DE1907605A1 - Process for stretching and heat treatment of polyester threads - Google Patents

Description

As is known, polyester threads show a high degree of crystallinity and a high melting point and others excellent properties, for example high resistance to heat »chemicals and light, great strength and high modulus of elasticity. Because of these favorable properties, the threads are very important as clothing and industrial materials. In particular, took its importance as Cbrdmaterial for tires rapidly in the last time too. Although a number are particularly important There are requirements for Qordmaterial for tires the most important, that the material has a high strength, tensile strength, toughness, dimensional stability and fatigue resistance from

When comparing τοη polyester threads as cord material for chains with polyamide threads, e.g. Iylon-6, Iylon-66 and the like, the polyester threads show excellent thermal stability, but are the polyanide threads strength, elongation and mechanical fatigue resistance not necessarily superior. The followers were made of polyester thread, which made the high

9P9S40 / 15 88

Maintain biaxial stability, and furthermore have improved mechanical strength "- ₉ elongations" and fatigue resistance properties, have a far greater usability not only as tire cord "but also in the field of clothing and interior decoration"

Various attempts have already been made to improve these properties of polyester threads. For example, the Polymerisationegrad of the threads forming polymers was increased to try _s jsu filaments with high strength, elongation and fatigue resistance to manufacture. However, of course, the degree of polymerization cannot be increased above certain limits which are due to the operating factors, and the tests did not give satisfactory results. '. ■:.

In the course of extensive investigations over long periods of time, the present invention provided the desired solution to these problems with regard to the improvement of polyester threads.

The object of the invention is a new one Process for stretching and heat treatment for the production of polyester threads with high breaking strength, Elongation at break and large Young's Hodul

Another object of the invention is one Process for stretching and heat treatment that consists of • There is an excellent and new combination of streok stages and heat treatments to produce polyester threads manufacture that are particularly suitable as tire cord,

high da si · high toughness, fatigue resistance and natural ktits-! 7a conversiont-7rehaltni · (Ji conversion of strength of the outer yarn).

909 8 4 07 1S8 8

Dae inventive method for stretching and Heat treatment τοη undrawn polyester threads, the Contain at least 85 mol of ethylene terephthalate units, consists of the following stages, which are to be carried out in the order given

(1) stretching the first stage "wherein the unstretched filaments by 1.1 to 4.0 at temperatures ranging faohe τοη be stretched 40 to 100 ⁰ C;

(2) stretching of the second stage, these stretched filaments still at a temperature in the range τοη 10 to 85 ⁰ C, but lower than they were used in stage (1), at a stretching ratio in the range from 1.2 to 7.0 times, which is at least 80 # of the maximum stretch ratio, can be stretched)

(3) First heat treatment, the threads being heat-treated at a temperature in the range τοη 55 to 12O ¹ Cj but higher than in step (2) while they are subjected to a tension equal to the thread length during the heat treatment 95 to 130} t of that value immediately before treatment, and

(4) «wide heat treatment, with the threads at least once at higher! temperatures than in level (3) were applied, and at least one stage of heat treatment at a temperature not below from 110 ^ is carried out «to be heat treated, the filaments at each stage being subjected to a tension which is the length of the filament during the treatment holds at $ 95 to $ 130 of the value of the immediately preceding level, and continues to the

909840/1518

Tension exerted on threads at each stage of stage (4) is set so "that the thread length after the end" level of level (4) at least $ 90 of those values « immediately before step (3) becomes · The characteristic features of the invention are continuously the following: Production of a highly oriented, but non-crystalline, stretched thread from Polyester by “white-step stretching of non-stretched Polyester threads at relatively low temperatures, such as they are indicated in steps (1) and (2); Manufacture τοη stretched threads from polyester with a uniform structure both in the vertical direction parallel cur thread axis from the stretched threads from high oriented, but not yet crystalline material a first heat treatment under tension according to step (3); Manufacture τοη polyester threads τοη very uniform? Structure both in the direction perpendicular and parallel to the thread axis from the stretched threads of the highly oriented and highly crystalline material through a single-stage or multi-stage second heat treatment in the Level 4)·

The obtained in this way according to the invention Polyester threads have a remarkably high breaking strength and elongation at break because of their excellent properties Structure and have a very high toughness. At her Used as soap cord, they have excellent fatigue resistance and high strength conversion rates. ratio. Since they still have very high Young's modulus values, the disadvantage is - Tön flat FIeeken remarkably improved in comparison to EU nylon tire cord * Thus, the inventions stand out. available polyester threads significantly compared to conventional products

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out as si · equilateral in all of the sahlrelohen important mechanical properties look excellent behavior·

The critical feature of the method according to the invention lies in the combination of the steps (1) to (4) listed below. As you can see from the following examples and comparative comparisons »lose, even if only a condition of the Sahi rich gatekeepers listed working conditions of the tier levels outside of the range listed, «the polyester threads obtained, the properties of the polyester threads obtainable according to the invention, i.e. the equilateral superiority in sahi rich mechanical Properties,

In Fig. 1 is a stress-strain curve τοη in accordance with a design of the invention Polyester threads produced by the process are silted. In Fig. are stress-tendon cures τοη corresponding to a further embodiment of the method according to the invention obtained polyester threads and τοη according to usual Process made polyester threads sung

The method according to the invention is explained in detail below.

The non-stretched ones used according to the invention Polyester threads are made up of high molecular weight polyethylene terephthalate "i.e. a polymer which has at least 85 mol-tf, up to 90 mol-ji" of recurring Structural unit possessed by the following formula

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Unstretched threads can be such »the naoto. desired commonly used spinning process has been spun

Thus the expression "polyester ^{N" is used} in the sense that it also includes a polyethylene terephthalate modified by the addition of not more than 15 Hol-Ji of other ether-forming units. The following are listed as such other ester-forming units present in smaller quantities: Bi - Ethylene glycol _for other polymethylene glycols with 1 to 10 carbon atoms, hexahydro-p-xylylene glycol, aromatic sicarboxylic acids, such as isophthalic acid, dibenzoic acid, p-terphenyl-4,4 "-dicarboxylic acid, and hexahydroterephthalic acids, aliphatic adiatic acids, such as hydroxy adiatic acids , and similar connections.

The polyester threads used according to the invention also include threads.

The properties of the unstretched threads are not critical, but thread bits with an inherent viscosity of at least 0.5 and a birefringence in the range from 0.0005 to 0.0120 are preferred. In the case of non-stretched threads with a birefringence outside the range listed, there is a deposit due to the formation of lack of stretching or an increase in thread breakage during the spreading operation. Torsugly · the appearance · of the non-stretched threads is not higher than 1.35 g / o » ² · Otherwise it results in a · increasing tendency to thread breakage during stretching ·.

Si · di · properties of the polymers and the values indicating the threads were determined in the following manner

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The inherent viscosity of a polymer becomes ale Bora des Polymerisationgradee dee polymers, accordingly given in the following equation

lim In c-> O C

In the formula, ^ r normally means the relative viscosity, which is obtained by dividing the viscosity of a dilute solution of the polymer by the viscosity of the solvent used, which are determined at the same temperature, c means the polymer concentration in the solution, given in g / 100 ecm · The intrinsic strengths given in the present case were calculated from the ^{values determined at 35 8} C using o-chlorophenol as solvent »

It is known that the load-elongation curve and the breaking strength and breaking elongation values calculated from the curve are variable in shape and value according to the length of the test specimen and the rate of elongation. In the present case, the tension test was 20 cm long samples at a stretch rate of 5056 / min. Carried out under standing conditions (2Q ⁰ C, relative humidity 65 #) using an Iistron drawing device

The "degree of inclination of the load-elongation curve ¹ 'is given by the differential coefficient of strength to elongation at each point of the load-elongation curve, ie the degree of the tangent, line correction of the values in line with the decrease in the paddling values, which are associated with the Stretching, was not performed

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According to the present process, dl * unstretched polyester threads are first subjected to a stretching of the first stage, where they are 1.1 to 4.0 times, preferably 1.2 to 3 »0 times _t at a temperature in the range of 40 to 100 ^° C., preferably 60 to 100 ° C., as described in step (1). Any heating media can be used in this step, but liquid non-solvents such as water and ethylene glycol are preferred.

