DE2357439A1 - METHOD OF DYING WOOL FIBER - Google Patents

Description

F km 3 WERKB HOEOHST AG.

formerly master Lucius & Brüning,

File number: HOE 73 / f 3 ^ 8 DR.CZ/W

Date: November 16, 1973

Process for dyeing wool fibers

Exhaust process for dyeing wool fibers under high temperature (HT) conditions or at boiling temperature, appropriate pressure-tight systems, such as HT-Jet dyeing systems, jiggers, reels, Skids, tree dyeing machines, systems based on the overflow principle o. a. well known. In general, depending on the system and dye class, dyeing times of 60 to. 180 minutes needed to control the exhaustion of the dyes so that level dyeings can be achieved. Under the thermal conditions of these processes, the affinity of the dyes is greatly increased, so that you can use these long dyeing times for leveling Have to claim. *

It has now been found that on bobbins made of wool or from mixtures containing such, with anionic dyes after an HT rapid dyeing process or dyeing at boiling temperature contrary to expectations, experiences and ideas of a person skilled in the art even with dyes that are otherwise difficult to color or dye combinations then perfectly level dyeings in (compared to known processes) significantly reduced dyeing times can be achieved if the specific thermal properties of the fibers are taken into account and the wound

', Brings fiber material into a pressure-tight dyeing container and means by displacing the air and filling the autoclave

ι Saturated steam or superheated steam to temperatures between 100 ° and 110 C heated, in a separate one, but by ■ - · .. " Pipes connected to it, also pressure-tight approach in the case of ■

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ORIGINAL INSPECTED

the entire dye liquor prepared and also ^{heated to temperatures between 100 and "RO 0} C, whereby by special control of the temperature within the limits mentioned and the vapor pressure in the" two closed systems as well as by applying external pressure it is ensured that it forms a relative Overpressure of 3 to 10 at (= 2.94 to; 9.81 bar), preferably 3.5 to 8 at (= 3.43 to 7.84 bar), comes in the batch container, then the hot dye liquor through the differential pressure within 3 to 60 seconds simultaneously from the inside and from the outside into the dry or wet bobbin and finally leads to the dyeing in the usual way to the end.

The principle of the present invention is that in a HT container a dye liquor with the selected pressure and Temperature conditions are set and from there by means of pressure (pressurized steam, compressed air, pump pressure) in another, steam-filled as well as with den.Wickelkkörern made of wool fibers, z. B. wound threads or piece goods rolls on dye trees, loaded Autoclave is transferred. This is done in such a way that one can use appropriately large pipelines, Pumps and a distributor valve press the liquor into the winding body from both the inside and the outside at the same time. on In this way it is possible to distribute the liquor evenly in the dyed material in an extremely short time without deforming the lap or threads. In general, times of less than 60 seconds, mostly even less than 30 seconds, are required for this taken. This rapid "shooting in" of the dye liquor is achieved by applying a high pressure on the side of the batch container (Pressure difference 3 - 10 at). The dye container is vented beforehand by means of pressurized steam and the goods are preheated at the same time » The textile material can be dry or pre-washed, whatever can be carried out in the dye container itself.

The dye container. Is pressure-tight, well insulated and with a Provided heat exchangers of high capacity in order to be able to keep the dyeing temperature constant.

The fleet itself is heated in the preparation vessel to etv / a 105 ° C to 110 ⁰ C, and then injected into the vapor-filled dyeing vessel. As part of this process, the dye container,

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as long as there is the corresponding differential pressure, even when it is closed The valve must be completely filled, as the previously existing steam condenses as the pressure rises.

A modification of this method according to the present invention consists in that the dye container filled with pressurized steam a condensation system that can be shut off is connected. As a result, a relative pressure difference is also formed, as a result of which it is in turn possible to completely fill the dye container with the dye preparation when the vent valve is closed.

