DE19860187B4 - Finishing of sewing threads in the pull-out process and finishing agents for this - Google Patents

Abstract

A method for finishing sewing threads in the pull-out method using an anti-aging bath with an anti-aging agent which comprises an anti-aging agent composition based on an aqueous emulsion of a dialkylpolysiloxane and an organic buffer system which buffers the anti-aging bath in the pH range from 3.0 to 4.5, characterized in that that the buffer system comprises a mixture of organic acids selected from formic acid, acetic acid, citric acid and sulfonic acids and that the buffer system comprises polyacrylates and / or polymethacrylates.

Description

The invention relates to a method for finishing sewing threads in the so-called Pull-out procedure using an anti-aging bath with an anti-aging agent, which one on an aqueous emulsion a dialkylpolysiloxane based aviva drug composition and comprises an organic buffer system.

Such compositions for the treatment of fibers are known from the EP 0055606 A1 known, the pH of this composition should be in the range 2.5 to 7.0.

The finishing of sewing threads or -Yarning is a very difficult process, but it is of the utmost importance for the Goodness and Usability of the end product is. An optimal finish protects the sewing thread the extremely high load on such a thread during the sewing process acts. Due to high sewing speeds, the constant transition from standing to gliding (the so-called stick gliding change or stick-slip) and due to high friction when penetrating the sewing material (e.g. shoe leather) a sewing thread enormously challenged.

A good leveling agent must therefore reduce the friction of the thread, both at high sewing speeds as well as at the transition from Stand for gliding (stick-slip).

In most cases, such sewing threads are made Made of polyester, polyamide or polyester / cotton. When sewing the sewing needle very hot due to the friction, in extreme cases up to 400 ° C. There the melting point of synthetic fibers is well below 400 ° C, would one simply melt such thread, if not the sewing thread finish would provide effective heat protection. This can be done through careful Selection of the product composition can be achieved.

For the application of such finishing agents on the sewing thread there are two fundamentally different techniques:

Zwangsauvlikation

Here the thread is forced with the finishing agent. This is done in a rewinding process, i. H. the thread is unwound from a bobbin, runs through an application device, in which the finish is applied, and is then again wound on another spool. The technical term for such Application device is called Galette.

A godet consists of a trough, in which the product is located. A profiled metal disc turns in this trough and decreases depending on the speed of rotation the disc and viscosity the finish with a certain amount of product.

The sewing thread is defined with Speed passed the profiled godet disk. By Coordination of the speed disc / thread can be a defined Product order done.

Finishings that are applied on a godet, can are in emulsion form or 100%. With the latter then one speaks of so-called cold melts. The thread must be used for emulsions frequently still dry, which is a disadvantage.

There is also a so-called single-lub hot applicator as an application device known. This is also the basic principle of the godet, d. H. a single thread is activated by a defined product order. The single-lub hot applicator is a heatable one Device. The product feed takes place by means of a precision pump. in the Applicator will apply the product immediately before hitting the Thread heated. So a "melt" is applied to the thread. For the single lub Hot application come only 100% products, d. H. no emulsions, in question. Such products are generally viscous at room temperature and only liquid as a melt. Such products are therefore also called hot melts. It can be higher quality Finishing agents, e.g. B. high molecular weight silicones and waxes used than with cold melts, which is why the effects are achievable better.

• – Verwendung von 100%igen Avivageprodukten, daher keine Nachtrocknung nötig
• – sehr gute Gleichmäßigkeit, weil sehr präziser Produktauftrag
• – keine Verschmutzung der Maschinen (Emulsionen neigen zum Antrocknen)
• – sehr gute Aviviereffekte

The advantages of this special forced application are:

• - Use of 100% finishing products, therefore no drying is necessary
• - very good uniformity because of the very precise application of the product
• - no pollution of the machines (emulsions tend to dry out)
• - very good finishing effects

All these advantages of the different possibilities there is an important disadvantage to compulsory application: the operational effort and thus the costs.

Will be sewing threads in large Apparatus colored, where easily 1,000 kg (e.g. divided into approx. 400 Individual spools of 2.5 each kg) can be driven in one batch. In the case of forced application, therefore 400 bobbins are rewound to make the finish, which is on the single thread done to apply. This is rewinding of each individual coil very time-consuming and / or requires a large number of winding devices and Applicators.

Pull-out application

About 20 years ago were first possibilities found sewing thread additives to apply in the so-called pull-out process, d. H. whole dyeing lots are following coloring equipped with a finish in the apparatus. The cost advantage of one such process is enormous.

