DE1928740A1 - Fiber structures with permanent elasticity and crease resistance - Google Patents

Description

The invention relates to fiber structures a, such as s, B. Yarns, knitted waxes, woven textile fabrics, non-woven sextile fabrics, ready-made clothing sticks and the like, which guarantee a permanent elasticity wad SaitterbaatäBdigkeit aind, xuad especially on hosiery for women, which have an excellent smoothness, softness and stretchability "as well as on the manufacture of the same ^

The term "fiber structure", as used in this description and in the claims, means a structure composed of staple fibers ^ endless Mk & mi or a mixture thereof, such as S ₀ B ₀ yarns, strands, hatchets, nets , knitted goods, woven fabrics θ j, non-woven fabrics, pilse, filter cloths, substrates for synthetic leather, garments and the like.

To the characteristics, especially the elastic algae shafts, of fiber structures «a verbaesem, it was usual to work an elastomeric polyurethane yarn into the structure eisura,

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What, however, requires a complicated process, of which it cannot be said that it is the cheapest way to manufacture a textile fabric with a light weight _, among other things, the following processes have generally been put into practice to achieve crease resistance: (1 ) Increasing the elasticity of fibers in the structure (by applying a resin finish with a condensation resin), (2) producing a sizing effect on the structure (by finishing with a polymerisation resin or latex), (3) smearing the fibers (through

) with a silicone resin or an E & mle2.on of polyethylene), In fact, the above method (1) does not cause any increase in elasticity, in particular improvement in elastic recovery from stretching of knitted or woven fabrics, although it improves the resistance to hitter ·. With the method (2) the Paeern is tried "to fix the structure in ianeinsa" of, so that they do not slide and be displaced, the structure Venn deformed or is folded; dieees process yields, ledach "in * n disadvantage" because "the Strwktm ** example of! PextJJlßtoff _t» Μ tends a ssharfen Saitterung. Such a disadvantage is reduced if a resin is applied, but that softening alone is sufficient

"Not enough for a complete selection of all stfects" originally expected from Schlishtmig. At a glance, the above-mentioned method (3) appears, since silicone type softeners or fasseratjnreleuxigBffiitt ©! sss £ are applied to the surface of the 3? aaer However, the resistance to bending and abrasion is strengthened, and the tensile strength of the resin itself is so small that it is impossible to obtain durability from the object treated with this type of agent of retention and interdependence

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expected"

On the other hand, in order to give i & serstructures, especially wool structures, shrinkage resistance, it is important to apply a chemical finish to prevent irreversible shrinkage of the fibers (a Pilsung effect), which is achieved by mixing the fibers in the wool pulp. According to the interpretation of Speakman, Harris and many other chemists that fungus is based on a differential friction effect (DFB) of scales on the surface of the fiber and also on the extensibility and high elastic recovery of wool fibers in water, an approach was made! proposed by method and attempted to produce a shrinkage resistant kait & u . Example of such methods and (4) modification of the scales in order to reduce the SFE, (5) covering of the scales in order to eliminate the WE * (δ) introduction of cross-links in the molecular structure of the fiber to reduce its To improve the modulus in the sweet state, thereby improving their resistance to a force of defoxmation, and (7) connecting points of fibers to make their movement relative to each other. For the method (4) oxidizing agents _β such as s, Bo were inorganic or organic chlorinated compounds or Monopersehw <5feleäure _s used? which have the ability to break open cysteine "binds" reagents "Since these agents were used in the form of aqueous light sings in general practice - in which the wool fibers" swell _- it was impossible to treat the fibers, however, because their scales are attacked on their own without their Hindan destroyed werdea _o In the method (5) cellulose! Silikonhai ^e were ae, melamine resins ttsw ₀ as Beschichtuugeffld, ttel used, but it was dex only one method * drenssflächeiipolymerisation of nylon with practical Who-t venreMet but ee

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can not be said that this method is far satisfactory, and indeed used as Vernetzungisnittel because of the hard handles the finished structure, "The process (6), wherein the diisocyanates, acrylic monomers or Methaerylmonomere, and the method (7), such as, _e Bo the so-called ianaeet method in which methylolmelamine is used and the so-called Pontex method in which a rubber latex is used are disadvantageous for practical reasons, due to poor hand feel and durability of the resulting product, as well as the high production costs in all cases · As explained above, it was previously difficult to prevent the filing contraction without a harsh grip, a reduction in fiber strength, a yellow discoloration etc. _{o of} the treated fiber structure occurring at the same time "

Furthermore, stretchable women's hosiery were previously available with a so-called "torque yarn" knitted, which by a false twist or high twist process produced ivt; however, the torque yarn increases the cost because of its slow speed Manufacture and furthermore it has the disadvantage that the knitting process is difficult because of the high torque For this reason, there has recently been provided a method of making stretchable stockings by a soft method an added monof & the adt of a latent Crimp is knitted, the thread aua consisting of at least two fiber-forming thermoplastic synthetic polymers, which have a different shrinkage when heated, in which thread the two components adhere to each other and in eccentric to each other over the entire length of the Thread are arranged, whereupon the resulting hosiery with the help of steam or another Brhitzungsmedium for

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Development of the crimps of the composite threads heated will".

However, stretchable hosiery, especially stockings, made from a xueaanengeeeitsste tfanof & dan are "generally such a disadvantage that they have thread loops on their own surface which are formed on the crimped threads when the stockings shrink" whereby another body in contact with it is slightly hemmed in, so that a ladder appears in the stockings. Ss is possible to run the formation to some extent To prevent extent by ending with so-called no- ^ running Haschen knits, but stockings with non-running hash have both stretchability and Softness inferior properties. In particular stockings, the main part of which is composed of a Hono £ ad "n s", generally a lower softness, since a thread with relatively high titer must be used in the stocking s sufficient strength so, give, and reduce emanation the non-running mesh the softness Eoch further The softness of the stockings can be improved somewhat by adding a multi-ply yarn of 15 to 30 that made up of 2 to 5 pieces Thread is used to make the main part of the stockings, but also stockings that are made from a single thread thread with composite threads consist, possess, general Disadvantages, such as a weakening of the eyesight as well a reduction in regression a & s elongation, and arwar due a mutual resistance to practice of the Monofödan which the multi-thread yarn consists of · But even here the softness is not completely satisfactory «

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A method for reducing the tearability of stockings knitted with a compound thread from old Reöhtsaaasehea, and for increasing the stretchability and softness of stocking on which have been knitted with non-running stitches from a tightly knitted thread ₉ consists, for example, in giving the stockings a softness with the aid of an emollient * However, the usual emollients, which contain oils and surface-active agents as all main components, give fiber structures with an extremely low durability against washing «,

To overcome the above problems, various studies and development work have now been gexaacht the finishing of fibrous structures with regard to these various favorable © properties su lend "Here, the facts have been found that a physical treatment let preferable to a drastic chemiechen treatment wad this let a poly" * but required for the coating of fibers, which has the ability to form a thin and tough film, the ability to adhere to fibers and a durability against mechanical stresses, such as pressure and stretching, tesi did "toad which" still does not swell in Waeser * Hierssu according to the use of a Silikonelaatosers with an excellent elastic recovery from chording nit high properties, etc. proposed ·

Sa is eztllatoffe an object of this Brfinäung how »· Β · Gterne, knitted goods, woven l'non ·" * woven text create ils t off s, finished · Kl "iduftgsstflek · waa d® '^ lAiehim _Ä s" that with a permanent HLastisiit & t, a permanent Shi.tterbestäaöigkeit, a permanent Sinlaixfhe »

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resistance - and a durability against hashing are ο

Another object of the present invention is to be highly-extensible knitted textiles, especially women's hosiery, to provide a permanent (dullness,. a increased softness and a longer usability "have *

Another important aim of the present invention is to © in process for the production of PaseretruJrburen, which a · permanent elasticity, crease resistance, shrinkage resistance and Wasöhbestäadlgkeit and especially hooh-etreek « Able steam stockings were made with a permanent smoothness, an increased softness and an extended shelf life create that easily and cheaply produced on a technical scale can be provided «

Other features and advantages emerge from the following description «

The above goals are achieved through. homogeneous application of a non "aqueous solution ™ $ a Polyorganosiloxaavorpolymers in an amount of not more than 10 wt. and a Eatalysators on the fiber structures and then subjecting the resulting structure under an Wärmebehandl-img of 70 bit 200 ⁰ C to initiate polymerization of said Prepolymer sau. End to lead, using a polysiloxane. attached to the structure with an elongation at break of at least $ 50, a tensile strength of 1 to 50 kg / cm ² and a hardness of 5 to 50 °

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The polyorganosiloxane prepolymer to be applied, according to the invitation, is a linear polysiloxane which, as Sndgruppexx Hyäraiygruppen, directly bonded to its silicon atoms! it can check represent wherein S and E ¹ each low Aliylgruppen having 1 to 5 carbon atoms, such as zobo Hethyl-, ethyl _f propyl, butyl and pentyl groups, or by the general formula HO- (SIER QO * _n -H - CH = CH ₂ , - ^ "^, -OH ₂ -CH ₂ -OP ₃ , - (CH ^ -CH, -NCO, -OCE, etc. There are numerous compounds which fall under this definition ₀ Xm general are used as main components, those compounds which low iüJfcylgruppen contain as Seitaiketten such as contain ₀ poly (dimethylsiloxane) -diol and poly- (diäthy3j3iloxan) ~ diol, or those compounds which have aromatic groups as a side chain, "as ζ · Β, poly (methylphenylsiloxane) diol and poly (diphenyl-8ilozan) diol. A polyorganoeilozan prepolymer, the main component of which consists of poly (lower alkyl8iloxane) diol, is preferred according to the invention. Venn H and R 'for example phenyl groups instead of CH ^ Groups, then the heat resistance of the prepolymer is increased, and if ITltri lgruppen be introduced, then the Ölbeetändigkeit is verbeasert _e The invention is, however, in view of the nature of the side chain ^ not beßchränkto addition, R and R 'are identical or different groups mentioned his _o Together with the above "n connections can" -ach alkylhydrogenpolysiloxanes, like z _e B _o Methylhydrogenpolysiloxane, are used effectively »

The non-aqueous solution of the polyorganosiloxane prepolymer can contain polyether compounds, such as Z ₀ B ₀ polyoxyethylene alkyl, polyoxyethylene alkylphenol ether, polyoxyethylene alkylphenol, polyoxyethylene alkyl phosphate, etc.

