IMPROVEMENTS IN OR RELATING TO THE TREATMENT OF COTTON SEED OIL MUCILAGE AND OTHER FATTY MATERIALS CONTAINING PROVISIONAL
Year: 1883

page_text: LETTERS PATENT to James Longmore of Liverpool in the county of Lancaster
for an Invention of "IMPROVEMENTS IN OR RELATING TO THE TREATMENT OF
COTTON SEED OIL MUCILAGE AND OTHER FATTY MATERIALS CONTAINING
PROVISIONAL SPECIFICATION left by the said James Longinore at the
Office of the Commissioners of Patents on the 15th August 1883.
JAMES LONGMORE of Liverpool in the county of Lancaster
"IMPROVEMENTS
IN OR RELATING TO THE TREATMENT OF COTTON SEED OIL, MUCILAGE AND OTHER
FATTY MATERIALS CONTAINING EXTRACTIVE COLOURING MATTERS FOR THE
OBTAINING OF VALUABLE PRODUCTS THEREFROM
This invention is applicable in whole or in part to Cotton seed oil, its mucilage
or soap, and to Palm oil or soap made, therefrom. I will describe the process for
the manufacture of soap from cotton seed oil mucilage.
The fatty acids are first freed from the excess of water and other matters
contained in the Mucilage by acidification with sulphuric or hydrochloric acid;
acetic acid, nitric, and one or two other acids can be used with care in place of
these, but they are not so advantageous. The mucilage if sufficiently weak or
unsaponified to be in a liquid state, can be allowed to stand for a time and the
free oil or partially saponified oil rising to the surface can be skimmed off.
The black fatty acids as prepared by either of above methods are then saponified
with caustic soda lye from forty to eighty degrees Twaddle and the resulting
soap separated by using an excess of caustic lye as described in the specification
of my patent No. 5465 dated 16th November 1882.
Caustic soda lye can be replaced as a separant by carbonate of soda.
The great bulk of the colouring matter having been removed in one or two first
operations with caustic lye as described in specification of my patent aforesaid,
further decolourization inay be effected by the following processes; these can
however be applied at a previous stage, but in practice it will be found better to
proceed as directed above. They are applicable also to bleaching cotton seed oil,
palm oil, palm oil soap, and other like matters. The partially decolourized soap is
boiled in the close state for some time with five to ten per cent or a greater or less
percentage of finely powdered per oxide or bydrated per oxide of manganese, and
the fatty acids then liberated and bleached by decomposing the soap and manganeso
by boiling with sulphuric or hydro-chloric acid. The quantity sufficient being
Drine AJ1

page_text: found by adding acid, a little at a time, till the soap is decomposed and the fatty
acids rise. The boiling of the soap with the manganese can be conducted under
pressure and by reason of the higher temperature etcetera thus obtained, a better
bleaching is effected. The great bulk of the manganese can be recovered without
decomposition if desired by allowing it to precipitate from the soap by standing, or
the soap can be opened to a curd, and the manganese withdrawn with the lye. In
either case to thoroughly remove the manganese and effect the bleaching,
decomposition with acid will be necessary.
Another method is to bleach the fatty acids obtained by acidifying the partially
decolourized soap before described, with bichṛonate of potash or other known
oxidizing agent or by agitation with a mixture of per oxide of manganese and
hydrochloric acid, or by common salt, oxide of manganese, and sulphuric acid. The
blenching of the raw or partially decolourized cotton seed oil mucilage, soap, crude
cotton seed oil soap, palm oil soap, and other similar materials can also be effected
by the addition of chlorine gas, pure or preferably diluted or chlorine water to the
soap while in the close state. It will be seen that many variations of this method
of bleaching can be made; a greater quantity of gas can be combined with the
water by means of pressure, or the operation can be conducted in a close vessel
into which a certain amount of the soap and gas or soap and chlorine water can be
forced, and the agitation effected by boiling or mechanical means, or the chlorine
gas may be condensed to a liquid state and used in that form..
The soap either immediately after saponification or after being partially
decolourized as described, can be freed of colour by the addition of chalk, carbonate
of lime, or other inert material in a finely ground state. The process is as follows;
a quantity of finely powdered chalk etcetera is added to the soap while in the close
state and well incorporated by boiling or mixing. The chalk when in sufficient
quantity has the effect of causing the soap on the addition of salt or strong caustic
lye to separate in a state of fine division, and thus yield up its colour more readily
than when soparated in the ordinary manner or as described in the specification of
my said patent No 5465 of 1882. When salt is used in separating, the lyo must be
sufficiently alkaline to effect the solution of the colouring matter. The lye is to bo
separated by allowing the whole to stand and decanting, or by means of a vacuum
filter or filter press.
The operations of closing the soap with water and opening with lye is to be
repeated until the soap is quite decolourized.
Economy in labour can be effected by combining the vacuum filter and mixing
vessel in one; a perforated false bottom or other similar apparatus covered with a
filtering medium can be fixed in the bottom of the copper or vessel used, and the
lees after separation pumped through. The first portion pumped out, if it consists
of unseparated soap that may have filtered through during the process, is returned
immediately to the copper before the pumping off is completed; during the pumping
off to prevent the filter bed becoming choked by the soap and lime settling on it,
the contents of the vessel should be kept agitated
When the mixture of soap, chalk, etcetera is decolourized, the soap can be
dissolved to as thin a solution as practicable and the earth used removed by
filtration; the dissolved soap can then be made into curd in the usual manner;
or the mixed soap, chalk, etcetera can be treated with sulphuric or hydrochloric
acid and the resulting fatty acids separated for use. Chloride of Calcium
formed in this process can be recovered by evaporation and crystallization.
The manufacture of the colouring inatter and the recovery of the lyes used, is
described in specification of my said Patent No. 5465 of 1882, when the latter is
offected by supersaturation with carbonic acid the resulting carbonate of soda can
bo recausticized with lime in the usual manner.
For the manufacture of Potash soap from mucilage, potash lyes must be
substituted for soda in the operations described

