DE1910526U - ARTIFICIAL THREAD. - Google Patents

Description

Patent Attorneys RA. 798 71 0 * 12-11-64

DR.-ING. WALTER ABITZ

DR. DIETERMORF

Munich

November 12, 1964 L-84 / R

Ε »Io DU PONT DE NEMORS AND COMPANY 10tii and Market Streets, Wilmington 98, Delaware, V ° StoA <

Artificial thread

The invention relates to melted elastic structures, in particular threads made of synthetic, segmented ₉ elastomeric copolymers on which there is a polyamylsiloxane-containing lubricant or lubricant preparation »

Elastic threads made of rubber or a segmented elastomer ₉ »B. of the spandex type, as is well known, generally require a Schmälzpräparation

1 -

"Gluing" of the yarn in other areas, resulting in, "endure erratic circuit voltages yarns The classic lubricants for rubber = _s is a" ber, the Taik _5, which can also be used for lubricating of spandex threads as lubricants many disadvantages ο The Talk problematic in terms of cleanliness as well as the risk of dust "because in the area where the finishing and processing of the thread material takes place, the talc is scattered" In addition, talc-coated threads cause serious abrasion problems in both the spinning machines and the treatment devices.

Oils should be a worthwhile substitute for talc in order to eliminate these disadvantages »It has been generally recognized, however, that oils cannot be used for narrowing rubber threads due to their negative effect on the physical properties» A solution to this problem when using. Oils resulting in spandex threads Prob = lems associated with the USA Patent 3,039,895 is available, according to which a textile oil ₉ as mineral ^ as a preparation for threads of synthetic, segmented, elastomeric Mi-sehpol ^ · = merisaten usable _s is when in fine particles of certain metal soaps dispersed in it _o This represents a considerable advance in the field of the preparation of threads of the spandex type ₉ but because of the necessary availability

- 2 -

the fine soap parts in the Pxäparationen according to the aforementioned Patent specification, improvements are still desired, especially with regard to a tendency of the dispersed Solid particles in the preparation troughs settle, and an accumulation of deposits in thread guides and needles of knitting machines and other devices on which the elastic threads are processed ο Well-known liquid preparations for spandex threads also have the drawbacks, su a tendency to favor the discoloration of the threads with regard to an antistatic protection much too to leave something to be desired or have an unpleasant smell ο

The present invention provides elastic threads with a soak malt preparation which can be processed without difficulty, in particular a stable preparation which does not need to contain any particulate solid material and which nevertheless gives adequate frictional properties on the threads. The elastic threads according to the invention have a sliding finish _P which (1) can be used on the threads in "smaller amounts than was previously necessary, (2) the fences - plasticized and (3) provides antistatic protection without discoloration promote ο Further advantages and details of the purpose result from the following description ο

According to the invention, these parts are achieved with an elastic structure in the form of a thread made of a synthetic, segmented, "elastomeric! Copolymer, which has a sizing preparation that has a smaller proportion of a polyamylsiloxane component with a viscosity of about 8,000 as the essential constituents up to 20,000 cSt and a larger proportion of a polydimethylsiloxane = component with a viscosity of about 5 to 100 cSt ο It has shown that, surprisingly, the polyamylsiloxane with Yer = twist in connection with the polydimethylsiloxane not only results in a superior gliding ability of the elastic thread ₉ without having to disperse solid particles in the preparation, but also obtain a substantial degree of anti-static protection Fadeil more pliable and on top of this e way made easier to process The statement made here that the polyamylsiloxane is present on the elastic thread is not limited to the fact that the total amount of the component is present on the surface of the thread, but the polyamylsiloxane can also be partially absorbed »

L-84 / R

The polyamylsiloxane that is used in combination with the polydimethylsiloxane the advantages according to the invention results is a liquid, trifunctional polyamylsiloxane with unique Properties »It is obtained by hydrolysis and condensation of n-amyltrichlorosilane, which in turn according to the USA patent = writing 2,632,013 by converting trichlorosilane and pentene-I can be obtained ο The hydrolysis of the amyltrichlorosilane will in a medium made up of isopropyl ether and water through = performed ο It is washed several times and the hydrolyzate is neutralized by reflux treatment with a mixture of sodium carbonate and water, removes the ether and the water, dissolves the hydrolysis product in toluene and subjects it to a reflux treatment with sodium hydroxide, for another condensation equation cause weight reduction au, with the remaining water as Azeotrope with toluene is removed "The product is then filtered, whereby a liquid with a viscosity in the range from 8000 to 20,000 cSt is obtained. “A polyamylsiloxane with a yiscosity in the range from 13,000 to 17,000 cSt is used according to the invention preferred*

