IMPROVEMENTS IN LIBERATING THE COLORING MATTER OF MADDER AND SIMILAR VEGETABLE SUBSTANCES FROM THE LIGNEOUS MATTER OR CELLULOSE WITH WHICH IT IS COMBINED IN THE PLANT
Year: 1868

page_text: PROVISIONAL SPECIFICATION left by George Tomlinson Bousfield.
at the Office of the Commissioners of Patents, with his Petition,
on the 21st January 1868.-A communication from abroad by
Alfred Paraf, residing at Boston, in the County of Suffolk, and
State of Massachusetts, United States of America.
I, GEORGE TOMLINSON BOUSFIELD, of Loughborough Park, Brixton,
in the County of Surrey, do hereby declare the nature of the said
Invention for "IMPROVEMENTS IN LIBERATING THE COLORING MATTER OF
MADDER AND SIMILAR VEGETABLE SUBSTANCES FROM THE LIGNEOUS MATTER
OR CELLULOSE WITH WHICH IT IS COMBINED IN THE PLANT," to be as
follows:-
Dry madder root, for example, contains about seven per cent. of
coloring matter combined with about thirty-eight per cent. of ligneous
matter, and about fifty-five per cent. of sugary matter. In the ordinary
process of dyeing and printing madder colors only about half the
coloring matter is utilized, and this portion is obtained by tedious
processes requiring a large amount of manual labor. The object of
the Invention which constitutes the subject matter of this Patent is
to liberate the coloring matter of the madder root or similar plant
from the ligneous matter, so that practically the whole amount of
coloring matter of the plant may be utilized.

page_text: The Invention is based upon the fact that cellulose becomes
soluble when in the presence of cupric oxyde with ammonia, and the
first part of the Invention consists of a compound process composed
of two operations, which are, 1st, the solution of the cellulose of the
plant by the action of cupric oxyde with ammonia; 2nd, the separation
of the copper from the coloring matter that has been set free from
the cellulose by the preceding operation.
The Invention consists, further, of the combination of the said two
operations with the separation of the surgary matter of the plant
from it.
In order that the Invention may be fully understood, I will proceed
to describe the several modes in which the principle of the Invention
has been applied when operating upon madder root. The madder
root previously dried and reduced to powder by grinding or by other
means is washed with water by several successive operations until
the sugary matters are separated and removed, which may be
ascertained by testing the wash water for sugar with Bareswell's
liquor in the usual manner. The damp washed madder root drained
from the water is next subjected to the action of cupric oxyde with
ammonia by steeping the damp root in an open vessel in aqueous
ammonia in which copper turnings have been placed. This operation
may be conveniently performed in an earthenware vessel fitted with
a perforated cover which permits the access of air. In performing
this operation it is expedient to use one pound of metallic copper
and seven gallons of aqueous ammonia for each pound of ligneous
matter to be removed. Thus assuming that the madder root contains
38 per cent. of ligneous matter, 38 pounds of copper turnings and
about 260 gallons of aqueous ammonia may be used for each 100
pounds of dry ground madder root. In the presence of the copper
the aqueous ammonia and the air (which has access through the
cover of the vessel) the ligneous matter of the plant is gradually
dissolved while the coloring matter and copper form insoluble
compounds which remain in the liquid in the form of a precipitate.
The operation requires generally several days during which the
materials should be occasionally stirred; the ammonia in the liquid
also must be renewed which is conveniently effected by passing a
current of gaseous ammonia into the liquid in the vessel. The gaseous
ammonia for this purpose may be produced in any of the modes known

