IMPROVEMENTS IN TREATING, CERTAIN VEGETABLE DYE-STUFFS OR PREPARATIONS THEREFROM, SO AS TO OBTAIN A COLORING SUBSTANCE OF INCREASED PURITY
Year: 1856

page_text: "1"
LETTERS PATENT to James Higgin, of the City of Manchester, in the
County of Lancaster, Manufacturing Chemist, for the Invention of
"IMPROVEMENTS IN TREATING, CERTAIN VEGETABLE DYE-STUFFS OR PREPARATIONS
THEREFROM, SO AS TO OBTAIN A COLORING SUBSTANCE OF INCREASED PURITY."
14.
44
PROVISIONAL SPECIFICATION left by tho said James Higgin at the Office
of the Commissioners of Patents, with his Petition, on the 28th November
1856.
I, JAMES HIGGIN, of the City of Manchester, in the County of Lancaster,
Manufacturing Chemist, do hereby declare the nature of tho said Invention
for "IMPROVEMENTS IN TREATING CERTAIN VEGETABLE DYE-STUFFS OR PREPARATIONS
THEREFROM, SO AS TO OBTAIN A COLORING SUBSTANCE OF INCREASED PURITY," to bo
as follows:
Some vegetable dye-stuffs, amongst which madder may be named, contain
certain substances such as poetic acid, colored resins, and other matters which
are injurious in dyeing, by masking and rendoring dull the shades produced.
By the use of solutions or mixtures capable of combining with these substances,
and either removing them from the dye-stuff or forming with them compounds
insoluble in water previous to dyeing, I find that purer and clearer colors
are produced, and I propose to effect this by mixing the dye-stuff with water
and a sufficient quantity of the substance or substances I employ to combine

page_text: with the impurities, and either allowing the mixture to stand cold or assisting
the action by heat, and when the combination is properly effected the dye-stuff
may be strained out and used as an ordinary dyeing, or may be pressed and.
dried. The substances I employ for this purpose are alkalies, alkaline earths,
salts of alkaline earths, or salts of alkaline reaction, though certain neutral
salts and substances can in some cases be used with effect.
SPECIFICATION in pursuance of the conditions of the Letters Patent,
filed by the said James Higgin in the Great Seal Patent Office on the
28th May 1857.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, JAMES
HIGGIN, of the City of Manchester, in the County of Lancaster, Manufacturing
Chemist, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Twenty-eighth day of November, in the year of our
Lord One thousand eight hundred and fifty-six, in the twentieth year of Her
reign, did, for Herself, Her heirs and successors, give and grant unto me, the
said James Higgin, Her special licence that I, tho said James Higgin, my
executors, administrators, and assigns, or such others as I, the said James
Higgin, my executors, 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, exercise,
aud vend, within the United Kingdom of Great Britain and Ireland, the
Channel Islands, and Isle of Man, an Invention for "IMPROVEMENTS IN
TREATING CERTAIN VEGETABLE DYE-STUFFS OR PREPARATIONS THEREFROM, 80 AS TO
OBTAIN A COLORING SUBSTANCE OF INCREASED PURITY," upon the condition (amongst
others) that I, the said James Higgin, by an instrument in writing under
my hand and seal, 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 immediately after the date of the said Letters
Patent.
NOW KNOW YE, that I, the said James Higgin, do hereby declare the
nature of my said Invention, and in what manner the same is to be per-
formed, to be particularly described and ascertained in and by the following
statement (that is to say) :-
Madder and plants of the same species, and most preparations therefrom,