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Impart properties and take away from the structures of a waxy handle _'s included in the Polyoxyäthylengruppe the above Polyätherverblndungen The number of moles of oxyethylene units, preferably "wipe about 5 and 40, but ettsäureestern at Polyoxyäthylenf and polyoxy" äthylenalkylphosphaten that area should be between 5 and 20. A suitable number of carbon atoms of the alkyl groups in the compounds is as follows:

Connection number of coals—

Substance atoms in the alkylarappa

Polyoxyethylene fatty acid esters 12-18

Polyoxyethylene alkyl ethers 10-18

Polyoxyethylene alkyl phenol ethers 4-12

Polyoxyethylene alkyl phosphate '10-18

Polyoxyethylene sorbitan fatty acid esters 10-18

In addition to the above-mentioned compounds, a polyethylene glycol can also be used old a degree of polymerization of 1 to 4 ο 000 and especially effective from 40 to 2,000 »

A suitable amount of polyether charges to be added to the non-aqueous solution is 1 to 50 wt. based on the polyorganosiloxane prepolymer »and preferably 3 to 20 <xewo- #. These polyether compounds can either can be used individually or in a mixture

In general, the degree of polymerization of the prepolymer can be selected according to the intended purposes. For example, a polymer with a degree of polymerization of about 50 to 2,000 has a considerably high viscosity,

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such as about 30 to 1OGoGOO Ce & tistoke, so that it is sweckaassig to use a solvent »If on the other hand the degree of polymerization is between about 20 and §0, then the prepolymer because of its low viscosity and its Honing easily in the form of an -aqueous EBiu3.si.CB be used"

A mixture of a prepolymer with a different chemical structure or degree of polymerisation can of course also be used. Since the above-mentioned polymer should be polymerized by a heat treatment into a polymer kit with the above-mentioned physical properties? iet Polyiaerisationsgrad the prepolymers on einsn high value limited such _e B "minimum ens 5O ₉ Torsmgeveit» © mindeetene 100 "whereas the one that is used for tObliche Erweiohongsmittel and Wasseralyweiiirangsnitiel of prepolymers * is not more than 50 is" so that it is in accordance with essential to the present invention is a non-aqueous solvent as d & e

medium or to use as a thinner for the prepolymer *

. As such, a polyorganoeiloxane can easily be obtained by hydrolysis of, for example, organohalosilanes, Organoalkoxysilanes, etc. aweoks polyaerization, by means of polycondensation, clay Ollgcmerea eiaee (Pclyorgeaoflilaran) -diolß odex * duroh Opening polymerization of a cyclic polyorganoeil ^ xane with a »low molecular weight,

• The Vorpolyeer becomes a larstebahafidlung and through help d «e Efttalyeatore in« transformed into sfth «e S3xueitaM7 ns« of that. Molecular weight more than a hundred thousand and several Hundreds of thousands to several millions are "dae" of these

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Manufactured in a wise manner © Elastomer can be more or less networked and / or contain branches in the molecule or can be made up of linear Molecules exist.

When © rfindungageaässen method, a non-aqueous solution is * contains generally 0.1 to 10 wt. "# Polyorganoelloxankomponente, at room temperature in an amount of the Paseretruktur by means of dipping, .KLotaen, syringes Ubw _o not more than 10 Weight - $ »Poly organosol oxane component applied. i> xa Kon · 'concentration dee polyorganosiloxanes recording uawo be appropriately controlled according to the shape of the fiber structure, the type of Faeena etc., Adaorptionsmsnge the Polyorganoeilexankostponent ^ ~ #' vm to no more than 10 percent. beaogen the Structure,

In the case of the process, an inorganic acid, such as S & iseäiare imä Sofcreiafeleaiare, an alkali, such as caustic potash or caustic soda, in alkali silanolate, which is derived from organic silanol, an inorganic isolaee salt, such as ZoB, can be used as a catalyst in the process. Ferric chloride * a metal oxide such as _lead oxide, silicon oxide and interest oxide, etc. can be used.

The most suitable are metal salts in an organic acid, such as s »B _o dibutylzine dilaurate, difetylssinn tiactoate, dibutylainn suecinate, Einn (lX)» octoate txuA oleylatvsrbinduBgen from Zimu The above mentioned SJatalyators can be used individually or in a mixture.

The amount of the catalyst described above can be added in a suitable manner according to the type of poly applied. organosiloxane prepolymers, its £ oBzentratI <m _f d-sr treatment

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'conditions ναού. The type of catalyst used can be determined, but ei © is usually 0.01 to 5.0% by weight, 6 and preferably 0.1 to 1.0% by weight, based on the polyorganosiloxane component in the prepolymer applied

May further susätzlich catalyst mentioned above SRAM, an organic silane compound, such as "an isocyanate silane compound, a JJLkoxyeilan, an acetate a Silanverbinng etc. may be added for the ale Beechleuniger Vemetzungareaktion, the adhesion of the Polyorganoeiloxans vm. On the Paaerßtruktur to Terbeeaern · As a further catalysts for effecting the Vernetzungereaktion, peroxides can be prepared as used eg "benzoyl peroxide, and a bi- or polyfoaktionelle verb ^ jadung as aB wad a triol a Yinylverbindung can be incorporated into the Polymerisationamaterialien, a polymer having crosslinks or branches to be produced in the Molectile.

If Faaerstrukturen containing polyamide fibers, treated, then it is preferable in the solution of the prepolymer a small amount of a compound having a Affini did incorporate for polyamides, such as _c, a compound having amino groups Iminograppen, carboxyl groups, amide groups and urea groups , and compounds having a reactivity with polyamides such ₀ B _e formaldehyde as a result of the above measure the adhesion between the fiber structure and the polyorganosiloxane improves _s and especially the durability of the liability is "greatly increased, the above-mentioned compound is usually in in an amount of not more than 15 - # based on the polyorganosiloxane added

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Examples of non-aqueous solvents which can be used when erfindnngsgemässen procedures "are toluene" xylene, benzene, perchlorethylene, trichlorethylene, gasoline for industrial purposes, chloroform, Kethylchlorofora, methylene chloride UAW _o These solvents can either oneness or be used in a mixture.

A curved silicone resin for a textile finish non-aqueous solvent, which is available on the market, tried but the formed® Harssfilm showed a low one Elongation at break, low flexural strength and poor durability when washing »

The fiber structure on which a Polyorganosiloxanvorpolyjaex and a catalyst has been applied * is then subjected to a heat treatment at 50 to 200 ⁰ C, xm its reaction xu · End lead. The optimal © temperature during the heat treatment depends on the type of fiber structure being treated, on the polyorganosiloxane and the catalyst applied and on the adhering amounts of polyorganosiloxane and the catalyst and is generally related to the treatment time.A temperature below 50 ° C It is advantageous because the polymer with the desired physical characteristics is not achieved or an excessively long process is required. If the temperature ^{goes above 200 °} C., damage occurs, such as, for example, discoloration and degradation of the treated. Article and decreased elasticity · The preferred range of the treatment temperature is 100 Me 180 ° C.

The treatment time is generally in the region of 20 seconds to 60 minutes and in particular in the range from 1 minute to

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10 mins.

Dae Yorpolyser is converted by a heat treatment and with the aid of the catalyst in a Hetswerk having a molecular "weight of several hundred thousand comprises} where a tough elastomer having an elongation at break of at least 50 <ß _f a tearing" - strength of 1 to 50 kg / cm and a hardness of 5 to 50 is formed.

™ Bishex · were for the purpose of keeping animals from Tüohers for

Raincoats uew _"y waterproof 'M gagserabgtoaseiKie properties * iron, PiMshirag ^ YerfalireBi wi® ss" B · Role & fairy "coating, Messerbasoliiehtuiig and Strsichmasserbescliichtung of taffeta, canvas from synthetlaaher fiber _s PersenniJsgtucfc. and so on with an Acrjlhars or a UrethaBharss around such planning procedures filmaia d @ r Bogeuaunteii Quis tung, so that with these procedures the advantage and the grip of Baeietuohss are lost. Since the aim of the above coating process lies in a vase-tightness of the object and there, according to this process, a Hargfilm

^ is placed on the surface of the fiber and connected to it, the object receives a guoraiaxtigea grip, so that the fiber itself can no longer be felt mm τγ @ γ «turning Harsea, various phyai & alissiier Mg © ss © Mftaa of the pole attached after the polymerization treatment, the amount of the attached Polyoex» mm, he2w & Bgßmä®n _a invention fulfills the above-described bollard »dae has been , msä daa on the Mm ^ jhatxvu ^ wc; adheres visr Iw dl «, laeers-k structure einiBporagiiiiKrl been I & fe, the

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Elongation at break of at least 50 %, a tensile strength of 1 Isis 50 kg / cm ² and a hardness of 5 Ma 50 ° ₀

Further, the "shows preferred polymer when in the form of a A string or a thin ribbon is an elongation at break of at least 80 36, preferably t OO $ »and one module of a maximum of 1 g / den,

The elongation at break, the tensile strength, and the hardness are determined according to JIS-C-St 23 as follows

Elongation at break and tear strength ;

A hantelföxroiges Ssststuok is aue a Silikongurmnlplatte cut formed on a glass plate or in a Porsellanböhälter by polymerizing the same solution of Polyorganosiloxanvorpolymer how the invention eie on di © faserstnaktur gem & B we applied & g hergsstell ^ wurd © "M * Gj? Ö38" dea TeetstiöskE "is 5 ϊβπι width 20 length before rniä 3 sss or ί2ΐ ₀ the Seetstüok wis fi less · Diefce for the straight part of a InstroE-Uriiiereel-EaiieioiL ^ -Xeeter (3ie2 ge @ tellt dur-oli astron _{(Sagineering?!} - Corporation, USA) asit -ainer stress rate of 500 pounds 25 asm / min to two. Eeissen stretched, and then the iaaximBle BeXastu? 3g and the length of the straight part are determined.The elongation at break and the tear strength are calculated by the following formulas:

- ^L t ** ^L 0 χ 100

¹ O

where Eg is the percentage lengthening when eating, L _{Q is} the original length (am) of the straight part, iißd L .. is the length

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(am) the straight part when tearing let; and

where T _{33 is} the tear strength (kg / cm), F _{33 is} the maximum load (kg) and Δ is the cross-sectional area (cm) of the straight part lato

If four values are obtained from repeated (tests with respect to oof Eg or, then the four pieces of tea are denoted as S 1, S ₃ , S, and S, which have the following relationship to one another;

From this, Eg or T ^ is determined according to the following equation *

or T ₂ = 0.5 S ₁ + 0.3 S ₂ + 0.1 (S ₃ + S ₄ ).

Hardness ;

Sin Teetsttiok with a flat surface and with a thickness tob at least 12 mm is made »If its thickness is less than 12 mm, then several such pieces of tea are placed on top of each other until a total thickness of 12 or more is obtained Endurance tester of the spring type introduced. This tester has a flat pressing surface, which is equipped with a hole with a diameter of at least 10 mm, a vertical pressing needle which goes out of the Looh and over the pressing surface and is located in the center of said hole, and a pointer which the amount of movement of the handle according to the hardness ä® & Teatetücks

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indicated

If the elongation is less than 50 % , the film produced is so brittle that a fiber structure with permanent blastiness, wrinkle resistance, shrinkage resistance and durability in washing cannot be obtained 800 & The tear strength is 1 to 50 kg / oa ² and above

2 2

preferably 3 to 20 kg / cm. If aie is less than 1 kg / s then the film produced is so brittle that the resulting fiber structure is unsatisfactory because the mechanical strength is too low. On the other hand, when the tear strength is over 50 kg / egg, the handle becomes the treated one The fiber structure deteriorates considerably, whereas the hardness increases o The hardness should be 5 to 50 ° and preferably 8 to 30 ° if the hardness is less than 5, then it is Film formation possibility is insufficient, and on the other hand is one Hardness exceeding 50 ° is not affected, as the treated fiber structure becomes hard and the surface deteriorates noticeably

Another important factor for achieving a fiber structure with permanent elasticity, smitter resistance, shrinkage resistance and durability against washing as well as good quality is the amount of polyorganosiloxane adhering to the fiber structure * According to the Brfinduog, a maximum of 10 G «w - # stick of de "Polyor ^ nosiloacan with dan aforementioned physical properties of the fiber structure or be impregnated into the fiber structure" the Meng "of liable or einimprägnierten polyorganosiloxanes is usually in the range of 0.05 to 10, preferably 0.2 to

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5 wt .- #, based on the fiber structure. When the amount is less than 0.05 wt .- ^, then the effect of the treatment is unsureichend, and if he other hand, 10-turn ~ £> exceeds ₉ then there will be drawbacks such as a reduction dee Kompresaienagrades \ md the Bausehigkeit and continue to chalky * spots arise ο

Fibrous materials to which the present invention can be applied are natural fibers, synthetic fibers, regenerated cellulose as well as grains thereof in staple fibers, endless threads or (mixed with the same. Examples of natural fibers include full silk, cotton, hemp, etc. Examples 'for synthetic fibers are poly eater, polyamides, polyureas, polyacrylonitrile, polyvinyl alcohol, Polyolefia © _f polyvinyl chloride, polyvinylidene chloride, polyurethanes uew _e are examples of the regenerated en Cellules Viekoserayon, cupra, Cellttloeeaoätat, cellulose triacetate uem _o

The fiber structures can be made of staple fiber yarns like 2.B spun staple fiber yarns, needle-punched non-woven fabrics and the like, but the directional process is more favorably applied to structures, which contain at least 20 % endless threads, such as ß.B. Yarns, knitted Varen, woven fabrics _t finished garment and dergleieiiea that, the Fons of Oernaträngen "chug, piece goods" * hosiery, foundation garments, Eandsohuhe and the like · FQR the texture of the Faserstruktor applies that a coarser texture bit provided the greatest effects can be. The present invention does not naturally apply to knitted animals, woven fabrics and non-woven fabrics are limited.