The trifunctional polyamylsiloxane obtained in the above manner is different from the conventional trifunctional Siloxane resins are quite strong in that the aim is to reduce residual chloride and hydroxyl to a minimum ο The conventional, trifunctional siloxane resin systems are made

To achieve ■ known generally made with the express purpose of a sufficient hydroxyl to secure a proper cure and or "or alkoxy content» In Mnaus contain conventional resin systems bifunctional units _s to improvements in the properties to maintain and ensure niederviseose properties. " The reason "why the polyamylsiloxane resin differs so much in its behavior τοη closely related substances is not completely clear ο A possible explanation for its behavior can be that the siloxane polymer is obtained in the form of cyclic chains instead of in a strongly crosslinked!" Form "One of the outstanding properties of polyamylsiloxane is its compatibility with conventional dimethyl silicones and with mineral oil"

The polydimethylsiloxanes, which are combined to obtain the erfindungsge = Mäss used preparations with the Polyamylsiloxanen are familiar silicone oils ₀ The PoIydimethylsiloxane with viscosities of about 5 to 100 cSt at 25 ° G represent solvent for the Polyaraylsiloxane is, both at 25 C a homogeneous Forming a mixture ο You can work with mixtures of any component «■

The segmented copolymers from which the elastic threads according to the invention can be obtained consist of segments of a high-melting, crystalline polymer ₉

alternate with segments of a low-melting, amorphous polymer ο The crystalline ₉ high-melting segment can e.g. Bo can be traced back to a polyurea, a polyurethane, a polyamide, a bis ~ ureylene polymer or a polyester, and the low-melting, amorphous segment Z ₀ Bo is based on a poly == ester ₈ a polyether or a hydrocarbon polymer o The explanation of such a segmented copolymer the polymers of the spandex type are used. The segmented copolymers can have a linear or a crosslinked structure

Those in various patents, including the United States patent specifications, are useful in practicing the invention 2 929 801, 2 929 802, 2 929 803, 2 929 804, 2 957 852,

2 962 470, 3 009 901, 3 023 192, 3 037 96O ₅ 3 040 003,

3 044 987, 3 044 989, 3 044 990, 3 071 557 and 3 097 192, ■ described segmented copolymers ° As described in these references, such segmented copolymers in thread form result in elongations at break above 200 "fo ₉ an elastic recovery (or recovery from tensile stress) of about $ 90 and a tension decay (under continuous tension) of less than about 20 $ “The terms elastic recovery and stress decay are described in US Pat defined

The application of the preparations according to the invention to the threads made of the segmented elastomers can be carried out in a conventional manner. In general, required to achieve advantageous antistatic properties of such a preparation an amount that is at least about O ₉₀₂₅ i "of Polyamylsiloxane respect present on the weight of the untreated elastic Fadens5" can be an absolute minimum amount of the poly = amylsiloxans for all cases, however, do not specify _o According to nature, it is desirable ₉ that the static charge "is minimal in the course of the thread ο With conventional spandex threads, a maximum value of the static charge of ± 1000 V _{9 is} determined at a thread speed of 18.3 m / min" in the manner described below , acceptable =

There is no decisive upper limit for the polyamiloxane amount ₉ but in general amounts above about 2% are unnecessary practical considerations with regard to viscosity and ease of application also determine the amount of the various components in the preparation. The expert can select the percentages light enough to the required percentage of polyamylsiloxane on the threads receives _o For general purposes, calculated as the practical upper limit a Yiscosität the preparation of about 100 cSt at 25 ° G ₀ This Höchstviscosität is with a mixture of about 50 fo polyamylsiloxane obtained with a viscosity of about 8000 to 20,000 cSt at 50 f> polydimethylsiloxane having a viscosity of 20 cSt

The total amount of preparation to be applied to the threads is not critical, and there is a limitation for practical considerations o Since very large amounts, such as 12 ^C J>, can lead to the preparation dripping off the threads, smaller amounts should in most cases be used Find use <=

