Pad dyeing process for wool

Vinylsulfonyl dyes, if padded from acidic liquors, produce on wool merely dyeings having a poor yield and only moderate fastness properties if the pad-beam method is used. It has been found according to the invention that padding from weakly alkaline liquor (pH 7-9) with sodium bicarbonate as fixing alkali and subsequent batching (6-24 hours) of the material produces good coloristic results especially on wools with a low-felting or non-felting finish.

The present invention relates to a pad cold batch process for dyeing wool 
with reactive dyes. 
Cold pad-batch dyeing processes for wool have been long known to the 
colorist. Therein the textile material is padded with acid, metal complex 
or reactive dyes from an room temperature for a certain period. In 
addition to the dyes used for that purpose, the padding liquors used 
usually contain high amounts (up to 300 g/l) of urea. Under these 
conditions, reactive dyes, in particular those of the vinylsulfonyl type, 
are fixed only incompletely and produce reduced fastness properties. 
Practical circles have long expressed the wish to be able to offer solid 
dyeings which match prints with reactive dyes on wool in hue and which 
were prepared with the same dyes in an inexpensive manner. Apart from 
simplified stockholding, the background to the demand is probably chiefly 
the desire to obtain in the case of compose articles agreement with 
respect to the appearance of the shade in artificial light, which is 
pivotal in the case of wool articles, not only in the printed but also in 
the solid-dyed portion of the textile material, which is otherwise not 
present when different types of dye combinations are used for such 
patterning purposes. Moreover, matching the shade of the dyeing in line 
with an existing printing recipe presents much fewer difficulties. 
The previously addressed situation thus led to the stated object to develop 
an inexpensive dyeing method which requires little expense on hardware, 
namely a pad cold batch method for dyeing wool with reactive dyes, which 
does not have the abovementioned shortcomings and disadvantages of the 
state of the art. 
This object is achieved according to the invention by padding the fiber 
material at a pH value between 7 and 9 with aqueous liquors containing the 
dissolved reactive dyes and then, to fix the dye, batching this dyeing at 
temperatures of up to 25.degree. C., preferably within the region of room 
temperature, in the moist state under the established weakly alkaline 
conditions for 6 to 24 hours, in general 12 to 18 hours. 
The fixing alkali used for the reactive dyes in the padding liquors 
according to the present invention is sodium bicarbonate in amounts of 5 
g/l to 40 g/l; preference is given to using 20 g of sodium bicarbonate per 
liter. 
This method of working in an alkaline medium, as it is practiced by the 
claimed process, was however completely novel to the wool dyer, since 
according to his previous notions it was likely that such a procedure 
wherein the textile material is stored for long times to effect fixing 
would result in damage to the wool by the alkali. 
However, experimental studies of these matters have shown, surprisingly, 
that the degree of damage which is done to the wool does not exceed that 
which occurs regardless in the other dyeing methods having the stated 
objectives. On the contrary, the degree of damage is distinctly lower than 
in conventional processes in which the liquor contains high amounts of 
urea (up to 300 g/l). By contrast, the process according to the invention 
dispenses with the use of urea. 
It is admittedly true that the fixing of reactive dyes from an alkaline 
medium by batching was also previously proposed in European Patent 
Application EP-A1-0,126,026 for the dyeing of silk or silk-containing 
blended fiber materials. But silk, in particular wild silk, is regarded by 
those skilled in this field as much less sensitive to alkaline influences 
than has been assumed for wool. For instance, the degumming of silk is 
effected by means of alkaline sodium carbonate liquors. For the previously 
mentioned motives, therefore, the use of alkaline conditions was generally 
ruled out for the treatment of wool fibers. When measures of this kind 
were occasionally impossible to dispense with, they were carried out in 
each case in as short a time as possible and only from ammoniacal baths. 
Application of the experiences gained with silk to the use on wool was in 
these circumstances not in any way obvious. 
Suitable reactive dyes for carrying out the process according to the 
invention are all chemical compounds which are mentioned in the Colour 
Index, 3rd edition 1971 and supplements 1975 under the generic heading 
"Reactive dyes" and which are capable of entering a covalent bond with OH- 
and/or NH-containing fibers. 
The padding liquors used can contain in addition to the dye other 
assistants of the customary kind such as wetting agents or assistants for 
promoting or preventing dye migration, if this should be found to be 
necessary. 
The claimed process is in general carried out as follows: 
The wool textile to be dyed is padded at about room temperature with the 
padding liquor which contains dye, sodium bicarbonate and possibly 
assistants. The liquor pickup can be between 50 and 130% on weight of dry 
fiber, depending on the nature of the material to be dyed. 
Thereafter, to fix the dyestuff, the moist cloth is batched at about room 
temperature for 6 to 24 hours, which is customarily effected in the 
rolled-up state by slowly rotating the beam. Advantageously this measure 
is carried out with air substantially excluded, which is obtained by 
wrapping the beamed cloth in a plastic sheet. If the liquor pickup is 
suitably low, the moist textile material can also be batched in the 
plaited state. Subsequently the completed dyeing is rinsed, washed and 
neutralized. 
Using the present invention it is possible to produce in this way dyeings 
having a good color buildup and high fastness properties, even if dyes of 
the vinylsulfonyl type are used. 
Particularly good results can be obtained when dyeing wools with a 
nonfelting or low-felting finish (for example chlorinated wools or wools 
finished by application of polyimine or polyacrylic resins).