Such a finishing process only takes about one hour, but then a complete batch is fully equipped and only needs to be dried, which is necessary after the dyeing anyway.

The finishing process is normally carried out on a fresh bath after dyeing or bleaching, ie after rinsing the apparatus used for dyeing and bleaching, into which water is added first, followed by the finish. Alternatively, the EP 0 187 136 A2 plan to carry out finishing directly in the dye bath. This method is partly used in practice, but has not been able to assert itself properly, because after staining there are always rinsing and post-cleaning processes and part of the finishing agent is removed again. The associated wastewater problem (the main component of the sewing thread additives is usually silicone) has not been solved.

This is tempting at first glance simple and inexpensive The pull-out method has a number of difficulties in principle that have not yet been optimally resolved.

A) Uniformity the finishing pad

While in the case of forced application, a clearly definable and even finishing layer is achievable, this is exactly one of the pull-out methods Major difficulties.

When finishing sewing threads this on big Cross-shaped coils wound up (one speaks therefore of packages). The fleet circulates through the standing goods, usually alternately from the inside to the outside and from the outside inside in a certain pumping rhythm. Through the resistance that opposing the cross coils of the fleet when flowing through them are comparative high pump capacities are required to ensure sufficient fleet throughput achieve.

Nähfadenavivagen for the Extraction processes are usually emulsions made of silicone, paraffins, possibly waxes and additives. The emulsion stability of such Avivagen has to to be such that the shear the pump and the flow work does not break the emulsion (this would result in two separate Lead phases). On the other hand, on Nevertheless, an even and complete bath extract at the end of the treatment the finish has occurred, d. H. the conditioning agents available in the bathroom are said to be practically complete absorbed by the treated sewing threads his. Control of stability sewing thread emulsions therefore represents a tightrope walk.

• – Emulgatorauswahl und -menge bei der Herstellung des Avivagemittels
• – pH-Wert der Avivierflotte (je höher der pH-Wert, desto instabiler die Emulsion, desto kritischer aber auch die Scherstabilität)
• – Zusatz von anorganischen Salzen (meist Phosphatpuffer), welche durch die Erhöhung der Elektrolytkonzentration neben ei ner pH-Regulierung auch einen "Aussalzungs-Effekt" bewirken; dieser Effekt destabilisiert die Emulsion
• – Temperaturerhöhung über den Behandlungsverlauf (es wird beispielsweise kalt gestartet und während 30 min auf 65 °C aufgeheizt, dann noch 10 bis 15 min bei Endtemperatur gehalten, um so auch bei verringerter Wirkstoffkonzentration im Bad eine weitere Aufnahme durch den Nähfaden zu erzielen.)

In practice, the uniform and ultimately complete removal of the finishing agent is controlled with the following parameters:

• - Selection and quantity of emulsifier in the manufacture of the finishing agent
• - pH value of the finishing liquor (the higher the pH value, the more unstable the emulsion, the more critical but also the shear stability)
• - Addition of inorganic salts (mostly phosphate buffers) which, in addition to regulating the pH, also cause a "salting-out effect" by increasing the electrolyte concentration; this effect destabilizes the emulsion
• - Increase in temperature over the course of the treatment (for example, it is started cold and heated to 65 ° C for 30 min, then held at the final temperature for 10 to 15 min in order to achieve further absorption by the sewing thread even with a reduced active substance concentration in the bath.)

Achieving one over the Coil run throughout the same finishing pad is always a problem in practice. Even small fluctuations (process water, pH value, etc.) can be sensitive Upset balance. The finish is then enriched indoors or outdoors the coil. Quality fluctuations are the consequence.

B) completeness the bathroom pull-out

An optimally formulated sewing thread finish for the pull-out process must be like this be designed with available to the customer standing variation options - pH value, Electrolyte addition and temperature increase - in the end a 100% bath exhaustion results. Remnants of finish in the bathroom not only reduce the benefit, but also cause problems in wastewater. The exact setting a balanced balance of bath pull-out speed (even support over the whole course of the coil) and in the end complete bath pull-out is a very difficult matter.

A common, the current standard corresponding avivier recipe for the pull-out process looks like this:

amount used

• depending on quality requirements: 6.0 to 15.0% sewing thread finish (50% active ingredient emulsion)

pH for

• a) Polyamide (6.6) and polyester: 6.5 to 7.0
• b) Polyester / cotton: 5.0 to 7.0

For the sake of simplicity, the pH is adjusted with a buffer salt, e.g. B. with
0.2 to 0.5 g / l ammonium acetate or with
0.2 to 0.3 g / l disodium phosphate.