The preparation can be applied to the elastic threads by the usual methods, such as by dipping, padding or spraying. One can treat moving threads ;, z _{o 0} B spraying or baths, or any wicks or similar devices, one of which receive the preparation, lead "A convenient application is the filaments over a roll au.führen ₉ in a the Trough containing preparation is immersed ο If the preparation is continuously applied to spandex threads during spinning ₉ the trough-roller arrangement is preferably arranged immediately after the first driven feed roller ₉ with which the spandex threads come into contact after leaving the spinneret ο

The addition of a preparation containing polyamiloxane to the spinning solution, do ho the simultaneous spinning of both, results in convenient and advantageous application »The preparation components are added to the spinning solution and pressed it at the same time with the thread-forming fabrics from »Particular

this working method is advantageous when spinning from fine = titre, elastic thread «, z, Bc spandex of 20 den ο this Mode of operation does not require an applicator roller and allows a "lower spinning tension," which in the production of fine Titer is particularly important *

The essential components of the preparation according to the invention are the polyamylsiloxane and polydimethyl == siloxane, but may be added other ingredients, without any detrimental effect to the obtained with the essential ingredients sliding properties and antistatic properties "get au So you can ζ ο Bo minor amounts of other silicone oils, mineral oil, butyl stearate, methyl, ricinoleate, butyl acetyl _s oil soluble polyether · = glykoleη and alkylphenol ethers enforce isopropyl alcohol and trichlorethylene are also compatible with the Polyamylsiloxau and find him using _o Special plasticizers for spandex ~ threads can be used , but are generally not required when working with the preparation according to the invention due to the favorable plasticizing effect of the polyamylsiloxane. Such plasticizers include ethylene oxide = fatty acid adducts, e.g. B. a polyethylene oxide ester of stearic acid ο In some cases, you can use metal soaps, such as the soaps mentioned in US Pat. No. 5,039,895, ζ. Bo

Zinc stearate and magnesium stearate, in small quantities ,, d _o ho of less than about 2 Custom? S enforce ο However, one can on mineral oil and dispersed Peststoffe such as the aforementioned, while working with the preparation according to the invention fully = constant refrain. " The elimination of this material results in obvious advantages in terms of cleanliness and safety _etc.

The ■ 7 / egf all of the mineral oil from the preparations geinäss the invention of spandex and eliminating the need ₉ as magnesium stearate according to US 'Patent 3,039,895 ₉ to work out with dispersed solids ;, when working with the preparations according to the invention au obvious benefits in terms of cleanliness and safety <>

The melted9 elastic threads according to the invention are suitable for a variety of products in the braided as well as the non-braided state = the continuous threads are particularly suitable for corsetry ₉ belts, corsets _? Stocking = goods for medical and orthopedic purposes, woven or knitted visual clothing, socks and sock edges =, The pile mixes are suitable for a variety of elastic products or stretch = · products ₉ including woven, knitted and nonwoven fabrics for use in clothing With universal fit, shapely upholstery or ο cover material, rubber stockings and ribbons

P.A.060 'tB3-M.65

E 20 757 / 8k Gbm 4 «February 1965

E ₀ Ϊ »du Pont de Iemours

and Company L-84 / R

for purposes Schiemmgs "The invention further allows for stocking _9;? arene and elastic KTetswaren ^ as elastic. IuIl ₈ achieve a reduced streakiness «,

The following examples ^ in which Q? Eil ~ and percentages. Unless otherwise stated "on the weight beaiehen ₉ to further illustrate the invention, are _s without the invention being limited" In Examples 3 ₉ 4 and 5 the formation of static charges on the thread samples is determined using a "Keithley Electrostatic Voltmeter ⁵¹ " type voltmeter, by measuring the charge that accumulates on a matt surface when the sample is tested

at an angle of 70 ° with a load of 10 g and a relative humidity of 60 to 62 $ and a temperature of temperature from 22 to 23 ° C is passed over the stick o clay example 5 apart from that, the pad material is transported at a speed of 18.3 m / min ■> guided over the rod *

As the following examples show _s the physical properties of the elastomeric Padengutes not adversely affected by the presence of Polyamylsiloxans in the preparation When misstj strength., The Dehnungj the module, the voltage decay with continuous train and the elasticity or Zugerholung, substantially the same values as for the same elastic thread - which has no preparation j, obtained =, essentially corresponding

- Heue page 12 - '

results are obtained ₉ if mart in the spandex threadguH; In the examples, the polyether is replaced by a polyester or a lated polyurethane. Substantially corresponding results are also obtained when the bis-ureylene or urea segments of the spandex material in the examples are replaced by a urethane or amide Segment to be replaced.

