DK146450B - PROCEDURE FOR COLORING WINNED TEXTILE MATERIALS OF SYNTHETIC FIBER OR SYNTHETIC FIBER MIXTURES - Google Patents

Description

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(19) DENMARK

§ (12) PUBLICATION (s) 146450 B

DIRECTORATE OF THE PATENT AND TRADEMARKET SYSTEM

(21) Patent Application No .: 0824/74 (51) Filing Date CL3: D06B 5/12 (22) Filing Date: 15 Feb 1974 D 06 P 5/00 (41) Aim. available: 23 Dec 1974 (44) Submitted: 10 Oct 1983 (86) International Application No :- (30) Priority: 22 Jun 1973 DE 2331669 (71) Applicant: * HOECHST AKTIENGESELLSCHAFT; 6230 Frankfurt am Main 80; THE.

(72) Inventor: Hans-Uirich von der * Eltz; DE, Albert * Reuther; DE, Hans-Joachim 'Wassmuth; THE.

(74) Plenipotentiary: Engineering Company Budde, Schou & Co (54) Process for dyeing wrapped textile materials of synthetic fibers or synthetic-fiber blends

Methods of dyeing synthetic fibers by extraction methods under high temperature (HT) conditions have long been known in numerous variations.

The present invention relates to a method of dyeing wound textile materials of synthetic fibers or of mixtures containing such synthetic fibers, with water-insoluble® dispersion dyes by the extraction method, at temperatures of J 110-145 ° C, by which process the wound articles are heated. in a pressure-tight color container prior to dyeing and deaerating and then contacting the combined color tank heated separately at 110 ° C -145 ° C, which is placed under a relative overpressure of 5-10 atm (= 4.9 ° C). 9.8 bar) by transferring the color fleet from the intermediate container into the color container, after which the color processing is terminated by circulation of the color fleet.

Such a process is disclosed in DE Publication No. 1,785,278 and 2,203,401. According to the prior art, deaeration is effected by vacuum treatment of the treatment container and the textile material. This is done in order to be able to transfer the hot treatment float from the mixing container to the treatment container as resiliently and quickly as possible. Since only a partial vacuum can be obtained in systems of a technically practical size with the help of vacuum pumps, there is still a residual pressure which gives some resistance.

In addition, vacuum inevitably leads to a strong cooling of the overall system due to the expansion of the air or the evaporation of moisture, whether from the textile material or from the adhesive float. This is also the case when the system (apparatus and textile material) has been preheated before the evacuation, e.g. using water vapor. There is a significant difference in temperature between product and good looking, which gives rise to large irregularities in the fast contact.

According to FR Patent No. 1,067,236, this known source of error is countered by a further heating of the wet textile material by high frequency current.

It has now been found that even uniform dyes can be obtained even with combinations of several dyes which are otherwise difficult to dye, and at the same time substantial color-time shortening on wound articles of synthetic fibers or of mixtures containing such synthetic fibers. with water-insoluble dispersion dyes by a high-pressure extraction method which does not suffer from the disadvantages mentioned above.

This is done according to the invention by a method which is characterized in that the heating and venting of the wound objects are done by exposing them immediately before the transfer of the color fleet to an atmosphere of hot steam which has approx. color temperature and that the color fleet is passed through large-dimensioned pipelines within 3-60 seconds at the same time, both internally and externally, into the wound elements against the pressure of the air-free atmosphere of hot steam.

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The decisive difference in principle of the invention and of the technique described in DE Publication Nos. 1,785,278 and 2,203,401 is that the color container is not evacuated, but filled with saturated high pressure vapor of about the same temperature used in the subsequent color process until the temperature is equalized. The color container therefore always contains an atmosphere of steam. At the rapid transfer of the color fleet, which is also under high pressure, from the mixing vessel into the color container, the vapor in the latter residual is condensed as a result of the applied pressure difference, thereby even releasing the heat of condensation. There is thus no temperature decrease, which as described above can be disruptive.

In addition to the textile material already being exposed to steam to heat the wound items to color temperature, it has also been found in the method according to the invention that the pre-heated raft is simultaneously pushed into the wound items both from the inside and the outside, on the one side to achieve a uniformity in coloration, on the other hand to spare the items. Only in this way is isothermal rapid staining on wound synthetic fiber blanks possible with uniform staining result.

In contrast, in the known method, it is given in advance that the flow direction of the inserted fleet in the blanks is from inside and out (due to the applied vacuum) and it occurs unilaterally and differently according to the present differences in the density of the windings and at the same time. also different cooling and corresponding decrease in the dye content of the float. The result is, first and foremost, by light shades, an inequality in the staining that can no longer be removed. Experience shows that very bright tones cannot be used at all for impeccable staining by the vacuum method. A further demonstrable disadvantage of the vacuum technique is the uncontrollable deformation of the wound items and the influence of the primarily highly sensitive textured textile material to be dyed.