Bie threads of the second stretching in the second stage are then subjected in step (2) under the following conditions * Bie threads are at such a temperature generally range from 10 to 85 ¹ C, preferably 40 to 75% lower than the first in stage (Stage (T)) applied stretching ^{temperature is, preferably at least 10 0} O lower, with a stretch never behaves in the Berti oh of 1.2 to 7.0 times stretched, which is at least 8Q $ t of the maximum available stretching ratio is under the second stage draw conditions and is preferably within a range of 1.5 to 5.0 and is at least 90 pounds of the maximum draw ratio listed above. The type of pickling medium is not critical at this stage, but liquid photo solutions such as water and ethylene glycol are preferred. . ' . ■. - - _ \ ......:. "- Λ -

The protruding stretches of the first and second Stage can be known in practice with any Stretching device, as it is usually used, be performed·

Ber hler applied expression "maximum draw ratio" denotes the maximum draw ratio of the threads under the specific drawing conditions in which

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• m Q mm

no thread breakage · of course there is « maximum draw ratio of the properties of the au The stretching thread is also dependent on the scattering conditions, such as temperature, medium> in which the threads are stretched, Streokgeaehwindigkelt and the like. influenced.

The polyester filaments obtained as a result of the two-stage drawing are then subjected to the first heat treatment in stage (3) under the following conditions! The threads are bevorsugt at a temperature in the range of 55 to ⁰ C IZO ₉ 65 to 10O ⁴ C ₉ but which is higher than that applied in the stretching stage in the sweiten! Temperature, preferably at least IOTJ higher, heat-treated ·

During the heat treatment, the polyester threads must be kept under tension so that the thread length bsi 95 to t30 £ of the value immediately before step (3), i.e. the value after the end of the step (2). In other words, the threads are either stretched or stretched to a maximum of 30j £, or kept at the same length, or shrunk by a maximum of 5 Jf *

The polyether threads obtainable according to the invention have a pronounced pattern of shrinkage after dsm two-stage stretching of stages (1) and (2) in the manner described above and bsi during the Heat treatment of step (5) applied temperature conditions, and normally · one free · shrinkage of at least 20 £ · S «r expressions * free shrinkage" means the spontaneous shrinkage, given in Jt, 41 "occurs when the threads are exposed to the temperature conditions free of tension. Therefore, if the polyester threads are kept at a" state, this does not exceed

0098 40/16

5 erauglloht it shrinkage during heat treatment of the step (3) to receive the filament a sufficient voltage, since the free shrink ale far greater the allowed shrinkage. As a result, the threads never show changes in shape or configuration, such as forming tone crimps, and are devoid of relaxation or relaxation.

Thus, the term "heat treatment means under tension ¹ * ndlungsbedingungen such the heat treatment that the threads either on a limited shrinkage you no more than £ 5" which is far lower than the free shrinkage of the same threads under the applied Wärmebsh & be restricted, odeE ^{1 maintain} their constant length, or the threads are stretched with a stretching ratio of at most »30j6, whereby the threads are kept in the tensioned state.

The threads that have received the first heat treatment under tension in stage (3) are then further heat-treated in stage (4 ).This second heat treatment of stage (4) consists of single-stage or multi-stage heat treatments under tension. The treatment temperatures in all stages under tension of stage (4) must be higher than the temperature used in stage (3), preferably at least 10 ⁰ C higher »and in at least one stage of the heat treatment of stage (4) the threads of a heat treatment at a temperature not lower than 11CW, preferably not lower than 120 ⁰ C, and more preferably not lower than 150%.

In accordance with the present method, it is essential that in each stage of the heat treatments that the Form step (4), the threads are kept in a single state, so that they have a length corresponding to 95 to 130jt

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the value of the threads after the end of the going Heat treatment stage and before the relevant stage have, and they are given a tension to do so. Furthermore, the voltage in each stage must be set so that that the threads, after they have passed through the final heat treatment stage of stage (4), have a thread length corresponding to at least 90 ° C of the value of the threads after the stretching of the «wide stage in stage (2) and immediately before the first heat treatment in stage (3) own.

When the threads are in such a condition at everyone Stage of stage (4) are maintained, the heat treatments meeting the above two requirements, the threads are always under tension during the second heat treatment due to the same reasons as they are at the first heat treatment are described.

The limited or allowable shrinkage in the Heat treatments of steps (3) and (4) is preferably not more than 3 ^ t, and in general, satisfactory results are obtained if the heat treatments are carried out while maintaining a constant thread length or be carried out under stretches of at most 3O # and the filaments are not heat-treated with a shrinkage within the specified range. The treatment time in steps (3) or (4) is not critical. However, times in the range of 0.01 to 1000 seconds preferred. The heat treatments of the stages (3) and (4) can be carried out using separate gate directions or using a single heat treatment device containing multiple stages, in each of these zones or devices the Heat treatment is carried out separately for each stage

909 840/15

- 12 · * ■ - ■ -, ■■■ - -

liii © characteristic feature of the

driving consists in »that that
(fBE) significantly hHher is \ -as it
can be redeemed »because those listed above ©. h © 2? = * outstanding © combination of stretching · »uni heat treatment®« stages is used * Si © from the: above stages.ft) to (: 4) threads obtained can have a length © ¥ oa i «to TO = - fold »of those of the untwisted? @@ kten threads be @ its © n _9. -uncL- ■ -. due, achieving such extreme Hoker · '& ©©© at = _v'. streek relationae set "see Ulm Yort © ± 3L® _: <S @ o ^ ös * -. lying procedure most clearly aesau-s« ■ - '"": -

The heat treatment can also tempera door · -fi © ^ Stui © _; | 4) "up to 600 * 0 or even fflnmn increased -'wE-cIeng - .." if for example a bekss2! T »© 3? -Sslse-Ehltsose ¹ wqm Wiöiit · = · .. contact type is applied _e - '-. . ^: . . ^: ".

As explained above,

What are the characteristics of the present constitution i® nation d @ 3? Levels (1) to {4) s "-wob © i TerseMtiöso Hoüfite · = tion @ a within the specified 3®%®i@h.Q_ _ äeT s & lilreieh ^ a '.- Working conditions are possible ·" ■ "-. ■ - ■ - "-" :. -: - _"-: ^-: ~ - ~

Bsispieleweise can n ®h © iser present process erhaltemi
Characteristic type of

.. la 1st generally bekaimt _f IASS di © curve toe Polye.sterfäden eiae r © © © t and "one GT7 © it @ limit (yield point) shows · The side to ^.des-d;. ergen strain and low elongation lying ®- is referred to as the first yield point · and the other as the yield point · On the other hand, in the characteristic load 8-Dehnung®-Curv®, the presence of a first yield point is not very '/ significant very clearly &.

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shows, as can be seen from FIG. Also on the stress-awareness curve is the degree of inclination after the other Characteristically very low yield strength · In an optimal embodiment can polyester threads with a very excellent mechanical behavior that is completely different from that of conventional products iat, for example, minimum degree of freedom not greater as 9 g / d above the point of 7 »O g / d on the stress-strain curve, according to the invention can be obtained *

In one form of training the present procedure can, if stage (4) consists of two heat treatments and all heat treatments of stages (3) and (4) be carried out so that the threads are held under such tensions that the length of the thread in each Step 95 to tlQjf of the value immediately before the step, and if the voltages are still set are that the threads after the heat treatment of the second Step of step (4) have a length corresponding to at least 9O96, but less than 120? own.

In particular, polyester threads can sit this type of Load-elongation curve based on a form of the Invention, i.e. by the process cum Drawing and heat treatment of non-stretched polyester threads which contain at least 85 Μο1-? Ί and preferably at least »90 HOl-J * polyethylene terephthalate units, where the following steps are carried out in the following order: 1

ΐ-907605

(1) Stretching of the first stage “whereby the threads are 1.1 to 4 times 0-fold, preferably-the I ₉ .2 to 3.0 times, in a liquid optical solvent of one Temperature in the range from 40 to -1OO ⁰ C _6, preferably 60 to 100 * 0, are stretched,

(2) second stage stretching, this being © stretched. fäämi in a liquid bio-solvent of temperature in the range of 10 to 85 ⁶ C ₉ preferred. "- 40 751!» "which, however, is lower than di® in & ®r stage © (" I) eh · = * applied temperature, preferably at least «! 10 ⁰ C ηί®ατί. * ° - lower , with a stretching ratio of. 1 * 2- to T ^ O- * times, preferably 1.5 to 5.0 times, the-at least- ". 80 i »of the maximum stretching ratio, g © ° = be stretched,

(3) First heat treatment, the filaments b @ i temperature not below 6Q ⁸ C, but lower 100 ⁰ C and higher than the temperature applied in step (2) are heat treated while they are subjected to a tension, so that the fiber length during the treatment at 95 to 1T.5 # ». · before, sugsw @ is &, 95 to 11O56, the value immediately before this ©? Treatment is held, _

(4) (1) first stage of the second heat treatment _s where ii @ ? & Ά · η are treated at a temperature in the range from 100 to 170% while they are subjected to tension, ie the thread length during the treatment at 95 bi · 115 £ »precaution» w «i ·· 95 to 110 $, which holds the value immediately before this heat treatment, etc.

