DE1435621A1 - Synthetic fiber - Google Patents

Description

Q-631

EI DU POMT DS NEMOURS AND COVPANY lOtb and Market Streets, Wilmington 98, Delaware, V _n St.A.

Synthetic fiber

The invention relates to fibers or threads, in particular one elastomeric fiber made from polypropylene.

Much effort has been expended in attempting to make fibers from synthetic polymers which have many of the desirable features of fibers made from natural rubber without bulging their necks. The results of these tests varied, but overall no great successes were achieved. Usually the fibers obtained had in the elongation ranges _? In which most of the areas of responsibility are worked, exceptionally low moduli of elasticity, i. e. for the fibers there is a very low tension at the usable elongations and consequently one had to resort to coarse denier fibers in order to achieve a suitable elongation resistance.

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The problem of creating a fiber that, in the popular sense, is somewhat elastic »but not too elastic, still exists»

The polymers proposed so far are lacking for deformation Äur not only the desired degree of elasticityj, Instead, oils are used to produce the solutions proposed in the foregoing used*". ? olyaa.ri8 & te is also quite expensive and schv.sr

Faaern i? Ue axially crystalline, high molecular weight "polypropylene sli? D well beks & it, .Sjeigs of these fibers are swar in the literature ale "-hocheliiotiooV viewed, about usable elastic Fibers & uss Polyprcp.vleu have not yet been found, and allgeaela has the problem, valuable elastic PcIypTOpyle ^ faear ^ and Isrgleleha / a au create as equally beautiful, iex'ig t, la at® Sias ^^ s anäerar synthotischer Polyi'isrisata proved.

ψοτ11 * ϊ £ &τΛ'ύ ^ rfiadung represents a new? a.ser from PoIy- <r VirfUguag ,, which in particular has a useful ^ iVi _- UChen Slaatlaität, ie recovery from stretching, and into! »rough Qrad of stretch resistance _c you caclit üpfi'jsiöller a polypropylene fiber is available that is suitable for a variety of purposes where a certain

is very desirable, as for the purchase of car

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eltsen and covering of garden chairs, carpets and hoses. Further distributions and details of the purpose of the invention result from calibration from the following description.

The above objects are achieved according to the invention with one Polypropylene fibers achieve their physical structure sioh duröb ^ -orientation and a heat-stable orientations marks angles from 10 to 30 °. According to a preferred The embodiment characterizes the polypropylene fiber according to the invention by an inteeneity ratio of at least 1.0 and a heat-stable orientation angle of 10 to 21 °.

It has been found that a polypropylene fiber, the physical structure of which is characterized by ^ -orientation and a heat-stable orientation angle of 10 to 30 °, a very favorable combination of properties, including! good recovery from stretch. Such a Fueer has the following properties: a tenacity of at least 0.6 g / den, an elongation at break of 100 to 700 f., A springback (tensile recovery) from a stretch of 25 ί> wide and in the following Cycles of at least 82 Jt ', a ratio of the reciprocal values of the modulus of elasticity ("Naohgiebigkeiteverhltnie") at two different elongations (5 to 30 elongation) from 2 to 15, a tension at 5 $ ■ elongation between

909808/0793

0.1 and 0.8 g / den and a five-a-thousandths of 5 to about 25 g / den.

The polypropylene fiber according to the preferred iiusführungsforin the invention with / "- orientation, an F-IntensitätsverhSltnis of at least 1.0 and a tTAER iaestitbllen OrientierungewAnkel 10-21 ° has © ine resilience of elongation by 25 $> in the wide and. the following cycles, which contribute at least 85 i- and, as shown in the examples, also exceed 90 fi

For the sake of clarity, the following are various

Marking defined terms used.

