters resulting being contained in a pan are
subjected to a heat of from 250 to 400% Fahrenheit (with from 2 to 7% of
sulphuric aci. or. vitriol) for about 4 hours, with agitation, during which period
the undecomposed fats are decomposed into fatty acids, sulphurous acids being
at the same time evolved, and when the operation is completed the acidified
materials should present a rich blue color. This is now washed with water
heated by means of a jet of steam, and after drying is subjected to distillation
by means of fire and superheated steam, as is commonly employed in and
for the distillation of fatty acids. During the above process of heating the
crude fatty matters with sulphuric acids the resin present is precipitated to
the bottom of the pan, and may be recovered by means of alkalies or lime and
distillation.
We find in practice that a modification of the above process may be adopted,
we thus sometimes heat the cotton foots in a common boiler by means of fire
or steam heat until 50% or thereabout of the water has been evaporated off,
such water being present in the alkaline solution employed for the purification
of the cotton oil originally, and we find that during this evaporation of the
water contained in the foots the fats: are entirely saponified or combined with
the alkaline material used, and any glycerine present is separated, and may be
recovered in the subsequent process when the soap is decomposed. The
crude dark colored soap thus obtained we neutralize ör decompose with any
of the acids before mentioned, by which means we procure the crude fatty
acids. The products obtained by either of these processes are distilled by
means either of direct fire and steam, either at 212 degrees, or heated to a
higher temperature, as is commonly adopted for the distillation of fatty acids,

page_text: but in such case the distillation is only carried far enough to separate the fatty.
acids from the resin or resins contained in the foots, the latter requiring a
higher temperature to bring them over than is required by the fatty acids.
SPECIFICATION in pursuance of the conditions of the Letters Patent, filed
by the said Robert Irvine and Peter Brash in the Great Seal Patent
Office on the 19th January 1867.
TO ALL TO WHOM THESE PRESENTS SHALL COME, we, ROBERT
1BVINE, of Magdalen Bridge, in the County of Mid Lothian, North Britain,
Chemist, and PETER BRASH, of Leith, in the same County, Soap and Candle
Manufacturer, send greeting..
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Nineteenth day of July, in the year of our Lord
One thousand eight hundred and sixty-six, in the thirtieth year of Her
reign, did, for Herself, Her heirs and successors, give and grant unto us,
the said Robert Irvine and Peter Brash, Her special license that we, the said
Robert Irvine and Peter Brash, our executors, administrators, and assigns, or
such others as we, the said Robert Irvine and Peter Brash, our executors,
administrators, or assigns, should at any time agree with, and no others, from
time to time and at all times thereafter during the term therein expressed,
should and lawfully might make, use, exercise, and vend, within the United
Kingdom of Great Britain and Ireland, the Channel Islands, and Isle of
Man, an Invention for "IMPROVEMENTS IN THE TREATMENT OF CERTAIN RESIDUES
IN ORDER TO OBTAIN FATTY ACIDS THEREFROM, upon the condition (amongst
others) that we, the said Robert Irvine and Peter Brash, our executors and
administrators, by an instrument in writing under our bands and seals, or
under the hand and seal of one of us, should particularly describe and ascer-.
tain the nature of the said Invention, and in what manner the same was to
be performed, and cause the same to be filed in the Great Seal Patent Office.
within six calendar months next and immediately after the date of the said
Letters Patent.
"
NOW KNOW YE, that we, the said Robert Irvine and Peter Brash, do.
hereby declare the nature of our said Invention, and in what manner, the
same is to be performed, to be particularly described and ascertained in and
by the following statement, that is to say:-
Our said Invention consists in treating the material known as "cotton
seed foots," or the residuum containing the impurities separated from the oil

page_text: expressed or extracted from cotton seeds in its purification, by means of
alkalies or alkaline earths, for the purpose of obtaining the fatty acids present
therein in a pure or nearly pure state. For this purpose we treat the cotton
seed foots with any of the acids known as sulphuric, nitric, hydrochloric, or
phosphoric acids, either alone or with mixtures of the same, and the pro-
portion in which such acids are to be employed will depend upon the degree
of alkalinity of the foots to be operated upon.
In the first operation we have for our object the neutralization of the
alkali or alkaline earth which has been made use of to effect the purification
of the oil, and which is combined or mixed with the fats or fatty acids present,
as also colouring matters and resin. When sufficient acid has been employed
the alkali or alkaline earth present combines with the above-mentioned acids,.
forming a salt or salts therewith, and the impure fatty acid matters rise to the
surface, forming a layer on the surface on account of their low density, and
the resulting alkali or alkaline earthy salts either; dissolve in the water or sink
to the bottom.
In order to carry out our Invention we employ a metallic pan, heated either
by means of fire or by steam, and after the acid solution and the foots have
been thoroughly incorporated and mixed in a heated state the separation of
the salt or salts formed takes place, and the watery solution is drawn off by
means of a cock at the bottom of the pan. The crude fats or fatty acids
mixed with resins and coloring matters resulting being contained in a pan, are
subjected to a beat of from 250 to 400 Fahrenheit, with from 2 to 7 per cent. of
sulphuric acid or vitriol, for about 4 hours with agitation, during which period
the undecomposed fats are decomposed into fatty acids, sulphurous acid being
at the same time evolved. When the operation is completed the acidified
materials should present a rich blue color. These are now washed with water
heated by means of a jet of steam, and after drying are subjected to distillation
by means of fire and superheated steam, as is commonly employed in and for
the distillation of fatty acids. During the above process of heating the crude
fatty matters with sulphuric acid, the resin present is precipitated to the bottom
of the pan, and may be recovered by means of alkalies or lime and distillation.
We find in practice that a modification of the above process may be adopted.
Thus sometimes we heat the cotton foots in a common boiler by means of fire
or steam heat until fifty per cent. or thereabout of the water has been
evaporated off, such water being present in the alkaline solution employed for
the purification of the cotton oil originally, and we find that during the
evaporation of the water contained in the foots the fats are entirely saponified
or combined with the alkaline "material used, and any glycerine present is

page_text: separated and may be recovered in the subsequent process when the soap is
decomposed. The soap thus obtained we neutralize or decompose with any
of the acids before mentioned, by which means we liberate the crude fatty
acids. The products obtained by either of these processes are distilled by
means either of direct fire and steam, either at 212 degrees Fahrenheit, or
heated to a higher temperature, as is commonly adopted for the distillation of
fatty acids, but in such case the distillation is only carried far enough to
separate the fatty acids from the resin or resins contained in the foots, the
latter requiring a higher temperature to bring them over than is required by
the fatty acids.
Having now described and particularly ascertained the nature of our said
Invention, and the manner in which the same is or may be used or carried
into effect, we would observe in conclusion, that what we consider to be novel
and original, and therefore claim as the Invention secured to us by the
herein-before in part recited Letters Patent is,―
1st, the treatment of cotton seed foots or residues for the purpose of
obtaining the fatty acids contained therein, in the manner herein-before
described.
2nd, the saponification of the foots or residues herein-before mentioned
by concentrating the residual alkaline leys mixed therewith and resulting from
the purification of cotton oil, and the subsequent treatment of the saporified
and other products thus obtained, in the manner herein-before described.
In witness whereof, I, the said Peter Brash, on behalf of myself and
the said Robert Irvine, have hereunto set my hand and seal, the
Seventeenth day of January, One thousand eight hundred and sixty-
seven.
PETER BRASH. (L.S.)