After the entire dye liquor is in the dye container, i.e. after the shooting-in has been completed, a Circulation pump the dyebath is pumped alternately from the inside to the outside "and from the outside to the inside through the material roll. The The selected dyeing temperature is maintained. The final fixation of the dye now takes place in a short time. It is advantageous, at the high drawing speeds under these temperature conditions, mii; sufficiently high funding rates the pump to work. At 40 to 60 l / kg.min, the result is good Staining results. In the case of dyes or dye combinations that are difficult to be colored equally, a delivery rate of more is required can be worked as 60 l / kg.min.

i
Due to the characteristic of feeding the entire dye liquor into the dyeing vessel at high speed on and into the more or less dry material in the form of bobbins, the process differs from the dyeing processes carried out up to now, which, including their process variants, have been extensively discussed in the literature «, Thus, according to the invention, not only part of the dye liquor or a concentrated dye solution is introduced into the dye container, but the entire dye liquor is pressed in almost suddenly. It was not foreseeable that level colorations could be achieved under these conditions, since all anionic dyes (acid, chromium, metal complex and reactive dyes) have an extraordinarily high drawability at these temperatures.

In addition, it could not be expected that the dyestuffs would solutions at such high temperatures and pressure differences because of the. thermal properties of the fiber still allow for penetration into

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Winding bodies are suitable.

In the case of the claimed ver _f

drive out the fact that at the high temperatures used the drawability of the dyes can be fully utilized.

The good levelness of the dyeings is achieved in that it according to the method according to the invention, it is possible to inject the liquor extremely quickly, and thereby the goods to bring it into contact with it immediately and at every point and then to continue dyeing immediately with high liquor circulation.

The process described is normally carried out in an aqueous medium; however, it can also be used readily for dyeing from organic solvents are used. In the latter case, the process conditions are of course the to take into account the typical boiling point and vapor pressure of the solvent in question «

According to the process, the dyes used are the customary trademarks of anionic dyes in powder form or in liquid form Attitude to the application. Such dyes are in the Color Index, 3rd edition, under the class name "Acid Dyes" or "Reactive Dyes".

For the implementation of the "claimed method are wool and Their mixtures with synthetic fibers or cellulose fibers in any processing form suitable for the HT dyeing method or can be colored at boiling temperature.

When dyeing wool fibers, no additives other than leveling agents and chemicals for pH adjustment are required. The constant pH of the dyebath between pH 2 and 8.5 enables the colorations to be reproduced and is determined by known, suitable buffer systems achieved. It can be dry as well as wet or pretreated, e.g. B. chlorinated material be treated.

For level dyeing it is important that the liquor circulation j when switching is not interrupted, which is generally known is achieved by a four-way circuit or a flap control.

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Example 1 - "

Bobbins made of solid fibers are suitable in a dye container for high temperature dyeing and dyeing at boiling temperature, brought in. This container is then vented with saturated steam of 1.2 kp / cm and the goods are preheated in this way.

At the same time, the entire · Prepared for the dyeing necessary aqueous liquor amount, which is 10 times the weight of the goods and - based on the Weight of dry goods -

$ 0.7 of the anionic dye Acid Blue 41

(C.I. No. 62130),

a) 20 I » sodium sulfate crystall. and

3 $ sulfuric acid (96 $ ig) or

b) $ 20> sodium sulfate crystall. and .

$ 1.5> formic acid ($ 85). . ·

contains. Above the liquor level, a compressed air pressure of 5.5 kp / cm set.

The pressurized liquor batch is now heated to 105.degree. By opening a shut-off valve in a suitable distribution line, the heated liquor is allowed to enter the dyeing container within 7-10 seconds. The dye preparation should flow into the wound body both from the inside and from the outside. ^{A mixed temperature of 100 °} C. is then established after the liquor circulation has started. With alternating liquor circulation, the goods are now dyed for 20 minutes at the temperature mentioned. Finally, the colored material is rinsed with water in the usual way and dried.

A uniform blue coloration is obtained. .

Used in the above example instead of the blue dye mentioned

0.9 5 »of the anionic dye Acid Green 44, ; (C.I. No. 61590),

20 fo sodium sulfate crystall. and ··.

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. - 6 -

0.5 ^ acetic acid (60 follow) or
8 $ ammonium acetate

used, a uniform green color is obtained.

Example 2

Windings made of wool fibers are introduced into a dyeing container according to the instructions in Example 1, which is used for HT high-temperature dyeing processes and dyeing at boiling temperature is suitable. The liquor approach is carried out in the same way as explained in Example 1, in this case, however, using

of the anionic dye of the formula

1.5

of the reaction product of 1 mol of stearylamine with 12 mol of ethylene oxide,
J Sodium sulfate crystall. and
Acetic acid (60

20th 2

The dyeing process is then carried out as in Example 1, however here with a dyeing time of 30 minutes.