The amount can vary depending on the quality of the process water vary.

The pH range should be maintained during the entire treatment and neither in the stronger al calic area (deteriorating bath stability) in the more acidic area (deteriorating bath exhaustion).

fleet approach

Add water, add pre-dissolved finishing agent, possibly buffer salt solution add for pH adjustment, pH control, possibly pH correction.

Fleet ratio (mass ratio of goods: Fleet)

• 1: 5 to 1:15

temperature program

Let it run cold for 10 min, then at 1 to 2 ° C / min, Depending on the amount used, heat to 60 to 75 ° C until water-clear, d. H. complete Bath exhaustion. With small amounts of finishing agents used, this pulls Bath already below 60 ° C water-clear.

circulation

Only outside / inside or 3 min outside / inside and 1 min inside / outside

desiccation

After pumping out or centrifuging the drying takes place in the high-speed or pressure dryer at 100 to 125 ° C with changing circulation. Drying in a cabinet or high-frequency dryer is also possible.

C) Problem with changing the stick glide due to the electrolyte content of pH regulators, buffer salts, but also through the process water itself

After the finishing process in the exhaust process will then drained and dried.

In the drying process, there are as described above, several technical possibilities. All types of drying common is that the removal of residual water only over the surface of the bobbin possible is.

During the development work within the The present invention has found that electrolytes present in the water - originating from the water hardness or from the buffer additive - during the drying process on the package surface enrich strongly. Such salt residues lead mainly to the inside and outer layers of the winding body to worse yarn gliding values, but above all to dramatically bad ones Stick-slip properties of the thread.

"Stick-slip" or "stick-slip change" (HGW) means the sliding properties of the thread at the transition from standing to sliding. This property is with sewing threads and especially with embroidery threads a very elementary quality factor.

A perfectly equipped thread must one if possible have good stick-slip value. This property is measured on a special thread sliding value tester. The given below Values were measured on the Rothschild electronic tensiometer R-1192. there the thread was moved at a slow speed (0.7 m / min) over corresponding friction body deducted. The thread tension was set to 120 using a thread brake cN set.

The force / tension between the thread inlet and Thread take-off is measured continuously. A thread with good stick-slip properties shows an even behavior. A thread with poor stick-slip builds up periodically a thread tension, which then suddenly collapses again. The thread does not slide dynamically, but initially adheres to the always stronger thread tension leads to a sudden sliding. This Change then takes place periodically. Such behavior is extremely unfavorable for sewing processes because the thread tensions that occur to undesirable seam ripple phenomena, the so-called tension curl, to lead.

If such processes are recorded in a force / time diagram, it looks like this for a thread with very good stick-slip properties 1a shown.

On the other hand, threads with bad stick slip result in a veritable "sawtooth curve" as in 1b is shown.

The more pronounced the "sawtooth pattern", the worse is the HGW of a thread.

In addition to the even distribution of the amount of aviva in the winding body achieving a perfect HGW is one of the most important Factors for the goodness a sewing thread equipment.

The three diagrams show how much the HGW in the outer and inner layers of a winding body can be influenced solely by the electrolyte content of a process water 2a to 2c ,

2a shows the HGW in the outer layer of an advanced thread, process water with low electrolyte content (conductivity approx. 150 μS / cm).

2 B shows the HGW in the outer layer of an advanced thread, process water with a relatively high electrolyte content (conductivity approx. 800 μS / cm), otherwise the same conditions.

2c shows exactly the same thread as in 2 B after a brief rinse (60 sec) with ultrapure water.

These diagrams show how much the electrolyte content of a process water already negatively affects the quality of the HGW. By briefly rinsing with ultrapure water, the electrolytes that had accumulated during drying in the outer layer were removed solved, the initially very poor HGW is significantly improved.

Most used today Nähfadenavivagen for the Pull-out procedure is in the interest of a complete bathroom pull-out additional buffer additive (inorganic salts) necessary to destabilize the emulsion, whereby the electrolyte problem is further aggravated.

The object of the invention is a Process and a finishing agent tailored to this process to introduce with the over seen the coil winding consistently good HGW values can be achieved.

The above task is at a pull-out method for finishing sewing threads of the type described at the beginning Kind according to the invention solved, that as Buffer system an organic buffer system is used which the Aviva bath buffers in the pH range from 3.0 to 4.5.