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent and of
an Order of the Lord Chancellor filed by the said James Longmore in tho
Patent Office on the 23rd February 1884.
JAMES LONGMORE of Liverpool in the county of Lancaster
"IMPROVEMENTS
IN OR RELATING TO THE TREATMENT OF COTTON SEED OIL, MUCILAGE AND OTHER
FATTY MATERIALS CONTAINING EXTRACTIVE COLOURING HATTERS FOR THE
OBTAINING OF VALUABLE PRODUCTS THEREFROM
This invention is applicable in whole or in part to crude cottonseed oil or soap
(from damaged or good oil) or cotton seed oil mucilage.
The following describes the method of refining cottonseed oil mucilage :—
;
In the refining of crude 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 colouring matter contained in
the oil,
"
In the specification of my patent dated November 16th 1882, No 5465, I described
a method of obtaining from mucilage à refined brown soap (suitable for dyers' use)
also a dye or colouring matter.
My present invention consists of the preparation from mucilago of refined soap
or fatty acids of a white or yellow colour, essentially by bleaching the brown soap
previously obtained; also of improvements in the manufacture of the brown soap.
For the purposes of this invention the mucilage to be operated upon must be
free, or nearly free from albuminous compounds; these when present consist of the
finely ground portions of cotton sced which pass into the crude oil in the operation
of expression, and in the process of refining into the mucilage.
The most effective and simplest method of dealing with this substance is to
remove it from the crude oil before refining, by allowing the latter to stand until
the seed has deposited, or elso by methods of filtration. It can also be removed
from the mucilage by melting the latter at a low temperature and then standing it
until cold, the excess liquor of the mucilage is by this means separated and contains
the majority of the cotton seed in solution with a small portion of grease which is
rejected. Or the mucilage can be decomposed with acid at a temperature not
exceeding 90° to 100° Fahrenheit and the resulting grease and albuminous matter
treated with bisulphide of carbon, naptha or methyl alcohol by which means the
grease is dissolved out and the albuminious matter separated. The dissolving agent
is then distilled off in the usual manner.
These latter methods however are uncertain and troublesome, as compared with
that of previously treating the oil before it is refined.
It is essential that the mucilage should be freed from albumen for the reason
that the presence of the latter has the effect of preventing the separation by means
of caustic lye of soap from its solution; the effect varies with the proportion of
albumen present.
The mucilage is now treated as described in the specification of my patent
No 5465 November 16th 1882, if the percentage of grease, it contains is as high as
say 40 to 50 per cent; otherwise it will generally be found more economical to
first decompose and treat it as below:-
The mucilage is decomposed with sulphuric or hydrochloric acid (taking care to
use no excess of acid) and the resulting fatty acids after being allowed to settle and
the liquor drawn off, saponified with caustic soda lye of from 20 to 40 degrees
Twaddle (varying according to the percentage of water the fatty acids may contain)
the additions of lye being continued until the soap separates from excess and is

