IMPROVEMENTS IN MORDANTING AND OTHERWISE TREATING AND DYEING VEGETABLE FIBRES OR TEXTILE MATERIALS
Year: 1878

page_text: LETTERS PATENT to John Henry Johnson, of 47, Lincoln's Inn Fields, in the
County of Middlesex, Gentleman, for the Invention of "IMPROVEMENTS
IN MORDANTING AND OTHERWISE TREATING AND DYEING VEGETABLE FIBRES
OR TEXTILE MATERIALS." A communication from abroad by Paul Magnier
and Louis Frédéric Doerflinger, of Paris, in the Republic of France.
Scaled the 4th April 1879, and dated the 20th November 1878.
PROVISIONAL SPECIFICATION left by the said John Henry Johnson at the
Office of the Commissioners of Patents on the 20th November 1878.
JOHN HENRY JOHNSON, of 47, Lincoln's Inn Fields, in the County of Middlesex,
Gentleman. "IMPROVEMENTS IN MORDANTING AND OTHERWISE TREATING AND
DYEING VEGETABLE FIBRES OR TEXTILE MATERIALS." A communication from
abroad by Paul Magnier and Louis Frédéric Doerflinger, of Paris, in the Republic of
France.
This Invention relates chiefly to the treatment of vegetable fibres, and it consists
in bringing such fibres to the condition of cellulose when not naturally in this
condition, and then converting this cellulose into pyroxiline, which is deoxidised
without destroying the azotised matter, whereby the fibres thus prepared are not
only mordanted in a most advantageous manner, but may also be covered by the
action of a powerful current of dynamic electricity with a coating of silk or other
animal or analogous substance capable of taking a very brilliant dye.
The object of the improved mordanting process is to so prepare vegetable fibrous
or textile materials as to render them capable of being dyed or printed on under
peculiarly advantageous conditions.
This process is applicable to all textile materials, but although cotton, which
constitutes a natural cellulose, may be immediately submitted to the improved process
without special preparation, other textile materials, such, for example, as flax, jute,
alfa, or esparto, and the like, require to be previously brought to the condition of

page_text: cellulose, for which purpose various means may be employed, but the series of
operations hereinafter described has been found to effect a good practical preparation
of flax for example.
Flax, after having been bleached by the usual processes, is treated with a mixture
composed of, say, about six parts of ammonia marking 24 Beaumé, and, say, about
one hundred parts of flax, the ammonia being previously mixed with, say, about fifty
parts of water.
After the flax has remained for the space of, say, about one hour in the liquid
mixture, it is taken out and washed in a bath containing about the following pro-
portions by volume, viz. :-
100 parts of water.
15 parts of methylic alcohol.
After this washing the flax is rinsed several times in water, in order to remove
all traces of the substances employed.
The flax is then plunged in a solution of potash soap at boiling point, and allowed
to remain for, say, about half an hour in this solution, after which it is again washed
and rinsed in water, and afterwards dried in this condition if it represents cellulose,
which admits of being treated in the same manner as cotton, as hereinafter
described.
The cellulose is plunged for, say, about four or five minutes into a mixture com-
posed of one part by volume of nitric acid at a density of, say, about 1.420, and
two parts by volume of sulphuric acid at a density of, say, about 1.860.
By means of this operation the cellulose is converted into pyroxyline, which is
washed in water until the water so employed ceases to show any traces of acid, and
the cellulose in the condition, which is termed bi-nitrated cellulose, is then dried at
the lowest possible temperature.
The object of the next treatment is to deoxidise the bi-nitrated cellulose without
destroying the azatised matter, and for this purpose it is plunged into a closed
vessel sulphuric acid maintained in a liquid state under pressure, where it is
allowed to remain for at least thirty five minutes, a period which is generally found
sufficient.
The cellulose after this treatment is immersed in a bath containing, say, twenty
parts by weight of hyposulphite of soda, one hundred parts of water to twenty
five parts of cellulose. After this the cellulose is washed and dried, and forms
a product upon which any description of dyeing or printing operations may be
performed under the most favourable conditions.
The vegetable fibres may also be covered with a silky coating before being dyed,
in order to impart special brilliancy to them, together with other advantages.
