Improvements in, and Means for Use in, Mordanting and Dyeing Cotton, and other Vegetable Fibres.
Year: 1899

page_text: Date of Application, 16th Sept., 1899
Complete Specification Left, 2nd June, 1900-Accepted, 25th Aug., 1900
PROVISIONAL SPECIFICATION.
Improvements in, and Means for Use in, Mordanting and Dyeing
Cotton, and other Vegetable Fibres.
I, BENJAMIN WILLCOX, of 47, Lincoln's Inn Fields, in the County of London,
Patent Agent, do hereby declare the nature of this invention (which has been
communicated to me from abroad by the Badische Anilin & Soda Fabrik of
Ludwigshafen-on-Rhine, in the German Empire) to be as follows:-
".
Many attempts have been made to simplify and improve the process of dyeing
the colour known as Turkey-red, but the simplest process in general use to-day
is still very complicated, expensive, and requires a long time to carry it out.
Perhaps the process which is now most generally used is the so called new-
red" process, which can be carried out in the following manner. After the
cotton has been prepared in the usual way by boiling it, it is at first thoroughly
impregnated with Turkey red oil. For dark shades, this operation is prefer-
ably repeated. The goods are then thoroughly dried at a temperature of from
60° to 70° Centigrade. They are then treated with the mordant
solution; acetate, or basic sulphate of alumina. After this they are again
dried and then treated with chalk to thoroughly fix the mordant. This is
succeeded by a washing operation, and only after this complicated_treatment,
involving two drying operations can the dyeing process be begun.
The dyeing
can be effected-in a boiling bath, but if it be desired to obtain the brightest-
and then to steam the goods under pressure, to develope the colour. Finally,
shades it is necessary to dye at a temperature of about 65° Centigrade,
the dyed goods are brightened by boiling with a soap solution, preferably
under pressure, whereby the shade is rendered more beautiful and fresh and
the goods are freed from colouring-matter deposited on the surface and from
impurities. The foregoing process is much simpler than the older Turkey-red
mordanting and dyeing process, but, nevertheless it is very complicated and
the drying operations take a considerable time and render the process expensive.
My foreign correspondents have invented a process which is much simpler
than that herein before described. By the use of the process according to this
invention it is possible to avoid the following steps of the process herein before
described. It is unnecessary to steam the goods to develope or fix, the colouring
matter on the fibre. The drying process is unnecessary, both after mordanting
and after the dyeing operation. The treatment with chalk to thoroughly fix
the mordant which is essential in the process herein before described is un-
necessary.
The process according to this invention consists first, in treating the goods in
an oiling bath containing castor oil caustic soda, stannate of soda, sodium
aluminate, and sodium phosphate, and subsequently mordanting in a mordanting
bath which has a strongly acid reaction. The series of operations necessary is
rendered essentially simpler, shorter, and cheaper, by this invention without the
shades being less beautiful or less intense. The following example will serve to

page_text: further illustrate the nature of the invention. In it is described what is con-
sidered the best treatment for obtaining the desired results, using 100 lbs. of
cotton yarn, but the proportions employed can be varied without departure from
the invention.
EXAMPLE.
The preliminary boiling out of the yarn can be effected in the usual way by
heating under pressure for two hours in a solution containing one kilogram of
calcined soda, or one kilogram of calcined soda and one-half kilogram of sodium
silicate solution having a density of 40° Bé. After this boiling out treatment the
goods are swilled and freed from the excess of water in a centrifugal machine.
The next operation is the treatment in the special oiling-bath acording to
this invention. For this purpose prepare a castor oil soap in the following
way Dissolve fourteen kilograms of caustic soda, twenty-five kilograms of
sodium stannate, fifteen kilograms of sodium aluminate, (commercial), and ten
kilograms of sodium phosphate, in two hundred litres of boiling water. Then
add one hundred kilograms of castor oil, and boil until the oil is, completely
saponified. Dilute with water, so as to make up the mixture to eight hundred
and fifty litres. The oiling solution thus obtained should have a density of
nine degrees Beaumé.
The oiling can be effected in a small vat with a broad rim, or a machine can
be used in which the goods are passed through the solution. It is recommended
that about two pounds of cotton should be treated simultaneously with six
litres of the oiling solution obtained as herein before described and two litres of
water, which should be as free from chalk, as possible. For every further two
pounds of yarn one-half litre of oiling solution is added.
After passing the goods a second time through the solution the yarn is
thoroughly and evenly wrung out and dried at about 60° to 70° Centigrade.
The next operation the actual mordanting. For this purpose dissolve forty
kilograms of sulphate of alumina in two hundred and forty litres of boiling
water. Run off the clear solution from any sediment. The solution obtained
should have a density of about twelve degrees Beaumé. Immediately before
using add about six and fourth-tenth kilograms of ammonium chloride and
five and one-fifth kilograms of sulphate of magnesium, dissolved in one hundred
and twenty litres of boiling water. The mordanting solution that is obtained
should have a density of about seven degrees Beaumé. The yarn is again pre-
ferably treated in portions of two pounds at a time either in a small vat with.
a broad rim, or by means of a machine by which the goods are passed through
the solution. The mordanting solution is maintained at a temperature of from
about 35° to 40° Centigrade, and at first twelve litres of the solution are used.
For each successive two pounds, of yarn three-quarters of a litre more of the
mordanting solution are added. The goods are passed once through the solution,
and are then washed until the wash water no longer exhibits an acid reaction.
As aforesaid, the proportion of the ingredients used in the various operations
according to this invention can be varied. In this actual mordanting operation
it is essential that the bath should have a distinctly acid reaction, which is not
the case in the mordanting baths as usually employed. The addition of the
sulphate of magnesium is not absolutely necessary, but my foreign correspon-
dents have found that it has the effect of rendering it easier to obtain uniform
shades.
The actual dyeing operations is effected as follows:-
The dyeing-vat is prepared with from eight to ten per cent of alizarine paste,
containing twenty per cent alizarine. To this is added from one to one-and-a-
half per cent. of solid acetate of lime, dissolved in water the quantity used being
regulated according to the hardness of the water. The mordanted yarn, without
being dried, is introduced into this dyeing-bath, and treated therein for about
a quarter-of-an-hour at the ordinary temperature. After this the bath is gradu-

