DE1669373A1 - Process for melt spinning fibers - Google Patents

Description

PATENT ADVOCATE

MUNICH 5

REICHENBACHSTR. 51

TEL «3151

A / l 0527 W / P

Alled Chemical Corporation, New York, NY, USA Process for melt spinning of fibers

The present invention relates to the production of fibers from wet containing polyesters dispersed in polyamides.

Spinnable masses which are suitable for the production of spanked textiles, such as tire cord, curtains and articles of clothing, can be prepared by using a mass mixed in the sol containing polyesters, such as polyethylene terephthalate, and polyamides, especially nylon products, such as Polyoaproamld and Polyhexamethylonadlplneüuramid, contain extruded. In this case, the polymers can first of all be in the form of. Schnitzeln, mixed together brooken and then the

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Mixture in a screw extruder or similar Device are mixed as a melt, after which you can molten mixture extruded through a nozzle. In the melted Oemieoh the polyester is in finely divided Form dispersed in thorn polyamide before. usually scored such a dispersion is done by putting the lard in the extruder or similar device large shear " Subjects to forces and then through a pile

Sieves, a sand fruit or a similar fine filter pro3t, after which it is extruded through the nozzle and in a subsequent cooling zone is allowed to solidify to form threads * This KiShIzone is usually an elongated room » where temperature and humidity are carefully regulated. There is a coil at the bottom of this room for winding the threads.

The threads will normally be too. Ladies united »the then to improve their mechanical properties are subjected to a Ve rat reclcungs process. This scattering process is generally caused by that the yarn is stretched at a temperature below the melting point of each of its components, with one Orientation of the molecules along the thread axis © and thus an improvement in the strength of the yarn will be achieved «in the pre-defcung process normal rweleo for polyostor / polyamide compositions Ver »

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stretching aids of about 3.5 to about 6.5 are applied, where the ratio of length is used as the factor of elongation of the stretchable yarn su the length of the undrawn Yarn becomes bad. Xnne & ialb of this area will be low · ® stretching ratio during manufacture Used by textile yarns, up to those © ine great strength is not absolutely necessary. Holier VerstraekungsverHltnlse within the range mentioned are normally used in the production of yarns of high tenacity, for example of yarns for tire cord ”. The yarn can be used in a one-time process or experienced several successive stretching " whereby at least one of the stretching stages is most appropriate « st en bsi carried out at a relatively high temperature will. The Verstreekusig is preferably made with the help of a St recket if done, which precisely defines the area to be stretched.

After drawing, the yarn is on a pile or Coil wound up and ready for further use.

Gewünsehtsnfalla can also use the yarn before it is used be pre-twisted to improve the cohesion of the individual threads. In the case of the procedure described occur in spite of strict pre-calibration measures various difficulties on. So put bsispi © lst; ice drops that go through

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partial blockage of a nozzle and interruptions in the thread at or just below it the spinning orifice plate, a bsim spinning threads particularly troublesome problem. The problem of droplet formation when spinning a polyester / polyamide mixture is particularly uncomfortable when there is an extruder in the melting / mixing apparatus for more than one son senplatte used and thus the! Extruder with the greatest possible Economy is used. Because of these disadvantages, it has been particularly difficult to date, based on polyester / poly & mid mixtures the production speed in that described Increase procedure.

Gin can also tear off during the scattering process or the thread became tangled. With an Ab « Breaking of the yarn in the drawing zone is an interruption of the entire scattering process necessary. Am Entangling can occur when © in thread or several, each

however, not all of the threads in the yarn in the tangle zone will break. In such a case, the ends of the torn threads, which are directed towards the hulk, tend to wind themselves around the roll instead of running on to the twisting apparatus. Sometimes such a disturbance can be remedied without interrupting the process, but the properties of the yarn obtained can result

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• 5 ■ the entanglement will be worsened.

The aim of the invention is thus a practically complete one Elimination of the aforementioned disruptive factors.

The subject of the invention is a process for the production of a fiber by spinning a fiber-forming β-polyamide-containing compound which contains up to 50%, based on the weight of the mass, diapered on a fiber-forming polyester. The process is characterized in that the mass contains 0.05 to 0.6 parts by weight of a spinning aid which I) has a melting point of over 1 (XK and II), a mold release index of over 25 in pure polyamide, and 111) one contains straight-chain, saturated acyl group, the hydrocarbon radical of which consists of 12 to 22 carbon atoms.

The spinning aids of the invention are waohs-like and practice no painful effect on the polyester / polyamide-Oemlsch, i.e. they set the tensile modulus of the Mixture made fibers does not degrade. Spin aids with the desired properties are generally Long-chain derivatives: fatty acids such as laurine ", palmltine", Stearic or behenic acid. Metal salts, amides as well Aoyl-modified hydrazines of these acids are typical representatives for useful accessories, of which the following

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Table shows a number with their melting points and mold release indices .

