IMPROVEMents in Treating Fatty SUBSTANCES CONTAINING COLORING MATTERS, AND IN OBTAINING USEFUL PRODUCTS THEREFROM
Year: 1872

page_text: LETTERS PATENT to John Thom, of Chorley, in the County of Lan-
caster, and John Stenhouse, of Pentonville, London, in the County
of Middlesex, for the Invention of “IMPROVEMents in Treating Fatty
SUBSTANCES CONTAINING COLORING MATTERS, AND IN OBTAINING USEFUL
PRODUCTS THEREFROM.”
"
Sealed the 29th October 1872, and dated the 22nd July 1872.
PROVISIONAL SPECIFICATION left by the said John Thom and John
Stenhouse at the Office of the Commissioners of Patents, with
their Petition, on the 22nd July 1872.
We, JOHN THOM, of Chorley, in the County of Lancaster, and JOHN
STENHOUSE, of Pentonville, London, in the County of Middlesex, do
hereby declare the nature of the said Invention for "IMPROVEMENTS IN
TREATING FATTY SUBSTANCES CONTAINING COLORING MATTERS, AND IN OBTAINING
USEFUL PRODUCTS THEREFROM," to be as follows :-
14
11

page_text: cipitate is formed of the fatty matter with the earthy base, and that this
precipitate carries down the greater portion of any coloring matters which
may be present in such liquors.
Our Invention consists in adding to the soap liquors obtained by
clearing or brightening woven fabrics or yarns dyed or printed with
madder and its derivatives, munjeet and its derivatives, or various kinds of
artificial alizarines solutions, as above described, of the alkaline earths or
metallic oxides, muriate of lime being preferred. The precipitates con-
sisting of fatty and coloring matters are then collected. The greater
portion of the water is removed by subsidence, or filtration, or preferably
by both combined. The colored fatty matters are treated with sulphuric
or hydrochloric acid, preferably muriatic or hydrochloric acid, at ordinary
temperatures, the resulting muriate of lime being used for a fresh
quantity of soap liquors. The fatty and coloring matters thus obtained
are heated and allowed to-cool, and are then pressed, cold, and as much
water removed by pressure as possible. The pressed mass is again
melted and put into strong cotton or other bags, and is subjected, whilst
warm, to. powerful pressure, in a hot room being preferred. This
pressure separates the greater part of the fat in a state fit for soap
making and other useful purposes. The impure coloring matter
remaining in the bags can be treated with petroleum, naphtha, benzole,
bisulphide of carbon, oil of turpentine, or similar solvents of fat by
which a further quantity of fatty matter is removed. The resulting
coloring matter, chiefly combined with oxide of iron, or with alumina, is
either steeped in the cold state, or digested at a higher temperature with
sulphuric or other strong acids, muriatic being preferred. The eliminated
coloring matter is then washed with cold water until nearly or quite
neutral. The product is then fit for dyeing or printing purposes.
It can be dried before using, but we prefer it not dried. We find that
although petroleum or other solvent removes an additional quantity of
fatty matter that it is not necessary to employ it, and that a product
quite useful for dyeing or printing purposes is obtained without petroleum
or other fatty solvents, by merely macerating or digesting the pressed
stuff with acids, and washing as above described.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent,
filed by the said John Thom and John Stenhouse in the Great
Seal Patent Office on the 22nd January 1873.
TO ALL TO WHOM THESE PRESENTS SHALL COME, we, JOHN
THOM, of Chorley, in the County of Lancaster, and JOHN STENHOUSE, of
Pentonville, London, in the County of Middlesex, send grecting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her
Letters Patent, bearing date the Twenty-second day of July, in the
year of our Lord One thousand cight hundred and seventy-two, in
the thirty-sixth year of Her reign, did, for Herself, Her heirs and
successors, give and grant unto us, the said John Thom and John
Stenhouse, Her special license that we, the said John Thom and
John Stenhouse, our executors, administrators, and assigns, or such
others as we, the said John Thom and John Stenhouse, our exe-
cutors, administrators, and 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, exer-
cise, and vend, within the United Kingdom of Great Britain and
Ireland, the Channel Islands, and Isle of Man, an Invention for
"IMPROVEMENTS IN TREATING FATTY SUBSTANCES CONTAINING COLORING MATTERS,
AND IN OBTAINING USEFUL PRODUCTS THEREFROM," upon the condition
(amongst others) that we, the said John Thom and John Stenhouse, our
executors or administrators, by an instrument in writing under our, or
one of our, or their, or one of their hands and seals, should particularly
describe and ascertain 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 im-
mediately after the date of the said Letters Patent.
NOW KNOW YE, that we, the said John Thom and John Sten-
house, do hereby declare the nature of the 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) :-
:-
It has been long known that during the clearing or brightening with