The process next hereinafter described is employed in order to obtain a brilliant
dye in this manner by employing aniline colours, such, for example, as anileine,
mauveine, methyl, aniline, fuchsine, ethyl, sasaniline, dephinylamine, toluidine,
tannate of aniline, and chrysaniline, and the like, one hundred parts by weight of
vegetable textile material, which has been treated in such a manner as to azotise
the cellulose by transforming this body into pyroxiline, and by deoxidising by
suitable means, are treated with a mixture of, say, about ten parts of normal phos-
phoric acid and nine hundred parts of water, and allowed to remain for a space of
about one hour in this bath at a temperature of about 60°.
The textile material thus prepared is then placed in a closed vessel provided with
a false bottom or worm, so as render it capable of being heated by steam, the vessel
being constructed in such a manner as to hold the threads or fibres in a fixed
position. This vessel is filled with a solution of silk, marking 1-28 in an instrument
for measuring density, and prepared as hereinafter described; the vessel is then
closed, and steam is introduced under the false bottom or in the worm until the
temperature of the liquid which it contains is raised to about 180°.
The material is allowed to remain for at least 14 hours in the solution of silk, and
during this time a powerful current of dynamic electricity is caused to pass until
by suitable trials or tests no traces of silk can be discovered in this solution. By

page_text: this means silk is deposited upon the vegetable fibres, after which the material is
taken out and dried by any know method.
The solution of silk may be prepared in any suitable manner, or by the process
next hereinafter described.
To one part by weight of silk added 24 parts by weight of crystallisable acetic
acid, the same being placed with the silk in a closed vessel capable of sup-
porting a pressure of six atmospheres. After the space of, say, about one hour, the
solution of silk is withdrawn from the apparatus, and if it is found to be not per-
fectly pure a small quantity of basic acetate of lead is added, and afterwards
precipitated with sulphuretted hydrogen, after which the liquor is filtered and may
be employed in the operation hereinbefore described.
After the double treatment hereinbefore described, that is to say, after the
employment of the bath of phosphoric acid and the passage of electricity through
the vessel heated by steam, as hereinbefore described, and filled with the solution
of silk, in order to effect the deposition of the silk upon the textile materials, the
latter are ready to be subjected to a process of dyeing with any of the aniline
products hereinbefore enumerated by employing any of the means known in
dyeing.
By the use of this Invention new products are obtained of great commercial value
and utility to the public..
SPECIFICATION in pursuance of the conditions of the Letters Patent filed by
the said John Henry Johnson in the Great Seal Patent Office on the 17th
May 1879.
JOHN HENRY JOHNSON, of 47, Lincoln's Inn Fields, in the County of Middlesex,
Gentleman. "IMPROVEMENTS IN MORDANTING AND OTHERWISE TREATING AND
DYEING VEGETABLE FIBRES OR TEXTILE FABRICS." A communication from
abroad by Paul Magnier and Louis Frederic Doerflinger, of Paris, in the Republic of
France.
The said Invention relates chiefly to the treatment of vegetable fibres, and it
consists in bringing such fibres to the condition of cellulose when not naturally in
this condition, and then converting this cellulose into pyroxiline, which is deoxidised
without destroying the azotised matter, whereby the fibres thus prepared are not
only mordanted in a most advantageous manner, but may also be covered by the
action of a powerful current of dynamic electricity with a coating of silk or other
animal or analogous substance capable of taking a very brilliant dye.
The object of the improved mordanting process is to so prepare vegetable fibrous
or textile materials as to render them capable of being dyed or printed on under
peculiarly advantageous conditions.
This process is applicable to all textile materials, but although cotton, which
constitutes a natural cellulose, may be immediately submitted to the improved
process without special preparation, other textile materials, such, for example, as

page_text: flax, jute, alfa, or esparto, and the like, require to be previously brought to the
condition of cellulose. For this purpose, that is to say, for eliminating matter
foreign to cellulose, and especially substances of a resinous character, various means
may be employed, but the series of operations hereinafter described has been found
to effect a good practical preparation of flax, for example.