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findungagemässe method is laser constructive doors special effect hei, in particular for ladies hosiery, pass the aas continuous filaments alone. "But also if continuous filaments gacaeinsaia used with staple yarns, such as K ₀ B ₀ mixed yarns, mixed gewehte fabrics nm *, then such structures a permanent elasticity UBd granted excellent resistance as long as the content of the endless threads is 20 # or more «,

More than one treatment for semen will trump it, which one of the main topics forums of the present invention described in detail.

For the production of women's stockings can be both a · mehrfadigea yarn and a Konofadengam be used · However, according to is the invention "b @ To: r sug: _s like a multifilament yarn from 10" to 30 to and from 2 to 5 Fäiea T @ rw @:. Bfi © t _f the threads zusaaimengesetzte threads, aufweieea the oln © dureh ErhitsuEg entefiokel- · bare latent crimp. A method may ssn 3 aiisaMa <^ igee®tste Fa & dtsrch v manufactured eröea _s comprises the steps of:? Separate melting ^ on mindeßtens s * fei fiber-forming, thermoplastic synthetic polymer, extruding the molten polymers simultaneously through the same opening of the spinning head ₉ to create a uniform 3? aden, which consists of at least two components that. have a different shrinkage capacity when heated and which stick together and are arranged in an eccentric position to one another over the entire length of the bath, as well as stretching the extruded thread *

Stockings that come from a MeSirfadeagara bssitfess ^ are those

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its main part, for example the leg part, with a multifilament yarn has been knitted either individually or in combination with a monofilament yarn «Furthermore, a yarn can be made from a single compound thread with latent crimps can be used with advantage * Stockings made from a monofilament yarn are composed, are those whose main toil is knitted with a hono thread, and whose toes, heels » Soles and ribbons can be knitted with a weft thread

The main part of the stockings can be knitted with any kind of loop, for example with reverse stitches, non-running stitches (loaf stitch-resistant stitches), micromasohen, jacquards and the like. Hit the expression "stockings ¹¹ , as used here, are meant seamless women's stockings ©, tights and the like. It is superfluous to say that the other ropes of the stockings, namely toes, heels, ribbons, panties, etc., in some catfish Any type of yarn can be knitted.

One method of making stretchable stockings from a composite yarn yarn comprises the following steps: knitting, crimp development, dyeing and shaping the treatment according to the invention can be carried out before the coloring step or before or after the shaping step _o However, since stockings which are treated with a polyorganosiloxane are somewhat less dyeable, it is desirable to get rid of the polyorganosiloxane treatment after the coloring step aaaeiafuSireno it is preferred the

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to be carried out on stockings that have been shaped and which have then been left to relax in a sufficient amount of time, to eliminate their remaining shrinkage, since in this way stockings with the most uniform and balanced appearance and with excellent elasticity are obtained.

The dyed stockings then become a non-aqueous solution a PolyorganoBiloxanrorpolyyaers immersed, squeezed out, so that they receive a suitable inclusion, and for polymerization of the prepolymer dried after the excess drying stage can be followed by a baking or curing stage, if this is desirable in order to accelerate the polymerization reaction. Ss is avoided externally, the polymerization reaction, i.e. the hardening treatment to be carried out while the stockings are in a sufficiently contracted state, so care should be taken to avoid tension on the stockings largely au Termeiden

The amount of polyorganosiloxane fixed on the stockings is preferably 0.1 to 10 βον-οΗβ * based on the weight of the stockings, and in particular 0.5 to 3 <* e * «- 9to If it is too small, then the stockings tend to be a lesser smoothness, while if it is too large, they are not provided with a smoothness that goes beyond this and in the worst case the polyorgaaosiloxane hangs in lumps on the hooks, forming films on the hooks of the stockings, so that the appearance of the stockings is adversely affected »Since uniform adhesion of the polyorganosiloxane easily leads to the formation of a pilas, care should be taken to ensure that the prepolymer solution adhering to the stockings is kept in a uniform state during the drying stage.

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1828740

Since it is possible in most cases, aufeubrechen the film formed on the chasing and au eliminate, presumably an intense voltage on the stockings is applied, can bob. such a step following the hardening treatment. For example, it is very cheap to treat "stockings with a Folyorga ^ oslloxanvor" polymer after dyeing and then to carry out the hardening treatment before molding, since a large part of the film mentioned is removed by the tension during molding.

Stretchable stockings obtained by the process of the present invention exhibit extra-good softness, smoothness, extensibility and durability, as does quality. comfortable seats, due to the »Polyorganosiloxane» located on it. These effects can be further improved by adding a multi-thread garx to the main part, ie the leg part, the stocking kit. is knitted, which is made up of composite. "Furthermore, the softness and flatness of the preserved" stockings are made up of threads

essentially so stable that they cannot / cannot be reduced by Vaechen.

The smoothness achieved by the process according to the invention is far better than that obtained by treatment with a conventional emollient containing a silicone oil (an aqueous mixture of silicone oil, etc.) "furthermore have stockings made according to the process of the present invention a great flatness ₉ the likelihood of being hoisted due to a scratching "of accidental snagging less late stockings ₉ main part with a" Mehrfadftogarc g "etrloi reisae », still other threads the Sana dia stockings

909850/1617 bXd ORIGINAL

Stockings produced by the method according to the invention have also been shown to have excellent recovery potential from stretching.

There is a considerable tendency for the appearance of stockings, the main part of which is not knitted in a monofilament yarn. iet is deteriorated ₉ when dis Msnge the adhesive polyorganosiloxanes increases, while in the case you been stockings "knitted aue the buckets Mehrfadengara SiHd _8, the above-mentioned tendency is reduced.

As is apparent from the above description of the preferred embodiment of the present invention, the fiber structure of the present invention exhibits excellent tensile resilience and bridging resilience due to the action of the incorporated poly-gaaosiloxam as part of the laser structure, and therefore the laser structure obtained ait a permanent reliability ußd KMtt © rb © gtäB ^ i ^ ieit ssn & gß rüßtet and shows a smooth running resistance and build-strength when washing »

The Asfringen eiaes Esicsfiaisäfe on Passrst2 * afctur © 3a who in the. Rewarded with the Äusfoildüiig -won Kreuauiigkontaktert linked in the structure, the SteolrU & r, especially sextile fabrics, has given a flat handle » waä. ee was unvenaeiabar that the Streckbarksit of such Stnaktur © n _s not like SB knitted goods, due to the formation of Kreusungskontakten to öamsehlin ^ n ^ versehlechtert wurdl jfSci ^ M ^ ff * $$ &> punched structure only stable but also shows a Satisfactory stretchability, since the resin used according to the invention has a high tensile strength or even ZgM-gkait acfweiet

BATH ORIGINAL

903850/1617

if ea is present at intersection points of fibers «,

In addition to the astonishing improvement in the elasticity and enitterbeatability of fiber structures, the invention features Procedure has the extraordinary feature that a crease-proof finish on silk structures without deterioration their grip can be obtained and that a shrink-proof Finish can be obtained in wool structures. In particular, wool structures with WaGh-and-wear properties can be used are obtained which are durable with respect to washing. that the fibers are treated with a non-aqueous solution in which the fiber does not swell, so that the fibers are not deformed and their shape is completely natural State maintained

Another great advantage of the present invention is that the fibers are not broken down and that the tear resistance the structure is noticeably increased Have been obtained an elasticity and dimensional stability, so that they are easier to cut and put in clothing can be processed than the untreated! textiles «,

Another important merit of the present is that when Faeeratnakturen with an Is PolyorganosiloacanvorpolyaereE @ rämi ₉ ül® Ö4o contain the mentioned polyether compound

Structures excellent antistatic 3igeag © lii £% .jä sogriva

whereas most harafinielies do

ORIGINAL BATHROOM 90 98 50/1617

easily accumulated static electric charge accumulation of problems with which the static charge is connected, such as 2.B «the fact that an electrically charged body is easily contaminated, difficult to process and inconvenient to wear, can be eliminated by the present invention. Moreover, the application of the polyether compound removes a waxy Crriff d r Faseretrukturen, which is sometimes caused by a Polyorganoslloxanfinish, especially if the adhering amount exceeds the prepolymers over the preferred Grenswert.

Another advantage of the fine structure according to the invention possesses, lies in the fact that, although the formability of the structure according to the invention compared to the untreated structure is slightly lowered, the structure is colored anyway can be, which is a great advantage. So far has been the dyeing of fiber structures, such as textiles and finished garments, with the help of a reel or ' Over-the-sun dyeing machine carried out, in which process wrinkles, in particular line-shaped rakes, were caused on the structures has excellent elasticity and tenderness, if the crease is chewed in water, so that the above difficulties mentioned are eliminated »Such an advantage has never been obtained by a conventional harsfining process until it has been stabilized and has cnesleel effects Polyorganosiloxanes according to the invention are in use.

A common silicone resin for a sextile hooking bit low degree of polymerisation and it is a non-aqueous Solvent that was available on the market was

909850/1617

Tried, but the hair film formed showed a low one Elongation at break, a low flexural strength and a low Durability in washing.

The invention is illustrated in more detail by the following examples Bas word "part" when used in the examples »Means" part by weight ". The procedures for determining the permeability (Load for elongation, degree of elasticity), compressive elasticity (Degree of zompreselons, degree of buckling) »tear-resistant-P speed, degree of elongation, crease resistance and shrinkage, as well as the hashing and dry cleaning conditions in the examples were as follows:

ZngelaatigJtät t

1) Load for elongation

One sample with an effective length of 10 esa and one Width of 2.5 cm is on an Instron-UniTe ^ al-Tene.iOß «- Tester stretched at a rate of extension of tO cm / ain, and then the load (g) becomes corresponding to a certain constant elongation j of the sample load for elongation fixed " placed·

2) Degree of air quality

The degree of iCLastiBility is given by the following equation:

ELaeti »itatßgrad ^{1 X}

where 1. (ob) is the length of the sample , if a "BeXaatisa ^ of 500 g in the same weight" is applied in (1) above,

909850/1617

the sample
Ip (cm) is the length / let measured after standing for a Hinute under the load trad anachlieseendem standing for one minute without load and _e iet 1 (cm) the original length of the sample.