The disadvantages mentioned above are avoided by the method of the present invention. By exposing the textile material to steam in advance, it is not only vented, but first and foremost it is heated to the color temperature, which lastly applies to the apparatus as well. This eliminates the temperature differences that occur in the supply of heated color floats by the vacuum technique and which cause large affinity differences, primarily at temperatures above 100 ° C. In the process of the present invention, the color fleet meets the same temperature conditions everywhere and is thus not cooled locally.

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Coincidences in the flow paths by the vacuum method are deliberately countered by the method of the present invention by pressing the color float simultaneously at both the inside and the outside, in addition to the circulation pump being started, while the float is being pressed into the material to be dyed. Thus, the wound items are exposed only to flow pressure differences, but not to the high pressure difference between the mixing vessel and vacuum. The pressure in the color container is solely determined by the temperature of the float. A pressure difference only arises from a difference in the pressure in the mixing vessel and the vapor pressure given by the temperature of the float. As this difference in pressure acts on the wound elements both from the inside and the outside as well as the opposite way, there is no need to fear a deformation of the blanks.

The principle of the present invention is that a color float is placed in an HT container with the selected pressure and temperature conditions and from there conveyed by pressure (vapor, compressed air, pump pressure) to another autoclave filled with steam and with the wound fibers of synthetic fibers, e.g. coiled filaments or piece rolls on color bars. This is done by pushing the raft simultaneously, both internally and externally, into the wound elements via similarly large dimensioned pipelines, pumps and a distributor valve. In this way, even with textured synthetic threads, the float is evenly distributed in the material to be dyed in an extremely short time without deformation of rolls and filaments. This requires time of less than 60 seconds, usually even less than 30 seconds. This rapid "push-in" of the color fleet is achieved by a high pressure on the side of the mixing vessel (pressure difference 5-10 atm), which according to the invention is most conveniently produced by compressed air. The color container is pre-frozen for trapped air with pressure vapor, and the product is preheated at the same time. The textile material can be dry or pre-washed, which can take place in the color container itself.

The color container is pressure-proof, well insulated and equipped with a high capacity heat exchanger to keep the color temperature constant. The float itself is heated in the mixing vessel to approx. 140 ° C and then pressed into the vapor-filled color container. Within the scope of this process, the color container, insofar as there is a corresponding difference in pressure, can also be completely filled by closed valve because the vapor present in it condenses with increasing pressure.

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A particular embodiment of the process according to the invention is characterized in that the wound items are exposed to a saturated water vapor atmosphere and that the color container is connected to a blockable condensation line to increase the relative overpressure, which in turn makes it possible to completely fill the color container with the dye preparation at closed air. -ningsventil.

After the entire color float is in the color container, that is, after completion of the insertion, the dye bath is pumped alternately from the inside and the outside and from the outside and in through the material roll by means of a circulation pump. The selected color temperature is maintained at the same time. Now, the final fixation of the dye will take place in a short time. At the high extraction rates under these temperature conditions, it is advantageous to work with sufficiently high transport services of the pump. Over 60 liters / kg / min good color results are obtained. For dyes or dye combinations, which make it more difficult to color evenly, a transport performance of more than 80 liters / kg / min must be worked.

By the peculiar feature of introducing the entire color fleet into the color container at high speed and into the more or less dry material in the form of coiled blanks, the method differs from the hitherto color processes performed so far, which, together with their process variants, have been thoroughly addressed in the literature. Thus, according to the invention, e.g. not only a portion of the color fleet or a concentrated dye dispersion into the color container, but the overall color fleet is pressed in almost stroke. It is not foreseeable that even staining under these conditions can be achieved, as all dispersion dyes have an extremely high drawability at these temperatures.

Furthermore, at such high temperatures, pressure differences and possible turbulences, it is not expected that the dye solutions are still suitable for penetration into wound subjects. Furthermore, it is surprising that even when combining several dispersion dyes, the dye dispersions remain stable, pinning these aggravated operative conditions and not prone to agglomeration.

The fact that the extraction ability of the dyes can be fully utilized at the high temperatures used, is found to be a significant advantage of the process of the present invention.

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The process described is usually carried out in aqueous medium. However, it can also easily be used for coloring based on organic solvents. In the latter case, of course, the process conditions must take into account the boiling point typical of the particular solvent and its vapor pressure.

As the dyes, the conventional trademarks of dispersion dyes in powder or liquid formulations are used. Such dyes are described in Color Index, 3rd edition, Volume 2 under the class designation "Disperse Dyes".

Suitable for carrying out the process of this invention are all synthetic fiber fibers in any processing form which can be stained by the HT staining method. However, the novel method is preferably used for textured fibers of polyamide and of linear polyester material because such fibers are particularly prone to being stained unevenly due to their thermal pretreatment in the texture.