T a b e 11 e I. 14> Run form »
index Added compound melting point, ⁰ C 130 40 Ethylene bis »(Btearylamld) 13 * 38 jMtethylene «bis- (stearylamide) 132 42 Ethylene bis (behenic acid amide) 167 40 N, N ^J -hydrazine ~ bie = (stear ylamid) 120 35 p "Fhenylen-bia" (stearylamide) 181 34 1,4 »phenyl stearate stearyl amide 162 29 PpP ⁹ -Diphenylätho r-bis - (palmit yι.
amide) 171 37 ρ, ρ ^ϋ ° Diphenylmethyl-bia °
(stearylamide) 223 33 ρ, ρ ⁵ «Dipheny linefchyl -bis«
(law ylamid) 260 42 p, p '~ diphenyl-bi8 ~ (st6arylamid) 270 42 Nat riufflst earat 145 35 Sodium palmitate 1 * 8 33 Barlum stearate 125 39 Calcium atearate 215 27 Copper stearate 159 40 Lithium stearate 125 38 Mangraeeiiaoistearate 32 Sinketcarat

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As used to determine the mold release index attempt polycaproamide ^ pellets were that 0.2 # contained homogeneously mixed to be tested according to the invention Spinnhili'smittelß of, a "Van ~ thorn ^R" SpritzguSmaschine that at a Heekzylinderternperatur (RSAR cylinder tonperature) 185 ⁰ C., and a Forratemperatur was operated by 8ZC. the pressure in the spray line was maintained at 77 »^ kg / cm, the injection time (injection forward time) was 5 seconds and the mold open time 2 seconds. the front» m zylindertemperafcur was set so that the melt viscosity required to fill the mold without the polymer running out of the mold between its two halves is achieved. The mold used is a disk with a diameter of 5 cm and a thickness of 0.32 cm, which with one in the middle of the bottom of the mold and with the bottom of the mold in the same direction Injection plunger with a diameter of 1.27 ora is mounted horizontally on a flat surface. The mold is made of stainless ™ steel. The melting time is 5 minutes, the injection time 10 seconds and the »clamping time 15 seconds. To test the tendency of a mass to separate from the mold, the force required to force the molded disk out of its mold is determined by measuring the pneumatic pressure applied to the piston. For comparison, the same experiment is carried out with a sample

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the same polyamide, but not a mold release agent contains, carried out.

The mold release index is as the percentage of decrease for pressing out the mass to be examined existing compacts from the mold required pressure compared to that of a compact that does not have a mold release agent contains, defined pressure to be applied. If at-φ for example the expression: for the pure polyamide

7 »7 kg / cm and for the sample to be examined 4.2 kg / cm is calculated, see the porcelain separation index to C (7.7 ■ = 4.2) / Γ, 7] * 100 β 45. The one according to the present Invention usable spinning auxiliaries must after this Test method have a mold release index greater than 25.

When carrying out the experiment, temperatures, pressures and dwell time are observed and recorded so that Comparable it and reproducibility of the results are guaranteed. At the beginning of each test series, the injection molding machine is cleaned with standardized pure polyamide, whereupon the system with the polymer to be examined is cleaned until the results remain the same can be achieved, which is usually repeated after 20 to 20 times Operations is the case. During this time, the optimal operating temperatures and fuel pressures are also determined. After cleaning, the printouts become

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ten successive injection molding operations the means formed and as an expression of the subject to be examined Polymer / admixture mixture retained.

As Spinnhilfsnilttel preferably have the alkali and Alkaline earth salts, since these compounds can be obtained easily and at low cost in practically pure form »In particular sodium palmitate and stearate are preferred, since excellent results can be obtained with these two substances ^ j can achieve.

The spinning aid can be added to the mass at any convenient time during the dry or melt ripping or introduced into the polymer during the polymerization. Ea can be added as a solid or as a solution or as a slurry, in the latter two cases a low-boiling liquid which can easily be evaporated is used for dissolving or slurrying. A spin agent in the form of solid particles during the dry Vermlschens faserblldenden the polymers is preferably admixed _p by being simply added to the trookenen Teilchongemisch and the whole anahlleßend mixed by stirring or other mixing process. During this mixing process, the spinning aid is evenly distributed over the surfaces of the polymer particles.

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According to the invention, good results can be achieved with compositions * which contain only 5% by weight or even less polyester. The above-indicated difficulties However, increasingly larger when the concentration increases to polyester "Accordingly, the method erfindungsgemäBe Ins" special advantage in compositions whose polyester content is 20 or more weight - is.%.