According to the invention, the buffer system comprises a mixture of organic acids, selected from formic acid, Acetic acid, citric acid and sulfonic acid. The buffer system according to the invention contains polyacrylates and / or polymethacrylates. A preferred sulfonic acid is the amidosulfonic acid.

The basic principle of the present Invention is based on the fact that an organic acidic buffer is used (compared with the usual Buffers that are selected around the neutral point in conventional finishing methods). In addition to a corresponding selection, the acidic pH stabilizes one Aviva drug the emulsion of the Aviva drug composition.

As a result, surprisingly, that this The "sawtooth behavior" of the HGW value described above is largely repressed becomes. This also applies if the preparation of the Aviva bath relatively hard or electrolyte-rich water is used.

The pull-out finishing methods known so far therefore find in the weakly alkaline-neutral or at most weak acidic pH range (6.5 to 7.5) instead, because it was previously assumed that only so the for a complete bathroom pull-out, d. H. a full exploitation of the Active substances present in the bath, required destabilization avivage possible is.

In contrast, the method according to the invention chooses one much stronger acidic range from pH 3.0 to 4.5. Nevertheless, surprisingly, is also in this pH range is a controlled bath extraction that is complete at the end possible, without the At the end of the treatment, the temperature should be raised above the usual level would.

This even applies to process water different Quality, d. H. the bath exhaustion the finish can be even with hard or electrolyte-rich process water, by reducing the buffer quantity and the temperature / time curve to a harmonious pull-out speed and a clear water at the end Bath pull-out is set (more detailed information on this below ) Was added.

The coordinated application of Softening agents and acidic buffer systems can be used in both classic Way as so-called post-avivage, d. H. the avivage will after draining the dye bath and rinsing the goods are newly prepared in the apparatus and used directly in the dye bath become. In this so-called dye bath finish, however, inevitably occur, as described above, by the subsequent cleaning / rinsing required Avivagen losses on.

• – der Auflagenegalität über den Wickelkörper, die häufig unbefriedigend ist;
• – schlechte Gleit- und insbesondere HGW-Werte, in den Innen- und Außenlagen bei Puffersalzzusatz oder elektrolytreichem Betriebswasser (wie bereits oben beschrieben).

The method according to the invention therefore also deviates fundamentally from the previously pursued concept of pull-out finishing in the following relationship. The previously pursued concept of pull-out softening was to reduce the emulsion stability of a sewing thread lubricant by shifting the pH in the direction of neutral-weakly alkaline and / or by adding buffer salt and then to achieve a bath exhaustion by increasing the temperature. This concept has so far had two fundamental problems, namely

• - The level of support over the winding body, which is often unsatisfactory;
• - poor sliding and especially HGW values, in the inner and outer layers with buffer salt addition or electrolyte-rich process water (as already described above).

• – Die Gleichmäßigkeit der Avivagenverteilung über dem Wickelkörper übertrifft die Ergebnisse der herkömmlichen Verfahren.
• – Das erzielbare Gleitwertniveau ist dabei mindestens gleichwertig mit dem der besten herkömmlichen Avivagemittel.
• – Das erfindungsgemäße, saure organische Puffersystem resultiert in sehr guten HGW-Werten nicht nur in den Innenlagen der Wickelkörper, sondern auch in den jeweils außenliegenden Lagen der Wickelkörper. Dies gilt sogar bei stark elektrolythaltigem Betriebswasser.

The coordinated system of aviva active ingredient and acidic organic buffer system according to the invention surprisingly shows three elementary advantages over the conventional method of operation:

• - The uniformity of the finish distribution over the winding body exceeds the results of the conventional methods.
• - The achievable level of sliding value is at least equivalent to that of the best conventional finishing agents.
• - The acidic organic buffer system according to the invention results in very good HGW values not only in the inner layers of the winding body, but also in the outer layers of the winding body. This applies even to process water with a high electrolyte content.

In terms of further reduction The organic buffer system essentially becomes of electrolyte problems free of inorganic ions.

It is preferred to ensure that the aviva bath has a total electrolyte content that has electrical conductivity of the bath of 1,000 μS / cm or less caused. The upper limit of the conductivity of the bath to 900 μS / cm or less set.

Preferred buffer systems according to the invention in the aviva bath ensure that already existing cations are at least partially immobilized, preferably be complexed. This carries obviously to hamper the migration of the Ionic Shares in the drying process, So that the in the outer locations the winding body observed worse HGW values due to electrolyte enrichment be avoided.