Flax, after having been bleached by the usual processes, is treated with a mixture
composed of, say, about six parts of ammonia marking 24° Beaume, and, say, about
one hundred parts of flax, the ammonia being previously mixed with, say, about
fifty parts of water. After the flax has remained for the space of, say, about one
hour in the liquid mixture, it is taken out and washed in a bath containing about
the following proportions by volume, viz. :-
100 parts of water.
15 parts of methylic alcohol.
After this washing the flax is rinsed several times in water in order to remove all
traces of the substances employed.
This preliminary part of the operation may also be performed in the following
manner, videlicet:-
:-
.
The flax, after having been bleached by the usual processes, is placed in a bath
composed of hydrate of potash or soda of a density of about 1.03 and a tempera-
ture of about 100° centigrade, and is allowed to remain for a period of, say, about
two hours in this alkaline solution, after which it is rinsed several times in
water.
The first part of the operation having been carried out according to one or the
other of the two methods hereinbefore described, the operation is proceeded with as
next hereinafter described.
The flax is plunged in a solution of potash soap at boiling point, and allowed to
remain for, say, about half an hour in this solution, after which it is again washed
and rinsed in water, and afterwards dried; in this condition it represents cellulose,
which admits of being treated in order to convert it into pyroxiline in the same
manner as cotton, as hereinafter described.
The cellulose is plunged for, say, about four or five minutes into a mixture com-
posed of, say, about one part by volume of nitric acid at a density of, say, about
1420, and about two parts by volume of sulphuric acid at a density of, say, about
1.860. If the cellulose be allowed to remain for more than 4 or 5 minutes in the
mixture, although no advantage will be obtained, the cellulose will not be injuriously
affected by such prolonged immersion.
By means of this operation the cellulose is converted into pyroxiline, which is
washed in water until the water so employed ceases to show any traces of acid, and
the cellulose in this condition, which is termed bi-nitrated cellulose, is then dried at
the lowest possible temperature.
The means employed by preference for performing this drying operation consist in
placing the bi-nitrated cellulose in a hermetically closed receptacle, from which the
air is exhausted until the pressure is reduced equivalent to about three eighths of
an inch of mercury.
The object of the next treatment is to deoxidise the bi-nitrated cellulose without
destroying the azotised matter, and for this purpose it is plunged into a closed vessel
containing sulphurous acid, maintained in a liquid state under pressure, where such
cellulose is allowed to remain for at least thirty five minutes, a period which is
generally found sufficient.
The cellulose after this treatment is immersed in a bath containing, say, about
twenty parts by weight of hyposulphite of soda and about one hundred parts of
water to about twenty five parts of cellulose.
The object of the last described operations being to deoxidise the bi-nitrated
cellulose by the action of sulphurous acid in a nascent state after the said cellulose
has been dried at as low a temperature as possible, the same result may be obtained
by immersing the cellulose in a bath of bi-sulphite of soda, upon which phosphoric
acid is caused to act so as to produce the sulphurous acid required.

page_text: After the cellulose has been subjected to the operations herein before described, it
is washed and dried, and it then forms a product which may be dyed or printed in
any required manner under the most favourable conditions.
The vegetable fibres may also be covered with a silky coating before being dyed,
in order to impart to them special brilliancy, together with other advantages.
The process next hereinafter described is employed in order to obtain a brilliant
dye in this manner by employing aniline colours, such, for example, as anileine,
mauveine, methyl, aniline, fuchsine, ethyl, sasaniline, dephinglamine, toluidine,
tannate of aniline, and chrysaniline, and the like. In carrying out this process
vegetable textile material, which has been treated in such a manner as to azotise
the cellulose by transforming this body into pyroxiline, and by deoxidising by suit-
able means, is taken in the proportion of, say, about one hundred parts by weight, and
treated with a mixture of, say, about ten parts of normal phosphoric acid and nine
hundred parts of water, and allowed to remain for a space of about one hour in this
bath at a temperture of about 60° centigrade.