page_text: ally heated so that in about three-quarters of an hour it boils and the boiling
is continued for from one to one and a half hours. Finally the goods are well
swilled.
The next operation of "brightening" can either be effected in an open vat,
or in closed apparatus under pressure. The water to be used is boiled with
from two, to four, kilograms of calcined soda to every one thousand litres, the
quantity of soda used being according to the hardness of the water. Remove
the scum that forms. Add an emulsion of five kilograms tournant oil and two
and a half kilograms of soap, and one kilogram of potato starch. The soap
and potato starch are each separately mixed, or dissolved, in hot water, and then
the oil is added. Introduce the yarn into this solution, and treat for from one
to one and a half hours, preferably under a pressure of one atmosphere. Wash
the goods well and dry.
Dated this 16th day of September 1890
JOHNSONS & WILLCOX,
47, Lincolns Inn Fields, London, W.C.,
Agents.
Improvements in and Means for Use in Mordanting and Dyeing
Cotton and other Vegetable Fibres.
I, BENJAMIN WILLCOX, of 47, Lincoln's Inn Fields, in the County of London,
Patent Agent, do hereby declare the nature of this invention (which has been
communicated to me from abroad by the Badische Anilin & Soda Fabrik of
Ludwigshafen-on-Rhine, in the German Empire), and in what manner, the same
is to be performed to be particularly described and ascertained in and by the
following statement:-
-
Many attempts have been made to simplify and improve the process of dyeing
the colour known as Turkey-red, but the simplest process hitherto in general use
is still very complicated, expensive, and requires a long time to carry it out.
Perhaps the process which is now most generally used is the so-called " new-
red" process, which can be carried out in the following manner. After the
cotton has been prepared in the usual way by boiling it, it is at first thoroughly
impregnated with Turkey red oil. For dark shades, this operation is prefer-
ably repeated. The goods are then thoroughly dried at a temperature of from sixty
degrees to seventy degrees Centigrade. They are then treated with the mordant
solution; acetate, or basic sulphate of alumina. After this they are again
dried and then treated with chalk to thoroughly fix the mordant. This is
succeeded by a washing operation, and only after this complicated treatment,
involving two drying operations can the dyeing process be begun.
The dyeing
can be effected in a boiling bath, but if it be desired to obtain the brightest
shades it is necessary to dye at a temperature of about sixty-five degrees Centigrade
and then to steam the goods under pressure, to develope the colour. Finally,
the dyed goods are brightened by boiling with a soap solution, preferably
under pressure, whereby the shade is rendered more beautiful and fresh and
the goods are freed from colouring-matter deposited on the surface and from
impurities. The foregoing process is much simpler than the old Turkey-red
mordanting and dyeing process, but, nevertheless it is very complicated and
the drying operations take a considerable time and render the process expensive.
My foreign correspondents have devised a process which is much simpler
than that herein before described. By the use of the process according to this