(4) (2) "wide" step "dtr" wide heat treatment, whereby di® Fid · »continues to be above 170 ° C Fe »fer» treated while under tension subject to a * that increases the length of the shop during loading *

$ 90 84O / 1h *

ORIGINAL / MSPECTED

treatment at 95 Ws 115 ^ ₉ preferably 95 "to 110 $, the value is held immediately before this heat treatment, the tensions exerted on the threads in stages (1) and (.2) of stage (4-) bo are that the thread length after step (2) of step (4-) at least $ 90, but less than $ 120 * preferably at least $ 95 »but less than $ 120, the fourth immediately before the previous step © (3) If the polyester filaments having the above-described type B © la © tung ~ strain -. curve characterized by the Satsaehe © us ₉ that in their use as Eeifencord the cord gear considerably improved fatigue resistance and FestigkeitsuMv / andlTinggverhältnisse plays the violin "" .-. - ■

Various methods for determining the resistance to wear of tire cord have been proposed, and the results of the various © !! methods versuohsme-today not always ₈ correspond. general- ^ eäoöh can check siehsn ₅ of the secure circuit äaß ₉ in the Pail, the comparison of the Ermüdungsbeständiglceit L? & aen ₉ siad composed of identical polymers, those _9, the greater toughness (strength χ Dehnung- s 1/2} violins, also have a higher fatigue resistance »That is why the toughness is used as a measure of the fatigue resistance in the present Pail. As mentioned above» the threads have a load ^ dahnungscurve that was obtained in the tensile test , wherein the degree of skewing after the second yield point is very low, has great toughness, As a result, when yarns of such filaments are twisted together to form a tire cord, the cord exhibits high fatigue resistance.

Also the fact that the degree of inclination is close to the "wide Yield strength is very low, shows that the Feetig-

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chain conversion ratio during manufacture Cordes from leaa yarn becomes very high ·. * "

BarUbeEfcinfeus. is © s aueh m & glieh «- with elsei? Further different types of covering) = Dehnungs ^ & rarre according to a further embodiment dea? Share out invention. ".-" ■■

Seigt a @ a high ÄHfauaga-Yetang-Modm! . * md © inest «Gil larger fflaximal ^ n Heigimgsgmd aa®h öer ^; © rstea St2? E © k «greas © als feti Beiastimga-BeliamH ^^ ittrrosi τοη fiMi'Cli. © ä" ■ 'Poljestes? Fäd © a <, Ia © inea estr ^ siesi-FaIX diesel ?; Belas-tusigs ^ D ^ hmaiigSrEKrTö eats äes ¹ ffiasiaa.1 © ßraä first StresIsgTOnze on the
between that-. Urspanang and i © .r first SteöekgÄas © ^ vii © from Pig β 2. © 3? Si @ ht! Ieh · .Sin
? erl.alt © a teitf never.
In äes ¹ Figo 2 the Xurven fm ")

won erf ± & äwagsg üliehsn j

fäi@2i.ait © iaer derartigiia can w®rden obtained, for example _p if heat treatments la stages (5) mad | kept 4) _s indsia dis threads Aatex "© ISIES ¹ Spanraag so öa £ the Paögnlänge in | @The treatment

des Westes immediately Tor de ^ ¹ treatment of the Spaniards in such a way, .be ■ threads near the final stage of the. According to Stuf® (4), store a length corresponding to 120 to 150 $ of the value immediately before the heat treatment of the Stuf® (3).

In particular, polyester threads with this type of load-elongation curve can be used according to the following

909840/1588

described embodiment produced

After that, polyester threads of this kind are used after the 7th «

2jur.

drive along routes and heat treatment of KleJätge ··

stretched polyester threads containing at least 90% ethylene terephthalate contents, with the the following stages are carried out in the specified order «

Be stretched (1) stretching the first stage, the sichtgeatreokten filament by 1.1 to 4.0 times in a liquid-Hloht LSsungsmittel from a temperature in Bereioh of 60 to 100 ⁰ C}

(2) Stretching the "wide stage, wherein these stretched filaments in a liquid Mioht solvent at a temperature in the range of 40 to 75SJ". but lower than the applied in stage (1) temperature, times 7.0 by at least 1O ⁰ C in a stretch ratio of 1.2 to DAC at least 80ji the maximum Streckrerhältnisaes is, are stretched;

(3) first Värmebehandlungv wherein the stretched on this · catfish threads al, "are treated at a temperature in the range 65-120 ⁰ C, which is higher in the stuf * (2) temperature applied, while they are subject to such a voltage , since £ the thread length during the heat treatment is kept at 100 to 130 ° C of the value immediately before this treatment} and

(A) »extensive heat treatment, the threads being heat-treated at least once at temperatures that are always higher than those in stage (3), and in at least one stage the heat treatment is carried out at a temperature aioht undercalf τοη 120T, whereby the threads in each stage bucket

909640 / Ulf

- 1ß -

are subject to such a tension that äl © 100 to 1305ε of the value of the immediate level is maintained, and where furthermore, the tensions exerted in one-stage or multiple stages (4) are set in this way Fade length after the final stage of stage (4-) <s ± n®n ; value of 120 to 150 £ of that rferte @ 'usimitt © lb @ E ^> tos · of stage (3).

The threads with the kw% load-elongation curve described above show how high strength and high continue to have characteristic properties, as well as dimension © »tabili tat, serrung due to an elongation below latlv low. Because of this type of thread, it is valuable as a material for constant use gisferdeg't v © rd "© n ^: o--""'

The reason why polyester filaments, which in the rest of the world have a large number of excellent similar properties at the same time, can be obtained by the present processes _f is mutlion of the following *

When the polyethylene terephthalate polymers structure due to the excellent combinatlon of the Streokr and heat treatment steps granted to the invention the molecular orientation is determined by this scattering process greatly increased, causing the formation of a cross ^ Cutting anisotropy is largely prevented, and ullen the control unit is regulated in a suitable manner, where the Quersohnittsaniiotropi · varäieden * With the

'and ordinary Sjtreskverfahren, attempts to achieve © ines hohsn "Ausmaßes'der- orientation invariably always @ in® Strukturuneinheitliohkeit towards the cross section ₀ If, however ein® unit" borrowed © structure de © cross sections © is desired, high draw ratio can not se be achieved, "why was © s rs®hnitt in ä®z practice impossible ^ Polyestsrfäden with © inheitliehOE Qu © manufacture ,, DI® are highly oriented country, © ine .höh © strength besaitsen" D. "h ₉ gewöhnliehen method fail b © i sol © h®a threads, .. di @ are uniformly in Hächtmig fi © s Hadias and are highly oriented, d, _e h _e threads with a liohsn? ®shalteiii © οθι? Ee @ tig & © it / Dehnung ₉ - SMhig «Iteit and E ^ fatigue resistant & eito The error is presumably caused by, dis" Tarsckiafienea 7®Ttoswang & n or Yerserruagen τ @ ^ »- p dl © ΐϊβΙϋ Streeksn in don iEmer © a and ämsseren. Ä®s threads appear,> unfi_ ii® usual procedures in this correct no © Yerfeeisspung bringQn, through. ds @ Torli © gend (S method niwä Mng © g © a © i? folgr @ ioh this ffichtlichlosit in complete peace, st @ ll © nd®m the extent of the new combination eyelet struck = w && hsiailiingsstufen - eliminated ».

Si © according to the invention
with. excellent property® »uad siafl not xmr-for industrial uses ₉ for example w © is © as B@ifen.oord»: but auoh. to clothing zv / eeken. usable »At the ^; For the latter use, the threads can be used as they are or staple fibers can be used according to silk silk.

The invention will be explained in detail below of working examples which are for illustration only and not limit the invention.

