Separation of Colouring Matter therefrom.
Year: 1887

page_text: Date of Application, 15th Nov., 1887
Complete Specification Left, 15th Aug., 1888
Complete Specification Accepted, 21st Sept., 1888
to the Separation of Colouring Matter therefrom.
We, GEORGE TALL of 5, Gladstone Avenue in the City of Chester, Oilcake and
Seed Broker, and WILLIAM PHILLIPS THOMPSON of 6, Lord Street, Liverpool in the
County of Lancaster, Patent Agent for the said George Tall, do hereby declare the
nature of this invention to be as follows:-
At present cotton seed oil is deprived of its coloring matter by means of caustic
alkali. By this means a variable amount say seven and a half per cent. of the oil is
lost in the mucilage.
This invention has for its principal object a new or improved process for extracting
and utilizing the brown colouring matter from cotton seed and some other oils, and in
obtaining the oil clear and colourless, or nearly so.
In carrying out the invention, we shake up the cotton seed or other oil, or under
special circumstances, the crushed seed with a saline solution capable of uniting with,
and dissolving the colouring matter, but not of combining with the oil. We prefer
for the saline solution to use washing soda dissolved in water or a solution of mono-
carbonate of potash.
The process as at present experimentally worked is as follows:-
To one pint of crude cotton seed oil add half a pint of pure water, boil and agitate
the two together, and adding at the same time about one ounce of washing soda and
continue boiling and agitating for about thirty minutes until the crude oil is well
struck and becomes a light colour. It is then allowed to settle, the oil run into a
washing tank and again boiled and agitated with lime water until it arrives at the
colour required. It can then be brightened by acid unless required for eating
purposes. If for the latter use, it is separated by decantation and washed with pure
water, then boiled till it becomes bright.
Either before or after the lime has been used, but preferably instead of using lime
we may simply add a lot of thoroughly dried clay, preferably Fuller's Earth and stir
it up with the oil, keeping it stirred up and heated for about fifteen or twenty minutes,
then allow the clay to settle and filter, or put the whole of the clay and oil into the

page_text: filter press. On a large scale it will be better to place the oil and Fuller's Earth in a
closed pan (with diaphragms), capable of being rotated so that every time it revolves,
the oil and clay will have to fall through the diaphragms, or in place of a revolving
vat with diaphragms, a rapidly reciprocating chamber about half filled with the oil
and clay can be used.
The clay employed in this operation when it ceases to have the required effect can
be washed preferably by boiling in water, or, first in a weak caustic soda solution, and
then in water, and after drying, is, again ready for use.
The saline solution charged with colouring matter, if still containing oil, can be
purified therefrom by shaking it up with mineral naphtha, and separating the two
liquids, it is then treated with hydro-chloric acid or other precipitant of the colouring
matter and the brown floculent deposit which separates, is filtered out and can be used
as a dye with suitable mordants, with or without the addition of aniline dyes; if an
alkaline solution of the colouring matter be required the washings can be used directly
without the precipitation.
To separate the colouring matter from the seed direct, a plan we do not recommend,
the seed is first crushed then heated to coagulate the albumen, then heated with the
washing soda solution, with vigorous stirring, then drained and then pressed. The
oil, however, will still contain a considerable quantity of colouring matter, requiring
further refining, we, therefore, recommend first extracting the oil, then separating
the colouring matter, and only mention this latter plan, as a possible but much
inferior alternative to prevent others claiming it.
The concentrated solution or the dry colouring matter and soda can be used directly
as a dye solution, when an alkaline solution is required in dyeing without other
preparation than dilution. If, however, the colouring matter be required pure, it is
precipitated from the solution by hydro-chloric acid or other precipitant, washed and
dried. The colouring matter is either sold in this state or treated with other reagents
to vary the colour.
The colouring matter is also useful for fixing aniline dyes.
WM. P. THOMPSON & Co.,
Of 6, Lord Street Liverpool,
Patent Agents for the Applicants.