After the usual completion, a uniform purple color is obtained.

example 3 '

Windings made from wool fibers are made according to the instructions in Example 1 placed in a dye container, which is suitable for HT high

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- 7th

temperature dyeing process and dyeing at boiling temperature suitable, is «The liquor approach is carried out in the same way as in Example 1 explained, but in this case using

1.2 $ of the 1 ^ chromium complex compound of

anionic dye of the formula. . -

0.6 fo of a mixture of equal parts of the reaction product of 1 mole of 2-heptadeeyl-4-ethyl-4-hydroxymethyl-oxazoline with 90 moles of ethylene oxide and the transfer product of 1 mole of 2-amino-2-ethylpropanediol-1,3-stearic acid ester with 90 moles of ethylene oxide,

5 fo ammonium sulfate or ammonium acetate and 1 fo acetic acid (60 $ ig).

The dyeing process is then carried out as in Example 1, however here with a dyeing time of 30 minutes.

After the usual completion, a uniform yellow coloration is obtained. . ". '

Example 4 . ·

Windings made from wool fibers are made according to the instructions in Example 1 placed in a dyeing container, which is used for HT high temperature dyeing processes .and dyeing at high temperature "is suitable. The liquor preparation is carried out in the same way as explained in Example 1, but in this case using

50 9822/078 8 J -:.

2 % of the anionic reactive dye of the formula

IT = N- ^0H ■ - GH

1.5 i ° of the implementation product of 1 mole of stearylamine with

12 moles of ethylene oxide,
• 4 fo acetic acid (60 $ ig) and
3 - $> ammonium sulfate.

A Preßluftäruck of 5.5 kp / cm is above the liquor level set.

The pressurized liquor batch is now heated to 105.degree. By opening a shut-off valve in a suitable distribution line, the heated liquor is allowed to enter the dyeing container within 7-10 seconds. The dye preparation should flow into the wound body both from the inside and from the outside. ^{A mixed temperature of 100 °} C. is then established after the liquor circulation has begun. With alternating liquor circulation, the goods are dyed at the stated temperature for 40 minutes. Then an addition of to the dye liquor takes place

5 ^e / o sodium trichloroacetate

and then a further treatment time of the goods of 20 minutes at 100 0. Finally, the dyed material is treated with water rinsed warm and cold. A uniform red color is obtained.

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-Β.

Example 5

Windings made from blends of polyester and wool fibers (im Ratio 55:45), are in one. Dye container, suitable for HT high-temperature dyeing, introduced. This container will then vented by saturated steam of 1.2 kp / cm and thus preheated the goods. ■

At the same time, the entire -prepared for the dyeing necessary aqueous liquor amount, which is 10 times the · weight of the goods and - based on the weight of the dry goods -

1.96 fo of the disperse dye of the formula 0 OH

X = s mixture of 40 # = H. 60 <fo =

0.72 fo of a disperse dye consisting of

approximately equal proportions of compounds of the formulas 0 HH-CH ₂ OH HH ₂ 0 Qj ₁

and

H-CH ₂ OH

1.36

of the anionic dye of the formula

so.

4.5 g / l of efilled. Carrier based on methylnaph-

- ■ ·· ■ · - - thalin

0.3 i ° of a mixture of equal parts of the

. Reaction product of 1 mole of 2.Hsptadecyl-4-ethyl-4 ^ hydroxym0 ^ hyl »-0xa2; olin with .

S09822 / 078i

^ ₁₀ ,

90 moles of ethylene oxide and

of the reaction product of 1 mol

2-Amino-2-ethylpropanediol-1,3-stearic acid ester with 90 moles of ethylene oxide,

4 $ ammonium sulfate or ammonium acetate and
1 io acetic acid (60%).

contains. A compressed air pressure of
5.5 kp / cm set.