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example 1

Non-straight polyethylene terephthalate fibers with an Elgen viscosity of 0 * 81, a size of about 6100 d / 250 threads and a birefringence of 0.0015% in normal white were melted about 2.0 times in a 100 ca long warm aqueous bath from 85 ° C and further to 3 ° C in a further 120 µm long warm aqueous bath of 65 ° C. The threads were then strengthened in a 120 cm long warm water bath at 85 ° C while stretching to 1 "05-fach® wärmefee * is what the" extensive heat treatment "followed, in which the threads were ^{wrapped in two windings on a hot whale""v®& 12G 5} C and 150 -bb 'diameter in two windings , .. & ma were stretched IO56 and then ®iaer further HeiSwale © -.? was developed by 180 ⁰ C and 150 mm diameter routes spell were the "äd @ n included in a" speed of 100 m / min * Di © had an SrSSe of 860 denier and of 12.5 g / d, an elongation at break voia module of 2000 kg / mm ^2. The toughness was ₀ 94 gA "same Sara was * u a Beifencord @ v n 860, grant a right llnter ^ zwimung of 56 ₉ 5 per 10 m and a anschließend® OheriBwirnung strands and a left side Zwlrmmg of gen 10 per cm made · If the measured © accordingly in that from 1000 d / 2 overft - became ₉ 'it was 20.2 kg. The strength conversion ratio up to the production of the yarn sum Cord was calculated from ratios and was ΘΙ96

9098A0 / 158Ö

- ■ 21 -

ComparativeTersuoh

Loosely stretched PolyäthyXenterephthalatfäcien with a low viscosity of 0.81, a size τοη about d / 250 threads and a birefringence of 0.0015 _f, which had been spun in the usual way "melt", were treoked and heat-treated under the following conditions. The results are summarized in Table I. In these experiments, the following standard conditions were used in all cases, unless otherwise stated in the table. First stage stretching

100 ca long aqueous bath with a stretching ratio of «2.0-faoa Stretches of the »wide level» 120 cm long aqueous bath τοη Stretch ratio »3.0-faoh (maximum stretching ratio «3.4)

First heat treatment

120 ca long watery bath pink $ Ό

Stretching over 5jt Second heat treatment!

(1) temperature 120 ^ C

Hot whale 150 aa in diameter Routes around 10Jt

(2) temperature 180 ^;

Hot whale 150 mm in diameter Stretches around tOji recording speedi about 100 a / min.

909840/1581

Τ · »· '' Conditions of establishment. -

* r.;, ^: ■. ■■. ■ '■.' ■■ - ¹ -; ■ ..: ■ ·. , ..

fab !! I.

Streokbarkelt (ΪΙΧΚ ^Χ ) properties

Break- Deh- Young-
consolidation of the module
speed _v (si) (kg / aa ² ) (g / d
(g / ä)

Tough cord

footiness (transferred to the value for

1000 d / 2) (kg)

Firming

keitu »-

Wall-

lung

▼ he

never lasts

Stretch the first Stage

Temperature 30%, lower than 40 ° C

Occasional Bruoh des Sinfadene during the stretching of the first and «long stage. Stretching not feasible.

First stage stretching ' : '. '\ Tea temperature' 110 * 0, higher ale

Terdiokungen were during the stretch " the «wide level formed .. stretch difficult to perform

INJ (S3

Stretch the first

«1.0

lower than 1.1 {M des Streekene dexr "wide step"

(6.7)

12th

1250

0.53

9098Λ0 / 1δ $ 8

Table I (continued)

First stage stretching DR * 4.5, higher than 4.0 (IiE dee stretching of the second stage - 1.2)

Compression @ n tiurden formed during the second stage scattering

Second stage routes:

Temperature * 5 ⁰ C, lower than 10 ⁰ C

Verdiokungen were made while stretching the second stage formed

Second stage routes:

Temperature «90 ^ C, higher than 85 ⁰ C and the, temperature when stretching the first stage

(7.6)

7.0 16

1100

0.56 -

Stretch the first

Stages

Temperature (T ^) χ DH

- 75 »C χ 2.0

Stretch the second

Stages

Temperature (T ₂ ) ζ

· ■ 80 * 2 x 2.6, Τ «higher than T ₄

(6.0)

3.8 13

1300

0.57 -

Ö0984Ö / 1S8Ö

is

O ₁

• π

4 * 1 03

ft!

it*

in

eaca!

ο dreary

φ V

4th s

«Ι

, s «ι m © λ ©

»Sr»,

JtA

■ #

¹ ^ W

of

»4»

S4 a ea

4 »

"O

«■ *

ι OrN

03

¹ ^ p

«Β

4 »

lea ω

ORIGINAL

table I (continued)

U second

BQK

(1) i routes in the

Stage (1) in the

lower than the Seapera "
door feel the «ret« »W & me- ■ wide warning b # - ₉ .0 ti 1350 0.49> - £ iaiet «£ lge« wide towers flllirl »ar 9.2 12th 1280 15th Se "per * ter" 1 © 0 * C
lower than 11OC r 'r. 0.53 - Sweite ¥ ür & §l) «annex (1) s (δ.3) 9.0. 1300 16 οΟ £ Ι2> ^ 3ΰΒΰΐΦ & USA ι mf a Level Ci)
at sweitexi strength? al @ J »! i 17th JSwelte WftTg # teft1iflwCy wing, (1) s ■ '■■ ■. (€ »i) '. ■■' ■ ^; stMsiBKr sie 3Öji Stretching the step (£)
let 4's, ssweiteÄ ' _: "\ ■ 13th Sweite WSrjRt ^ eliÄiadluisg (2) ι 19th ! wide WSlciß «» * haMlw, TEtg (2) s

FafiBotems' s ^^

909840/1588

18076-5 /

Aue the .. 'Vert «a of the previous table; results in ee:.; ; > sioh "that" falls any de? 8tre © 3e- imd Wärmebelrnnd ™ Λί lungs under a rule outside of this invention. rsiöhe "lying conditions'-dusohgefO & rt is" entweä ©? ' the stretching can be done - let »ofier-, fells one; / StreeJEK_- availability given let »eesaatatreolörerMltiäls. TBl'low let · Ia some cases scan da »@esa» tatreolnrliältnis fBH Be on the inventive KXSezi BereloM. / jedooh ^ / be » ait sea then the products eehleeiit® llgeiäsehaften and do not result in any satisfying cord «?

Example 2 - _:. '-._-, ■} "; ^:

Liehtgeetreekte Folyäthylentdreplitlmlatfää®n with "iner BigenTlskoeltät of 0" 92 _f a size τοη about 7200 d / 250 1Men and an Itoppelbreeh ^ Bg 7on O ₉ OOSe ₉ di "was in the usual way aeheelsgeeponnen © a ₉ . ward @ nw to 2.0-

in a 100 en long warm aqueous. l & d -won 90 ⁰ C ..; furthermore about 3 _tons of «oh® in © iaem 120 sa laagen wamea wäligen sed tor 70 ⁰ C geatreekt. Senn were iie threads three consecutive ¥ 8raebenaiiSlung®ii subjected to Veiee in ä @ r ^ n ^ and successful aneehlieasenä in a Ge "aonwindlgkeit won 100 a / sain, aufgewiekelts The filaments were in a 120 long warm eft wSSrlgen Saä 90 * 0 under Streekung 10 $ w & raeben & ndelt, then ®isi © HEIS walie of 150 * 5 and 150 whether Baresaeeser mu an Wärsebehandlung under a tension of 10 $ Streekung gewiokelt and sehlieBlieli a leiSwalse of 200 ⁰ C and 150 BB Burenmeeser under Streokung us 10 ^ waved. Approximately 3 am obtained in this way had a & röSe toü 1000 denier and a brewing strength of 15 »5 g / d« an elongation of and a Tcung-Ifoäel ir @ n 1900 kg / aa , Bie ber @ ohnete

909840/16 88

Thickness was 1 »03 .g / ά * This« yarn tone 1000 denier was twisted with 53 windings J® 10 om in a right-hand twist and white strands received »int ObeE'swirnuög sueaamess * where you can see a» twist on the left alt 53 Howkliängen j® 10 om connected and a maturity aoord of 1000 ä / £ was obtained "The cord strength was 21 _v 3 kg and the" B®lmnng 18 ^ "Aue eieeen values became- the f®: 8tigkeiteiäM"& iiiliUQgeT®rhaltiiie the transfer & 9 & Garnes la äen OeM reoknet, sincee amounted to 80 ^. "'.-.""■■ .-.