As explained in some examples, preparations containing polyamylsiloxaa and polydimethy isiloxane show "good behavior when used in extremely low consentrations on the thread material" Although an absolute minimum amount for all uses of the spandex thread material cannot be given, "it is generally required For narrowing the thread material at least about 1 fo preparation »Preferably, the preparation is used on an elastic thread material according to the invention in an amount in the range of about 2 to 4 ^ ₉ based on the weight of the thread material =

In the following examples, before the polyamylsiloxane-polydimethylsiloxane preparation is applied, a multi = fil of a coarse titer formed by the growing together of many smaller threads. On the other hand, a single mono · = Press out and treat fil or fine-titer single threads 2. Β »of 6 denier or below, first treat with the preparation and then collect on a continuous cord that

Stack can be cut ο The elastic staple fiber can then, as in üSÄ patent specification 3 00? 227 described » with inelastic staple fiber with the formation of mixtures are mixed together, which are suitable for the formation of elastic yarns » The batch mixes can also be obtained by the melted continuous filament cable is mixed in a corresponding manner with a cable made of inelastic continuous filaments and then cuts the cable mix on a stack (according to USA patent specification 3 077 006) ο

At sp 1 e 1 1

Polytetramethylene ether glycol (molecular weight about 2000) PsP'-methylenediphenyl diisocyanate are intimately mixed in a molar ratio of 2 moles of diisocyanate per mole of polyether glycol and reacted for 90 to 150 minutes at about 96 ° C to form a pol ^ ätförs having isocyanate end groups ° G cooled, Xsoe ^ änat-Endgrüppen polyethers having a speed of 173 ISSE ilen / std "into a mixer and are a current N ₉ BW) imethy! acetamide 27 ₉ 6 O? rush / h ₀ to" The Geraisch (solids content 39 <fa) is continuously discharged into a pipeline and fed to a second mixer in which it is "acetamidstrom containing 9.1 $ m intimately with a dimethyl>» xylylenediamine and O ₉ 6 <fo _{diethylamine?} at a total speed of 1O ₉ 3 parts / hour. is supplied, mixed, the Yerweilaeit

3> to 4 min * and the temperature rises from about 40 to 90 ° C »The emerging polymer solution contains about 33.7 1" solids and has a viscosity of 1450 P at 40 ° Co. The polymer has an inherent viscosity ) of 1.27 "at 25 ° C in hexamethylene! phosphoramide at a concentration of 5 O ₉ g / 100 ml Lösungo The polymer solution is then coated with a slurry of titanium« dioxide in dimethylacetamide ₉ a solution of poly-iüFsN-diethyl · = ß-aminoethyl <= methacrylate) in dimethylacetamide and a solution of 4 ₅ 4 ⁵ = butylidene ~ bis = (6- = terto-butyl-m ~ cresol) in dimethylacetamide in such proportions ₉ that the finished mixture 5, 5 or » 1 io of each additive ₉ based on the elastomer = solids ρ contains ο

The above mixture is heated to a temperature of 70 ° G and spun in a conventional manner in a dry spinning shaft, the individual threads being brought into contact in the shaft and forming a coalesced multifilament of about 420 denier (46 tex) _{hang together o} As it emerges from the shaft, the overgrown multifilament is treated with a preparation of the following composition;

Polyamylsiloxane (viscosity 10,000 cSt) 10 io polydimethylsiloxane (viscosity 20 cSt) 90 f

This preparation is applied to the spandex threads in a concentration of about 1.5 3.8 fo ₉ based on the spandex weight. The spandex thread treated in this way shows essentially no tendency towards adjacent threads when it is unwound from a bobbin stick, and can be handled with very low voltage ,, As a comparison experiment, preparations (e.g., Bo writing with a content of 5 i ° of dispersed magnesium stearate according to United States Patent "3,039,895) mineral oil = basis of the prior Technique to achieve the same low tension when unwinding the threads from a wrapped package in an amount of about 12 to 15 Qewofo required "With preparation concentrations of only 1 to 4 fo these known preparations cannot prevent breaks when unwinding the spandex thread material."