page_text: and
contain, in addition to the coloring matter, certain substances, such as pectine,
pectic acid, resins, &c., which do not act as true coloring matters, but become
attached to the mordants during the process of dyeing, and also form com-
binations with coloring matter, which fix to some extent on the white or
unmordanted parts, and consequently require further operations to give lively
pure colors and good whites. I act on the dye-stuffs so as to prevent tho
pernicious effects of the above-named injurious substances, by either removing
them wholly or in part by substances capable of dissolving them, or by forming
compounds with them insoluble in water to prevent their action during dyeing.
Now although my processes are successful when operating on madder or
munjeet, especially when fermented or steeped, it is better to act on thoso
preparations which have been treated with acids, such as garancine, garanceux,
or extracts from them, and it is to this class of preparations that I most
particularly refer. I take garancine or garanceux made by the well-known
process of boiling or steaming madder with an acid, and wash it thoroughly
with water. It is a common practice, in order to save timo, to neutralize the
last portions of acid remaining in the garancine by a wash containing a small
quantity of an alkaline or basic substance, giving sometimes a slight excess of
alkali, so as to ensure the neutralizing of the acid; but I prefer to wash with
water only till tho acid is washed out. I then put the garancine into a vessel,
which can be heated in any convenient manner, and add sufficient water to
make it tolerably fluid. I then introduce the substance which I wish to
combine with the impurities in the garancine, and heat the mixture to as bigh
a temperature and for as long a time as may be found necessary for the
particular sample of madder in operation; generally a temperature at or near
the boiling point of water, and of about two hours' duration, is found to produce
a good result; but owing to varieties in the constitution of different madders
these details will vary, a less heat and a shorter time answering better for
some madders than others. The proportion of purifying agent will also vary
for the same reasons. When the operation is considered complete the mixture
is allowed to cool, then transferred to a filter and washed with water till the
soluble impurities are sufficiently washed away. The purified garancine is
then in a fit state to use in dyeing, or may be pressed, dried, and ground to
fine powder.
The substances I use to purify garancine or preparations of madder, as above,
are alkalies, alkaline earths, or such combinations of these bodies with acids as
will, when boiled along with pectic acid, combine therewith, forming either
compounds soluble or insoluble in water, observing that those substances
which combine with the pectic acid are generally found to combine also with

page_text: the colored substances, not true coloring matters, such as resin, &c. It is
advisable however not to make use of those salts of alkalies or alkaline earths
which easily yield oxygen or which are generally termed "oxydisers." Some
organic substances, not salts, are likewise available for the above purpose, such
as mucilage, glue, sugar, and generally any substance which when boiled or
heated with pectic acid combines therewith, is applicable to purifying pre-
parations of madder, as above described.
In order, however, that my Invention may be more clearly understood, I
will describe the method I use for Turkey madder of the finest quality. After
making it into garancine in the ordinary manner with sulphuric acid, and
carefully washing out the acid used in the manufacture, I put in a vat a
quantity which represents five hundredweight of madder; I add about two
hundred gallons of water and a solution of arsenite of soda, made by boiling
seventeen pounds of chrystallized carbonate of soda dissolved in water, with
excess of arsenious acid, for half an hour, filtering out the undissolved arsenious
acid and using the clear liquor only; I then heat the mixture to the boiling
point or nearly so for an hour; when cool I put it in a filter and wash it
with two hundred gallons of water or till the arsenite liquid is all washed
out. The garancine is then ready for use or for drying and grinding.
Many salts may be used instead of arsenite, though this gives very good
results, and for some purposes a very short duration of time of the treatment
with heated mixtures or solutions is necessary, and although a better effect is
produced by filtering the purified garancine and washing with water, yet a
certain improvement may be effected by treating garancine or preparations of
madder with a purifying agent, at a temperature above the natural temperature
of water, for a time sufficient to form combinations with pectic acid, &c., and
then cooling down to the ordinary temperatures at which dyeing operations
are usually commenced, and dyeing goods at once without previous filtering
and washing.
When garanceux is operated upon it is advisable to take only about half
the quantity of the purifying agent which is given to garancine, all other
circumstances being alike; and when extracts of madder or garancine con-
taining pectic acid or resins (but freed from vegetable fibre) are oporated
upon a much less quantity of water will suffice.
Having thus described the nature of my said Invention, and the manner in
which the same is to be performed, I desire it to be distinctly understood that
I do not confine myself to the precise details herein set forth, so long as the
spirit of my Invention is retained; but I claim as my Invention, and which to
the best of my knowledge and belief has not been hitherto used within the

page_text: realm, the use of alkalies, alkaline earths, salts of alkalies or alkaline earths, or
other substances capable of combining with the pectic acid, resinous or other
impurities of madder or preparations therefrom, at temperatures above the
natural temperature of water, for the purpose of removing or rendering
innocuous those impurities.
In witness whereof, I, the said James Higgin, have hereunto set my
hand and seal, this Twenty-seventh day of May, in the year of our Lord
One thousand eight hundred and fifty-seven.
Signed, sealed, and delivered by the within-
named James Higgin, in the presence of
JAMES HIGGIN. (L.B.)
E. J. HUGHES, Patent Agent,
Manchester.