The proportion of organic acids in preferred aqueous buffer systems is 10 to 40% by weight. Preferred mixtures of organic acids are:
5 to 20% by weight of citric acid monohydrate
1 to 8% by weight of amidosulfonic acid
5 to 20% by weight of formic acid
the percentages by weight refer to the proportions of the acids in the aqueous buffer system.

A portion of the buffer system, often acetic acid, can be added to the aviva active ingredient composition from the outset. Here proportions of 0.4 to 1% by weight based on the total weight come of the finish agent preferred.

More preferred aqueous buffer systems include Polyacrylates and / or polymethacrylates with a share in the buffer system formulation from 1 to 10% by weight.

A is preferably used as an aviva active ingredient Dialkylpolysiloxane with a viscosity of 350 to 10,000 cP, preferred 800 to 5,000 cP, at 25 ° C used. A dimethylpolysiloxane is further preferred as the dialkylpolysiloxane used. The dialkylpolysiloxanes are in the Aviva drug composition preferably contained with a content of 15 to 40 wt.%.

The aviva drug composition can in addition to the dialkylpolysiloxanes, paraffin waxes, ester waxes, emulsifiers, Contain polyglycols and / or preservatives.

Preferred aviva drug compositions several emulsifiers are used side by side. This will be in the individual further below explained.

The ester waxes are preferred in the range up to 4% by weight in preferred aviva drug compositions used.

Polyethylene glycols as preferred Representatives of the polyglycols preferably come with a content of 1 to 4% by weight used in aviva active ingredient compositions, where polyethylene glycols in a molecular weight (Mw) range of 2,000 to 20,000 as particularly cheap have proven.

Preference is given to the process according to the invention the Aviva bath at room temperature first the Aviva active ingredient composition and then added the buffer system.

The Aviva drug composition and the buffer system are preferably prediluted (factor = 10) before can be added to the Aviva bath.

The temperature of the Aviva bath is in the course of the extract finish after adding the active ingredient composition and buffer system to approx. 65 ° C raised. The temperature is raised gradually over the Treatment time, for example with 1 to 2 ° C / min, preferably with a Rate of approx. 1.2 to 1.7 ° C / min.

For example, the Avivage pre-diluted are specified, and after 5 minutes of circulation of the liquor, the prediluted buffer according to the invention are added, followed by a further 5 min at room temperature an increase in temperature at a rate of 1.5 ° C / min 65 ° C for approx. 30 min. The fleet is at this elevated temperature while circulated another 15 min and only then drained, drained and dried the fleet.

The invention further relates to a softening agent for use in that described above A method comprising an Aviva active ingredient composition, which is based on dialkylpolysiloxanes, and on the other hand an organic one Buffer system for buffering in the pH range from 3.0 to 4.5 comprises. The Buffer system according to the present Invention includes a mixture of organic acids, selected from formic acid, Acetic acid, citric acid and sulfonic acids. The buffer system includes Polyacrylates and / or polymethacrylates. A preferred sulfonic acid is the amidosulfonic acid.

Usually the aviva active ingredient composition and the buffer system sold separately packed. This enables the softening agent according to the invention exactly to the conditions existing on site at the customer, d. H. in particular, adjust process water and the sewing thread qualities to be treated. However, the aviva drug composition can be part of the buffer system included to stabilize the emulsion by lowering the pH.

As mentioned earlier, Dimethylpolysiloxane is preferably used as the dialkylpolysiloxane. The dialkylpolysiloxanes used will preferably have a viscosity of approx. 350 to 10,000 cP.

The finishing agent according to the invention or its Drug composition can Paraffin waxes, ester waxes, emulsifiers, polyglycols and / or preservatives be clogged.

Paraffin waxes are preferred, which have a melting point in the range from 50 ° C., preferably 60 ° C. and higher. The melting point should more preferably be below 100 ° C. to ensure sufficient abrasion resistance of the waxes.

The emulsifiers are preferred Fatty acid amine condensation products and / or castor oil ethoxylates include.

The fatty acid amine condensates are preferred those in which the fatty acid component contains a C ₁₄ -C ₂₀ fatty acid or a mixture of such fatty acids.

The amine component of the condensate is preferably selected from aminoalkylalkanolamine and dialkanolamine, the respective alkyl-functional groups being C ₁ -C ₄ -alkyl groups.