page_text: derivatives, munjeet or its derivatives, or with the various kinds of
artificial alizarine a considerable quantity of valuable coloring matter
leaves the dyed or printed goods, and remains in the waste soap liquor.
It has been also long known that by adding earthy or metallic bases, or
their salts, or solutions of such bases or salts, such as those of lime,
alumina, baryta, magnesia, to the colored waste soap liquors, such as
are above referred to, a precipitate is formed which contains fatty matters
associated with coloring matters thrown down from the waste
liquor.
Our Invention consists in the use of a process of treating precipitates
of the character above referred to, so as to recover therefrom so much of
the coloring matters as will be found valuable for dyeing purposes, and
which, having due regard to economy, it may be worth while to recover,
and also to recover in a useful form the fatty matters which were present
with the said coloring matters.
The mode in which we carry our process into practical operation will
be well understood from the following description, in which with the
object of making it completely intelligible, we will describe the entire
operation of first producing the precipitates, and then of treating them
by our process. We run a solution of muriate of lime (which we prefer)
into the waste soap liquor until no further precipitation takes place, and
the mixed liquors are then run into a pit or cistern, or we run the
solution of muriate of lime into the pit either before or after we run in
the waste soap liquors. When the pit or cistern is about full of the
said liquors milk of lime is added until free lime remains in the mixture;
about twenty gallons of milk of lime containing about forty-three pounds
of quicklime being sufficient for twenty thousand gallons of the soap
liquor, the whole being well stirred up, so as to insure a uniform mix-
ture, having a slight excess of lime. The whole is allowed to settle
about twelve hours, when the supernatant liquor is drawn off. The
precipitate contains the fatty and coloring matters previously contained
in the waste soap liquor. We then pump this precipitate or run it off into
a wooden vat or other receptacle, and add to it an acid, taking especial
care to use it in such quantity as only to decompose the compounds of
fatty matter with their base or bases, wholly or nearly so, but not in
quantity sufficient to decompose the compounds of coloring matter
with their bases. In practice we find that to thirty-five thousand eight

page_text: hundred and sixty pounds weight of this precipitate an addition of three
hundred and ten pounds, or thereabouts, of muriatic acid of commerce
containing thirty-three per cent. of dry acid, or thereabouts, is sufficient.
This is done at the usual temperature of the air.
If in any case some of the precipitates proposed to be operated upon
have already been treated with acid, we in such case examine them by
analysis or otherwise, so as to ascertain in what proportion the acid has
been employed in so treating such precipitates.
If the acid should be found to have been used in about the same pro-
portion as that above indicated the precipitate will be in a state we find
to be suitable for use according to our Invention.
If the precipitate on examination shall be found to have been treated
with too small a quantity of acid, it should be further treated with such
an additional quantity as may make it about equivalent to the proportion
above indicated as being suitable. If it shall be found that an excess of
acid has been employed so as to have removed not only the base or bases
of the fatty compound, but likewise the base or bases of the valuable
coloring compounds, then it is possible (as shewn hereafter) to add or
restore bases which will replace those removed injuriously by the excess
of acid, and such a method is in that case to a certain extent equivalent
to our process of treating the said compounds, because the mischief that
arises from the coloring matter being free from base, and so rendered
soluble in the grease or fatty matter is to some extent prevented,
though not nearly so well as by our process above described.
Having then properly prepared the precipitates by the acid treatment
which wholly decomposes the fatty compounds with their bases or nearly
so, but which does not decompose the coloring matters with their bases,
we next draw off the whole of the matter so treated on to a suitable
filter, preferring to use a flannel stretched on a wooden frame for the
filter; this filter being so placed that the liquor draining from it, and
which is chiefly a solution of muriate of lime may be run off into and
mix with a fresh quantity of soap liquor; the fatty and other materials
left on the filter are removed, and we then heat them until they have
reached such a temperature as to melt or agglutinate the colored fatty
substance; we then allow the whole to cool and then press in bags or
cloths to separate from it as much of the watery solution as possible.