In a particularly preferred embodiment of the process according to the invention, a spinning aid is used in conjunction with fiber-forming polyester / polyamide materials which form 10 to 50 parts by weight of the fiber-forming polyester in the form of microfibres in a mass of 50 to 90 parts by weight of polyamide contained dispersed. The polyamide is also characterized in that it has no more than 40 such end groups * which react with the polyester in the melt. The polyester is long-chain and has a glass transition temperature in the amorphous state of at least 50 ⁸ C * as measured by differential thermal analysis, while the glass transition temperature of the polyamide * is lower. The reduced viscosity of the polyamide, measured at a concentration of 0.5 g of polymer per 100 ml of ^T * solution in o-chlorophenol at 25 ⁴ Cf, is in the range from 0.9 to 1.4 and the ratio of the reduced viscosities of polyamide to polyester is about 0 * 9 to 2 * 0. The mass is in

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all mixed in as a melt tind foai at one temperature from about 50 to about 285 ^, i.e. about 10 to 40 "C above the melting point of the higher melting component the nozzle extrudes.

In the preferred embodiments of the invention, polycaproamides and polyhesamethylqiiadipins & urearoids are used, although other polyamide components which are made from polyamides of monomers having 4 to 14 carbon atoms can also be used. Preferred polyesters are, for example, the polyethylene phthalates, in particular polyethylene terephthalates , albeit other condensation: products of dibaaiger acids, for example of
Naphthalene ~ 2,6 ~ and ~ 2,7 ~ carbonic acid, with polyhydric alcohols * such as ethylene or propylene glycol, or sterically hindered glycols can be used.

The following examples illustrate the invention; Examples 1, 3 and 5 are commercial examples.

Pellets made from polyethylene terephthalate were used as the polyester cap used with the following properties:

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Melting point (determined by thermal Differential analysis

End group content in mill! Equivalent each kg polymer

Carboxyl 55

Hydroxyl 65

Reduced viscosity in o-chlorine « phenol 0.80

Glass transition temperature, determined by thermal differential analysis

Pellets made from polycaproatnide were used as the polyamide with the uses the following properties:

Melting point (determined by animal differential analysis)

End group content in mill equivalent each fcg polymer

Carboxyl 72

Amino 20

Reduced® viscosity, determined in ο -chlorophenol

Glass transition temperature "determined by thermal differential analysis

In a circulating mixer, 55 parts by weight of polyamide pellets and 45 parts by weight of polyester pellets were mixed for 1 hour. The granular mixture was then dried to a moisture content not exceeding $ 0.07 and as a melt at 279 "C in an extruder with a diameter of 8.9 cm rotating at a speed of about

23 »1 rpm was operated, mixed, with an outlet pressure

"""2
of about 267-2 kg / cm was produced. The temperature of the

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BATH ORIGINAL

- 15 polymer on leaving the extruder was 279%.

The molten Oemisob was untur a Oruok of 196.9 kg / cm ² and at a temperature of 265% through a filter stack, which is pumped from a number "of screens and a sand bed consisted" and by a DUsenplatte with 204 circular openings with the following Dimensions extruded: length · of the nozzles! »7526 mm; Diameter 0.4572 mm; Entry angle 60 °. The threads obtained passed through a cooling chamber which contained air at 27.8 ° C. and 65% relative humidity, which flowed in the same direction as the threads at a speed of about 8.2 ohms / min. The Qarn. was wound onto a cylindrical bobbin under a tension of 35 g at an oeso speed of 347 * 7 m / min below the cooling chamber, after it had been lubricated shortly beforehand with 4.2 pounds of its weight on a (. The yarn thus obtained possessed a denier of about 6772 and a birefringence of 0.004.

The yarn then went through a process of twisting subjected by moving it from a closed oot feed roll onto an upper draw roller and from there in a soling around a statlontre keramisohe Streoknadel (or needle stick) of 3.8 om diameter to oinor

Contact heating plate, which has a temperature of 185%, and

dl «leads around a lower Zlthwalse with an oohllefllioh in five soles, /

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5 * 52 times the circumferential speed was rotated as the upper drawing roller. That way, dad got yarn on stretched the 5.3 faehs of its initial length.

Subsequently, the yarn hurries a speed of 256.2 m / min using a ring guide (ring «= ' traveler device) in such a way that the yarn was twisted by 0.2 win = fertilize per cm. The one obtained in this way Yarn had the following properties:

Denier 1279

Elongation at break, % 14.7

Tensile Strength, g / denier 8.56

Tear strength, g 10 9 ^ 7

Tensile modulus, g / denier 7?

Shrinkage, % 12

The following phenomena were observed during the production of 89.7 kg of yarn:

Drops / hour at the spinneret 2.43

Reiflvorgiinge / kg on the pull «and Twist device 0.299

VerwioklungenAe at the 2 ... Qh- and Twist device 0.689

Example 2 The procedure is practically the same as in Example 1

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with the deviation, aai the spinning mass sodium stearate added tsurde «A comparison osr in both examples The results obtained clearly show the superiority of the dope containing sodium stearate.