'from' ■ Kiohtgeetreect Fäöeii / Polyätnyleiiterephthalat »it

an EigenTiekosess γοη 0.92, dimer size r @ n about

6100 δ / 120 threads land a Boppolteechyiig τοη 0 _? 0020 _t which in the usual way eehmslsgdaponnen w ^ rdsin WbTSn ₉ y billion us, the 3iO-faehe in a 100 mm warm water bath ψοη 35 ⁸ C ₉ uod w © itsxfeir & um de.el§O «f & @ k® @ in®a 120 oi long, warm watery watery b > * 1 T © a 73 ⁶ C g @ etr®ekt * The threads were spellbound in a 120 sm lasagea% rasm © M wlSrigsn bath of 90 ⁰ C under a Spammng ^ ön 1C ^ Sti? Eekuag wtes®treated _β As wide Wänaebea® ^ € liiiig, di © fM © a amf © ine HeiöwalBc from ^{150 0} C and 150 mm bio-fiber under a tension of 8 $ Streetang A further K ^ ißwals © from 195 ⁸ C tmä 150 aa Iteahaieeeer under a tension of 1OjS stretching-.wound · Barauf the threads in a "sesohvindigkeit of 200 a / ain, peeled off» Bas ®rfealt © s .® uArm had a breaking strength of 12 ρ 8 g / d, a © BrueMeiaamiag of 16 $ _ρ a lounge nodnl of 1850 kg / aa and ® a yeastness of 1 _? 02

..- 28 »ν ■■■■ ;: .--. ■■ ■ '. ■■■' ■ ■ -.-. -

19076Ö5

Hichtgeetreokte threads made of belyethylene terephthalate with a? Intrinsic viscosity of 0.8O ₉ a size of about 6100 de / 250 2 threads and a? Birefringence of Q, 0015, which had been eehmelzgespönnen in the usual way _f were su one? 15 em long sample fitted. That was us the 2.0-fold at a speed tois, 10 ^ / ain ", in an aqueous bath of 55 * G - using a? St? Eokvo ?? ioh.tung voia Hshastntyp and furtherMia 3 _r 2 ^a > faeke in a? HesenwiMigkeit of 50 ^ / sIjj., Aqueous bath of 4-5 ^ stretched. The sample was then in water of 170% while maintaining the? Konetantea ^: Fsdeis "length 'heat" treated "lt _t on it in" a S-lliepaGitoA τοη 120 ⁰ C under tension of 20 ^ stretch xmi sohli "Sli © ii la a Silioonölbaä of 180 ⁸ C under a tension ψ & η StreekuMg treated. B & a obtained Ctara had a strength of 12 _f ö g / d *. Time Bruohdehnuiiig of 1SfI _f © inen

of 2000 kg / wsr and one - Zlhigkftit. ' Tom _$ 1 08 g / d.

Liohtgestrekte P @ lyäthylente? «phthal & tfldeii old

a league & viekoeität ron 0 ₉ 8O _f one? Stark® v © n about 6100 d / 250 threads and one? Birefringence of O ₉ OOiP _9, which had been melt-spun in the usual way, was about 2.0-fold in a 100 em long warm aqueous bath of 70 ° C and furthermore about 3 ₉ 2 ** t && h & in one 120 am long warm aqueous bath of 45 ⁰ C in a? Streokgtsßhzahl of 40 am / min, treetop. The threads sucked in were pulled off after removal from the water bath. The sample was then in a 120 en long

909 84 0 / TSS8

from 80 ⁸ C heat treated with constant junction length gsfe «-! ton ward * _e 2wr» wide heat «- the /! rob®, in a» 100 © »! engin silicon-

120% treated under aimer savings of 25 $ stretching »ad weiterfein iß ®in®ai 100 em longs Siliooaölb & i tob 185 * 0 under a spansuHg tös 6jl itrekung accepted. The silicone oil 'vttrd · τοη removes the preserved sam, which amieheBend in a sea depth of 40 m / w ± n * mutgtnommsn tmrd »*! Fts @ & rn hattt ®iae 0rö £ * ▼ on 760 IDsnter,« ine strength tob 11 , 8 g / d, a Bruehdehsaimg toe 20 ^ unß «iß®a Yöiing-MoäKl τ © η, 1900 kg / nr © ie bereenntt * SMhigkeit des Ee © diskt © 9 bastrv ^ 1.18 ^ g / d. 1 «? Srgl» iefeeawe © k * n becomes · »di« · gleieaea: ^ ijubtg «·« stretched ' WSÄ9M \ m da «4 ₁ 3 ™ t fe @ ß® Sur @ h Wieklisiig% uf« inen E ^ isdorn rcia 90% and 60- w® Jkm®hm®t $ z®%? _O «titifMa μ das t _f 3 ~ £ a®he on a 50®» Isagss H «i ^ flat © ¥ © a 190 ^ ge« etreokt and. on a 5® ®m ifSBg® »]? l £ tt $ fön 210 ⁸ C

egg"

aal ten imrdesi * Bafj Sars, srard «aneehlyingl im« iziesr G * - fortitude of 60 V ^ ^ ο «ufg @ £ oafieii _e - Mm _ © ^ malt®a · 0arn had a GfrÜBe tone TIOO P * © i« ^ ₉ a lämefcf ·· * ■ igkeit '▼ on 9 i.5 g / d »a® BrucM ^ lunaag Ten 13 _S 8 ^ · -issiäl« Inen Yoiang-HöduX Ton 1259 leg / who · Me bereo ^ aete SSIiigktit des Oarncs was O _t 65 g / d.

Here you see? <$ ad the erfindmmgsg®a £ S <f product sarkftnt secures strengths aside file duct The first one also has one

? oly% thyleßfer "$ hthal &tfläen" with a voa 0 _t 1 & ₉ a β "81β Töa about € 100 i / 250? aden and a 3> oppelbre <3huiig of 0.0016, which is ttttreher

909840/1508

-30-- 1

Weis "sehmelswereponnen
length © of 10 cm cut @ m, t
2 ₉ 0-faohe in one

contraption

in © ines wäfeig®n bath from 3G ⁸ C in a G @ Böhwi'ndigk; @lt 1QQ $ / mi, n _e stretched · This® sample maä <® 4am during 5 utes in a silicone oil bath of 8Ü®C below :? ' © iner of $ 6 elongation
Heat treatment for 10 minutes in a silicone oil bath - stretching under a tension of $ 22.00 _o That

Yarn had an elongation at break of 12.5 g / _{e 9} of 17 $ and a Young »Moiiil yum 2050 Ig / m. The calculated toughness of the product was -1.06" g / d

Example 1 / * '.:,' ■■ _. .

lieatgeetreokt «Polyätlivldnterephthalätf äda.n _:. with '";■"■'; - '- ■'"._ a signature viscosity of 0.80, @ ia @ r strength © of about, 6100 d / 250 F18« n unö a Döppelteeehung r @ n ; 0ϊ, was 0015, '· ά ± @ "' echmelsg®spennen in the usual way _uaren: were around 2 _s Ö £ aeh © in a 100 cm long warm aqueous bath of 93 * C and continue Fähe 0 to the 3 ' in ®ineia 120 em long warm wäSrigen bath of 65 "C in bucket Streokgeschwindigkeit of 100 m / mln * stretched. Di · wicks were removed from the water bath and then in a 120 om lengths warm aqueous bath of 93 ⁰ C under stretching by 10 Thereupon the threads were wound on a hot whale of .15CW and 150 in diameter in two windings but heat treatment under a tension that resulted in an elongation of 10 pounds, and then on a Hessian whale of 220% and 150 in Durohnesser sur Heat treatment under one

9098Λ 0 / 1S88

Tension giving $ 10 elongation, wrapped. The yarn obtained was then clay dtr roller in a speed τοη 1Q0 m / min, deducted. Bas yarn had a value of 860 denier, a breaking strength of 11.8 g / dj an elongation at break of $ 18 and a Young » Module τοη 1800 kg / rough. Her calculated toughness was 1.00 g / d.

Beispi®I 8

Highly stretched threads made of polyethylene terephthalate with an Eigenviekoeitat τοη 0.80, a thickness τοη about 6100 d / 250 threads and a birefringence τοη 0.0015? The usual whiteness was smelsversponnsn 2.0 times in a 100 cm long warm aqueous bath τοη 80 ⁰ C and further to the 3 ₉ 0 times in a 120 am long warm aqueous bath τοη 40 ⁰ C in a Streekgeacmd-Sidigkeit of 40 ra / miii »streekt- · The threads were then frs.it and wound up ygm water. The stretched threads in this manner were placed in a 100 cm long silicone oil τοη 80 ⁰ C under 5 $ stretching irärmebehand®lt _t then in a 100 cm long Silisonölbad τοη 120 ⁰ C under a tension, the $ 12> Streokung Terursachte _a and schliesslioh in a 100 on long silicone oil bath Tpa 185 ⁰ C under a tension that resulted in a stretching of the threads. The yarn obtained was freed from silicone oil and _{wound up at a speed of 40 m / min e} , the yarn obtained had ®in® breaking strength of 12.8 g / fl, an elongation at break τοη 14 ^ _{9 and} a Toiang initial modulus τοη 1950 kg / mm »The maximum value of the differential coefficient of strength and elongation near the first strength limit was 23ΟΟ kg / mm. The thermisch® shrinkage of the yarn at 20Q ⁰ C was 14.0 $, so daS.es "ine shows high dimensional stability.