The plasticizing effect of the Pol ^ amylsiloxans is from the The following values can be seen on a rib knitting machine from Scott & Williams DRG design is made using two of the spandex threads described above and four 100-denier puff = n ^ ion threads a typical belt material knitted round, whereby Samples with spandex prepared in different ways (see table) are produced »The number of breaks During the knitting process, comparable amounts of knitted fabric are given in the following table =

preparation

10 <? O Pol ^ am ^ lsiloxane -s- 90 fo Pol ^ dimethylsiloxane

$ 100> poly dimethylsiloxane

Preparation on the thread, jo

3.8 5.4

Number of fractions

The Yorteil of PoljamylsiloxanSj, a conformable effective Fadengut give au, is recognized by a comparison with this component not containing preparation, in which a relatively high number of ruptures at the entrance of the thread in the V / irknadeln ο results in order to achieve an effective behavior _9, the is equivalent to that obtained with the preparations according to the invention ₉ , a mineral oil-based preparation containing magnesium stearate is required in an amount of about $ 12

i e 1

On intergrown spandex multifiles of 420 den (46 tex), which have been produced according to example 1 ₉ , preparation © ?! of the following additions in the following amounts to «·;

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preparation preparation
on the Fa
dengut s ^C / o Deduction
voltage <
G 10 _s 5 - no O Friction =
ι, force 5,
S. 9 _S 5 10 fo polyamylsiloxasi
-f 90 io polydimethyl-
siloxane 1.3 For a measurement too
high" 14th 3.9 1.2 100 io polydimethyl
siloxane 3.2 0 ₉ 8 1.9

$ 95> mineral oil (No. 50) 15.3 1.0 15 _S 5

+ 5 f ° magnesium stearate

(dispersed according to

USA patent

3 039 895)

Under the withdrawal tension in the table above, the voltage is au understand that one sum withdrawing the yarn good overhead from the package 82 ₉ 3 m / min ο required The frictional force mentioned in the table is equal to the Kraf t _9, the one to overcome the friction between guide and running = the thread is required and is determined by means of a Poppe tension friction measuring device at 91 ₉ 4 m / min, under input load of 10 g on a GXpO ^ rod with a matt surface at a wrap angle of 70, as shown in the table values j results in a preparation containing polyamylsiloxane the same or better running · = · and withdrawal tensions at lower preparation concentrations than the prepaxationexi of the prior art,

Example 3

Has been prepared in a verwachsenes multifilament of 420 (46 tex), that according to Example 1 ₉ preparations are applied in the form of various amounts-at Polyamylsilöxan in polydimethylsiloxane having a applicator ₀ Man foe · = adjusts the charging of the yarn samples ₀ result

Polyamylsiloxane
in the preparation =
tion, io preparation
on the thread =
well, $> Polyamylsiloxane
on the thread =
Well, # Static
Charge j Y 0 3.3 0 -1800 * 1.0 2 ₉ 2 0.02 = 1500 7.5 2.7 0.20 = 750 1O ₉ O 3.2 0.32 = 400 0 8 _S 8 0 . = 800 0.75 6.2 0.05 = 600 1O ₉ O 7.1 0 ₉ 71 +200

The static charge mentioned in the table is determined at a thread speed of 91.4 m / min ο (this speed means a more severe antistatic test than a thread speed of 18.3 m / min) »The table values show that very small quantities at PoIv = amylsiloxan on the Fadengut as 0.2? S, already give a substantial reduction of the static charge of the thread material provided with the Polvdi = methjilsiloxan preparation and that about 0 ₉ 7 i ° are sufficient to make a transition from the negative in to get the positive area =

■ = 19 =

Be 1 "pi e 1

On an overgrown multifil of 420 den (46 tex) ₉ which has been produced according to Example 1, preparations in the form of various amounts of polyamylsiloxane with a viscosity are made

-O

of 16 1J0 cSt at 25 C in polydiinethylsiloxane with an ¥ iseo ~ sity of 10 cst at 25 ° with an applicator roller The static charge of the thread sample “Results” is determined

Polyamylsiloxane
in the preparation
tion, fo , 5 preparation
on the thread
good, ok Polyamyl oxylaxane
on the thread =
good, ok Static
charge, ¥ O , 5 O O • MO 000 O , 0 1.1 O = 2,000 2 1.1 O ₉ 028 = 1,000 7th 1.2 0.09 = 400 10 1.3 O ₉ 13 = 200