The polyethylene terephthalate pellets were the same as those used in Example 3. The polyeaproamide pellets possessed the following characteristics:

Melting point (determined by thermal Differential analysis)

Kndgruppengetialt in Hilli equivalent each kg polymer

Carboxyl 75

Amino 18

reduced viscosity in o-chlorophenol 1.10 Oil transition temperature (determined by thexroisehe differential analysis) 48SJ

55 parts by weight and 45 Polyaniidpellets Oew. parts of polyester pellets with 0.2 weight "parts Natriurasfccarat Fons in a dry powder i hour in Qinara Urawälzmischer \ TG:. W: j: CHT, Ό && granular öemisoh vrarde 'Jis za a moisture content of less than 0.07 ° and then dried in an 8.9 cm diameter extruder, which was operated at a rotational speed of about 35 rpm, as a melt of about 278 °. The discharge pressure at the extruder was about 246.12 lcg / cm and the temperature of the polymer melted into the extruder

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The molten mixture was passed under a pressure of 246.12 kg / cm ² and at a temperature of 265 * C a filter stack made up of a number consisted of sieves and a bed of sand, pumped and through

a nozzle plate with 204 circular openings with the following dimensions extruded: length of the nozzles 1.7526 mm; Diameter 0.4572 mmj entry angle 60 °. The threads obtained descended through a cooling chamber containing air of Sk 27, BK and 65% relative humidity, which in the same direction as the FKden flowed at a speed of about 2.2ebm / min. The Oarn was under, a tension of 35 g at a speed of 359 "? m / min below the cooling chamber on a cylindrical bobbin, after it had started with 4.5 # of its weight shortly before lubricated. The oarn thus obtained had a denier of about 6727 and one Birefringence of 0.0OJJ.

The yarn then went through a warping process subjected, by moving it from a closed loading * «rollo (cot foed roll) to an upper Zletetalze and from there in a loop around a stationary ceramic straightening needle 3.8 cm in diameter to a contact heating plate that has a Temperature of 185 * C, and finally in five Sohlingen around the lower drawing roller, which with a 5.58 times eo The upper drawing roller was rotated at a great initial speed. In a dloso way, the yarn was on that

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5.3J8 times its initial length.

The yarn was then wound up at a speed of 256.2 m / min using a ring-traveler device in such a way that the yarn was twisted by 0.3 turns per cm. The yarn obtained in this way had the following properties:

Denier 1257 _-

Tear, % 15.6

Tensile Strength, g / denier -8.67 Tear strength, g 10 892 Tensile modulus, g / denier 77

Shrinkage, % 12th

The following phenomena were observed during the production of 88.8 kg of yarn:

Drops / hour at the spinneret 0.47 l

RöißvorgHngo / kg on the pulling and Twist device 0.022

Verwloklungen / kg on the pull and Twist device 0.044

Example 3 The same) η polyethylene terephthalate pellet *

as used in example 1. The PolyocproamldpellotQ

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the following properties:

Melting point (determined by thermal differential analysis) 22SK

End group content in NIII equivalent per kg of polymer

Carboxyl 71

Amino I ^

reduced viscosity in o-chlorophenol 1.0 Olas transition temperature (determined by thermal differential analysis) 45t

In a circulator, 55 parts by weight of polyanide pellets and 45 parts by weight of polyester pellets were mixed for 1 hour. The granular mixture was then mixed up to a moisture content of not more than O, O39 £ dried and used as Sohmelze at 275 ¹ C in an extruder having a diameter of 8 9 whether, which was operated at a rotational speed of about 23.5 QPM * " , with an Auslafidruok of about 210.96 kg / cm? was generated. The temperature of the polymer leaving the extruder was 275 ^

The molten oomiseh was pumped under a pressure of 203.93 kg / cm and at a temperature of 26% through a filter stack consisting of a number of sieves and a bed of sand and extruded through a diamond plate bit 204 circular openings with the following dimensions: lung of the nozzles 1.7526 mi diameter 0.4572 mmj entry angle 20 °. The PHden obtained descended through a cooling chamber, the air from

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BATH ORIGINAL

27.8 ¹ $ 65 C and relative humidity contained "in the same

Direction as the thread with a dizziness of about

2.2 obm / min flowed. The yarn was under tension of 35 g at a speed of 359 * 9 m / min below the cooling chamber wound on a cylindrical spool " after it briefly: before with $ 4.4 of its weight »at one

Lubricant had been applied. The yarn thus obtained possessed

about 6712 denier and birefringence of 0.00228.

Subsequently, the oam underwent a dispersion processS8 subjected «by moving it from a closed cot feed roll to an upper orphan and from there in a loop around stationary ceramic ones 8tredewfcl of 3 * 8 om Durohmesser asu a contact heating plate, which had a temperature of 185%, and sohlleflloh in five Solingen led around a lower drawing roller with a bucket 5 «58 times the circumferential speed was rotated as the upper drawing roller ·. That way the yarn was on the fifth of its initial length rotten.