EXAMPLE 1 
A fabric made of wool without an antifelting finish is padded with an 
aqueous liquor at room temperature (25.degree. C.) which contains per 
liter 
20 g of the dye Reactive Orange 16 having the C.I. No. 17757, 
5 g of a wetting agent based on isotridecyl alcohol reacted with 8 moles of 
ethylene oxide per mole of alcohol and 
20 g of sodium bicarbonate. 
The liquor pickup is 95% on weight of the dry fiber material. The cloth 
treated in this way is then beamed in the moist state resulting from 
squeezing off the excess liquor and to fix the dye is batched at room 
temperature by slowly rotating the beam for 24 hours. 
Thereafter the dyeing thus produced is first rinsed with water at 
40.degree. C., to remove dye portions not fixed to the substrate and 
nonreactive hydroxy dye portions formed by hydrolysts from the 
vinylsulfonyl dye is washed at 80.degree. C. by treatment with ammonia in 
an alkaline medium at pH 8.5 for 15 minutes, is rinsed once more with 
water and is then neutralized with acetic acid. 
This gives a brilliant orange dyeing on the wool having very good fastness 
properties. 
Fastness tests before the ammonia aftertreatment have shown that the 
covalent bond between fiber and dye was formed beforehand during the 
batching time. 
EXAMPLE 2 
A wool fabric with a nonfelting finish by application of polyimine resin is 
padded with a liquor at 20.degree. C. which contains in addition to water 
per liter as further components 
10 g of the dye Reactive Blue 19 having the C.I. No. 61200, 
5 g of a wetting agent based on a reaction product of 1 mole of isotridecyl 
alcohol with 8 moles of ethylene oxide and 
20 g of sodium bicarbonate. 
The liquor pickup is 85% by weight. This padded fabric is then beamed and 
to fix the dye the beam is left to rotate slowly at room temperature for 
10 hours. 
Thereafter the completed dyeing is thoroughly washed at 40.degree. C. with 
water and is finally neutralized by treatment with acetic acid. 
This gives a level, fast brilliant blue dyeing on the wool. 
EXAMPLE 3 
A wool jersey made of chlorinated wool is dyed as follows: 
Padding at room temperature (25.degree. C.) and with a 100% by weight 
liquor pickup with an aqueous liquor comprising per liter 
30 g of the dye Reactive Black 5 having the C.I. No. 20505, 
5 g of the wetting agent used in Example 1 and 20 g of sodium bicarbonate. 
Thereafter beaming of the moist cloth and batching of same at room 
temperature on a slowly rotating beam for 20 hours. 
The ammoniacal aftertreatment of the dyed wool fibers is effected as in 
Example 1. 
This gives on the textile material a level anthracite dyeing having good 
fastness properties. 
EXAMPLE 4 
Fabric made of chlorinated wool is padded with an aqueous liquor of the 
following composition per liter: 
15 g of the dye Reactive Blue 2 having the C.I. No. 61211, 
5 g of a nonfoaming, anionic wetting agent mixture and 
20 g of sodium bicarbonate. 
The padding temperature is 25.degree. C., and the liquor pickup is 100% by 
weight. After beaming, the padded fabric web is stored at room temperature 
for 16 hours on a slowly rotating beam and is then finished as described 
in Example 2. 
This gives a level blue dyeing on the fabric.