The content of the fatty acid amine condensate in the aviva active ingredient composition is preferably 1 to 8% by weight; in the case of the use of castor oil ethoxylate it is Proportion preferably 0.5 to 5% by weight.

Different emulsifiers are more preferably used side by side, for example in a preferred formulation of the active ingredient composition
0.5 to 5% by weight of castor oil ethoxylate,
1 to 5% by weight of fatty acid aminoalkanolamine condensate and
0.2 to 5% by weight of fatty acid dialkanolamine condensate
contains.

Preferred castor oil ethoxylates have an EO degree of approx. 100 to 400.

The organic buffer system will preferably selected so that it at least parts of inorganic cations that occur in the Aviva bath, is able to complex.

In addition to organic acids, preferred constituents of the organic buffer system are acrylate and / or methacrylate homo- or copolymers. The molecular weight M _w is preferably 2,000 to 10,000, more preferably 2,500 to 5,000.

Particularly preferred ingredients of the buffer system are copolymers of acrylic acid and maleic acid a monomer ratio from 1: 1 to 3: 1.

These and other advantages of the invention will be explained in more detail below with reference to the drawing and the examples. It show in detail:

1a : a so-called HGW value diagram, which can be assigned to a thread with a very good, so-called stick-slip;

1b : HGW value diagram of a thread with poor stick-slip;

2a : HGW value of an outer layer of an advanced sewing thread when using process water with a low electrolyte content (conductivity approx. 150 μS / cm);

2 B : HGW value in the outer layer of an advanced sewing thread under treatment conditions as with 2a , but with a process water with a relatively high electrolyte content (conductivity approx. 800 μS / cm);

2c : HGW value diagram of the thread according to 2 B after rinsing with ultrapure water for 60 seconds;

3 : Time / temperature diagram of an Avivier pull-out method according to the invention;

4a : HGW diagram for a sewing thread equipped according to the invention;

4b : HGW diagram of the advanced sewing thread according to 4a , but without the buffer according to the invention;

5 : Time / temperature diagram of a dye bath-finishing method according to the invention;

6a : HGW diagram of a sewing thread treated in a dye bath extract with conventional finishing agent

6b : HGW diagram of a sewing thread treated in the dye bath extract with a finishing agent according to the invention; and

6c : HGW diagram of a sewing thread treated in the dye bath extract with a finishing agent according to the invention ( 6b ) after further aftertreatment according to the invention.

Using the following sample recipes and 3 to 6c the invention will be explained in more detail.

Example 1

A specific formulation for the aviva active ingredient composition is as follows:
30% by weight dimethylpolysiloxane with a viscosity of 1,000 cP (at 25 ° C)
10% by weight paraffins with a melting point of 60 to 65 ° C
2.5% by weight of ester wax (Hoechst Wachs KLE)
3.5% by weight emulsifier based on tallow fatty acid aminoethyl ethanolamine
0.3% by weight emulsifier based on specific fatty acid amine condensate products, for example tallow fatty acid diethanolamine condensate
1.3% by weight emulsifier based on castor oil ethoxylate with approx. 100 to 400 mol EO
3.0% by weight of polyglycol M _W , 12,000
0.6% by weight of acetic acid (part of the buffer system)
possibly usual preservatives
Rest of water

As mentioned above, the share of 0.6% by weight of acetic acid a component of the following in the aviva active ingredient composition still described in detail buffer system, which, however is already required in the aviva active ingredient composition, to keep the emulsion there stable.

The buffer system according to the invention is otherwise composed as follows:
approx. 5% by weight acrylic acid / maleic acid copolymer M _w approx. 2,500 to 5,000; Monomer ratio 1: 1 to 3: 1
approx. 13% by weight citric acid
approx. 5% by weight amidosulfonic acid
approx. 14% by weight of 85% formic acid
Rest of water

The aviva active ingredient composition defined above is used in the aviva bath in a concentration of 10% by weight. The buffer defined above will in an amount of 1.5 g / l added to the Aviva bath already mixed with the Aviva active ingredient composition. The addition occurs in each case (cf. 3 ) at 20 ° C and at a distance of 5 min, each in 10 times prediluted form.

It is dealt with in the present example a polyester fiber yarn (Nm 80/2) in a package with a liquor ratio from 1:10.

The conductivity of the process water is approx. 800 μS / cm, d. H. the process water is relatively rich in electrolytes. The circulation the fleet is set to cycle 2.5 minutes from the inside to the inside Outside and then 4 minutes from the outside inside in constant Repetition.