.Four pieces of cloth are laid over each other, then the total Dieke (t mm) is measured after a load of 10 ^ g /

2
cm has been applied for one minute, then the thickness

(t .. am) measured ^ after a further load of 3 00 g / cm Minute inserted * 1st been Imae thereto is the thickness mm) measured _s nacMem di Proh @ © © a further minute without loading

steaea- ^ elaaaesa been iet _e Wiiii Then the Eompreeaionsgrad ibid the EUclcbildungsgraä dureh determined the following equations:

Degree of compression (%) t -
= T X 100 Depreciation rate {$) V X 100 ~ 4-. 3 ■ * i _ 4-

sine sample with a © ffektiTsn Lirage - ^ QB 20 esa edge of a width of 15 cm on an Instro3a ~ tiiiiTe3P8aL - *! E © nsion-®ester with a stretching speed tob 20 cia / fflin is stretched _? then wisÄ the LiiTsge (L. em) of Pr © "be in accordance with the load of 4 i £ gg @ iaess © So L e ^ · is the urspriißglicsii © iänge the Prelbe» Dar

© rglfet ^ afc d @ im © ms of the following

C ^) - «- = η joe

BATH 909850/1617

Crease resistance :

The crease resistance is determined according to method B described in JIS L-1079-5 »22.2 B, which corresponds to the so-called Monsanto method, which is described in AAl ¹ CC 66-1959 T or in ASTM D 1295-60 T. _e

Degree of shrinkage :

- Broadcloth (65 ^ polyester staple fiber / SS $> cotton) -

Measurement is carried out according to Method F-3 in JIS L-1042 as follows

executed;

1.36 kg of a sample cloth are taken out with a sufficient amount / brought into a washing machine. Steam is supplied to the washing machine at the same time as work begins in order to increase the temperature of the water quickly until it reaches 100 ^° C., whereupon the supply of steam is interrupted and soap powder is added in an amount of 0.05 wt .- # "Bach a 40-minutes if soaps is the hot Waaser replaced by clean, cold water, the temperature is rapidly raised to 60 ⁰ C, followed by a further 10 minutes gewaechen" the washed Sample cloth is dried on a flat bed press and the distance between markings previously made on the sample cloth is then measured. From the average values obtained from three solutions in each case in the direction of the weft and warp, the shrinkage value is calculated. calculated using the following formulaί

Degree of shrinkage {%) = = - £ - = - _{£ -jqO}

JU

where L is the distance before washing uml L ³ represents Aöstaaö

9 0 9 8 5 0/1617 ^BAD OFUGINAL

washing is o -! Textiles made of wool and wool / silk -

The measurement is carried out according to the IWS method as follows:

On the Brobentuch there are three groups of marks in the direction of attached by warp and weft.

1 kg of the sample cloth are used together with 25 1 of water, which is 0.45 4% by weight sodium hydrogen phosphate, 8% by weight sodium conohydrogen phosphate and 0.05% by weight of a nonionic surfactant. Contains agent, placed in a washing machine, soaked for 15 minutes and washed for another 5 minutes * After the Drying by steaming press' the degree of shrinkage is measured and in the same way as in the case of the sheet calculated·

Vases s

Washing is carried out continuously for 2 hours at 25 ° C. in an aqueous solution of 2 g / l Monogen (the trademark of a neutral Soap made by Daiichi Kogyo Seiyaku K «K · being), with a bath ratio of 50: 1 and an automatic Washer whose direction of rotation is reversed is used will,

Dry cleaning t

The dry cleaning will age at 25 ° G for 3 hours

50-fold Badmeng © Perohlorfithylen executed » Tear resistance :

The measurement of the tear resistance is carried out according to method C,

909850/1617

1828740

did that described in JIS L-1079, as follows:

Brei Testettteke with 6.5 cm width and 10 cm length will », in the Directions of warp and weft on a Blmendorf-ElnreiS tester attached.

The middle of the long side of the Xestetücks is incised by 2 cm. The maximum load (kg) is obtained when the remaining width of 4 × 5 cm is torn apart wildly »is determined.

example 1

Sin Doppeljjerseytextilatoff (length in the direction of the wales 70 mm / 50 Maschenreilien), the ylon with a falask G® "zwirnten textured l! ~ 6-Gara of 70 which was knitted with 18 Fades / 2 strands at 70 ⁰ g for 20 minutes washed long la a 30-fold Badmenge which tg / l of a surfactant and tg / l Sodaaeche contained, dried (density _t wales 30 / inch;. Masehenreihe & s 45 / iach) old (the solution of the Welter Zusaiasensetzung described below receptacle 100 ) geklotst and DSAA reheated again dried at 6Q ⁰ C for 2 minutes at 150 ⁰ C.

The textile fabric obtained in this way (density ₉ rods 37 / inch; Masohenrei & en: 45 / incii) contained 1.5 polyorganosiloxanes, had a good soft hand, good drapability and excellent elastic recovery from stretching, and was also resistant to creasing.

BATHROOM OHIGSNAL 909850/1017

Composition of

Trlchloräthylenlösung With 15 Gewo- ^ Dimethylpolysiloxandiol, a content of 20 mol- # ^ -GyanopropylXBethylBilGescasaeinheiteiQ and a

Degree of polymerisation (P) of about 1,200 100 parts

Sixm (II) -oötoat «. ···· .. ··. ··········« ···. .... 2! Hurry

Methyltriolooyanate silane 2 parts

IndustryTjensin <, <> ·. «Ο,. ··. ·. · ... ··. ·······. ·· 900 parts

For the purpose of comparison, treatment was carried out in the same manner as above, with the exception that a conventional silicone finishing agent EB 714 (manufactured by Shin-etstt Kagaku Kogyo KK, V: about 30) which had been used for all Waeserabweiaurgsfiniehing was used, wad with the further difference that a bath of the following standard was used:

Composition of

ES 714 (manufactured by SMa »2tga
Catalyst B7 (manufactured by Shin-etsia

j / ο · s «u r ο ο ο c Q ο» »& C 'ο ο β ο β s t,» κ · a »« e c:> ι tiU Ιβΐΐθ

* »*. ₄ =. ο,., _t *. _{& o β α β c} . _e <>. * * * _a * * 950 parts

The above-mentioned polyorganosilos ^ O-ösmig raad FB 714 were polymerized to fafein with aines? Diöke VOA 0.7 Baa herzustelleno The first "panel obtained Q aeigte Äio below-mentioned physical Mgensehaftea" while the EB 714 obtained from panel so brittle * rar ₉ characterized in that the elongation at break and tear strength are not measured konnteno
Elongation at break. 752 #

Tear strength S l ^ _; r / cm ²

Hardness n 0 °

BATH ORIGINAL

303850/1617

The tensile elasticity and the compressive elasticity of the treated fabric and the untreated fabric are shown in Table 1 for comparison. The tensile elasticity shown in Table 1 was under an elongation of 30 % in the course direction. measured"

909850/161 7

Tabel

I. Uabehaadelter
object Zvgtlastlzitat
before washing ELaetlei-
degree of activity Pressure stability Rüok- after the washing look-
picture-
Degree near the dry BUok-
£ ^ ad treated counter
etand
Comparison, for deli * -
nnsg (g) 80.3 ▼ before washing 71.2 preselone *
Degree (*) - Koa—
preseione-
degree ($>) • 152 94.3
87.8 Koa-
preaelone-
degree (^) 94.3
82.3 - 92.5
71.5 • 92.2
73.2 120
130 18.9 19.8
16.2 20.3
17.5 20.6
19.2

Example 2

The fabric obtained in Example 1 was immersed in a dye bath of the composition mentioned below at 25 ° C, the bath ratio being 30; 1 waso After the temperature had been raised to 95 C _v which took 40 minutes, the boiling was continued at this temperature for another 60 minutes «

The dyed fabric of the present invention showed a good effect and uniform dyeability in Ver _f . sum of untreated textile fabric. Furthermore, it was only slightly wrinkled, the elasticity of the textile remained satisfactory, and the dimensional change in the textile was negligibly small. The results are shown in Table 2 below.

Table 2

Contraction of the textile

near «hissing

Dndiated blessing trend

Object treated in accordance with the invention

0.5

rejLne (3D

Tensile elasticity

Stressgo for expansion

(B)

148

123

KLa-

stisi

activity

78.8

92.5

Pressure availability

Compression

17.8

21.2

HUok bildo

70.8

93.2

90Sa50 / 1617

ORIGlNAL BATHROOM.

55 -

The percentage contraction of the textile is shown by the YeAaltnie the Längemrerluats after drying to Large before drying in percent,,

Example 3

A fabric of double half tricot, with a Hohseidengara of 21 to had been knitted with 7 threads / 2 strands was at 1OO ° C 1 capable long in the 40-fold amount of a bath, which was washed 3 g / l PcfcSaschenseife contained _s, then subjected to Baumfärbimg in a bath containing 10 wt ~ fi direct Deep Black e & C (trademark for a direct dye, the Ciba Go "is prepared by,) and incubated at ioo ° c .on a frame dryer dried (density Maschenstäbohen.: 42 / inch; courses: 46 / inch) _o the thus dried fabric was immersed in the solution having the composition shown below, squeezed under a pickup of 60 #, again at 80 ⁰ C dried and then 2 minutes' at 12O ⁰ C heat treated o

The fabric obtained in this way (density, gauge; 42 / inch; crochet stitch; 45.5 / inch) shows excellent crease resistance and elasticity _P so that it was useful for women's clothes and gloves.

Composition of

Trichloräthylenlosung with 15 wt _e -5 £ Dimethylpoly "siloxanediol containing 5 mol # ~ Hetbylhydrogen3iloxan

retrieved contains (S ?: about 900) .. _Ο · .. · * ο.ο ··· αο 100 parts

Dibutyltin dilaurate., ... 0 ........................ O 3 parts

Tetraethoxysilane α .. · ... »♦ _o 3 parts

Perchlorethylene o _S. 900 parts

909850/1617 6AD ORIGINAL

For the sake of comparison, a treatment was carried out in the manner given above, with the difference that a bath of the following composition, which contained ES 724 (manufactured by Shineteu Kagaku Kogyo E ₀ K ,, £: about 30}, was used:

Composition of treatment solution (for comparison) ; KS 724 (manufactured by Shin-etsu Kagaku

Kogyo KoK.) 50 ropes Catalyst PD (manufactured by Shin-etsu Kagakn Kogyo Κ, Κ.) · Ο 10 ropes Peroblorethylene o950 parts

The result of the comparison between the two fabrics is Approved in the following table 3:

Table 3

Reliability Return
biido
Degree Crease resistance (%) Bunny
line after the
Dry cleans
gene Ha
shen «
line Invention before washing 96.5
93.2 before washing 79.4
58.3 Ma-
small- 77 ₉ 7
66.6 avasser counter
was standing
comparison Koa-
pressure Bunny
rod 77.1
58.3 22.0
19.3 77.7
57.2

The above-mentioned polyorganosilozane solution and KS 724 were individually polymerized and shaped in safein. The one from the former obtained table shows the following physical

909850/1617

see properties, while the board obtained aua ES 724 so it was brittle that it was impossible to measure the elongation at break asu » Elongation at break 650 pounds

Tear strength 6 kg / cm

Hardness 10 °.

Example 4

A skein (500 g) of incorrectly twisted textured Hylon 6 yarn with 70 denier from 18 piles / 2 strands was immersed for 1 minute in the bath used in Example 1, whereupon it was dried in a centrifuge to a water content of 22 pounds introduced and then dried in air. The dried yarn was heat-treated for ^{10 minutes at 150 ° C.}

The amount of polyorganosiloxane fixed on the yarn obtained was O ₉ 3 wt.