page_text: invention it is possible to avoid the following steps of the process herein before
described. It is unnecessary to steam the goods to develope, or fix, the colour-
ing matter on the fibre. The drying operation is unnecessary, both after mor-
danting and after the dyeing operation. The treatment with chalk, to
thoroughly fix the mordant, which is essential in the process herein before
described is unnecessary.
The process according to this invention consists first in treating the goods
in an oiling bath containing castor oil, caustic soda, stannate of soda, sodium
aluminate, and sodium phosphate, and subsequently mordanting in a mordant-
ing bath containing sulphate of alumina and ammonium chloride which bath is
more acid than the bath usually employed.
The series of operations necessary is rendered essentially simpler, shorter
and cheaper, by this invention without the shades being less beautiful, or less
intense.
The following example will serve to further illustrate the nature of the inven-
tion and the manner in which it can be performed. In this example I describe
what is considered the best treatment for obtaining the desired results. as
applied to 100 lbs. of cotton yarn, but the proportions employed can be varied
without departure from the invention.
EXAMPLE.
The preliminary boiling out of the yarn can be effected in the usual way by
heating under pressure for two hours in a solution containing one kilogram of
calcined soda, or one kilogram of calcined soda and one-half kilogram of sodium
After this boiling
silicate solution, having a density of forty degrees Beaumé.
out treatment the goods are swilled and freed from the execess of water in a
centrifugal machine. The next operation is the treatment in the special oiling-
bath according to this invention. For this purpose prepare a castor oil soap
in the following way. Dissolve fourteen kilograms of caustic soda, twenty five
kilograms of sodium stannate, fifteen kilograms of sodium aluminate (com-
mercial) and ten kilograms of sodium phosphate, in two hundred litres of boiling
water. Then add one hundred kilograms of castor oil, and boil until the oil
is completely saponified. Dilute with water, so as to make up the mixture to
eight hundred and fifty litres. The oiling solution thus obtained should have
a density of nine degrees Beaumé.
The oiling can be effected in a small vat with a broad rim, or a machine can
be used in which the goods are passed through the solution. It is recommended
that about two pounds of cotton should be treated simultaneously with six litres
of the oiling solution, obtained as hereinbefore described, and two litres of
water, which should be as free from chalk as possible. For every further two
pounds of yarn one-half litre of oiling solution is added.
After passing the goods a second time through the solution the yarn is
thoroughly and evenly wrung out and dried at about sixty degrees to seventy
degrees Centigrade.
The next operation is the actual mordanting. For this purpose dissolve forty
kilograms of sulphate of alumina in two hundred and forty litres of boiling
water. Run off the clear solution from any sediment. The solution obtained
should have a density of about twelve degrees Beaumé. Immediately before
using add about six and four tenth kilograms of ammonium chloride and five
and one-fifth kilograms of sulphate of magnesium, dissolved in one hundred and
twenty litres of boiling water. The mordanting solution that is obtained should
have a density of about seven degrees Beaumé. The yarn is again preferably
treated in portions of two pounds at a time, either in small vat with a broad
rim, or by means of a machine by which the goods are passed through the solu-
tion. The mordanting solution is maintained at a temperature of from about.
thirty five degrees to forty degrees Centigrade, and at first twelve litres of
the solution are used. For each successive two pounds of yarn three-quarters

page_text: of a litre more of the mordanting solution are added. The goods are passed
once through the solution, and are then washed until the wash water no longer
exhibits an acid reaction.
As aforesaid, the proportion of the ingredients used in the various operations
according to this invention can be varied. In this actual mordanting operation
it is essential that the mordant should have a more acid reaction than usually
employed. The addition of the sulphate of magnesium is not absolutely neces-
sary, but my foreign correspondents have found that it has the effect of ren-
dering it easier to obtain uniform shades.
The actual dyeing operation is effected as follows:-
hardness of the water.
The dyeing vat is prepared with from eight to ten per cent of alizarine paste
containing twenty per cent alizarine. To this is added from one, to one-and-
a-half, per cent. of solid acetate of lime dissolved in water, the
quantity of acetate of lime used being regulated according to the
The mordanted yarn, without being dried, is introduced
into this dyeing bath, and treated therein for about a quarter of an hour
at ordinary temperature. After this the bath is gradually heated, so that in
about three quarters of an hour it boils, and the boiling is continued for from
one, to-one and a half, hours. Finally the goods are well swilled.
The next operation of "brightening" can either be effected in an open vat,
or in closed apparatus under pressure. The water to be used is boiled with from
two, to four, kilograms of calcined soda to every one thousand litres of water,
the quantity of soda used being according to the hardness of the water. Remove
the scum that forms. Add an emulsion of five kilograms of tournant oil, and
two and a half kilograms of soap, and one kilogram of potato starch. The
soap and potato starch are each separately mixed, or dissolved, in hot water,
and then the oil is added. Introduce the yarn into this solution, and treat for
from one to one and a half hours, preferably under a pressure of one atmos-
phere. Wash the goods well and dry.
Having now particularly described and ascertained the nature of the said
invention and in what manner the same is to be performed I declare that what
I claim is: —
1. In dyeing cotton or other vegetable fibres, with mordant dyeing colouring
matters, the employment of both the oiling bath herein before described and
the mordanting bath also hereinbefore described.
2. In a process for mordanting cotton, or other vegetable fibres, the use of an
oiling bath prepared from castor oil, caustic soda, stannate of soda, sodium
aluminate, and sodium phosphate.
3. In a process for mordanting cotton, or other vegetable fibres the use of a
mordanting bath containing sulphate of alumina and ammonium chloride.
4. The process for the mordanting cotton yarn and dyeing it Turkey-red, here-
inbefore described in the example.
Dated this 2nd day of June 1900.
JOHNSONS & WILLCOX,
47, Lincolns Inn Fields, London, W.C.,
Agents.