page_text: The colored fatty substance removed from the bags or cloths if
thought desirable may be heated to such a temperature as to evaporate
or separate the greatest portion of the water, taking care not to raise the
temperature so as to decompose the alizarine or other valuable coloring
matters contained in the substance; in practice we prefer not to exceed
212° of Fahrenheit's thermometer.
i
In the case of treating a fatty mixture from which those portions of
the bases which existed in combination with the fat are entirely removed
and those portions of the base or bases combined with the coloring
matter are either partially or entirely removed, we proceed by reintro-
ducing a base or bases in sufficient quantity to combine with the useful
coloring matter.
The following bases may be employed for this purpose:-Lime, its
hydrate or acetate; baryta, its hydrate or acetate; strontia, its hydrate
or acetate; magnesia, its hydrate or acetate; finely powdered oxide of
lead, oxide of zinc, oxide of iron, oxide of manganese, or the acetates of
the metals just mentioned.
We find that alumina, hydrate of alumiņa, or acctate of alumina can
also be used, provided that the fat and coloring matter be made neutral
or slightly alkaline, ammonia being usually employed for this purpose.
When the coloring matter has combined with the alumina we make
the mass slightly acid by the addition of a small quantity of acetic or
other acid, and then proceed to heat it. The bases and salts which we
prefer are lime, its hydrate and its acetate, oxide of iron and its acetate,
these being cheap and effective agents.
The quantity of the above bases to be added will be dependant on the
quantity of coloring matter mixed or combined with the fatty matter.
In practise we find that the quantity of coloring matter associated
with the fat varies so much that no definite quantity of these oxides or
their solutions can be here stated, and we find it necessary to make an
experiment in order to decide upon the proper amount to add to the
mass about to be operated upon in each case.
Having added the requisite amount of a suitable base or salt, we keep
the mixture melted, but not at a higher temperature than 212 degrees
Fahrenheit, and well stirred for about an hour, when the useful coloring

page_text: matter will have combined with the base or bases introduced, leaving
the compound substantially in the same state as if only the amount of
acid necessary to combine with the base or bases of the fatty compound
and not with the base or bases of the coloring compound had been
added in the first instance.
When we employ a solution of any of the above-mentioned bases either
in water or acetic acid, we mix the colored fat with water, to which we
add the proper quantity of the dissolved base, the quantity being pre-
viously determined by experiment; we then heat the colored fat to a
temperature not higher than 212 degrees and agitate it with the solution
of the base until the color associated with the fatty matter has com-
bined with a sufficient quantity of the base to render the combination
insoluble or nearly so in the petroleum oil or other fat solvent, or in the
melted fat, when the subsequent hot pressure is performed. We then
collect the compound matter so obtained and heat it in a suitable vessel
at a temperature not exceeding 212 degrees until the whole or the
greater portion of the water has been removed. We can now extract
the whole of the free fatty matter, leaving separated so much of the
coloring matter as is practically useful for dyeing purposes; this we do
by macerating or digesting the mass with petroleum oil, naptha, benzole,
bisulphide of carbon, oil of turpentine, or similar solvents of fats, filtering
and pressing out the solution of fatty matter. The valuable coloring
matter chiefly combined or mixed with alumina, oxide of iron, lime, or
with all these or other substances, is thus obtained in a separate state,
freed or nearly so from fatty matter.
In practice however we have found it more advantageous to proceed
as follows: We heat the combined coloring matter and fatty materials,
when prepared with the requisite acid treatment as above described, to a
temperature of 212 degrees Fahrenheit's thermometer or thereabouts..
We put them into strong bags or cloths and subject them whilst hot to
a pressure in the way well known in the trade of extracting oils or fats
from solid matters containing them, until as much as possible of the
fatty matter has been squeezed out. The small quantity of fatty matter
then remaining will in practice not be found to be injurious in the
subsequent process of making a useful dye stuff from the colored
residue. If however it be thought necessary more completely to separato