The fleet approach, which is under pressure, is now increased to 110 ö
heated. By opening a shut-off valve in a suitable distribution line, the heated liquor is allowed to enter the dyeing container within 7-10 seconds. The dye preparation should flow into the wound body both from the inside and from the outside. A mixed temperature of 104 ° C. is then set after the liquor circulation has started. With alternating liquor circulation, the goods are now dyed for 30 minutes at the temperature mentioned. Do the dyeing
the dyed material is rinsed with water and the staining
is then with an aqueous bath containing:

2 g / l of an emulsifier, based on a mixture of

40 ia of the reaction product of 1 mol
.: Castor oil with 36 moles of ethylene oxide,
42 $ o Phenylkogasinsulfonat (Ca-SaIz) and
18 fa isopropanol, as well

0.5 ccm / l acetic acid (60 "follow)

aftertreated for 10 minutes at 75 G.
A uniform blue coloration is obtained.

Example 6 _t ·.

Windings made from mixtures of polyacrylonitrile and Y / oll fibers (in a ratio of 50:50) are suitable in a dye container
for HT high temperature dyeing and dyeing at boiling temperature. This container is then vented with saturated steam of 1.2 kp / cm and the goods are preheated in this way.

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At the same time, the entire amount of aqueous liquor required for dyeing is prepared in a batch container, which is 10 times the weight of the goods and - "based on the weight of the dry goods - ₌

0.5 i ° of the cationic dye of the formula CH

® Y-N =

IT

/ AV

ZnCl,

0.75 i ° of the anionic reactive dye of the formula

π C-CO-NH-OH

1 fo of the reaction product of 1 mole of stearylamine with

12 moles of ethylene oxide,
1 fo of the reaction product of 1 mole of stearyl alcohol

with 2-5 moles of ethylene oxide,

Contains 20 $ polyethylene glycol of molar weight, ~ 6000

"and .

X cem / l acetic acid (60 ^ ig) to adjust the pH-Y / ertes of the fleet to about 5,.

contains «Above the liquor level, a compressed air pressure of 5> 5 kp / cm set.

The pressurized liquor mixture is now heated to 108 ⁰ C. By opening a shut-off valve in a suitable distribution line, the heated liquor is allowed to enter the dyeing container within 7-10 seconds. The dye preparation should flow into the wound body both from the inside and from the outside. It then turns after the start of a liquor circulation Mischtemperater of 103 ° C. · In mutual liquor circulation is the "commodity colored than 30 minutes at 103 ° C. Hach cooling of the fleet to 80 ⁰ C takes place a

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12 -

* Ibfc

Addition of

5 $ ammonia (25 $ ig)

80 O. Finally, the dyed material is warin with water

and another .Treatment time of the goods of 10 minutes "at 80 ⁰ O. Finally ι and rinsed cold.,

A uniform red color is obtained.

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Claims (5)

'- HOE 73 / f 348 claims: 1. Process for dyeing textile materials made from wool or from Mixtures containing such in the form of wound bodies with anionic dyes according to the exhaust method, characterized in that that he the wound fiber material in a pressure-tight brings dyeing vessel and heated by displacing the air and filling of the autoclave by means of saturated steam or superheated steam at temperatures zwischen_100 ° and 110 ⁰ C, in one of them separate, but connected thereto by piping, as the pressure-tight container approach prepared the entire dyeing liquor and also heated to temperatures between 100 ° and 110 ⁰ C, being closed by special control of the temperature within the stated limits and the vapor pressure in the two Systems and by applying external pressure it is ensured that there is a relative overpressure from 3 to 10 at (= 2.94 to 9.81 bar) comes in the batch container, then the hot dye liquor through the Differential pressure within 3 to 60 seconds simultaneously from the inside and from the outside in the dry or wet Y / ickel body press in and. finally the staining comes to an end in the usual way. 2. The method according to claim 1, characterized in that the Differential pressure for transferring the liquor from the batch container to the dye container is generated by compressed air. 3. The method of claim 1, characterized in that the . The dye container before the dye liquor is pressed in with HD- · ■ Steam flows through, vented, filled and with the goods ) is preheated. . · ■ 4. The method according to claim 1, characterized in that the The dye container before the dye liquor is pressed in and after ». 509822 ^ 0788 pulling with high-pressure steam to generate a relative pressure gradient connected to a lockable condensate line will. 5. The method according to claim 1, characterized in that the anionic dyes are acid, chromium, metal complex and Reactive dyes are used. 509822/0788