909840/15 88

-32— ■■ · ■: ■

19076U5

To ..Yergleioheeweoktn were identical «stretched fä & en around the 4 # 3-fold® by means of a» ®a H®is4®J »aes τοη 90 ⁰ C and 60 ms diameter gö a tr * ec tj daim furthermore in dta maximum stretch ratio tob 11 ₉ 3-faohea on '. a 30 en long hot plate τοη 190 ⁰ C on strike, among other things * finally on a 50 cm long Heisplatt® of 210 ⁶ C, with the constant thread length being wmM® "would be @". The yarn obtained was at a speed of 60 a / min, wound up Ba yarn had a gross strength τοη 9 * 5 g / a and © int BrueMtnung _e The Toung * Änfangesi6stil was 1250 kg / aa “ Bi®

Thermal view at 20O ⁰ O was 2S ₉

! fiohtgeetrtokts Polyäthyleatr «plathal & tfä4®ia with a Sigenriskoeität τοη Ö _g ? 8 _s a strong v © sa g.twi. 6t00 d / 250 filaments, and a B6pp "LBRE * chuag τοη Q _{9 #} 0020 the wares in the usual catfish achaslsTtreponntn _r ^ ms ämn sur a Probtnlähgt to τοη to geeehnitten, Bie sample was around 2.0 Fähe in a bath wmSrigen τοη 7Ö * € at a speed τοη 25 ^ mia _e using a stretching device voa Eahm @ ntjp and furthermore, among other things, the 5f4- £ a @ he in an aqueous bath τοη 30 ⁶ C at a speed τοη 100 ^ / ain. Stretched · BIeae Prob® was then allowed to stretch in Sllloon oil τοη 80 ⁹ C-under tension "dl® 6 # lg", for 5 minutes and then in a silicone ¹ ! τοη 125 * 0 under a tension allowed 20ii stretching »for 5 minutes uM borrowed in Sili @ onul τοη 18O ⁰ C under a tension" Si © stretching resulted in 10 minutes would have been> The yarn obtained had a breaking strength of τοη 12 ₉ B § / d,

909840 / 1S8 @

a deft of 15 $ uM «a loungWuifÄiigaBOdul of 2000 kg / ma?» Ber a & xiß & le Blfferentialkoeffisient the firmness aur DtfeBung ssea the "ret" ja Streekgrense was 2400 'kg / aa · The theraieehe SoluraBpfuiig de * Samea la Siliooßöl of 20Q ^ S was 15 _s 8fl.

Siohtgestreokt · FolyätlijleaterephthAlatfldeii ait a ¹ SigeaTlsioaitat v © n 0.81 "a SröS® tob about 6100 d / 250 load and ..-- a- B @ ppelfer® © lwing τθβ. O ₉ OOI5 »who were in ilbllohsr Weis® sehiseXsTereposmen, wtsrden aai d & e 2 ₉ ®-faofo« in »ine» 100: © a. lemgea «araen väSrigea lad toh 85 ⁸ C ws & w« it®rMii .'- over dae. 5 "0-f * e! Ie in a 120 ob Xfmgen wmeis
. ^ uan were the

in follow®Ma ^ ¥ ®ls® imterworf «si you were treated in a 120 or a long w & gw * n watery bed hair dryer under a tension from 'iff Itreekung ₉ then as» wide tfäraebehandXung eat egg ^ ess 80 ® «lft®g® ü iilioonüXbad of 120% under a tension τοη 5 $ Streökusf and eehlleä <borrowed in »ine» 80 es long SIliooniilöad τ @ η 200 ⁸ C under a tension, so ds © dl®; fade length kosetaat was applied, wlrsetoeoelten. Bieden were then at a sea speed ¥ on 100 a / aln, auflekelt · The received · Sarn had a value of 1 @ 00 Denier uad: '- had a brewing strength of S ₉ A S./^* a Beto ^ Kf- ... τοίι 22 '^ ₉ a Toung module τβη 1600 kg / ss and «Ina läalgkelt v © n 1.03 i / d. With «ZugfestigkeltsYereuek, tor aiaiBal® 9ra4 was the weight at de? ! • lastunga-Behnungf-Iiar ^ ® ia .des feil near the "wide Streokgrense 4" 5 g / do Bleeee Sarn old 1000 Senler was in 53 Wloklungesi 10 each as reoht-

909840/1588

19Ö76O5

underside on the side geswig-at _y miä 'ämm ' wörd © ä strands of this »itelms & i ©! ¹ ¥ © rawii®t, «or $ uf © is® liiikm- sided twisting with 53 -Weklungdn j® 10 e® of a tire @ o? Al8 wb 1000 d / 2 e? Follows $ _e . The • in® Brueiif @ 8tigk®it τοη 18 kg tnid «ine Daten®! tos, Bas festigkeiteuKwandluagaverh d @ s Cordes from the G & ro fraud

Line-stretched polyethylene terephthalate threads
an EigenTiskoeität of 0.81 _y elnam ¥ ®rt τοη @twa
6100 d / 250 filaments, and a Doppelbreshuiig ¥ on 0.0015., Dl © iii conventional manner echmelsTersponnen were, were subsequently && conditions laid n © g stretched and wäraebehandelt. Fmlls In the following fatell® II
nothing else is indicated®% @ ni @ t ₉ mzsä® at & Bmtli © h®n ¥ er °. suohen Si® listed below © a
applied

First stage stretching

100 whether long watery baths Streekrrehaltnls * 2.0-faeh Stretching the wide stage

120 ö "long watery bath from Streekrerhäitnls" 3.0-faoh First heat treatment

120 ca long aqueous bath of stretching us $ 3
Second heat treatment %

(1) 80 whether long silicone oil bath of Stretching around i5ji

(2) 30 oh long silicone oil bath τοη 200 ⁸ C maintaining a constant thread length.

The results are summarized in Table II susasaesa.

909840/15 88

Table II

Ownership

Yer- Production conditions Streokver- Bruoh- Deh »Tough * - Srafl Cordfestig- Festig-

suohs- hold firmness to ability new »Ir. (TDR) speed (#) (g / d) end. (ttberftOirt on 'wandluinge-

(g / d) share the value of inherited

the 1000 da / 2) nis

S-S »(kg) (5t)

■ '■, cart

Stretch the first

Step:

DH * 1 ₉ 0 (5.4) 8.8 15 «10 t4.2 81

lower than 1.1

(DE while strengthening the

iwide level * 5 «Ö) ,, ■

Stretching the second "

Step"

Temperature «90 ^, (6.5) 7.0 16 - 12 - - ^ j

higher than 85 ¹ C and the _s

Temperature in the

first S treokatuf « ■ , ' , ..', ,,, ■ '" ..., ·. ^ ₁₁ / _;

Streoken the first

Stuf® »

Tea temperature (T ₁ ) χ DE.

»75« C χ 2.0

Strengths of the second (5.4) 8 _f 9 16 - 15 14.0 79

Stage

Temperature (T ₂ ) χ DH

«80« C χ 2.6

R ₅ higher than T ₁ . · · - ^

' ^: · ' ^! -i—— ■■ ■■ i O

9 0 9 8 4 0/1588 p

Table II (continued) Single stage second Heat treatment: temperature

₁ ) * DR

* 80 «C χ 1.03,

T ₁ lower than that

First heat treatment temperature

Thickenings were formed

Second heat treatment (1) s Shrinkage by 10% more than 5%

(5.6)

8.6

18th

13.8

80

Second heat treatment (1): A stretching of the stretches by 40 pounds »stage (1) in the more than 30 pound second heat treatment was not .... ' . feasible

Second heat treatment ^) "Am routes on routes by 40 £, the step (2) in more than 30> the second heat treatment was not dureh-. . . manageable

909840/1588

Example Tf

Highly stretched threads made of polyethylene terephthalate with a low viscosity of 0.80, a value of about 6100 d / 250 threads and a birefringence of 0.0015, which had been melted in the usual way, were made to be 2.0-threading in a 100 cm long warm aqueous bath of 70T and further to da * 2.95 times in a 120 µm long warm aqueous bath of 4-5 ⁰ C at a speed of 40 m / min, stretched. The threads were then removed from the water bath and wound up. The stretched in this manner the sample was heat treated in a 100 cm long Silioonölbad of 80 ⁰ C, the FadenXLänge was kept constant, then in a whether long Silioonölbad of 130% wherein a shrinkage was us 2 $ allowed, and finally in 120 a 100 omlangen silicone oil bath of 190 ⁰ C under a tension of 3 $ stretching heat treated · Sann the sample was free of silicone oil, and wound at a rate of 20 m / min ·.

The yarn obtained was 1050 denier, a strength of 8.4 g / d and an elongation at break of 26jt. The minimum slope of the curve above the point of 7.0 g / d on the stress-strain curve, which when pulling » test obtained was 4.6 g / d and the calculated Tenacity 1.09 g / d.

The yarn then received an underwire on the right-hand side to an extent of 51 turns per 10 om and swel strands were sueammen verswlrai, resulting in a left-sided Twisting with 51 turns j · 10 es fUisohlod · thereby a tire board of 1050d / 2 was produced, the »ine Cord strength of 15.9 kg and a tensile strength of 28 ^

9098A0 / 1588

19076Q5

pointed. From these values the fixed-time conversion ratio became in the manufacture of the cord from the yarn calculated au 90? δ.