At the end of the thread the yarn was fed at a speed of 256.2 m / min using a ring traveler device in such a way that the yarn was twisted by 0.2 turns per om. Daa received on these catfish Yarn had the following properties:

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Denier 1260

Elongation at break, 15.9 pounds

Tensile Strength, 8.3 g / denier

Tear strength, g 10 458

Access modulus, g / diameter 34

Shrinkage, % Xi

The following appearances were made during manufacture observed from 39.4 kg of yarn:

Drops / hour at the spinneret 3.0

Rg eat processes Ag on the pull and Test device 0.1Oi

Vertficklungen / kg on the pull and "Ewist device 0.81

Example 4

The procedure is practically the same as that of Example 3 with the deviation that sodium palmitate is present in the spinning mass is. A comparison of the b ^ äen Bs & games invites the superiority of the spider masoids containing sodium fissure recognize clearly.

The polyethylene terephthalate pellets, dl © according to this example were used, were the same as those in example! used.

The Folyc & proamid «P <sllet9 possessed the following properties

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Melting point (determined by thermal differential analysis) 222 ¹ C

Group content in milll equivalents each leg polymer

Carboxyl 79

Amino * 3

Reduced viscosity in o-chlorophenol I ₄ O

aias transition temperature, determined duroh thexnisohe differential analysis 45U

55 (Jew. Part · polyamide pellets and 45 dew. Parts polyester pellets were vexvisoht with 0.1 parts by weight sodium palmitate in the form of a dry powder for 1 hour in a circulator. The granular mixture was up to a moisture content of <up to dried, and then, to vermisoht 0.0295 * in an extruder of 8.9 cm diameter dor was operated at a rotational speed of about 26 UpH as a melt at about 275 C ^1. the AuslaSdruck in the extruder was about 20 ^, 93 kg / cm and the temperature of the polymer admitting the extruder

The geeohmolsene Oemisoh was under a pressure of 161.74 kg / cm * and at a temperature of 275 ⁰ C through a filter stack, which consists of a number

consisted of seven and a bed of sand "pumped and through one DUaenplatte with 204 circular openings with the following ^ Dimensions of the extruded tubes 1.7526 mm Durohmesser; 0.4572 BMf back ride angle 20 °. The threads obtained A cooling chamber ran downwards, the air at 27.8 ° C and 65Jt ^ relative humidity contained in the glelohsr direction SfU the F * den old a QoeohwindlfHeit of about t, 8 cm / fine m strente. The oarn was pulled under a tension of 35 g

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at a speed of 244.65 n / min below the KÜhlkananer wound on a cylindrical spool, after shortly before with $ 4.5 of its weight at one Lubricant had been applied. The yarn thus obtained possessed a denier of about 7026 and θ ine birefringence of 0.00i4.

The yarn was then subjected to a Veratrackungaprozöss by pulling it from a closed feed roll (eot feed roll) to an upper draw / fold and from there in a loop around a stationary ceramic needle of 3.8 om diameter to oinev contact hot plate, which is a Temperature of 165 * 0 possessed “and finally in five loops around a lower drawing roller a led »the one with a 5 * 78 times so was rotated at high peripheral speed like the upper drawing roller. In this way the yarn became 5.72 times its initial length scattered.

The yarn was then transported at a speed of 256.2 m / rain using a ring guide (ring-travoller device) wound up in such a way that it learns by 0.2 turns Jo om was twisted. The yarn preserved on the catfish bosaS has the following properties:

Denier 1267

RelSdtnung, Jf 15.0

1 0 9 8 1 9/1 8 8 0 bad original

Tensile Strength, 8.2 g / denier At the same time, g 10 389 Tensile modulus, g / benier 84

Shrinkage, % 10

The following phenomena were observed during the production of 50.3 kg of yarn:

Drops / hour at the spinneret 0.67

Tearing process on the pulling and testing device 0.119

VerwioklungenAg on the pulling and riveting device 0.119

Example 5 There were polyethylene terephthalate pellets old as follows Features used:

Sohaelx point (determined by thenl differential analysis) 250t λ

End group content in milli-equivalents each kg polymer

Carboxyl 5 "

Hydroxyl 65

reduced viscosity in -chlorophenol 0.80 Olast transition temperature (determined by thermal differential analysis)

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The polycaproamld pellets used had the following Eggs:

Melting point (determined by thermal Differential analysis)

End group content in milli-equivalents each leg polymer

Carbonyl 77

Amino 5

reduced viscosity in ο-chlorophenol 1.09 glass transition temperature (determined by differential thermal analysis) 48 ⁸ C

In a tJmwglzmische? 55 parts by weight of polyamide pellets and 45 parts by weight of polyester pellets were verraleoht for 1 hour, The granular mixture was then up to a FouchtlgScaite "content of not more than 0.033 $ dried and as a melt at 274 C in an extruder ¹ cm having a diameter of 8.9, which was operated at a rotational speed of about 18.7 rpm, with a mixed _f AuslaSdruok of about 210.96 lcg / crn was produced. The temperature of the polymer on leaving the extruder was 275%.