page_text: to the Separation of Colouring Matter therefrom.
We, GEORGE TALL of Gladstone Avenue, in the City of Chester, Oilcake and
Seed Broker, and WILLIAM PHILLIPS THOMPSON, of 6 Lord Street, Liverpool, in the
County of Lancaster, Patent Agent for the said George Tall, 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 :-
At present cotton seed oil is deprived of its colouring matter by means of caustic
alkali. By this means a variable amount, say from three to seven and a half per cent.
of the oil is lost in the mucilage. This matter that is lost too, is mostly stearine, which
is the most valuable part of the oil. This mode of depriving the oil of its colouring
matter further gives a disagreeable taste to the oil, so that it cannot be used for food
purposes without very expensive treatment.
Now, our invention is designed to avoid this waste, and to make a more perfectly
refined oil, and consists in separating the colouring matter by substances mixed
mechanically with the oil, but not combining with it, and having a greater affinity or
attraction for the colouring matter than the oil has, and so separating the colouring
matter alone from the oil.
The two substances which we prefer to use are:
1. A solution of an alkaline carbonate, preferably nearly boiling, to take the great
bulk of the colouring matter.
2. An absolutely dry, absorbent, solid material, such as thoroughly dried fuller's
earth, preferably at a temperature of 300 degrees to 400 degrees Fahrenheit.
Our process as at present carried out by us in refining ordinary black cotton seed
oil made in England, from Eastern cotton-seed is as follows:--
To each gallon of oil, we add half a pound of washing soda dissolved in half a
gallon of water, and agitate the whole together, preferably at about 100 degrees
centigrade for about 30 minutes, or until a sample of the mixture on standing divides
into a light coloured nearly transparent oil, and a brown solution. The brown liquor
is then separated and utilised as hereafter described. A second agitation of the oil
with fresh alkaline solution can be performed if desirable, but in place of this, we
prefer to add to the nearly clear oil about one quarter or half a pound of thoroughly
dry fuller's earth to the gallon, and again agitate, preferably at a temperature of about
300 to 350 degrees Fahrenheit. This fuller's earth takes up any remaining colouring
matter, and also destroys or removes a peculiar disagreeable taste, leaving the ou
almost tasteless and colourless.
Other absorbent earths and clays in an absolutely dry state can be used instead of
fuller's earth, but are none of them so efficacious.

page_text: The fuller's earth has the faculty of destroying the taste and colour of oil already
nearly deprived of its colour by mono-carbonate solution, but is not found so efficacious
with oil clarified by the use of caustic soda as ordinarily practised, as the bad taste of
that oil is not, in our experience, removed by it.
After it is found on testing, that the disagreeable taste and colour have vanished,
the oil is decanted or filtered clear of fuller's earth in a filter press, or centrifugal, or
other apparatus, and is ready for use.
The fuller's earth can be used till it is no longer effective, then well boiled at
ordinary atmospheric pressure in carbonate of soda solution with constant agitation,
and again in water to wash it, then thoroughly dried at about 300 to 400 degrees
Fahrenheit when it can be again used.
The dark solution obtained from the first washing of the oil by an alkaline carbonate
solution is used at once as a solution for dyeing various shades of brown to yellow
with a mordant, or it is treated with hydrochloric acid till the colouring matter
separates as a flocculent deposit. Some other acids or even salts, such as common salt
can be used as precipitants, but hydrochloric acid is best and on the whole, cheapest
for this purpose.
The deposit is then filtered from the solution, washed and dried, and is a valuable
colouring inatter, available for use by dissolving it in an alkaline solution, such as
carbonate of soda, and employing such mordants as are used to fix fustic and other
vegetable dyes.
In the foregoing, we have spoken only of mono-carbonate of soda solution for
washing the oil, but mono-carbonate of potash and some other combinations of
alkalies with weak acids, and having an alkaline reaction, will also act, but mono-
carbonate of soda is so much cheaper and better than the others that it is needless to
mention them.
Having now particularly described and ascertained the nature of the said inven-
tion, and in what manner the same is to be performed, we declare that what
we claim is:-
1. The process of treating crude cotton seed oil which consists in well washing it
at a suitable temperature with a solution of an alkaline monocarbonate, till the great
bulk of the colouring matter has combined with the solution, leaving the oil nearly
clear, separating the soution and precipitating the colouring matter by means of hydro-
chlori id, treating the partia ly clarific oil with well dessicate 1 fuller's earth, till
and rallying the tuber's earth by washing in
ly on the tor's arth, and then
l
with
water, sal
2. The improvement in the process of treating cotton seed oil, which consists in
agitating it with chemicals having an affinity for the colouring matter but not for the
oil, whereby the colouring matter leaves the oil and dissolves in or adheres to the
chemical, and can thus with the chemical be mechanically separated from the oil.
3. The improvement in the process of treating cotton seed oil, which consists in
agitating the oil with aqueous alkaline monocarbonate solution until the colouring
matter has been taken up by the solution, then allowing the two to stand and decanting,
substantially as described.
4. The improvement in the process of treating cotton seed oil, which consists in
agitating the oil successively with aqueous solution of monocarbonate of soda, and
with fuller's earth successively, and separating the oil from the foreign matters after
each operation, substantially as described.
3. The improvement in the process of treating cotton seed oil, which consists in
washing the crude oil with aqueous alkaline monocarbonate solution, till the greater
part of the colouring matter has left the oil, and joined the solution, then using this
solution at once as a dye solution with a mordant.
6. The improvement in the process of treating cotton seed oil, which consists in
washing the crude oil with aqueous alkaline monocarbonate solution, till the greater

page_text: part of the colouring matter has left the oil and joined the solution, then precipitating
the colouring matter with hydrochloric acid, and filtering and drying, whereby the
colouring matter is obtained in a concentrated form.
7. The improvement in the process of treating cotton seed oil, which consists in
5 regenerating the spent fuller's earth by boiling it in an aqueous solution of an alkaline
monocarbonate, substantially as described.
WM. P. THOMPSON & Co.,
Of 6, Lord Street, Liverpool,
Patent Agents for the Applicants.