IMPROVEMENTS IN THE UTILIZATION OF RESIDUES OBTAINED IN THE REFINING OF COTTON SEED OIL AND IN VALUABLE PRODUCTS OBTAINED THEREFROM
Year: 1882

page_text: LETTERS PATENT to James Longmore of Liverpool in the county of Lancaster
"
for an Invention of IMPROVEMENTS IN THE UTILIZATION OF
RESIDUES
OBTAINED IN THE REFINING OF COTTON SEED OIL AND IN VALUABLE PRODUCTS
OBTAINED THEREFROM
"
PROVISIONAL SPECIFICATION left by the said James Longmore at the
Office of the Commissioners of Patents on the 16th November 1882.
" IMPROVEMENTS IN
JAMES LONGMORE of Liverpool in the County of Lancaster,
THE UTILIZATION OF RESIDUES OBTAINED IN THE REFINING OF COTTON SEED OIL
AND IN VALUABLE PRODUCTS OBTAINED THEREFROM
"
In the refining of Cotton Seed Oil, the oil is treated with Caustic Soda, when a
mucilaginous precipitate of Soapy matter technically called " Mucilage" is thrown
down carrying with it the colouring matter contained in the oil.
This substance has hitherto been chiefly used in the arts as a rough Soap or
adulterant of Soap or for the manufacture of Stearine therefrom.
My invention is designed for the purpose of utilizing this article by extracting
valuable matters therefrom chiefly Refined Soap and Colouring Matters.
My invention consists essentially of forming a solution of the Mucilage by
melting; adding water or soda lye, Caustic or carbonate and thereby, or by means
of common Salt or other known separant, effecting the separation of the Soap;
the colouring matter is dissolved and remains in the excess of liquor, which can
then be removed by means of a filter or drawn or pumped off and treated as
hereinafter stated.
The process I at present prefer to adopt is as follows:
The Mucilage is placed in a suitable vessel, and saponification completed by
boiling with an excess of Caustic Soda Lye of the requisite strength; or should the
Mucilage used contain an excess of water, the soda can be added solid in that case
the Greenbank Alkali C, may be found preferable. the Soap is then separated by

page_text: means of Common Salt, Carbonate of Soda or other known separant, or if the Lyes
The Lyes
be used sufficiently strong, the addition of Salt et cetera is unnecessary.
which contain in solution the colouring matter are then allowed to settle by standing
and can be drawn or pumped off and the preceding operations repeated until the
required degree of purity of the Soap and extraction of the colouring matter is
reached when the soap can be finished into bars or otherwise in the usual manner;
or treated with dilute mineral or other acid and the fatty acids skimmed off as
they rise.
--
After Saponification is effected and in the concluding operations, boiling may be
dispensed with, and Carbonate substituted for Caustic Soda to effect the solution of
the colouring matter if found advantageous.
Should the Mucilage bave been made with Potash or should a Potash Soap be
required, strong Potash Lyes must be substituted for Soda in the foregoing operations
and any use of Common Salt et-cetera dispensed with. The processes before given
will also be found applicable to other classes of dark soaps
After filtration (if thought necessary) the Lyes are neutralized with a suitable
acid, such as acetic, sulphuric or hydro-chloric, or with an alum or calcium salt, such
as alum, sulphate or acetate of alumina or calcium chloride whereby the colouring
matter is precipitated.
The lake or precipitate formed as the case may be is collected on a filter washed
and dried.
The colouring matter being removed if desirable the liquor is freed from any
excess of acid, by means of chalk or other form of calcium and evaporated till a
large quantity of its component salts have crystalized out when the remaining
mother liquor is added to a fresh batch of liquor and is treated anew.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent filed
by the said James Longmore in the Great Seal Patent Office on the
16th May 1883.
JAMES LONGMORE of Liverpool in the county of Lancaster
"IMPROVEMENTS
IN THE UTILIZATION OF RESIDUES OBTAINED IN THE REFINING OF COTTON-SEED
OIL, AND IN VALUABLE PRODUCTS OBTAINED THEREFROM
"
In the refining of Cotton Seed Oil, the oil is treated with Caustic Soda, or
Potash, when a mucilaginous precipitate of Soapy matter technically called
mucilage," is thrown down, carrying with it the coloring matter contained in
the oil.
#
This substance has hitherto been chiefly used in the arts as a rough soap, or
adulterant of soap, or for the manufacture of Stearine therefrom.
My invention is designed for the purpose of utilizing this article, by extracting
valuable matters therefrom, chiefly Refined Soap and Colouring Matters.
My invention consists essentially in forming a solution of the mucilage by
melting or the addition of water, then adding sufficient caustic alkali to complete
the saponification and separate the soap from the lye thus formed. The lye which
contains nearly all the coloring matter in solution is drawn off, and fresh water
added until the soap again dissolves or as it is technically termed "closes," when
it is again separated with caustic lye, and the alkali removed. The process if
necessary is repeated three or four times, until the coloring matter is sufficiently
removed. The slightly colored lyes of the latter washings can be used for the first
operation with fresh mucilage, it first being dissolved as directed, and the lyes
being increased to the strength necessary to form the soap and separated as here-
after described.
The process I prefer to adopt at present is as follows.
The mucilage is placed in a suitable vessel, and if as is usually the case, it
contains sufficient water to form the excess of lye necessary for its formation into
soap, and the solution of the coloring matter, it is melted by the application of heat,
without further addition of water Caustic Soda Lye of the strength of 30 to 50
degrees Twaddle, or preferably to avoid unnecessary increase of water and as
furnishing a better result powdered caustic soda such as that supplied by the
Greenbank Alkali Works Co. Limited St Helens Lancashire, is then added in suc-
cessive portions (time being allowed between each addition for it thoroughly to
dissolve and amalgamate) until saponification is completed, the additions being
continued until the soap separates from the lye and is well open.
If the mucilage be of good consistence and contain little water, sufficient is added
to dissolve and melt it and the process proceeded with as above, the saponification
and separation being effected by means of lyes or if the whole amount of water
necessary to form the requisite lyes be added in the first instance the powdered
solid caustic can be used. The lye which contains in solution the coloring matter,
is separated by settling and decantation or by filtration.
To further purify the soap and free it from any remaining coloring matter, water
is then run in until the soap dissolves and technically "closes" fresh caustic or lye
of about 20° to 30° Twaddle is again added and the operation repeated till the
soap is sufficiently refined. It is then finished into bars or otherwise in the usual
manner, or treated with dilute mineral acids and the fatty acids skimmed off as
they rise.
It will be seen from the foregoing that the ordinary use of salt in separating
soap from its solution is avoided, owing to its lessening the solubility of the
coloring matter in alkaline lyes, thereby materially retarding the operations. If