The molten mixture was under a pressure of 246.12 kg / cm, and? Ei a temperature of 265 ⁰ C through a filter stack, which consisted of a number of screens and a sand bed, pumped by a DUsenplatte with 204 circular openings with the following dimensions extruded: lung of the nozzles 1.7526 ram; Diameter 0.4572 mm;

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BATH ORIGINAL

Eint rode »angle 20 °. The fibers obtained descended through a cooling chamber, the air of 27 * 8% and 65Ji relative humidity, which flows in the same direction as the threads at a speed of about 3.2 obe / min te. The yarn was tightened under a tension of 35 to 45 g Speed of 359 * 9 «/» in below the cooling chamber wound on a cylindrical bobbin »after it shortly before with $ 4.00 of his oewioht ·· to a »lubricant had been provided. The yarn thus obtained had a denier * number of about 6666 and a birefringence of 0

The qarn was then subjected to a scattering process by moving it from a closed feed-roll onto an upper roller to report slip losses, and from there in the sole length of a stationary ceramic scattering needle }, 8 on Durometerssser su a contact heating plate "which has a temperature of 185%, and finally led in five soles from a lower drawing roller" which was turned with a speed of 5.48 times as large as the upper 21-shaft. In this way the yarn was stretched to 5.22 times its initial length.

Ansohllefiend became the Oarn at a rate of

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BATH ORIGINAL

256.2 m / min using a ring guide (ring traveler device) wound in such a way that the yarn was twisted 0.2 turns per om. The oarn obtained in this way had the following properties:

denier 1265 Elongation at break, % 14.5 Tensile strength «g / benler 8.73 Tear strength, g 11 043 Zugoodul, g / denier 75 Shrinkage, jf 12th

The following appearances were made during manufacture observed by 788.7 kg of yarn!

Drops / hour at the spinneret 0.375

ReiflvorgangsAg on the pulling and Twist device 0.161

»Tangles at the pulling and twisting device 0.251

Example 6

The procedure according to this example is practically that of Example 5 is the same with the difference that in the present example, 0.10 * sodium stearate is used as a spinning aid and that an extruder for two liners was used. Comparing the results of the

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BATH ORIGINAL.

Examples 5 and 6 show that the number of Tropfmje Hour is practically the same in both examples. However, the throughput per hour according to Example 6 is 29.62 kg compared to only 14.813 kg according to Example 5- The use of the Spinning aid according to the present invention thus enables polyester / polyamide mixtures to be spun with a much higher production speed than before »without the drop formation at the same time on dtr Spinneret is increased.

The polyethylene terephthalate pellets were the same as those used in Example 5.

The polycaproamide pellets had the following properties:

Melting point (determined by thermal Differential analysis)

End group content in mill. Equivalent per I.

kg polymer

Carboxyl 70

Amino 17

Reduced viscosity in o-chlorophenol 1.04

aiasttbergeng temperature (determined by thermal differential analysis) 48 * €

Egg made from 55 weight polyamide pellets and 45 weight parts Polyester pellets containing 0.10 parts by weight of sodium stearate

109S19 / 1886 bad or / q, _Nal

was mixed in a circulator for 1 hour. The granular mixture was dried to a moisture content of up to 0.035 # and then in one Extruder of 8.9 in diameter, which was operated at a speed of rotation of about 30 rpm, as a melt of about 2745! mixed. The outlet pressure at the extruder was about 210.96 kg / cm and the temperature of the polymer leaving the extruder

The molten mixture was under a pressure of

246, IS kg / cm * and at a giner temperature of 25 ^ ^e C through a filter stack made up of a number consisted of seven and a bed of sand, pumped and through two Extruded nozzle plates with 204 circular openings each with the following dimensions: lungs of the nozzles 1.7526 mm; Diameter 0.4572 mm; Entry angle 20 °. The filaments obtained underwent descending a cooling chamber, the air of 27.8 ¹ S and 65 $ relative humidity contained in the same direction as the flowing FKden at a rate of about 2,2cbm / min. The yarn was wound onto a cylindrical bobbin under a tension of 35 to 45 g at a speed of 359.9 m / min below the cooling chamber, after it had been provided shortly beforehand with 4.5 # of its oil of a lubricant. The yarn so obtained had a denier of approximately 6616 and a birefringence of 0.0043.

109819/1886

The yarn was then subjected to a stretching process! by it possessed of a geschloasenen Beschiolcungs "roll (cot feed roll) to an upper drawing roller and from there in a loop around a stationary ceramic" stretch needle of 2.8 cm diameter to a contact system "including a temperature of 155 ⁰ C and finally led in five loops around a lower drawing roller, which was rotated with a circumferential speed of 5 * 56 times ao as high as the upper drawing roller. In this way the yarn was drawn to 5.3B times its initial length.