page_text: the remaining portion of fatty matter, the mass remaining after hot
pressure is macerated or digested with petroleum oil or other solvents of
fat in the manner above described. In this case, as well as in the case
of separating the fatty matter by petroleum oil or other solvent of fat
without previous hot pressure, we recover the solvent by distillation in a
retort or other suitable vessel.
Whether obtained by hot pressure or by solution and separation of the
solvent by distillation, the fatty matter, when separated in the manner
above described, will be found to be somewhat colored by coloring
matters of little or no value, but it will not be found to contain alizarine
or other valuable coloring matter of madder, munjeet, or artificial
alizarine; or if it do contain such it is in so small a quantity as to be of
little or no practical importance. The fatty matter, although somewhat
colored, will be found to be capable of being profitably used for soap
making and other purposes. But if it be thought desirable to purify it
still further, it may be distilled in a retort with or without steam being
blown into it in the manner well known in the trade of making or
purifying stearic acid and other fatty matter.
We have now the valuable coloring matter separated from the fatty
matter by petroleum oil or other solvents, or by hot pressure with after
treatment. by petroleum oil or other solvents of fats, or by hot pressuro
alone, which we prefer, and we now proceed to describe the manner by
which this is purified, which however we do not claim as being of our
Invention-We put the coloring matter thus left, after having sepa-
rated wholly or nearly so the fatty matter, into a wooden or other 2
suitable vessel containing water, and add to it a suitable acid, preferring
sulphuric or muriatic acid, in such quantity as to have an excess of acid
after the macerating or boiling, and either allow the mixture to stand
until the bases are separated from the coloring matter, or we heat or
boil the mixture until we arrive at the same result. In practice we find a
that one hundred pounds of the colored pressed residue with about
twenty pounds of rectified sulphuric acid of commerce, or about sixty
pounds of muriatic acid of commerce, and about ten gallons of water,
make a suitable mixture when boiling is employed. When the mixture
is not boiled more of the acid is required. We prefer boiling the 3
mixture.

page_text: After boiling a sufficient time to produce the required results, which
is in general about two hours, the coloring matter should be washed
with cold water until all or nearly all the acid is removed, as is practised
in the making of garancine. We now drain off on a filter as much of
the water as possible, and the pasty residue, consisting of alizarine or
other coloring matter, of madder and its derivatives, or of munject
and its derivatives, or artificial alizarine mixed with other organic
matter, is left in a state suitable for dyeing or printing, or we can dry
and then grind the substance into fine powder for use in this state, or-we
can separate the pure coloring matter from the other organic matter by
alcohol or other solvents of the coloring matter of madder and its deri-
vatives, of munjeet and its derivatives, or artificial alizarine, in the
manner well known in the trade of making extract of madder.
Having now described the nature of our Invention, and the manner of
carrying it out, we wish it to be understood that we make no claim
generally to the precipitation of waste soap liquor with or without
,coloring matter by the addition of earthy or metallic salts, or earthy
oxides, or oxides of other metals, such process having been in use before
the date of this Patent; nor do we claim generally the separation of fatty
matters from solid substances containing them by hot pressure; nor do
we claim generally the treatment of substances containing the coloring
matter of madder and its derivatives, of munjeet and its derivatives, nor
of artificial alizarine with acids, these processes being well known; but
we claim, the manufacture or recovery from the precipitates of waste
soap liquors of the two practically separated products, namely, the
valuable coloring matter with little or no fatty matter, and the fatty
matter in a useful state with little or no mixture of valuable coloring
matter, in the manner substantially as above described.
Also, we claim the process of treating precipitates from waste soap
liquors by operating upon such precipitates as have been treated with
the requisite amount of acid, in the manner and for the purposes sub-
stantially as above described.
Also, we claim the process of treating precipitates from waste soap
liquors by operating upon such precipitates as have been treated with
1

page_text: the fatty and the colored compounds with bases, in the manner and for
purposes substantially as above described.
the
In witness whereof, we, the said John Thom and John Stenhouse,
have hereunto set our hands and seals, this Sixteenth day of
January, in the year of our Lord One thousand eight hundred
and seventy-three.