page_text: used to excess in lyes of ordinary strength it quite destroys the said solubility, a
little may be used however in assisting the separation without much harm, but is
not to be recommended, as it has also a deleterious effect upon the coloring matter
itself. After the extraction of the coloring matter it can of course be used in the
ordinary way to finish with. Soap being insoluble in alkaline lyes above a certain
strength that is about 10 to 14 Twaddle, to separate it from the excess of water
added will require that water being brought up to the strength named by the
addition of caustic and it will therefore be seen that the quantity of lyes to be
used will vary in exact proportion to the water contained in or used with the
mucilage or soap, the strength of course being greatly a matter of choice, a strong
lye requiring less in quantity to effect the separation and vice versa. I do not
recommend however the use of above 80 degrees Twaddle and prefer it at the
strengths already named.
The removal of the coloring matter will be greatly facilitated if after the first
operation or at any subsequent stage the soap is what is technically called "fitted"
that is it is dissolved or closed by the addition of water and the head or fob boiled
out the whole being allowed to remain quiescent for 2 days when the usual separa-
tion takes place, the excess of alkali together with the coloring matter being carried
down and is contained in the lower stratum of soap or technically nigre which is
then removed and can be treated with a fresh batch of mucilage the soap being
operated upon as before.
Should the mucilage have been made with potash or should a soft soap be
required Potash Lyes must be substituted for soda in the foregoing operations
though of course the saponification of a Potash Mucilage can be completed with
Soda and vice versa.
The strongly dark colored lye when drawn off is filtered and either super-
saturated with carbonic acid or neutralized with acetic sulphuric or hydrochloric
acid or with an alum sulphate or acetate of alumina, or soluble calcium salt such
as chloride of calcium and the coloring matter precipitated.
The Lake or precipitate formed as the case may be is collected on a filter washed
and dried.
The coloring matter being removed the liquor is freed from any excess of acid
other than carbonic acid by means of chalk or other form of calcium and evaporated
till a large quantity of its component salts have crystallized out when the remaining
mother liquor is added to a fresh batch of liquor and is treated anew.
Having now described my invention and the best mode known to me of carrying
it into effect, I claim as my invention secured to me under the letters patent.
1
The manufacture of purified soap or fatty acids from cotton seed oil refuse
substantially as herein described.
2nd In the manufacture of soap from the residues obtained from cotton seed
oil the use of powdered caustic soda added by degrees until the soap opens
substantially as described.
3rd The extraction of a coloring matter or dye from cotton seed oil residues
by dissolving them substantially as described, and then causing a separation of
the soap by the addition of caustic alkali,
4th As a new article of manufacture the herein described coloring matter
extracted from cotton seed oil soap, or mucilage.
In witness whereof I the said James Longmore have hereunto set my hand
and seal this Eleventh day of May in the year of our Lord one thousand
eight hundred and eighty three.