The yarn was then wound up at a speed of 256.2 m / min using a ring traveler device in such a way that the yarn was wound by 0.21 Turns per cm was twisted. The yarn obtained in this way had the following properties:

denier 1257 Hoop elongation, % 1 *, 9 Tensile Strength, g / denier 8.89 Tear strength, g 11 181 Tensile modulus, g / denier 79 Shrinkage, % 12th

The following appearances were made during manufacture of 788.7 kg Often observed:

109819/1888 ⁸ ^ D original

ib69373 - 30 -

Drops / hour at the spinneret o / 37 Reissvörgüiiga / kg on the pulling and Twist device 0, Tangles / kg at the pull and Twist device 0.066 Example 7

When using the following spinning aids, the formation of less at the spinneret was in each case; as 1 drop per hour observed. The spinning auxiliaries were according to the invention in a polyester / polyamide mixture 50:70 used «where the polyethylene terephthalate used and polyoaproanjid similar to those used in Example 2 Components was procured and the mixture in analog Catfish has been processed into «yarn.

Added spinning aid Concentration? 0.2 Oew «» parts | c Λ ο ο Ίμ

Ψ Ethylene-bie- (stearylamide) ~ *

Methylene-bs- (stearylamide) ethylene-bie- (behenic acid amide) N, N'-hydrazine-bie- (EtearyliuBid) p-phenylene-bie- (atearylamide) 1,4-phenyl-atearate-etearylamide p, p ^e -diphenyl -Kther-bi · - (palmitylamide) p> p ⁸ -Diphenyl-methyl-bis - (»tearylamide)

109818/1886 _BAD or.g.nal

ρ, ρ ° -diphenyl-methyl-bis- (laurylamine)

P s P ^δ -diphenyl-bis (stearylaroid) Sodium stearate Sodium palmitate Barlum stearate Calcium stearate Copper stearate Lithium stearate Magnesium stearate Zinc stearate Example 8

A mixture aua 50 0EW. ~ £ polyethylene terephthalate and 70 poly cap ro amide, each polymer has the same properties as that according to Example had 2 eiifcspyeofeeiuäe polymer used was dry with various amounts, pulverförraigen sodium stearate mixed for 1 hour in a conical Umwälzralsoher λ. The granular mixture was dried to a moisture content of not "mixed more than $ 0,038, and then dried in an extruder of 8.9 cm diameter which was operated at a rotational speed of approximately S3 tJpM as a melt at about 265 C ^f. The outlet pressure in the extruder was about 210-96 kg / cm and the temperature of the polymer leaving the extruder was 265%.

109819/1888

^ßAD

The molten mixture was under a pressure of

140.64 kg / öin * and at a temperature of 26 & α through a filter stack consisting of a number consisted of sieves and a bed of sand, pumped and through a nozzle plate with 204 circular openings with the following Dimensions ext erased: length of the nozzles 1.7526 mm; diameter 0.4572 mm. The threads obtained passed through a descending one ! Cooling chamber, the air of 27 * 8 <C and 65 $ relative humidity which flowed in the same direction as the filaments at a speed of about 1.64 cbm / min. The yarn was under a tension of 35 S at a speed of

344.65 m / min below the cooling chamber on a cylindrical Coil wound up after it had just been with $ 4.6 of his Weight had been provided with a lubricant. The yarn thus obtained had a denier of about 6844 and one Birefringence of 0.0Q25.

The yarn was then subjected to a drawing process

subject by reporting hatching losses from a closed prey, ash ic kungs roll (cot feed roll) Christening an upper Zlehwalse and von There in a base around a stationary ceramic needle of 3.8 mm diameter to a contact heating plate, which had a temperature of 1 & 5K , and finally led in five base rings around a lower drawing roller, which was rotated with a circumferential speed of 5.73 times as high >: de like the top pinch roller. In this way the yarn was drawn 5.4O times its initial length.

^Sl "'" 109819/1888 .ad or.ginal

1b69373 - 33 -

The yarn was then run at a speed of 256.2 m / min using a ring guide (ring traveler device) wound in such a way that the yarn is wound by 0.2 WIn * fertilize for each cm twisted,

In the following Table IXI, the results are compiled without the addition of sodium stearate and with the addition of sodium stearate in four different proportions received:

T a ρ e 11 e III Sodium stearate 0.0 0.1 0.3. 0 * 4 0.6

Spun product, kg 288.1 127.3 239.2 236.9 90.6 Drops / hour 0.98 0.0 0.19 0.13 0.15 Tangles / kg 0.286 0.0 0.0 0.0 0.0 Tears / kg 0.189 0.035 0.033 0.0121 0.0066 denier 1258 I274 1265 1267 1263 Elongation at tear, # 15.5 14.8 15.1 15.2 15.3 Tensile strenght,
g / denier 9.75 9.50 9.46 9.20 8.55 Tensile modulus, g / denier 64.6 68.4 66.9 67.4 69 »* Veratreok'jee Pro
duct, kg 93.8 114.9. 147.7 163.8 8K8

The presence of the use according to the present invention ten spinning aid ·! affects the properties of

109819/18 »«

manufactured products not.