The treated yarn exhibited excellent elastic recovery from stretching. The treated yarn and the untreated Yarn were each knitted into socks (knitted stitches, walesj, 28 / inchj courses: 4t / inch). The socks knitted with the treated yarn were both in stretchability as well as in Passits better, showed a small change in the Density of the mesh, which is caused by a change in tension is obtained in the knitting process, and besides, that could Knitting can be done smoothly. The result is shown in the following table 4:

1617

Table 4

phyeikaliseh> - ^ sample
Features - ^^^^ Eompression
Degree (#)
Retraining
Degree (#) untreated
object
τ according to the invention Pressure elastic
activity Haschenetäb ~ -
chen 00
Row of stitches ( 21.6
70.8 treated subject Degree of elongation 140
6) 9 * 28.8
86.5 200
150

Example 5

A pique, in which a rayon yarn of 1Fj "lon with 32 threads was used for both the warp and the sock (density, warp: 65 / inch; weft: 84 / inch), with" 1t the in case " Bad game described padded 3 'and a Aafns & nth of & 5% squeezed and 3 minutes at 160 ⁰ C wämebehanäalto the fixed on the fabric was amount Polyorganoslloxan t, 3 wt ·· the result 1st in the following Table 5 gezeigts

BATH ORIGINAL

903B50 / 1B1 7

Table 5

Compressive elasticity {%) Review
manic
^ rad Crease resistance (%) Shot Inventions Eompression
Degree 94.2
80.2 chain 131
103 object
Untreated Gc
genetand 14.2
12.8 145
98

Example 6

A fabric of a roughened tricot, which had been knitted with a Nylon-6-Fadengam of 17 to and 18 filaments was heat-set at 170 ⁰ C, and after 20 minutes if washing at 70 ⁰ C in the 20-iachen amount of a In a bath containing 2 g / l of a nonionic surfactant, it was fluorescent with 1 wt -colored.

The fabric had a 38 / inch density in the Maechen rod direction and from 32 / inoh in the course direction,

The above-mentioned fabric made of roughed tricot was not padded with a solution of the composition below and squeezed out with an inclusion of 160 #. On that it was heat-treated at 170 ° C for 45 seconds to form a fabric to produce, which was equipped with a permanent elasticity and resistance to aging.

909850/1617

The mustard fixed the amount of polyorganosilo xan "was 4.9 wt .- ^.

Composition of the treatment strand s trichlorethylene solution bit 15 wt .- $ C dimethyl

polysiloxane diol (?: about 1,000) »180 parts

Sibutyl £ innootyl maleate laurate ··· < >. ·" 2 parts Phenyltriisooyanatsilan o ·. ·· · 2 parts Trichlorethylene 820 parts

For the purpose of comparison, a treatment was made in the same Way as stated above, with the difference that since KS 714 used in Example 1 was used. The result is shown in Table 6. The tensile elasticity was measured under a 70 wale elongation.

Table 6

Tensile elasticity Blastic
quote-
«Wheel (£) after washing Elaeti-
citizen
graä i%) untreated counter · "
was standing
Behan according to the invention
del item
comparison before washing 22.2
95.5
85.8 load
for the-
nune (gj 20.5
95.2
65.2 load
for expansion
nung ^ ßj 148
153
145 142
150
155

The above-mentioned polyorganosiloxane was polymerized and in processed a board with a thickness of 0.7 mm, which the

909850/1617

showed the following physical properties: Elongation at break 424 %

Tear resistance

hardness

3 kg / cm

Example 7

Satin textile fabric, which had been woven with a cellulose acetate thread yarn γοη 150 den with 60 threads as warp and with a top-dyed wool thread with a thread count of 60 as weft, was padded with the treatment bath used in Example 3 and squeezed out with a take-up of 80 JC. Br was then heat-treated for 3 minutes at 130 ^° C. in order to produce an elastic textile fabric which was provided with excellent lattice resistance. A comparison with the untreated textile fabric is shown in Table 7 below

Table 7

Crease resistance (%) Shot Invention details treated
object
Untreated item chain 77.8
61.6 81.7
54 »5th

Example 8

Mn sports shirt with half sleeves, with a wrongly twisted textured Polyecterngava of 150 den with 18 fiden / 2 stvihnen (ßechtsmasohen, density, Maschenetilbohens 25 / ineh; Maechenxeiheni

909850/1617

40 / was knitted inch) for 1 minute into a solution of the composition indicated below immersed and placed in a centrifugal separator to make it to a water content clay 40 i "au dry · After air drying, it was molded and 2 Hinuten at 160 ⁰ C heat-treated o The obtained sports shirt showed a good elastic touch and had a * satisfactory tensile elasticity, compressive elasticity and crease resistance. The amount of polyorganoslloxane fixed on the sports shirt was 0.6% by weight

Composition of the BßhandlungalÖ * sunjg : Trichlorethylene solution with 15 Sew - # Dimethyl-

polysiloxane diol (P: about 1,300) _o ..... » _e .......... 100 parts

Dibutylsinnoctyl maleate laurate,. · .. “» ..., .. ·. · ... · 0.8 ropes Phenyltriisocyanatsilane _e . ··>", ....... ο ........ ° 0.8 parts Trichlorethylene ....-.... ■■ ». ,, -" .. o ... 900 parts Example 9

Men's socks knitted with a textured nylon 6 feather yarn from the 32 thread / 2 strand (density, wales: 29 / inch; courses: 43 / inch) were immersed in a solution of the composition given below until au an uptake of 45 £ squeezed and then for 1 minute at 150 ⁰ C heat treated · the fixed amount Polyorganoeiloxan on the obtained socks was 1.1 wt <- # _o the socks were ausserdea an excellent Paeeitz and excellent elasticity ₉ Uxul one felt there is no fire in the Eussen, as is the case with nylon socks when they are worn "

909850/1617

Composition of the treatment solution ; TrLehloräthylenlösung with 15 Gew * - ^ dimethylpolysiloxanediol, which 5 mol ^ MethylhydrogenBiloxaneinheitiienutlt (P: about 500) ".. <> 160 parts

Dibutylsinndl laurate ...... « _Λ .. 3 parts

Tetraethoxyeilane _o · 3 parts

Ferchlorethylene ·· .. · .. <> .. ·. <, <> 900 parts

Example 10

A double jersey fabric which had been knitted with a false twisted Hy.lon 6-thread yarn of 70 denier with 18 threads / 2 strands was ^{washed "at 70 0} g in 30 times the amount of a bath containing 2 g / l a non-ionic surfactant contained, with 1.2? £ Hakkol BS cone (a trademark for an anionic fluorescent dye _s manufactured by Showa Eagaku EE) stained and dried. to the optimum amount of au study resin to be used, were the same Behandlungelösungen prepared, as were used in example 6, except that the concentration of the resin between 0.5 and 40 wt _o - / S was changed Bie above-mentioned dried fabrics were padded with the solutions, to a pickup of 175 #. squeezed and then dried at 80 ⁰ C and then 2.5 minutes at 150 ° C heat-treated · the compressive elasticity and crease resistance of the resulting fabric were measured and are shown in Table θ g They showed were as follows:

909850/1617

Table 8

• ι 909 ¹ Efl; Pi », d.Ii88Tiog S «* · Degree of compression (^) O 0.075 0.15 0.45 Q, 75 1.5 3.0 4.5 6.0 7.5 850 / ~ ——Jfenge dee fix.Silikons
physical —— * -. ^^^^ ) ■ » Degree of regression (£) O 0.13 0.26 Q, 78 1.31 ?, 62 5.24 7.86 10.48 15.5 co Maaohenstäbohen 18.6 21.1 22.4 22.4 21.9 20.8 20.3 19.6 18.5 16.3 I. Hasohenrelho 69.8 7ä, 6 82.3 83.5 85.8 84.8 85.2 87.5 86.2 84.3 Handle aohl 55.6 77.8 BO, 6 82.2 85.0 92.2 90.6 93.4 91.7 89.5 58.9 84.4 B8., 4 86 * 6 85, 6 87.8 88.9 90.6 90.0 88.4 . «Clv« Well Well Well Well Well Well Well some • tvae
Lt bad
I.

If the fixed amount of the resin exceeds 10% by weight, then The degree of compression and the grip decrease and come closer together those of a rubber coating o

Example 11

200 g of a 21 denier Eohseidengarns with 7 threads / 2 strands in Ροπή a strand were washed at 10O ⁰ C for 1 hour in 40 times the amount of a bath "which contained 3 g / l Potachese soap" and dried. The dried extrudate was immersed in a treating solution as used in Example 3, introduced into a centrifuge heat-treated (to him on a Vaesergehalt of 42 i> drying), air dried, and then 10 minutes at 105 ⁰ C.

The yarn obtained in this whiteness was put in a jet type skein dyeing machine in which it was immersed in the dye bath having a bath ratio of 40: 1, which a solution of 4.2 wt .- # Kiton Fast Violet R (trade oak for an acidic dye made by Ciba Co.) and containing 2% by weight of potash soap, boiled for 20 minutes, gradually dried, washed with water and then dried again. The resulting yarn had a good balance ! coloring, and the problems of disgusting feelings (lousiness) as well as the pimples that had previously occurred in silk dyeing techniques were eliminated and the feel of the yarn became lighter · A ladies' costume was made with three of the yarns obtained (Rechtsmasohen, Maschenstäbohens 27 / tachf stitches: 40 / inehj £ an article excellent in wrinkle resistance and elasticity was obtained. The results are shown in Table 9 below:

909850/1617

- 46 -

Tabel

Compression elasticity {%) - Suckling
duxucsjcrad Crease resistance (^) Meshes—
line Compression
BionßßTad 88
95 Mesh
stäbohen 63.9
80.6 untreated
object
aX * xι TIh Wl £ 8fii9B £ U9 ΟβΧ * 18th
24 49.5
80.6 object Example U2

Mn twill made of two wool yarns and two mixed wool / silk yarns (warp: worsted yarn with a yarn count of 2/54; lap: Kaxaa «» yarn with a yarn count of 2/54 and silk yarn τοη 2/21 den; view of the warp: 42 / inch; density of the lap worsted 38 / inoh and silk yarn "5β / Χτ '} xäe bit of the same Lößung as was used in example 1, padded (pickup: 66 fi) at 80 ⁰ C and then dried. 3 Minutes at 120 ° C «Szae treated to

The Xextilet obtained in this way contained «£ f. 0.98 wt Poly organo ei loian, showed a part-like elastleoh ^ Srlfi and improved wrinkle resistance, anti-creep resistance and durability in washing,

For the purpose of comparison, a treatment was made in the same Catfish as stated above, bit the difference that the " Comparative bath used in Example 1 was used

The tensile strength, the elasticity, the emitter resistance and

909850/1617

the shrinkage during washing (percentage of shrinkage and WoWo, do ho wash-and-wear properties) of the treated textile fabric β was compared with that of the untreated fabric β and with that of the comparative fabric in Sahelle 10 Compiled

Table 10

Teardrop
sturdiness
(G) 1,580 Shot Pressure elastic
aity (#) Return
hild.-
Degree Emitter
eternity
(Wrinkle Shot Permanent
home
To wash, Shot W & W 1,280 Com-
pree-
ionic
£ jrad 89.1 regression)
(*) 78.8 Schrum
exam (&) _ 6.5 Untreated **
delter
Counterstai chain 1,600 18.6 92.5 chain . 89.8 chain 1.3 step
2 · K472
Ld 1.310 22.2 90.5 86.1 81.2 8.2 4.6 step
4th Inven- Io 888
appropriately
"treated
object 20.2 92.5 1.0. step
2 Ver *
same 87.5 2.8

Example 13

A double jersey fabric knitted from a worsted 1/44 count (density, hash double crochet; 39 / inch; size range: 34 / inch) was hot packed to relax and a course density of clay 35 / inch was obtained with the same bath as qb in the example

909850/161 7

3 was used ge3d.ot.At (receiving 85%!) At 70 ⁰ C tmd dried 4 minutes at 120 ⁰ C Wärmebehandelto The resultierende.Textilstoff (density, Maechenstähchen: 38 / inch; Masohenreihe: / 35.5 inch) contained 1.28% by weight -56 polyorganosiloxane, exhibited a favorable soft handle and good drapability and possessed excellent recovery from stretching, crease resistance, durability in washing and water repellency.