The textile material thus prepared is then placed in a closed vessel provided with
a false bottom or worm, so as to render it capable of being heated by steam, the
vessel being constructed in such a manner as to hold the threads or fibres in a fixed
position. This vessel is filled with a solution of silk (prepared as hereinafter
described), marking 1.28 in an instrument for measuring density; the vessel is then
closed, and steam is introduced under the false bottom or in the worm until the
temperature of the liquid which it contains is raised to about 180° or 190°
centigrade.
The material is allowed to remain for at least fourteen hours in the solution of
silk, and during this time a powerful current of dynamic electricity is caused to pass
until by suitable trials or tests no traces of silk can be discovered in the solution.
By this means silk is deposited upon the vegetable fibres, the threads or fibres to be
operated on being stretched in a fixed position, as hereinbefore described, in such a
manner as not to be in contact with one another, so as to admit of the silk being
deposited on every part of the threads or fibres, which thus act as so many conduc-
tors of the electric current. When this operation is completed the materials are
removed from the vessel and dried by any known means.
The solution of silk may be obtained in any suitable manner, but it is preferred
to prepare it by the process next hereinafter described.
To one part by weight of silk are added about twenty-four parts by weight of
crystallisable acetic acid, the same being placed with the silk in a closed vessel capable
of supporting a pressure of six atmospheres. After the lapse of, say, about one hour,
the solution of silk is withdrawn from the apparatus, and if it is found to be not
perfectly pure a small quantity of basic acetate of lead is added, and afterwards
precipitated with sulphuretted hydrogen, after which the liquor is filtered and may
be employed in the operation hereinbefore described.
It has been ascertained that in obtaining the solution of silk for the purposes of
the said Invention, the weight of acetic acid may be varied by employing the acetic
acid in combination with heat and pressure, and producing corresponding variations
in the two latter. For example, assuming that it be required to dissolve a certain
weight of silk by the employment of an equal weight of acetic acid, a pressure of
from ten to twelve atmospheres will be required in a closed vessel, in which the action
of the inherent heat of the steam with the pressure of the latter will effect tho
solution of the silk in the acetic acid, or assuming that it is desired to employ a
greater weight of the acetic acid in the proportion of, say, two, three, or moro
parts by weight of the acid to one part of silk with the degree of heat and pressure
may be reduced in proportion.
After the double treatment herein before described, that is to say, after the
employment of the bath of phosphoric acid, in order to submit the bi-uitrated
cellulose to the action of nascent sulphurous acid, and the passage of electricity
through the vessel heated by steam, as hereinbefore described, and filled with tho
solution of silk in order to effect the deposition of the silk upon the textile mate-

page_text: rials, the latter are ready to be subjected to a process of dyeing with any of the
aniline products herein before enumerated by employing any of the means known in
dyeing.
The solution of silk prepared as hereinbefore described may also and by the same
means as those hereinbefore described be employed for imparting to woven fabrics a
gloss capable of receiving the most brilliant colors.
Having now described and particularly ascertained the nature of the said Inven-
tion, and the manner in which the same is or may be used or carried into effect, I
would observe in conclusion that what I consider to be novel and original, and
therefore claim as the Invention secured to me by the hereinbefore in part recited
Letters Patent is,―
First. The application to textile materials, which have been previously converted
into pyroxiline or bi-nitrated cellulose deoxidised without destroying the azotised
matter of a solution of silk or analogous substance obtained by any one of the
processes herein described or otherwise, the said pyroxiline or bi-nitrated cellulose
being first dried, and then subjected to the action of nascent sulphurous acid, and
the product thus obtained subsequently submitted to the action of a current of
electricity, while such product is immersed in a solution of silk or analogous sub-
stance in a closed vessel subjected to heat and pressure, all substantially in the
manner and for the purposes hereinbefore described.
Secondly. The application and use of a solution of silk or analogous substance
obtained by one of the processes herein described or otherwise to and in the glazing
of the yarns or threads of textile materials, or the glazing of woven fabrics, for the
purpose of imparting to the same a gloss susceptible of the most brilliant colours,
substantially as hereinbefore described.
In witness whereof, I, the said John Henry Johnson, have to this my Specifi-
cation set my land and seal, this Fifteenth day of May, One thousand cight
hundred and seventy nine.
J. HENRY JOHNSON. (L.S.)