From the following attempt to test a given yarn, on its tendency to form flattened beefs (flat spotting) «when it is used as a tire cord wlrcU is known that he realizes the behavior of yarns in tires, which are reinforced with them, reproduces well * It is a standardized test procedure that is carried out under the following conditions:

Conditioning the samples

1. Two 50.8 cm samples of chamois, denier 840 are placed in an oven (a glass tube * that is used for heating surrounded with steam with a dumbbell), the dry Contains nitrogen, hung.

2. Load each sample at 0.5 g / denier and open the oven 105ΐ heated! Temperature and load are 1 hour » long maintained.

"3. The oven is cooled to room temperature and the load increased to 0.75 g / denier; it will be 30 minutes long

maintain. 4 “The oven is heated to 105 ° C and this temperature

Hold for 1 hour. 5 «The oven is cooled to room temperature» and this

The temperature is maintained for 30 minutes. 6. The load is reduced to 0.90 g / denier, the oven on 103% heated, and the conditions become 60 minutes maintain.

10 ** 1 t / 1 888 8ADORiGlNAL

7. The oven is cooled back to room temperature and this Maintain temperature for 30 minutes.

The samples conditioned in this way are tested as follows:

8. The oven is ^{heated to 105 8} C and this temperature is maintained for 20 minutes.

9 «A sample (yarn B) for the load M for 5 minutes to 0.25 g / denier lowered, then the furnace is cooled to room temperature (approximately 20 minutes).

10. The load is increased for yarn B & to 0.5 s / denier.

After 30 seconds, the length of the samples is determined. The flat spot index is the tenfold difference in length, expressed in mm, of the two probers after reloading referred to in level 10. After this FrttfveKfatireii was for the yarn made using 0.11 wt. $ sodium stear & t was manufactured, a flattening index of 22 and for a yarn, which was made without the addition of sodium isoistearate, practical found the same flattening index. This value is well within the limits commonly accepted in trade will.

The yarns produced were also subjected to an adhesion test, namely the standardized "H ^ adhesion test",

109819/1886 ^ßAD

in which two strands of the yarn to be examined were used, which were coated with normal resorc in / formaldehyde latex or a polyester adhesive, and in which natural rubber was used as the elastomeric substrate. In the test method, the force (in pounds) is measured which is required to a strand cm eat in a length of 0.633 a Gummisohiohtstoff 1st embedded to pull in the axial Riohtung from its embedment, wherein the laminate at a temperature of 121 ⁰ C is held. To produce the laminate, the piece of cord treated with the adhesive is placed under a tension of 50 g in a mold between two sleeves. This sandwich unit is then vulcanized in the press for 30 minutes at a temperature of 138% and a pressure of 17.58 kg / cm. In such a test method it was found that the adhesion values of the yarns produced according to the method of Examples 5 and 6 agreed within the reproducibility limits of the method.

109819/1886

BATHROOM OHIGrNAL

Claims (2)

Ib69373 Pat e η t a η s ρ r Q c h e 1. Process for the production of a fiber by spinning a mass containing a fiber-forming polyamide "which contains up to 50 $ * based on the weight of the mass, dispersed in a fiber-forming polyester" characterized in that the mass 0 _p 05 to 0 , 6 Qew. "Contains parts of a spinning aid which I) a melting point of over 100 "C and II) a mold release index of over 25 in pure poly" oaproamid has and III) a straight-chain saturated one Contains aoyl group whose hydrocarbon radical is from 12 to Consists of 22 carbon atoms. 2. The method according to claim 1, characterized in that daS an alkali or alkaline earth salt of an aliphatic carboxylic acid is used as a spinning aid. 2. The method according to claim 2, characterized in that sodium stearate, sodium palmitate or calolum stearate is used as the spinning aid. 4 «Spinnable mass, which contains a fiber-binding polyamide, in which 100 parts of Ctosant weight the mass up to to 50 parts by weight of a fiber-forming polyester 1098 td / 1 wasteland »ADORIGINAL are dispersed, characterized in that the Hasse also contains 0.05 Ms 0.6 parts by weight of a spinning aid which 1) has a melting point above IC (K and II) a mold release index of more than 25 in pure polyeaproamide and IXX) contains a straight chain, saturated ac ^ l group, the hydrocarbon residue of which consists of 12 to 22 carbon atoms. 109819/1111 BATH ORIGINAL