After adding the Aviva active ingredient composition (10% by weight) and subsequently 1.5 g / l of the buffer system according to the invention a pH value of 3.2 is established in the Aviva bath, which is no further needs to be corrected.

5 min after adding the prediluted buffer system is at a rate of 1.5 ° C / min while 30 min to the temperature of 65 ° C heated. The temperature of 65 ° C is held for a further 15 min. The result is a uniform, on End of treatment water-clear bath extract.

Then the fleet is drained, the goods are dewatered and dried. The so-called HGW value is then measured. The result is in 4a shown.

You can see that despite using very Electrolyte-rich process water with a conductivity of 800 μS / cm (the Avivierbad has a conductivity after adding the buffer system according to the invention of 849 μS / cm on) receives one optimally pushed back "sawtooth formation" that almost in the noise of the measuring device goes down, is obtained.

This approach became comparative repeated, with the only difference that the buffer according to the invention was omitted.

While the inner layer of the cross-wound HGW value curves similar to that 4a show, you can find a HGW course in the outer layers, as in 4b is shown. This means that, due to the buffer system according to the invention, an extremely strong damping of the "sawtooth formation" is possible even with an optimally selected aviva active ingredient composition. This is attributed to the fact that - although the conductivity of the Aviva bath increases slightly due to the addition of the buffer according to the invention (from 800 to approximately 850 μS / cm) - the migration tendency of the electrolytes when drying into the outer layers of the cheese is practically prevented, so that over the entire bobbin, ie in inner and outer layers, essentially the same yarn quality, ie the same good HGW behavior as in 4a shown, can be obtained.

Example 2

As already mentioned, the aviva active ingredient composition and buffer system according to the invention can also be applied directly during the dyeing. The procedure for a dtex 50/2 polyester core is described below:
The yarn to be wound in cheese package is first in the usual manner after z. B. pre-washed the following recipe:
0.5 to 1.0 g / l non-ionic detergent (e.g. PERLAVIN NIC / Petry)
0.5 to 1.0 g / l sequestering agent (e.g. PERIQUEST APG / Petry)
0.5 g / l soda calc.
Wash for 20 minutes at 70 ° C
Rinse warm for 10 min, 40 ° C
Rinse cold for 10 min

Then the dye / finish bath is added.
x% disperse dye
1 to 2 g / l leveling and dispersing agent (e.g. PERIGEN PME / Petry)
0.5 to 2 g / l according to the invention. Buffer system (example 1)
8 to 15% by weight according to the invention. Aviva drug composition (Example 1)

The pH value is set automatically to 3 to 4 and need not be further corrected.

Usually is the start temperature 40 to 50 ° C.

The fleet is preferably alternately the bobbin pumped, e.g. B. 2 min from the inside out, followed of 4 min outside inside.

After adding the dye, auxiliary agent, buffer system and anti-aging agent composition, treatment is continued at 40 to 50 ° C. for 5 minutes. Then the temperature is increased at 1.5 to 2 ° C / min to 130 ° C. After a treatment time of a further 30 to 60 minutes, the liquor is hot-drained or it is cooled to 80 ° C. and drained (cf. 5 ).

In the case of light colorings, hot and warm rinsing takes place. In the case of dark colorations, reductive cleaning may be necessary with
1 g / l anionic / non-ionic dispersant (e.g. PERLAVIN SRD / Petry)
3 to 5 ml / l sodium hydroxide solution 50%
3 to 5 g / l hydrosulfite
Treat for 20 min at 80 to 90 ° C, rinse hot and warm, neutralize with
0.5 to 1 g / l buffer system according to the invention

Then it is drained and dried.

6a to 6c show the HGW value of the outer layer of a polyester core yarn that has been finished in the dyebath using the above-mentioned process.

It was here again with electrolyte-rich Water (approx. 800 μS / cm) worked. The coloring was carried out with 2% by weight of disperse blue 56.

at 6a 10% of a 50% commercial, state of the art ( EP 0 187 136 A2 ) Appropriate finishing agent used.

A pronounced sawtooth curve resulted.

at 6b 10% of the aviva active ingredient composition described in Example 2 was used. Instead of using the preferred acidic buffer system according to Example 1, the pH was adjusted to 4.5 with acetic acid.

A better one has already resulted Stick-slip, but still with clearly visible scatter.

at 6c 10% of the aviva active ingredient composition described in Example 1 was used. In addition, 1 g / l of the preferred buffer system according to the invention was used both in the dyebath and in the neutralization after the reductive cleaning.