page_text: well
open; the whole is allowed to stand until the excess lye which contains the
principal portion of the colouring matter in solution has thoroughly subsided. The
time required is from one to three nights according to the quantity of the material
operated upon.
The brown soap thus obtained (and with which my previous process ended) is
further refined into pure soap or fatty acids by the following processes :-
No. 1. The soap either immediately after saponification or after being partially
decolourized as described can be freed of colour by the addition of chalk, carbonate
of lime or other inert material in a finely ground state. The process is as follows:
a quantity of finely powdered chalk, etcetera is added to the soap while in the close
state, and well incorporated by boiling or mixing. The chalk when in sufficient
quantity has the effect of causing the soap on the addition of salt or strong caustic
lye to separate in a state of fine division, and thus yield up its colour more readily
than when separated in the ordinary manner, or as described in the specification of
my said patent N° 5465 of 1882. When salt is used in separating the lye must be
sufficiently alkaline to effect the solution of the colouring matter. The lye is to
be separated by allowing the whole to stand and decanting or by means of a
vacuum filter or filter press. Where chlorine water is afterwards used however as
further described, this addition of chalk or other inert powder is of little use and
can be dispensed, with,
No. 2. The soap is melted or dissolved and if an inert powder. has been used the
said powder is filtered out or allowed to subside.
While the dissolved soap is boiling, chlorine water or bleaching powder made
into a cream with or dissolved in water is to be added gradually in portions until
the soap is bleached to the colour that may be considered sufficient or desired at
the time. For the full effect 5 to 10 per cent or more of bleaching powder will bo
required.
If chlorine water is used, the soap should contain a slight excess of caustic;
after the bleaching is completed the soap is to be finished in the usual manner
with salt.
'
If bleaching powder is used it will on completion of the operation be necessary
to decompose the resulting mixed lime and soda soap into fatty acids, with
sulphuric or hydrochlorine acid in the usual manner.
A larger quantity of chlorine gas can be combined with water by pressure and
unnecessary dilution of the soap thus avoided.
No. 3. The soap is melted or dissolved and an excess of caustic added (but
insufficient to open it), while boiling 5 to 10 per cent of finely powdered peroxide
or hydrated peroxide of manganese is to be incorporated and kept well mixed with
the soap for two or three hours; a manganate of soda is thus formed and the
colouring matter more or less bleached. The excess of manganese can be removed
by opening the soap to a curd and withdrawing it with the lye. The soap has
then to be decomposed into fatty acids with sulphuric or hydrochloric acid which
completes the bleaching.
No. 4 The brown soap can be decomposed into fatty acids and the fatty acids
bleached with bichromate of potash or other known oxydizing agents.
The best method I consider to be with chlorine water or bleaching powder.
For the treatment of crude cotton seed oil or soap the oil is saponified in the
usual manner and while in the close state manganese, chlorine water or bleaching
powder added, the operation being carried out exactly as described for the soap
from mucilage. The treatment with excess of lye is not necessary. The manufacture
of the coloring matter and the recovery of the lyes used is described in the
Specification of my patent No 5465, November 16th, 1882.
Having now described my invention and the best mode known to me of carrying
it into effect, what I claim is :—
1st. The improvement in the treatment of cotton seed oil, cottonseed oil
mucilage or other similar oils containing extractive coloring matter, which consists

page_text: in saponifying, adding an indifferent powder, separating with caustic alkali and
drawing off the coloring matter in the lye.
2nd. The improvements in the treatment of cotton seed oil, cotton seed oil
mucilage or crude cotton seed oil soap, which consists in fully saponifying, separating
the bulk of the coloring matter-when there is a large amount of it by means
of caustic alkali, and bleaching the remainder by means of oxidizing or chloridizing
agents, substantially as described.
3rd. The manufacture from crude cotton seed oil, cotton seed oil mucilago or
crude brown cotton seed oil soap, of soap or fatty acids of a yellow or white color,
substantially as described.
In witness whereof I the said James Longmore have hereunto set my hand and
seal this 20th day of February in the year of our Lord one thousand eight hundred
and eighty four.