For the purpose of comparison, a treatment in the same catfish was carried out as above, with the difference that used by the comparison test in Example 3, the bath was ₀ The results of the comparisons of the T ext ils t offe .ata d shown in the following Table 11:

Table 11

pressure Stoop Pressure- Chick Permanent rei tf & W Tensile elasticity .. 165 3 level 152 Blaeti- picture- elaetizitSt picture- ability leg hen (SO fi elongation) 4th ^B 158 citizen elasticity Degree (after Trok- Degree To wash 3tuf
2 (#) cleaning) Shrink Bela j (^) exam stung
(β) Maeohen 15.4 Koa- B9.5 pree- 88.2 rod pres- ionic chen sion Degree 84.8 untreated Ijrad - 1.3 step delter 95.0 94.0 O ι C 1.5 object 91.5 25.2 89.5 12.8 Invention 24.4 95.6 dgemäfi 88.7 treated object 27.3 2.2 comparison 27.5 24.8 10.1 25.2

909850/161 7

Example 14

HLn Küper, made with a Torelon yarn (trademark for a polyacrylic yarn manufactured by Toyo Rayon KK) (warp: Garnaahl 1/50; weft: Garasabl 1/32; density of the warp: 86 / inch; density of the weft : was 80 / inch woven), bit was a solution of the composition indicated below knotted (recording .: 60 _t s0 at 8O ⁰ C and then dried for 30 seconds at 17 (C wäraebehandelt the resulting fabric contained 1.62 wt?.. -Jt polyorganosiloian, showed a favorable elastic handle and excellent crease resistance »

the

Triehlorethylene solution with 15% by weight of dimethyl

polyslloxanediol (f: about 20σ) .......... ο 180 parts

Dibutylssinnootylnaleate laurate ».» .. • «.. o ... ·. ·« .. « 3 parts

Phenyltriisocyanatsilane ··· «. <> ··. ····. ··. · <>. ··. ····» · <> 3 parts trichlorethylene. · .. <> .... «> 820 parts

For the purpose of comparison, a treatment was made in the same Way as stated above "with the" difference that the same Bath as used in the comparative test of Example 1. The result of the comparison of the textile fabrics is shown in Table 12 below:

909850/1617

- 50 -

Table 12

Pressure resistance
(*) Back
image .- ^ Crease back
education (?,) Shot Crease back
education (#)
(after V ^ Fchen) Shot [Untreated
object Koepree
aionegrad 85.1 chain 87.3 chain 83.8 That treat
the subject
comparison 20.5 89.5
86.7 85.5 92.3
88.5 81.6 89.9
84.2 27.0
22.8 89.8
86.2 87.8
83.2

The above-mentioned polyorgano-jloxane solution was polymerized to produce a plate with a thickness of 0.7 a », an elongation at break of 424 ?

Example 15

Ski socks that were knitted with a woolen yarn and the toes and heels of a Hylon-6 yarn (composition: 85 ^ full and 15 % Hylon; density, masohenet rod: 5 / inch; hash row: 8 / inoh) were stronger north, the following ZusammensetEung dissolved in a solution soaked sur reduction treated .des Vaseergehalte to 100 Ji in a centrifuge and then dried for 1.5 minutes at 150 ⁰ C. The resulting contained 2.5 wt. felting tendency both with vasching and with »

909850/1617

Composition of the treatment solution: Triehloräthylenlösung with 15 Gew .- ^ Dimethylpolßiloxandiol, which 5 Mol- # Methylhydrogen-

siloxane units contains (P: approximately 1,200) 160 parts

Dibutylsine dilaurate _ββ 3 parts

l'öt.raäthoiysilan _o ...... 3 parts

Perchlorethylene ... ·,> · .. ·. · «840 parts

Compare the socks treated as above with those not treated Socks and socks made with a conventional enema Pinioh has been treated wine »is in the shown in Table 13 below:

labeile 13

Pressure Reliability ⁺
($) Retrograde
duBgsgrad Durability at
To wash 3ehnii) ipfung
ler mesh
rows (? 6) Pil _r
sensational
aeißun *: (Untreated
object
Inventiveness
appropriately treated
the subject
Comparison ¹ " ¹ "
(elnlauTbe-
stäMigaachen-
of the finish) Compress
degree of sion 84.6
96.5
86.6 Very conduction
the! Saechön-
etäbehen (^) 8.5
0.8
1.5 atark
weak
saittel-
Nasty 46.8
48.2
46.8 7.8
1.2
1.8

Remarks;

•H-

The Draekelaotiisität wu2 "d © with two on top of each other laid socks gemeseeiio

For comparison, the socks have been treated with an aqueous solution of 3.0% by weight Basolan DC (trademark for a anti-fouling agent for Violle, manufactured by Badische Anilin- & 3oda -]? Abrik AG) »

909850/1617

example ) 6

A strand of pure woolen yarn (500 g / strand) was soaked for 1 minute in the same bath as was used in Example 1), processed in a centrifuge to reduce the water content to 50 pounds and then subjected to air drying, whereupon a 15 minutes lasting cure at 100 ⁰ C joined. The amount of polyorganosiloxane fixed on the yarn was 0.78% by weight. No noticeable shrinkage of the yarn was observed and the yarn had a good hand. A sweater knitted from the yarn treated in this way had good grip and durability, and had excellent dimensional stability . In addition, the knitting was smoother with the treated yarn than with the untreated yarn.

A comparison between the two, sweaters made with the treated yarn. of the untreated yarn had been knitted, iat shown in the following table 14:

Tabel Büekbil-
application size 14th EIa-
stlzi- durability
while chasing line Felting Compressive elasticity
(#) charity
Cl) shrinkage
fan OK, 8
2.5 pretty much
strong
easy iompres-
slonsgTo 87.8
94.8 Bridle elasticity 76.2
88.2 Mfsupc Be
burden rod
chen Treated
object
Brfi / ndtmgegeaäß
treated Ge
object '38, 2
42.5 <«) 15.2
3.5 150
136

909850/1617

Example 17

A Fuji selenium textile, i.e. a textile made from a spun silk yarn with a yarn count of 2/140 ale warp and a spun silk yarn with a yarn count of 1/66 as filling (density, warp: 112 / inch; filling: 88 / inch) was padded with a solution of the composition mentioned below, squeezed out until an absorption of 70 $> and then cured ^{at 130 0} G for 2 minutes. The resultant fabric · _ä material contained 0.5 uew "-9t Polyorganoeiloxan and showed a" thick handle and an excellent crease resistance.

the

Triehloroethylene solution with 15 parts by weight of dimethyl *

polyailoxanediol (?: about 80) 50 ropes

Oibutyl sense octylaaleate laurate. Part 1 Fhenyltriisocyanatsilane <, ·· ... ··. · «1 rope Perchlorethylene ₀ 950 parts

The comparison between the fabric treated according to the invention and the untreated fabric is in the following Table 15 specified!

90 9850 / 161.7

Tabel

Tear resistance

(2)

Latvian

Shit

Compression elasticity (ji) chatter formation (56)

ror that

Dry-

clean

Grain- Püekpressione- | degree degree

after dot froze
Dry clean EEroeken {clean

Com-

pres-

sions-ferad

Kick chain

Made Lette

laugh at it! rocking clean

Shot

Jnbehan-

older

Jegenatand

Findings * according to be ~ he pretends

.920

»• 368

2,048

2,816

27.2

27.0

78.8

89.7

79.2

76.8

86.6

77.2

89.4

75.2

87.6

Example 18

TtIτι broadcloth that had been woven with a mixed spun yarn with a Qarnsahl of 40 and vLt 65 wt. - $ 6 Folyesteretapelfaeer and 35 wt .-? C cotton (density, warp: 120 / inch; weft: 70 / inch) was woven washed, bleached, fuloreszenssgefärbt, with the same solution as used in example 3, geklotst, squeezed to "u a pickup of 70 £ and then cured for 3 minutes at 160 G ⁰ · Ber resulting fabric contained 1.05 6ev.- 0i folyorganosiloxane and has a thick handle and good resistance to cold.

The properties of the treated fabric are common sloped with those of the untreated fabric in Table 16 below:

909850/1617

Table 16

Compressive elasticity (&, Back Crease recovery rate {%) learn
aen after this
To wash Shot Bn-treated
object
According to the invention
treated Ge
object before washing 75
83 before (
Vase] Shot chain 74.4
81.8 Compres- »
degree of sion chain 78.8
82.7 78.8
83.5 29.5
30.5 80.0
85.6

Example 19

A double jersey fabric (the lengthwise elongation in the wale direction was 70 mm / 50 stitches), which had been knitted with a false-twisted textured nylon 6 yarn of 70 denier with 18 FMen / 2 strands, was knitted for 20 minutes at 70 ° C in the 30- washed times the amount of a bath containing 1 g / l each of an anionic surfactant and soda ash , dried, padded with the solution of the composition described below (absorption; 100 %), dried again at 80 ° C and then for 2 minutes at Hardened at 150 ^{° C.}

Zusa mmensetzu n g the TrichlorätliylenD-dissolution with 30 wt -.% Dimethyl

polysiloxaiidiol prepolymer (P: about 400) «·. · ...» .. 100 parts

Dibutyltin dilauret * ..., ........ ,,. * <,. · ... ... · .. <> Part 1

Polyoxyethylene itatiiEonoiaurat ₀₀₀ .. * ». ···· .. · _ο χ Part ⁴

Perchlorethylene ₆ , _e . · ... «., ·. · ..... ^ ......... ₀ 900 parts

BATH ORIGINAL

909850/1617

192874Ö

Remarks: The amount of this polyether compound has been changed, BQ that they are 0, 3.3, 10, 16.5 and 30 (Jew. based on the polysiloxane prepolymer, where 5 kinds of solutions were made *

Textiles made with the Polyoxyäthylenaorbitazoaonolatirat containing solutions had been treated, showed in comparison a noticeably reduced horizontal feel to the fabric treated with the solution containing no polyether compound and antistatic properties as well as excellent elasticity »

The comparison of these fabrics is in Table 17 below shown:

Table 17

- ** ^^^ amount of
im, -ZT ^ *** - · ^^ added 0 3.3 10 16.5 30th Uribe-
han «* ~ '
delt
(Gray.) Axial handle
Compressive elasticity
Electrostatic
Heibunsadruek (V) ⁺ * be
Right
88.5
2000 strong
redu
adorns
88.2
700 strong
redu
adorns
87.8
400 strong
redu
adorns
86.2
200 strong
redu
adorns
84.8
150 72.0
5400

Remarks;

POBSL: polyoxyethylene sorbitan monolaurate

The determination of the electrostatic friction pressure was carried out as follows: A cloth was rubbed with a pure BaumifoHtuch at 1050 U / min at 20 ⁰ C and 65% relative humidity and then, the electrostatic pressure generated was measured.

909850/1617

Example 20

Men's socks (density, stitches: 29; row: 43) »which had been knitted with a wrongly twisted, textured Hylon 6 yarn of 70 denier with 32 threads / 2 strands, were soaked in a solution of the composition given below, in a centrifuge treated to reduce the Vassergehalte to 170%, dried at 70 ° 0 and then 5 gehartet Hinuten at 120 ⁰ C "

the B ^ hpivi T

U.N

Trlohloräthylenlösung old 15 wt. -S * Dimethylpolysiloxanediol, which 5 mol-9 * Methylhydrogen-

ailoxane units contained (P: approximately 500) 160 ropes

Oibutylsixmdilaurat i . ··.; ·· ..... · 3 parts Tetraethoxysilane .. ··· ..... · 3 parts Polyoxyathylenlaurylphoenhat parts χ ₁ ⁺ Perohlorethylene 840 parts

Remarks: The amount of this polyether compound was changed so that it was 0, 3.3, 10, 16.5 and 30 OeW ₀ - ^ f, based on the polysiloxane, whereby 5 different solutions were obtained «

The socks that contain the polyether compound Solution acted showed a sufficiently suppressed smoothness and an excellent elasticity, while those who treated with the solution containing no polyether compound showed a smoothness so that their soles were slippery and gave a dangerous feeling when worn.