Example 12

Highly stretched polyethylene terephthalate filaments with an inherent viscosity of 0.78, a value of about 6100 d / 250 filaments and a birefringence of, QO16, which had been melt-spun in the usual way, were cut to a sample length of 15 cm. The samples were 2.0 times in an aqueous bath of 68 ⁰ C at a rate of 1Q # / min. using a frame type stretching device and further 3.2 times in an aqueous bath of 40 ^° C. at a rate of 5> 0 ^ / min. The sample was then stretched · in silicone oil of 80 ⁰ C for 10 minutes, then in silicone oil of 120 ⁰ C for 10 minutes and closing lent; Heat treated in silicone oil of 185 <€ for 10 minutes. During these heat treatments, the sample was kept under tension so that the pad length was kept constant. The sample taken in air was sucked in carbon tetrachloride at room temperature to remove the silicone oil and dried. The yarn obtained had a tenacity of 8.1 g / d, determined by the method described above, and an elongation at break of 32 ^ · On the load-elongation curve, the minimum degree of inclination above the point of 7.0 g / d is only 4.1 g / d · M «calculated toughness is 1.29 g / d. The yarn natta has an inherent viscosity of 0.77 after the above-mentioned stretching and heat treatments.

909840/1588

Example 15

Non-stretched polyethylene terephthalate threads with an intrinsic viscosity of 0.78, a value of about 6100 d / 250 threads and a birefringence of 0.0016, which had been spun in the customary manner in clay, were cut to a sample length of 15 cm. The sample was 2.0 times in an aqueous bath of 68 ⁰ C at a rate of 10 # / min. stretched using a frame type stretcher and further stretched 3.2 times in an aqueous bath of 40T at a rate of 50 # / min. stretched. The sample was heat treated for 10 minutes in silicone oil of 80 ⁰ C !, for another 10 minutes in silicone oil of 120 ⁰ O and schließlich.während further 10 minutes in silicone oil of 185 ⁰ C. During the heat treatments, the sample was kept at a constant thread length. The sample was taken in air and then immersed in carbon tetrachloride at room temperature to remove the silicone oil and dried. The yarn obtained had a tenacity of 8.1 g / d, determined by the test method described above, and a gross elongation of 3296 · On the load-elongation curve, the minimum degree of inclination after the second yield point was 4.1 g / d. The yarn had a tenacity of 1.29 g / d.

Example 14

Non-stretched polyethylene terephthalate threads with an inherent viscosity of 0.80, a value of about 6100 d / 250 threads and a birefringence value of

en 0.0015, which was melt-spun in the usual way /,

909840/1588

were 2.0 times in a 100 cm long warm aqueous bath τοη 70 ⁰ C and further by 2.95 times in a 120 cm long warm aqueous bath τοη 45 * C at a Streekgesehvindigkeit τοη 40 m / min _# stretched · The stretched threads thus obtained were freed and wound up by Tom Waseer.

The sample was then heat-treated in a 100 cm long silicone oil bath τοη 80 ⁴ C while maintaining the constant thread length, further in a 120 mm long silicone bath τοη 130 ⁰ C with a shrinkage τοη 2 £ and finally in a 100 em long silicone oil bath τοη 190 ⁰ C under a tension τοη 3 $> stretching heat-treated · The yarn obtained was freed from Tom SilioonOl and at a speed τοη 20 m / ain. The yarn had a value of τοη 1050 denier, a greasiness τοη 8.4 g / d and an elongation at break τοη 26 $ ί On the load-tendon curve obtained in the tensile test with the yarn, the minimum gradient after the second yield point was 4 .6 g / d · The calculated tenacity of the yarn was 1.09 g / d · ■ '■

For Yerglelchszweeken a sample of the same threads stretched in the same way was placed in a 120 cm long silicone oil bath of 13W, allowing "shrinkage τοη 2f> , and furthermore in a 100 cm long silicone oil bath τοη 185 * 0 under a tension equal to 3ji Elongation revealed heat treated. The yarn was freed from silicone oil and wound up at a speed of τοη 20 η / min., Showed a value τοη 1050 denier, a tenacity τοη 8.2 g / d and a tension τοη 17 pounds. The calculated toughness of the equivalent product was 0.69 g / d. The stress-tendon curve obtained on the bela tensile test with the yarn was the minimum inclination * »

909340 / 1S88

degree iu ^ h of the wide Streokgrens «12 g / d.

Example 15

Lightly stretched polythene-inter "phthalate" dea "with an inherent viscosity of 0.80, a ¥" rt τοη about 6100 4/250 threads and a birefringence of 0.0016 ", which had been spun in the usual way soh" el ", were reduced by 2 _f 0 * faohe in warn water τόη 68 ¹ C at a speed of τοη 10 pounds / «in. and furthermore by 3.1 times in warm water of 40 ° C in an ooohwindifkeit τοη 50 ^ / Win · genreect. The threads treading on the “W” i ·· • had “in sptsifisohe“ Sewichtf • tiaat at 20 ^ C, toh 1.364 ”a double broadening τοη 0.185, a Ftetigbtit τοη 7 _f 4 f / d and a Bruehdehniing Ton 55ji. Diets? Threads were heat-treated in a “silicone oil bath τοη 80 * C for 10 minutes, in a“ further silicone oil bath clay 120 * C for IQ minutes and in a further silicone oil bath τοη 185 * C for a further 10 minutes. During this heat treatment, the threads of a voltage were subjected so that the Fadenllngβ constant fehalten was · "Di · * bsohlieiend abgeiogenen in air threads were τοη the Sllloonölaufnahme" it Tetraohlorkohlenstoff freigew & eohen, The product has "in" Bruehfestlf "ness tob B _t O g / ά and an elongation τοη 39? C *

2u? «? The same * w« ek * n were tightened in the same way «y * den in a» silicon bulge * d τοη 185 "CwIhWHSd 10 minutes treated, with the thread! Änf constant f - was kept, exhaled in the air and the Siliooa »! «It Carbon tetrachloride tntf «rat. Pie the thread had a breaking strength τοη 7.2 g / d and "in" elongation τοη

909840/1588

The calculated lanities of the two products standing at the door were 1.56 g / d fttr the loaded weight «« Bftfien fadtn and 1.32 g / d for the Tergleiohsfaden · Der int · »seigt aoait · 1η · welt grBlers tenacity.

Example 16

Liohtgestreokte Polyithyleneterephthalatfäden Bit • in «r SigenTiskositftt τοη 0.80,« in «r Stürk · τοη« twm 6100 i / 250 fidtn and a double width τοη0.0015, which were in Ublioher width tehmlimtr "poaan" n wos-dea the 1,4-ffeeh in a 100 ob long watery lad τοη 90 ^ C and wiiterain uot da · 4,3-faohe in a 120 ob laisgan «wnt an irrvious bath of 65% stretched. The fiden were banned in a 100 oa long waraen aqueous bath of 85V while maintaining the constant thread length wtrBatoena & delt and continued with a Heiiwalie τοη 160 ^ C and 150 bb SurohBeaaer in three windings and was treated with an extension τοη 3? Ί. As a result, the bits of a 500 bb long bela plate τοη 230 ^ C were contacted under a voltage that resulted in 3% scattering and at a speed of 120 a / ain. raised.

The tern obtained had a thickness of 1000 denier, a strength of τοη 8.4 g / ^ and an elongation at break τοη 20ji / d. Me calculate te IKaigkeit concerned 0 ₉ 84 g / d.