In the dyeing of polyester fibers, no additional additives other than dispersants and equalizers and the chemicals for pH adjustment are required. The pH value of the steam bath between 4.5 and 5.5 allows the stains to be reproduced with dispersion dyes and is obtained by known suitable buffer systems. Both dry and wet material can be treated.

It is important to achieve even coloration that the raft circulation is not interrupted by the switching, which, as is well known, is achieved by a four-way switch or a valve control.

. In some cases, especially when staining woolen yarn material, it has been found appropriate to pre-treat the product in the process of the present invention in about 5 minutes. 10 minutes at temperatures of approx. 60 ° C with an aqueous raft containing 1-3% by weight of the dry product weight, preferably 2% by weight, of a carrier-like aid favoring the dyeing, consisting of 85% by weight perchiorethylene and 15% by weight of an emulsifier mixture, e.g.

7.5 parts by weight of the reaction product of 1 mole of castor oil with 36 moles of ethylene oxide and 7.5 parts by weight of tetrapropylene benzenesulfosuric calcium.

Then, with or without intermediate rinsing, one can insert the hot raft containing the dye preparation.

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Example 1

Coiled items of textured linear polyester filaments are placed in a color container suitable for high temperature staining. This container is then freed from trapped air by saturated steam at a pressure of 2 kp / cm 2 (about 120 ° C) and preheated with the product. At the same time, prepare in a mixing container the total amount of float required for coloring which is 10 times the weight of the product and - based on the weight of the dry product - contains 1.3% dispersion dye of the formula

N = w * TH3 CN

0 OH

3 1 cm / liter acetic acid (60%) 1 g / liter 2,2'-dinaphthylmethane-6,6'-disulfonic acid sodium and 1 g / liter reaction product of 1 mole of isotridecyl alcohol with 8 moles of ethylene oxide.

Above the float level, an air pressure of 2.5 5.5 kp / cm is set using compressed air.

The pressurized beautiful mixture is now heated to 140 ° C.

When opening a blocking valve in a suitable distributor line, let the heated raft run into the color container in 7-10 seconds. The influx of the dye composition into the wound up takes place both inside and outside. After the start of the float circulation, a mixing temperature of 130 ° C is set. By alternating float circulation, the bath temperature is now raised to 135 ° C and the product is stained for 20 minutes at this temperature. Finally, the dyed material is reductively treated in the usual manner and dried.

A uniform yellow color is obtained.

If in the above example, instead of the said dispersion dye, the dispersion dye of the formula is used

6 H

II I

0 OH

a uniform red color is obtained.

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Example 2

Coiled items of textured linear polyester filaments are placed in a color container suitable for high temperature stains. In this container, the product is first rinsed with water at 60 ° C and the rinsing raft is discharged. Next, the method for dyeing the fiber material is further advanced, however the dyeing operation is carried out using 0.7% of the weight of the product of a dispersion dye from equal proportions of compounds of the formulas

NH₂O NH-CH90OH NH₂O OH

^ i ~ II i

OH O OH OH O NH-CH2OH

A uniform blue color is obtained.

Example 3

A knitted product of textured polyester filaments is placed wound on a color boom in a color container of Example 1. After closing the container, the product is treated for 10 minutes at 60 ° C with an aqueous raft containing 2% of the weight of the product of an auxiliary mixture of 85 wt% perchlorethylene 7.5 wt% turnover product of 1 mole of castor oil with 36 moles of ethylene oxide and 7.5 wt% tetrapropylene benzenesulfosuric calcium.

Then, this wash float is pressed into the mixing vessel by compressed air and 0.95% of the weight of the product is added by the dispersion dye of the formula

Br «

II

o of the weight of the product of the dispersion dye of the formula

0 O

TI II

j, Μ I N - R (R = lower alkyl)

II II

o and 1 g / liter of 2,2'-dinaphthylmethane-6,6, -disulfonic acid sodium and acetic acid to adjust the pH to 4.5. A pressure of 6 kp / cm with compressed air is generated over the mixing raft and the raft thus prepared is heated to 140 ° C.

The further coloring of the product is then carried out in the manner described in Example 1, however with 30 minutes of dyeing time at 130 ° C.

A uniform green color is obtained.

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Example 4

A woven article of linear polyester filament, in which the chain consists of textured filaments and the shoot of textured filaments, is placed wound on a color boom in a color container of Example 1. After closing the container, the air is removed from the container by blowing superheated water vapor ( 130 ° C) at the bottom of the container for 10 minutes, displacing the air through the overflow conduit to the open circulation. As soon as steam comes out, the overflow line is closed. The supply of steam is then continued until an internal pressure of 2.7 kp / cm is achieved in the color container. This vapor pressure is maintained for 5 minutes. In this treatment, the textile material is freed from trapped air and the apparatus is preheated. After 5 minutes, the pressure of the saturated steam is lowered to approx.