As these figures show, even very small amounts of polyamylsiloxane _9, such as 0 _s 025 ^ ₉ on the thread material, can reduce the static charge on the thread material to an acceptable level

E.g. example 5

There are preparations with different contents of the polyamylsiloxane and polydimethylsiloxane from Example 4 by means of an applicator roller on overgrown multifiles of 420 den

20 -

(46 tex) applied, which have been produced with the modification as in Example 1 _s that in place of p, p'-Metholendiphenvl ~ $ diisoc anates here an equivalent amount of 4 ₉ 4 ° ~ Methylendicvclohexvl-diisoc.yanat comprising 50 Mo1 $ is formed by the transjtrans = xsomer, and instead of the m ~ xylylene = diamine here an equivalent amount of 4s> 4 ° -methylenedi = (e $ clo = hexylamine), which is formed from the trans _s trans = xsomer is formed, are used ₉ whereby the thread material is free of all three additives related to the elastomer solids according to Example 1. The static charge on the pad samples is determined

Polyamylsiloxane Preparation Polyamylsiloxane Static

in the preparation - on the thread = on the thread = charge ₉ V

tion? jo gutg jo guts, <fo == _, ______ ===,

0 7 ₉ 0 0 = 1 100

2 ₉ 5 7 _s 0 0.175 = 60

B e i s ρ i e

On an overgrown multifilament of 420 denier (46 tex), preserved as in Example 1, preparations of the following composition are used Settlements applied in the following amounts = strands of thread are left to act in the ambient atmosphere for 77 days and determines the so-called b = Werto

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preparation

preparation

on the fade ngut ₉ fo

no

95 fo mineral oil
(No. 50) + 5 %
Magnesium stearate
(dispersed according to the USA patent
2 039 895)

10 fo polyamylsiloxane + 90 io poly dimethylsiloxane

3.9

b ^ value

in the form it has retained

O ₉ ? 0 ₉ 6

0.9

after

77 days

3.8

The ID values relate to the degree of yellowness of a PadeiaproTse, with the difference between the evaluation and the expression of the discoloration which arises during the action of the ambient atmosphere on the samples. The b-values are determined on the basis of colorimetric values obtained when examining continuous thread samples in which the threads are arranged in the form of a square with a side length of 7.6 cm a reflection meter of the type "Hunter. Refleetometer" is determined and the value is calculated in the manner described in more detail in the USA patent 3 095 322 »

As the table values show _9, the preparation containing the polyamyl silosan is superior to the preparation containing mineral oil and does not noticeably contribute to the yellowing of the sparide thread material

The explanation of the invention is provided by the model formed by a sample of a thread, example 4 "Ta ¹ OeIIe ₁ , penultimate line, corresponds to ₉ ie a 420 denier multifil" represents the 1.2 fo preparation on the thread (having 7j5 i ° polyamylsiloxane, based on the preparation, or "O ₉ O9 fo _s in relation to the thread} =

Claims (2)

RA. 798 710 * 12.11- & 4 1. Artificial thread made from a synthetic, segmented, elastomeric copolymer, with a visual preparation being provided on the thread, characterized in that the preparation is a mixture of a smaller proportion of a polyamylsiloxane component with a viscosity of about 8,000 to 20,000 cSt , determined 'at 25 ° G _s and a larger proportion of a polydimethylsiloxane component with a viscosity of about 5 to 100 cSt, determined 25 ° C, and the polyamylsiloxaa on the thread iia an amount of at least 0 ₉ 025 ° f ° des Thread weight is present " 2. Thread according to claim 1, characterized in that the preparation of about 2 ₉ 5 to 10 $ Pol ^ / amylsiloxane, Re st Polj'dimethylailoxan, is formed _o 5o thread according to claim 1 and / or 2, characterized in that the preparation is present on the thread in an amount of about 2 to 4% of the thread weight ₀ 4 ο thread according to one or more of claims 1 to 3 _S characterized in that the thread is a spandex thread « L-84A In that 5 = yarn according to claim 3 characterized _S the preparation fo the pole about 10 ^ at ^ lsiloxarss and about 90 Ψ of Polydimethy! Containing siloxanes ο