The comparison of the socks is shown in Table 18 below:

909850/1617

- 58 -

Tabel 18th

~ - ~ - ^^^^ amount of asuge-
Own- "** -— ^^ last POELP
shafts "" "" ■ - "^^ L ^ 0 J, 3 10 16.5 30th Gray Vacheiger grip
Pressure elasticity KU
slip
rig
92.2-
93.8 repentant
lates
92
93.5 siarlc
π you «-
z: .ert
! »0.8
92.8 strong
redu
adorns
90.2
91.8 strong
redu
adorns
88.5
90.8 78
72 Elastic regression at

Comments: * POELP: Polyoxy * tftylenlauvy! Phosphate

Example 21

Iylon-6 bit with a viscosity of 1.24 in m-xresol solution at 25 ° C and a hlsch polyester made of 9 parts of Hylon-6 and 1 part of polyhexa- ■ ethylenisophthalaiiid bit with a viscosity of 1.24 were melted separately, and the two aisles were extrudlert in the same öewichtsmengen side by side from an opening equal · aeitLg was 0.25 at the Purohvesser, wherein the Spiandüsenplatte a temperature of 280 ⁰ C exhibited, a uniform un Paden hersnistellen by the two polyamide components adhered to each other and in a side- by-side vezbaltnis were arranged over the entire length of the bath. The extruded sod was quenched in air, oiled, wound up on a tube at a speed of 700 m / min and then drawn to 4.1 times its original length to produce a monofilament yarn Y. of 15 denier Am multifilament yarn Y ₂ of 45 denier with 7 threads was essentially

909850/1617

received in the same white as above, with the difference » that the stretching ratio is 3.7 karat

The two yarns Y ₁ and Yp were each passed through a heated metal pipe having an inner diameter of 3 mm and a length of 50 cm in the relaxed state to develop slight crimps, and wound on a bobbin. When the yarn Y _{1 was} processed, then was the temperature of the heating tube 14O ⁰ C, the feed rate of 280 m / min and a is the Abzugegesohwindigkeit 211 m / min ,, When the yarn Y "™ has been processed, then was the temperature of the heating pipe 180 ⁰ C, the feed rate of 200 m / min and the take-off speed 150 m / min. Stockings were knitted with knitted stitches on a circular knitting machine equipped with 400 needles, using the above processed yarn Y. for the leg part and the above yarn Y ₂ for the toes, pereen and edge. After binding off, the knitted stockings were knitted at 100 ⁰ C for attenuated under a stress-free state for 30 minutes to develop their crimps, placed in a sack and ausgefomt in a dyeing machine of the rotating drum type colored "the colored socks were and steamed at 116 ⁰ C 45 Seknnden, for * drying of peeled off the form and left to shrink for 1 day in a room with 65 % relative humidity and at 25 ° C. «The resulting stockings were called" Stockings S ₁ * ", The stockings S ₁ were soaked in a solution containing 1 5 parts Polydimethylsiloxandiolvorpolymer with a PoIymerisatioBsgrad -one about 150, 98.5 parts of trichlorethylene and 0, CM part Bensoylperoxyö contained, on a centrifuge from uder "b au-. ansenLiesseiici been dried and designated deinn in hot 15 minutes at 165 G ^ getJ The ockneto be in this way ~ en stockings _f ISIT "stockings S _2"

BATH ORIGINAL 909850/1617

~ 60 ~

were, had 0.6 l " polyorganosiloxane",

Further stockings were produced in essentially the same manner as above, with the difference that, after dyeing, they were treated in an aqueous emulsion of a hardening agent comprising a silicone oil and a cationic surface-active agent (adhesion amount of the emollient B 1.1 wt. - $ Q contained «and then subjected to a deformation, whereupon the stockings were referred to as" Stockings BJ " _{or similar}

The stockings S 1 and S were very smooth and which, whereas the stockings S, had a somewhat hard grip.

The above mentioned stockings S., S ₂ ^and ^ j were worn by 60 people sum test »Bin consumer wore three pairs, one pair of each of the three different types of stockings, so that one pair was worn three times each until all were torn · Their lifespan was then determined. The stockings were placed in hot water with neutral soap after each day. washed after wearing. In this way, the relationship between the service life and the number of tears was observed in 60 pairs of stockings of one type, and it is clear that the number of unbroken stockings decreases inversely with wearing time. This relationship was determined by the exponential function of equation (1) approximated.

X at Ae "** (1)

where X: number of torn stockings As ATTKRtVl of the tested stockings (120) e: 2.718 (constant)
k: decrease coefficient
t: time

909850/1617

If equation (1) is applied, an average Xragelife is given by the reciprocal of the coefficient k, ie "t / k" The average life of the stockings S ₁ , S ₂ and 3 ~ was 75 hours, 82 hours and 2 hours · The socks e 3 had lost their softness after washing, whereas the socks S ₂ did not lose their softness and smoothness »

Too large an amount of the polyorganosiloxane led to undesirable results. In the following Table 19 the results of measurements of the elongation and the recovery of the leg part are shown in the case of stockings which were produced essentially in the same way as the stockings S ₂ , with the difference that the amount of the adhesive polyorganosiloxane differed

Table 19

Amount of adhesive Elongation (£) Regression (*) Polyorganosiloxanes (%) O 132 88.4 0.3 134 90.9 0.5 134 91.3 0.7 135 91.5 1.0 135 90.0 2.3 134 91.2 4.3 133 87.4

The procedure for determining the residual elongation and regression was as follows:

909850/1617

The distance (Lq) between the edge and the verse of stockings was measured"

Next, the strap of the stocking was fastened, and the stocking was hanging down, "with a load of 2 kg being attached to the lower end of the leg part." Later on, the distance (L-) between the edge and the heel was measured. Then the load was removed and 1 minute later the distance (L ₂ ) between the edge and the heel was measured again. The percentage of elongation and regression was measured by the formulas (II) and (III):

L ₁ L ₀ Percentage of elongation (%) »-4 —- ζ 100 (II)

L ₁ -L ₉

Percentage of regression 00 * rf-j * - χ 100 (III)

Io

Vis from Tatelle 19 * can be seen "the percentage regression is very small if the amount of the adhering polyorganosiloxane is greater than 4 £ ^{1" 1 From the} point of view of smoothness even an amount τύη less than 1 % gives good results "and a larger amount appears unnecessary .

Next, stockings 3 * 1 were "made essentially in the same way as in the manufacture of stockings S ₂ " with the difference that the leg part was trimmed with non-running stitches continued to have a good PaQsits. In contrast to this, ladder-resistant stockings * which were not treated with the Polyorgano83.lo.Tftn »were» a streokbarelt as well as a sole

BATH ORIGINAL 909850/1617

Example 22

Bylon-6 with a viscosity number tone 1 * 21 hone in m-cresol solution "at 25 ⁰ C and a copolymer of 88 Hylon-6 and 12 parts Polyhexametbylenisophthalamid bit were a Viskositätezahl of 1.2? Separately aufgesohmol & s and the two Sahmeisen were in the same quantities by weight of Se, ite side zusaimengefUhrt and at the same time from an orifice having a diameter of 0.25 m in a spinneret plate yon extruded 280 ⁰ C to a mono- ä threadlike produce "by ewei polyamide components adhered to each other and 3eite side-by-in a -Ratio were arranged over the entire length of the thread. «The extruded thread was quenched in air, oiled, wound onto a tube at a speed of 700 m / min and then stretched to 4 * 0 times its original length To produce a monofilament yarn Y ~ of 18 denier. Hultifaden yarns J ^ of 18 denier with 2 threads and Y, - of 45 denier with 7 threads were produced in essentially the same manner as above lt, with the difference that the _draw ratio of the latter yarn was 3.7 0 ·

A. each of the yarns Y ,, Y. and YV were passed through a heated (Ketallxohr with an inner diameter of 3 Bsn and a length of 50 cm in the relaxed state to develop slight crimps, au and as yarns Y _1. ,, Y ,. and Y _{1 ς} respectively on coils wound When the yarns Y and Y wurclen _processed? enteric the Oiemperatur was dee Erhitaungsrohrs 135 ° 0 'the Einlaiafgeechwijuiigkeit 280 m / min and the Abzugegeachvindigkeit 211 ϊα / _Εάη σ When that yarn Y _first treated was ^ then the em ~ perat'or of the Erhitiäuogsrohrs was 180 ⁰ C, the feed speed 200 m / min and ate KUgs speed 150 m / min _o stockings were knitted with Reehtsmasehea aixf an Eundetriökmasehin ©,

909850/1617 ^ö

which was equipped with 400 needles, the above processing

Gera X ₄ * for the leg part and the yarn Y _4c for the toes, Fer-14 15

was used sen and ribbons "After the binding off the geatrickten stockings were heated with saturated steam at 100 ⁰ C under a stress-free state for 30 minutes, to develop their crimps, placed in a sack and dyed in a dyeing machine of the rotating drum type. The dyed stockings were formed and ^{steamed for 45 seconds at 114 °} C., after drying, removed from the mold and left to shrink in a tree with 65 % relative humidity and 25 ^° C. «The resulting stockings were called" Stockings Sc "marked * The stockings Sj- were soaked in a solution that consisted of 1.5 parts of polydimethylsiloxane diol prepolymer with a degree of polymerization of approximately 150, 98.5 parts of peroxyethylene and 0.01 rope of benzoyl peroxide, spun off in a centrifuge and then dried and then 5 Hinuten helsser in air of 160 C cured the thus treated stockings were referred to as "stockings Sg ¹¹ and possessed 0.6 1» polyorganosiloxane. More stockings S "were prepared essentially in the same manner as obtained above, with the difference that the yarn Ϊ .., was used for the leg part _o Ea further stockings are produced in essentially the same way as indicated above tellt, with the difference that it an emollient were treated after dyeing with an aqueous solution, the country, a silicone oil containing a cationic surfactant (was the adhesive amount of the softening agent 1.0 wt _o ~ #), and then a molding subject The Stockings were referred to as "Stockings Sg",

The stockings Sg and _SQ were very smooth and soft, whereas the stockings S "and S" had a somewhat hard grip and a slight one

BATH ORIGINAL 909850/1617

Showed softness .:

- 65 -

Sg, S

₇ and 3 _Q were used for the test. she

The stockings S ₅ , Sg
were washed in hot water with neutral soap after being worn for a day ”. The S ₃ stockings had completely lost their softness after being worn 5 times, whereas the Sg stockings did not lose their softness and smoothness.

An adherent to groase amount dee polyorganosiloxanes led to undesired results "The following table 20 the results of measurements of the stretch and recovery are shown the leg part of stockings, waxen made essentially in the same way as the stockings Sg," it of Difference that the amount of polyorganosilozan adhering changed "

Table 20

Amount of adhesive Strain (#) Regression {%) Polyorganosiloxanes ( ^σ £) 0 145 84.0 0.3 151 90.5 0.5 150 91.9 0.7 163 92.1 1.0 162 91.5 2.5 163 91.1 4.5 169 86.5

The socks showed an elongation of $ 135 and a regression of $ 91.5

909850 / 16t7

The method of determining the percentage of elongation and the Regression was the same as in Example 21 above,

As shown in Table 20, is the percentage regression small when the amount of the adhering polyorganosiloxane is over 4 pounds · From the standpoint of smoothness, even amounts less than 1% give good results, and a larger amount appears unnecessary.