The result is an even stick-slip image.

Claims (27)

A method for finishing sewing threads in the pull-out method using an anti-aging bath with an anti-aging agent which comprises an anti-aging agent composition based on an aqueous emulsion of a dialkylpolysiloxane and an organic buffer system which buffers the anti-aging bath in the pH range from 3.0 to 4.5, characterized in that that the buffer system comprises a mixture of organic acids selected from formic acid, acetic acid, citric acid and sulfonic acids and that the buffer system comprises polyacrylates and / or polymethacrylates. A method according to claim 1, characterized in that as sulfonic acid Amidosulfonic acid is selected. A method according to claim 1 or 2, characterized in that that this Procedure as post-aging is carried out. A method according to claim 1 or 2, characterized in that that this The process is carried out as a dye bath finish. Method according to one of claims 1 to 4, characterized in that that this organic buffer system essentially free of inorganic ions is. Method according to one of the preceding claims, characterized characterized that the Aviva bath has a total electrolyte content that is electrical conductivity of the bath of 1 000 μS / cm or caused less. Method according to one of the preceding claims, characterized characterized that the Buffer system complexing agent for cations present in the Aviva bath. Method according to one of the preceding claims, characterized characterized that as Dialkylpolysiloxanes with a viscosity of 350 to 10,000 cP 25 ° C can be selected. A method according to claim 8, characterized in that as Dialkylpolysiloxan Dimethylpolysiloxan is used. Method according to one of the preceding claims, characterized characterized that the Finishing agent paraffin waxes, ester waxes, emulsifiers, polyglycols and / or preservatives. Method according to one of the preceding claims, characterized characterized that the Aviva bath at room temperature first the Aviva active ingredient composition, optionally with a part of the buffer system, is added, and then added the buffer system or the remnants of the buffer system become. A method according to claim 11, characterized in that the Temperature of the aviva bath after addition of the aviva drug composition and the buffer system is raised to approx. 50 to 90 ° C. A method according to claim 12, characterized in that the Temperature increase at a rate of 1 to 2 ° C / min, especially about 1.2 up to 1.7 ° C / min he follows. Finishing agent for finishing sewing threads using the pull-out method comprising an aviva drug composition based on dialkylpolysiloxane and an organic Buffer system, characterized in that the buffer system polyacrylates and / or Polymethacrylates and a mixture of organic acids selected are made: formic acid, Acetic acid, citric acid and sulfonic acids. Finishing agent according to claim 14, characterized in that the sulfonic acid amidosulfonic is. Finishing agent according to claim 14 or 15, characterized characterized that the Aviva active ingredient composition and the buffer system packed separately are, the aviva active ingredient composition optionally individual Components of the buffer system can contain. Finishing agent according to one of claims 14 or 16, characterized in that the aviva active ingredient composition comprises dimethylpolysiloxane. Softening agent according to one of claims 14 to 17, characterized in that the Aviva active ingredient composition dialkylpolysiloxanes with a viscosity in the range from about 350 to about 10,000 cP. Softening agent according to one of claims 14 to 18, characterized in that the Aviva active ingredient composition paraffin waxes, ester waxes, emulsifiers, Includes polyglycols and / or preservatives. Finishing agent according to claim 19, characterized in that that the Paraffin waxes have a melting point in the range of 50 to 90 ° C. Finishing agent according to claim 19 or 20, characterized characterized that the Emulsifiers fatty acid amine condensates and / or castor oil ethoxylates. A softening agent according to claim 21, characterized in that the fatty acid amine condensate is a C ₁₄ -C ₂₀ fatty acid amine condensate. Finishing agent according to claim 21 or 22, characterized characterized that the Amine component of the fatty acid amine condensate selected is from aminoalkylalkanolamine and dialkanolamine. Softening agent according to one of claims 21 to 23, characterized in that the Fatty acid amine condensate content Is 1 to 8% by weight. Finishing agent according to claim 21, characterized in that that the Castor oil ethoxylate content 0.5 is up to 5% by weight. Softening agent according to one of claims 21 to 25, characterized in that it Castor oil ethoxylate with a proportion of 0.5 to 5% by weight of fatty acid-aminoalkylalkanolamine condensate with a content of 1 to 5 wt.% and a fatty acid dialkanolamine condensate with a content of 0.2 to 5 wt.% Contains. Softening agent according to one of claims 14 to 26, characterized in that the organic buffer system complexing agent for at least parts of the inorganic Cations of the Aviva bath included.