Baa 9arn Bit 1000 Denier was ait on the right side 53 Wioklungen 10 each whether underswisted and two strands of the same susan with the formation of an upper swirl

909840 / 1SdS

twists, whereupon a left-sided twist with 53 Windings were made every 10 cm. This created a maturity » cord of 1000 d / 2 made · The cord had a strength τοη 15.4 kg and a tension τοη 24 # »where the Strength conversion ratio in the manufacture of the Cordes from the yarn, which was calculated from the goal values, was 92? T

Example 17

A non-stretched single thread made of polyethylene terephthalate τοη 1200 denier elt an ElgenTiskositat of 0.80 and a birefringence τοη 0 * 0035, which had been melted in the usual way, was about 2.0 times in warm water τοη 65 ° C in a © © soh speed τοη 1Q # / min. using a Tom frame type stretching device · Furthermore, the thread was stretched over 3.1 times in warm water τοη 45Έ at a speed τοη 100j </ min. stretched and then treated in waraea water of 65 ¹ C with stretching wa 1.1 times the heat. For the second heat treatment, the thread would continue to be treated in silicone oil τοη 12OT with an elongation of 15 $ and then in silicone oil at 180 ° C. with an extension of 10 a toung module of 1900 kg / mm,

YergleichsTereuch 3

Unstretched polyethylene terephthalate threads with an inherent viscosity of 0.90, a strength of about 5800 d / 250 threads and a birefringence of 0.0020,

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which had been eohmelsgesponnen in the usual way were further gestreokt by 4 "3-fold · by winding around a Heisdorn tone 92 ⁰ C in a conventional manner and around the 1 _# 3-fold to a 50 om long Heisplatte of 19OT" Subsequently, the threads on a 50 µm long hot plate of 210%, leaving a shrinkage of 7%, heat-treated and wound up at a speed of 80 m / min. The yarn obtained had a tenacity of 7.5 g / d and an elongation of 155 *. On the stress-strain curve, the minimum degree of inclination above the point τοη was 7.0 g / d 25 g / d. The calculated toughness was 0.56 g / d. The yarn count was 1100 denier and the inherent strength was 0.88. The same yarn received an underside twist on the right side with 51 turns of 10 cm each, and two strands of this were sewn together to form a top twist, followed by a left side twist with 51 turns of 10 cm each. keep. The £ ord had a strength τοη 14.4 kg and an elongation τοη 17j6. The strength / conversion ratio obtained when the cord was made from the yarn was

909840/1588

Claims (1)

Claims Process sub Streoken and sur heat treatment ▼ on non-stretched polyester threads which contain at least moles of ethylene terephthalate units gekennseiohnet that the following stages are carried out in the specified loan sequence (1) Streoken of the first stage, whereby the nlohtgestreokten Threads na 1.1 to 4 »0-fold at one temperature Ib are stretched from 40 to 100 * C, (2) Streoken of the second level, whereby these are treetoped Threads continue to be used at a temperature in the range of 10 to 85% but lower in stage (1), in a scatter ratio in the range of 1.2 to 7.0 times, the at least 80 * of the maximum Streekrerhaltnissee amounts to be stretched, (3) erete heat treatment, the threads in a Temperature range from 55 to 120% the aumer when it was applied in step (2), can be heat-treated, whereby it is of equal tension are subjected to the fact that the thread length during the Treatment at 95 to 130 * of that value immediately goal of this treatment wtrl, (4) »far * heat treatment * where the fide» once at higher temperatures * «1 · ml * Ib stage (3) has been applied, heat treated ., / "■■ ' ^: .' _: iim aiaieeteiit- tin «level of ¥ är * ebefe ** dlaiag with \ - bucket not below τοη 11O ^- C llegenäem fe * ye ** tijr are we carried out and the threads each * «? Jlimf · ■ ;; Z ■■ -. ^:: a "olohen Mm subject", 4a * 41 "Fmee" ~ would be at % $ »iff 130 * de« ****** *** ttwdtt «lb« r Stage gthÄliea weraea ^ ttBf die * mt * i · 9038A0 / 1588 original Filaments are set in each eo stuf · the step (4) applied voltages, DA8 the filament after the final stage of the step (4) ", however least 90? · Ί the Läng directly gate the step (3) beeitlen, 2. Method according to Anapruoh 1, daduroh .gekennaeiGhi & © t, .- that in step (2) one is cautioned by at least 1 (K, at least 15% lower exposure temperature than in the Stage (1) is applied. 3 Process according to claim 1 or 2, characterized in that the heat treatment temperature used in stage (3) is at least 1CWJ higher than the spreading temperature in stage (2), and that in all stages of stage (4 ) by at least 104! higher heat treatment * tempera doors, Wurd applied as si · in step (3) "B _t are employed. 4 · Procedure according to claims 1 to 3, which are identified «Eiohnet that the strife in stages (1) and (2) in a liquid that is a fieat solvent for which represents Poljesterfiden. 5. Method according to Aaspruoh 1 to 4, daduroh gekennaeiehnet that the threads near the stage "(3) at least once Sm öer stage" (4) feel a temperature that is not lower "X" 12CÄ, ttToravigt aioitt lower it is 15CW, be treated, 6 * TerfaJbrea according to claim 1 feie 5 »iaiiuroh g« k «im-» eiefejwt, did 4i «itreekrerliSiltiiieas * in the animal stages (1) Wa (4) m eiageetellt * £ * & Si« fäaen naok animal stage «ei »· Fe- bi» 1O-f * i »iie lyEng *« efenüber der » 7 * fffffagxftji 2taeh Aa * pru <sh 1 bi * 6, «T ^ ia £ 4i #« nf 4i «y« #a in | f £ · » (4) «weg *« ³ »** tpwmiKOt m eia« * 3t $ I] tt is, SsS 9038AO / 1SS3 BAD ORHSlNAi. Thread length after the final stage of stage (4) at least 9Ö #, but less than $ 120, preferably at least £ 95 » 3edooh less than $ 115 dee value immediately gate the Stage (5) becomes. 8. The method according to claims 1 to 6, characterized in that the tension exerted on the threads in each stage of stage (4) is adjusted so that the thread length after the final stage of stage (4) is 120 to 17OjC _9, preferably 120 to $ 150, the value of which will immediately become a level (3) gate. 9. The method of claim 1 to 7 sur stretching and heat treatment of niohtgeβtreckten Folyesterfäden, at least 85 MoIfS, preferably at least 90 MOI ^, Alkylenterephthalat®inheiten include, characterized _y that the following stages are carried out in the order given " (1) First stage drawing "wherein the undrawn filaments by 1.1 to 4" 0 times "preferably 1.2 to 3" 0 times in a liquid high-quality solvent having a temperature in the range of 40 to 100 ⁰ C, preferably 60 to 100 ⁰ C, are stretched, (2) Second stage stretching, these stretched filaments in a liquid Iloht solvent at a temperature in the range of 10 to 85 ⁹ O? preferably 40 to 75 ⁰ C, but lower than that employed in the step (1) temperature is preferably lower by at least 10 ⁰ C, multiple 7.0, in a stretching ratio of 1 ₉ 2 "bis, preferably 1,5- stretched to 5.0 times, which is at least 80 pounds of the maximum stretch ratio, (3) first heat treatment, the threads at a Temperature not below 60 * C, but lower 909840/1588 than 10O ⁰ C, which is higher than the temperature used in the step (2), are treated, whereby they are subject to such a tension that their length during the treatment at 95 to 115 $, preferably 95 to 110 $, of the value immediately Goal of this treatment is held, (4) O) first stage of the second heat treatment, where ·! the filaments are treated at a temperature in the range from 100 to 170 ^° C., being subject to such a tension that their length during the heat treatment is kept at 95 to 115? $, preferably 95 to 110 $, of the value immediately before this treatment , (2) second stage of the second heat treatment, the threads being ^{treated further at a temperature lying above 170 °} C., whereby they are subject to tension, so that their length during the treatment is 95 to 115%, avoiding 95-Ma 110 $, the value is held immediately before this heat treatment, where the tension exerted on the threads in stages (1) and (2) in stage (4) is adjusted so that the thread length after stage (2) of stage (4) is at least 90 $, but less than 120 ^ ₉ prevents at least $ 95, but less than $ 120, of the value immediately prior to step (3) above. 10. The method according to claim 1 to 6 or 8 sum Stretching and sur heat treatment of non-stretched Polyester filaments containing at least 90 col- £ ethylene terephthalate units contain, characterized in that the. carried out the following steps in the order given will i 909840/1588 (t) stretching of the first stage, whereby the etreokten threads are stretched T ₉ I to 4.0 times in a liquid lioht solvent with a temperature in the range of 60 to 100 ⁶ C,. (2) Scattering the »wide stage, with these geatreokten threads in a liquid flown-leeking agent at a temperature in the range τοη 40 to 75 ⁰ C, but at least 10 ⁰ C lower than used in stage (1), in a stretching ratio stretched from 1.2 to 7.0 times, which is at least 80 * of the maximum Streok ratio, (3) first · heat treatment, the threads being treated at a temperature in the range τοη 65 to 120 ⁴ U, which, however, is higher than the temperature used in step (2), while they are subject to tension, so that the thread length during the heat treatment at 100 to 130 * of the value immediately the goal of this treatment is kept, (4) »extensive heat treatment, whereby the threads are further heat-treated at least once at temperatures higher than those used in stage (3), and at least one« stage is carried out at a temperature not lower than 12O ^- C * The threads in each stage are subject to tension, so that the thread length is kept at 100 to 130 * the value of the immediately preceding stage, and there is still no exertion on the threads in every stage of stage (4). Tension »so ■. ".: - ■; be set, 4a * die? Ad« Jillft «· aa« h * # * toistufe der St »? · (4) 120 Um 150 * ** · W« rtee «» indirectly gate of the Level (3) .fc ** i! I§ **. \; ";;',: - ^; - ". '■. ■ __ 90984 0/1588