Example 23

Stockings S ₅ , Sg and S obtained in Example 22 were worn by 80 panelists. Each consumer wore three pairs, one pair of the three branches of stockings, so that one pair was worn for 3 days each until they were all torn been · your life was held »in this way, a connection between the life and the number of cracks at 80 Struapfpaaren a kind was observed" Ss is clear that the number of torn stockings with the gestation period decreases _β the relationship was by the exponential function of Equation (1) given above is approximated. The average lifespan of the stockings Se, Sg, S "and Sq" was 85 hours, 92 hours, 82 hours and "87 hours", respectively

the stockings produced according to the invention had a

longer" average / lifespan than the stockings that come with one

herkössBliehen J softening agents had been treated.,

Example 24

Bylon-66 with a viscosity of 1.15 szahl in m "fe§sollö * 8ung at 25 ⁰ C and a copolymer of 4 parts, nylon-66 vr» ^7> from ropes! Ylon-610 with a Viekositätassahl of ίί & iimMen

909850/1617 ORiGiNAL BATHROOM

separating melted, and the two melts were, in the same weight brought together side by side and at the same time from an orifice having a diameter of 0.25 ram in a spinneret at 290 ⁰ C pressed to prepare a monofilament, in which together the two polyamide components adhered and arranged in a side-by-side relationship over the entire length of the thread. The extruded thread was quenched in air, oiled, wound onto a tube at a speed of 600 m / min and then 3.9 times of its original length on a Ziehatif t drawn at 80 ⁰ C, share a filament yarn Xg of 20 to 3 threads out. A 7-filament hernial yarn Y ₇ of 45 denier was obtained in substantially the same manner as above except that the draw ratio was 3 »6. The yarn Y was given a twist of 120 turns / m, and / by a erhitsstes Netallrohr of 160 ⁰ C, the inside diameter of 3 mm and its length was 50 cm, with a feed rate of 600 m / min and a Absugsgeschwindlgkeit of 550 m / min passed _o The heat-treated in this way yarn Y _4, - was then applied to a pirn wound the yarn Υ "has been substantially wärraebehandelt for manufacturing a yarn Y ₁₇ in. the same manner as above, with dam, except that the feeding speed 250 m / min, the Abjsugsgesehwindigkeit 222 m / min and the temperature of Brhitznmgsrohrs 180 ⁰ C was * Stockings were knitted with ladder-resistant stitches on a seamless Run & Striekaiasehtne equipped with HOl needles, the above treated yarn Y., for the leg eil and the yarn Y ₁₇ was used for toes, heels and edges, laughing the binding off were knitted stockings with saturated steam at 100 ⁰ C under a voltage condition heated for 30 minutes and then further heated with saturated steam for 10 minutes at 120 ⁰ C. ρ to develop the ripples «, The rippled ones

BAD LOCAL GINAL 909850/1617

• 68 "

Stockings were then placed in a sack and dyed. They were then shaped and ^{steamed for 45 seconds at 119 0} O, • removed from the form after drying and left for 1 day to shrink in a bar with 65 relative humidity and 25 ⁰ O. the resulting stockings were referred to as "stockings Sg""the stockings S _g were soaked in a solution of 2 parts of a Polydimethyleiloxandiolvorpolymer ait Polyeerieationegrad of about 100, 96 parts of trichlorethylene and 0.02 parts of benzoyl peroxide was squeezed off in a centrifuge, so that various adhesive amounts were obtained, followed by drying. Then they were listened to in hot air at 150 ⁰ O for 3 minutes.In the following Table 2, the results of measurements of the elongation and the arching of the leg part for the stockings with various adhesive amounts of polyorganosiloxane are shown, which measurements are made in the same manner as in the above 'Example 22 were carried out.

Table 21

Amount of adhesive Strain (#) Regression (%) Polyorganosiloxanes (#) 0 192 80.4 0.3 208 84.9 0.5 212 90.1 0.7 215 89.7 1.0 209 88.2 2.5 223 89.5 4.5 230 82.6

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All stockings on which polyorganoslloxane was present a better softness than those «which had not been treated with bit polyorganoslloxane ..

Other stockings Sj ₀ , which had 0.5 wt .- ^ polyorganosiloxane, were produced in the same way as the stockings mentioned above, with the difference that a monofilament of 20 denier was used for the leg part. They stockings S ₁₀ had one Elongation of 181% and recovery of 86.2 Ji and had a rather hard feel which was undesirable, whereas the stockings Sq made according to the methods of the present invention had an excellent grip.

In general, stockings knitted from a multifilament yarn can be mixed with a better amount of polyorganosiloxane be provided polymer, as stockings that have been knitted with a Monofadeagarn. The larger adhesive amount of the prepolymer not only improves the appearance of the stockings but also in most cases intensifies their stray force

909850/1617

Claims (1)

Process for the production of a fiber structure with a certain elasticity, resistance to khitter and resistance to shrinkage, characterized in that a non-aqueous solution of a polyorganosiloxane prepolymer containing a polymerization catalyst for this is placed on a fiber structure, homogeneously in a quantity of not much than IO Ckw.-? 6 Polyorgano »slloccan component, based on the structure mentioned, applies, ψ and the resulting structure * of a heat treatment during a. subjecting temperature of 50 to 20O ⁰ C to initiate polymerization of said prepolymers to bring en end. 2 · The method according to claim 1, characterized in that the structure is made of staple fibers. 3 · Method according to spoke 1, characterized in that the laser structure sua at least 20 ßew.-flt from endless threads and there is a maximum of 80 Öew - ^ ans staple fibers _ 4 · The method according to claim 1, characterized in that the "The couple structure consists of endless lüden. 5. The method according to claim 1 _1, characterized in that the pas structure number is a knitted product which consists of a crimpable yarn of composite threads 6. The method according to claim 5 _9, characterized in that the knitted goods are Damenstrümpfβ, 7. The method according to claim 5 _9, characterized in that said yarn is a multi-thread yarn _{or the like} 909850/1617 19287A0 8o method according to claim 7t characterized in that knitted goods Daaenatrümpf θ are · 9ο The method according to claim I _1, characterized in that the PolyorganoBiloxanvorpolyoer contains as main component or main components-at least one linear polyeiloxane whose side chains consist of lower alkyl groups and which is selected from poly (dimethylsiloiaia) diol and poly (dißthylsiloxane) diol. 1Oo method according to claim 1, characterized in that the polyorganosiloxane prepolymer poly (dimethylsiloiane) diol as Main component and methylbydrogenpolysiloxane as a lifting component contain 11. The method according to claim t, characterized in that the polyorganosiloxane prepolymer contains at least one linear polysiloxane as the main component or main components contains an aromatic group as side chains and consists of poly (methylphenylsiloxane) diol and poly (diphenylsiloxane) diol is chosen 12o method according to claim 1, characterized in that said prepolymer has an average degree of polymerization of at least 50 13- The method according to claim 1 _p, characterized in that said prepolymer is an average polymer. has a degree of at least 100 » 14 ". Method according to claim 1, characterized in that 909850/1617 BAD ORIQINAL the non-aqueous solution of the polyorganosiloxane prepolymer Is a solution of an organic solvent which is selected from at least one of the following solvents: toluene »xylene» Benzene, perchlorethylene, polychlorethylene, industrial gasoline, Chloroform,. Methyl chloroform and methylene chloride 15o method according to claim 1, characterized in that organic the catalyst is at least one tin compound which is made from Dibutyltin dilaurate, dibutyltin dioctoate, dibutyltin sauce, Tin (II) octoate and gelat compounds of tin is selected 16 _{e The} method according to claim 1, characterized in that the catalyst is contained in an amount of 0.01 to 5 wt .- ^, based on the polyorgatiosiloxane component, _e 17o A method according to claim 1, characterized in that the catalyst ₉ is in an amount of 0.1 his 1.0 Gewo- ^ j included 'in the polyorganosiloxane. 18o method according to claim 1, characterized in that the catalyst contains at least one accelerator for a crosslinking reaction selected from the following group is: isocyanates of silane compounds, alkoxysilanes, Acetates of silane compounds, benzoyl perozyd, triols and vinyl compounds 19o A method according to claim 18, characterized in that the accelerator is no longer based on the Polyorganosilozankomponente contained in an amount of 15 wt than _o = $, _o 20. The method according to claim 1, characterized in that the non-aqueous solution continues to contain at least one polyether 909850/1617 _BA d ORtGiNAt 19287A0 Compound selected from the following groups is: polyoxyethylene alkyl ether, polyoxyethylene alkyl phenol ether, Polyoxyethylene alkylamine, polyoxyethylene alkylphate, polyoxyethylene sensor, titanium fatty acid ester and polyethylene glycol 21 ο Method according to Claim 20, characterized in that the amount of polyether compound present is 1 to 50 (Jew - ^, based on the polyorganosiloxane prepolymer, is » 22o Process according to Claim 2O _9, characterized in that the amount of the polyether compound contained is 3 to 20% by weight, based on the polyorganosilaxane prepolymer, _o 23ο method of claim 1 _v characterized in that the Wäxaebehandlungstemperatur IQO to 180 ⁰ C beträgto 24o method according to claim t »characterized in that the structure for 20 seconds to 60 minutes of said heat treatment is subjected. 25ο Method according to claim 1, characterized in that the structure takes one minute
Act is subjected the structure one minute to 10 minutes of the mentioned wazmebe » 26. The method according to claim 6, characterized in that the Bamers stockings have previously been subjected to a crimping development treatment. have been subjected to a case treatment «. 27 “fer-fslides aaeli Ansprueii 6, ctadorch gekeimseicliii- © t that i? Liegsage "ϊ & Έ -? - ¹ ^. \ :: -: & - - « d-ü. V G £ Z S ί '/ ^ Γ "' ^c - ■ - ^{D 0} ^ ¹ GINAL 28 · A process for the manufacture of stretchable stockings with a permanent flatness and softness, which is characterized by the combination of the following stages: knitting a stocking from a composite polyamide monofilament yarn; Developing the ripples; dyeing the stockings; homo "genes applying a non-aqueous solution in an amount of O ₉ 1 to 10 α by weight 96 of the Polyorganoslloxankomponente based on the stockings, containing a poly organosiloxanTorpolymers the stockings thereof, a catalyst for the polymerization, and subjecting the resulting stockings a heat treatment at a temperature λ is followed by molding, (boarding) c Heat treatment at a temperature of 100 to 180 ⁰ C, before 29 «Faeerstructure obtained by the method of claim 1 has been produced, characterized in that a maximum of 10 Ge * .- 56 of a polyorganosiloxane is based on it homogeneously attached to the fiber structure, soft ones Elongation at break of at least 50 #, a hot strength of. 1 cowardly 50 kg / cm and a hardness vcm 5 Ma 50 « 30 «fiber structure according to claim 29, characterized in that that it consists of staple fibers " 31 »fiber structure according to claim 29 $ in that it consists of at least 20 wt. 56 continuous threads usd 80 wt. 96 staple fibers» 32 · Fiber structure according to claim 29, daferuli that they aas endless flfciea. b 32, I; - " u, ' ■' ■ ί, Ι © ': \ 1) / -, r; τ BAD ORfGiNAL Yarn is made up of composite threads. 34o fiber structure according to claim 29, characterized in that it has the shape of women's stockings made of a
frizzy elitist yarn consists of composite threads » 35ο fiber structure according to claim 33t characterized that the yarn is a multifilament yarn 36. Fiber structure according to claim 35t, characterized in that it has the shape of ladies' stockings _a 37 · Fiber structure according to claim 29, characterized in that the elongation at break is 150 to 800 % _o 38o fiber structure according to claim 29, characterized in that the tear strength is 3 to 20 kg / cm ² «, 39 · Fiber structure according to claim 29t, characterized in that that the hardness is 8 to 30 °. 4Oo fiber structure according to claim 29t characterized that the fixed amount of the polyorganosiloxane 0.2 to 5 wt. ~% based on the fiber structure. 41 ο fiber structure, according to claim 29t, characterized in that the fixed amount of the polyorganosiloxane 0.3 to 3
based on the fiber structure, is o 909850/161 7