2 1.5 kg / cm and it is condensed by means of a cooling means.

Next, the color operation is carried out as in Example 1, and the transfer of the hot color float takes place against the residual pressure exerted by the vapor atmosphere in the color container.

Example 5

Coiled yarns of linear polyester and rayon filaments in a mixing ratio of 67:33 are processed and stained in the manner set forth in Example 1.

A polyolefin of the polyester filament fraction is obtained in the product. The staining of the cellulose filament portion can be done in one or two baths using suitable dyes, e.g. direct, reactive and leukocyte ester dyes and others.

Example 6

A linear polyester textured filament mask is pretreated in the manner given in Example 4. After preheating, the product is stained as in Example 1, however, using 2.5% of the weight of the product by a dispersion dye, 1Α6Λ50 consisting of a mixture of differently brominated diaminodihydroxy anthraquinones with less than 1 bromine per liter. molecule dye.

A uniform blue color is obtained.

Example 7

Coiled items of textured linear polyester filaments are placed in a color container suitable for high temperature staining. This container is then freed from trapped air by saturated steam at a pressure of 1.4 kg / cm and preheated with the product. At the same time, in a mixing vessel, the amount of float required for coloring is prepared which is 10 times the weight of the product and - based on the weight of the dry product - contains 0.25 $ of the dispersion dye of formula ^ CN, -v / C2H5

° 2K— = N —ΛΛ — N

\ = / \ = / CgH ^ CN

1 enP / liter acetic acid (60 $) 1 g / liter dispersant based on the condensation product of naphthalenesulfonic acid with formaldehyde.

Above the raft level, a compressed air pressure of 5.5 kp / cm 2 is set.

The pressurized beautiful mixture is now heated to 135 ° C. When opening a blocking valve in a suitable distributor line, the heated raft is allowed to flow from the pressurized mixing vessel into the color container within 7-10 seconds. Thereby, an inflow of the dye composition into the wound subjects must occur both from the inside as well as from the outside. A mixing temperature of 125 ° C is then adjusted. By alternating float circulation, the bath temperature is raised to lj55 ° C. Finally, the colored material is reductively post-dried and dried.

A uniform red color is obtained.

Example 8

The dyeing process carried out according to Example 1 can be carried out using 1% - based on the weight of the dry product - of the dispersion dye 2,6-dicyan-4-ni tro-2-acetylamino-4-die thylamino-azobenzene (West German patent no. 1,290,915) instead of the dispersion dye mentioned in Example 1, with a time commitment of 50 minutes for the color operation.

The plot mixture is heated in the pressure mixing vessel already during the still ongoing prior staining. The time commitment to the actual color process consists of the following processing steps in succession in succession: 1. Filling the color container with a heated raft to a temperature of 55 ° C, start of raft circulation and the formation of the necessary static pressure 0.5 min.

2. Heating the float from 125 to 135 ° C for 10 minutes.

3. Staining at 135 ° C for 20 min.

4. Shut off the color fleet 2 min.

5. Fill the color container with the finishing vessel already prepared in the mixing container 0.5 min.

6. Reductive finishing 5 min.

7. Shutdown of the after-treatment float and rinse at continuous water flow and drain 7 minutes.

8. Treatment with antistatic agents 5 min.

50 min.

The function control and temperature control takes place using the programming, control and monitoring elements developed by the measurement and control technique for appliance color.

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Example 9

Coiled blanks of textured, acidically modified linear polyester filaments are placed in a color bender suitable for high temperature staining. This container is then freed from trapped air by saturated vapor at a pressure of 1.2 kp / cm and preheated for 10 minutes with the product. At the same time, in a blending vessel, the total amount of stain required for coloring is prepared which is 10 times the weight of the product and - based on the weight of the dry product - contains 0.5 # of the dispersion dye of the formula ^ OT2-CH2. 0.1 cm 2 / liter acetic acid (60 # 's) and 5 g / liter glauber salt.

Above the raft level, an air pressure 2 of 5.5 kp / cm is set by means of compressed air.

The pressurized beautiful mixture is now heated to 110 ° C. When opening a blocking valve in a suitable distributor line, the heated raft is allowed to flow from the pressurized mixing vessel into the color container within 7-10 seconds. In this way, an inflow of the dye preparation into the wound items must be done both from the inside and the outside. A mixing temperature of 105 ° C is then adjusted. By alternating float circulation, the bath temperature is now raised to 110 ° C and the product is stained for 20 minutes at this temperature. To the dye bath is then added, via the open circulation, 1 g / liter of a color accelerator based on emulsified chlorobenzene and stained for another 20 minutes. The reductive finishing and drying is done in the usual way for the overall textile material.

A uniform violet color is obtained.