page_text: to chemists and the quantity introduced daily should be sufficient
to cause the solution of about twenty per cent. of the ligneous matter,
so that the operation may be completed in about five days. If any
of the copper remains undissolved at the end of the period and the
liquid still contains free ammonia, an additional quantity of washed
madder root may be added little by little until all the copper is
dissolved; on the other hand if all the copper is dissolved and some of
the madder root remains undecomposed metallic copper may be added
little by little until the madder root is substantially all decomposed.
The coloring matter being thus set free from the ligneous matter or
cellulose by the solution of the latter the next operation is the
separation of the coloring matter and copper.
This operation may be performed in several ways as follows:-1st,
the dissolved cellulose is removed from the compounds of the coloring
matter and copper by filtration and by washing the precipitate; then
the precipitate is mixed with alcohol, and a current of sulphuretted
hydrogen (H, S) is passed into the mixture; this substance decomposes
the compounds of the coloring matter and copper, setting free the
coloring matter and transforming the copper into an insoluble cupric
sulphide. The coloring matter dissolves in the alcohol as fast as it is
set free, while the cupric sulphide remains in the liquid in the form
of a black precipitate which is readily separated by filtration.
filtered alcoholic solution of the coloring matter may be concentrated
by boiling until the coloring matters will crystallize; or the coloring
matters may be precipitated by adding acetic acid to the alcoholic
solution until precipitation ceases, after which they may be separated
from the liquid by filtration.
The
2nd. The separation of the coloring matter and copper may be effected
by the use of a small quantity of alcohol in the following manner :-
The compounds of coloring matter and copper after the removal of the
dissolved cellulose by filtration and washing are mixed with water, and a
current of sulphuretted hydrogen is passed through the mixture until
precipitation ceases. The precipitate is separated from the liquid by filtra-
tion and is dried; after which the coloring matter is extracted by treating
the precipitate successively with small quantities of boiling alcohol.
The coloring matter may be obtained from the alcoholic solution as in
the previous mode.

page_text: effected without the use of alcohol in the following manner:-The
compounds of coloring matter and copper separated from the dissolved
cellulose by filtration are mixed (without previous washing) with a
dilute solution of hydrochloric acid (H, Cl) sufficient to transform the
copper into the protochloride of copper, and the excess of ammonia
into chloride of ammonium, the liquid is boiled for about ten minutes,
or until the copper is dissolved in the form of the chloride, while the
coloring matter remains in the form of a reddish precipitate, which is
separated from the liquid by filtration and washing.
4th. If the coloring matter is to be used at once for dyeing the
dissolved cellulose need not be removed from the compounds of coloring
matter and copper, but a sufficient amount of hydrochloric acid (H, Cl)
may be added to the liquid to combine with the excess of ammonia
to transform the copper into the soluble protochloride of copper and
to precipitate the cellulose. The coloring matter, being insoluble in
water and acid, remains in the liquid in the form of a precipitate.
The precipitated cellulose and coloring matter are then freed of the
chlorides of copper and ammonium by filtration and washing, and the
product remaining on the filter may be used in the same manner as
is practised in dyeing with madder root; but as the coloring matter
in this product is liberated from the cellulose and is only mechanically
mixed with it, in the same manner as it might be with any inactive
adulterating material, the dyer is able to utilize practically the whole
of the coloring matter of the plant, instead of only about half of it,
as in the ordinary method of using madder. The filtered solution of
cellulose obtained in any of the preceding modes may have hydro-
chloric acid added to it until the excess of ammonia is neutralized,
the copper remaining in the liquid is dissolved in the condition of a
chloride and the cellulose is precipitated. The liquid may then be
removed by filtration and washing and the product utilized for any
purpose that is expedient, one of such purposes being the manufacture
of paper. When using the product for this purpose it may be treated
with sulphuric acid in the manner practised for transforming paper
pulp into artificial parchment.
The material obtained by the above described operations designated
respectively 1st, 2nd, and 3rd, may be used advantageously for either
dyeing or printing, the material when used for printing being previously
mixed with the acetate of alumina or of iron, or a mixture of the two

page_text: to produce red, purple, or chocolate colors, and being also mixed with
gum or starch in the usual mode of thickening. After printing the
cloths should be steamed in the usual mode and washed with water
with or without soap. The material obtained by the operation designated
4th, is useful specially for dyeing.