The "orientation angle" is a parameter which reflects the orientation of the molecular axes of the material forming a fiber in relation to the fiber axis. It is indicated by the azimuthal extent of the intensity of the (040) interference sickle at 2Θ »16.7 °, these indices here according to G, Natta et al.,“ Atti acoad. Nassl, Llnoei, Hend «Classe ei. Fis * mat, e »Nat, ¹ *, θ 21, 365 (1956). The angles of orientation are based on the method of H. G ₀ Ingersol," Journal of Applied Physics ", 17, 924 (1946) on the device based on J ₉ E Owens and WO Statton, "Aota Chryetallographica", VO, 560 (1957). The muscle determined using the (040) sickle is a must for the crietallite orientation with respect to the fiber axis (C axis),

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The Ύ-orientation ¹¹ means the unusual orientation or the unusual material state in a body, which is recognizable by an X-ray diagram, in which, the (110) interference sickle at 20 · 14.0 ° intensity maxima at an azimuthal angle of more than 50 ° pointing from the equator. In comparison with the intensity maxima of the (022, 122) interference sickle at 2Θ = 28.6 °, the intensity maxima have a ratio of more than 0.6. This ratio (I * / I «^ is determined on a photometer radial curve, which is made with a microphotometer of the type" Leeds and Northrup Knorr-Alber Model 6700-P-1 "with a 0.01 mm width and 1.5 mm slot length The peak intensities of the maxima over the background scatter are determined as follows: For the vertex at 20 m 14.0 ° a straight line is drawn on the photometer curve, which connects the intensity values at 20 «9.3 ° and 20 = 11.3 °; one extends this inclined straight line below the vertex and uses your intensity value at the 20 vertex ale background value and subtracts it from the vertex value, v / oduroh the Qröese Iv * is obtained. For the vertex at 20 * 28.6 ° an inclined straight line is drawn showing the intensity values joins at 20 ■ 26.0 ° and 31.2 °; the value of this line with Soheitol is deducted from the Sobeitelwert, whereby one

dl «large l £ receives.

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Oriented fibers as with a ^ -intensity ratio less than 0.6 are subsequently oriented as "normal" referred to, oriented fibers with a ^ -Intensltäteverhttli-. nis of raebr than 1.0 are preferred.

"Latently oriented" is to be understood as meaning a structure that results in a ^ -orientation, if it is _{stretched 1 to 2 f} 5fuch and heated to οί> ° C for 10 minutes.

Under • 'heatest.aöiX "in connection with in the y-state""polypropylene iat au understand that the orientation angle changes to a temperature of 155 ° C by no more than 8 % at 10 minutes.

The "RUcicfecleiung ¹¹ (i" ucn referred to as TR) is the Pro8 # nt3t4tz over BaEnang % \ x by which a fiber goes back (all index number given), at SSX9 old 100 </ min "extended, 1 Min. On the Maxiauildehmang held ν.ηδ aasn sioh at the speed of 10Of Bebnuag / min, is allowed to erbolen. Unless otherwise close "give the counter values called the RUc! Suspension si'jä in dee second Zyklua on a tester 1 min. After the recovery e'er Cupids test according i'iedereinklemmung the Paeer Laset beet.

The ο "Ißcbgiabigkeltevör relation" (also ale Cii btaeiohnet) let equal Qlrxm fifth of the subtraction dt "Kohmertae ui'fiität" ffiodul9 at 5 $> Pehnunj von d ** t Mt $ '"*' t 4 ·· - 6 -

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ί! 6 5

tiiastizitStsmaduls feel 30% elongation obtained fourth and can through the Forn.el

are shown in which L, _Q and Lc mean the tension (in g / den) at the respective elongation. A high Nachgiebigkeits- verhältnls indicates a fiber which can be relatively easily stretched us 30 i "whose elongation at 5 £ but ft" et glelohe the force requires, for which a rubber band is an extreme example. A low yield ratio, on the other hand, indicates a fiber that can be stretched relatively more than 30 %, but by 5% more easily .

The initial modulus (also referred to as Mi , unit g / den) is obtained by extrapolation »by extending the starting point of the tensiona-strain-coefficient from 0 f strain straight to 100 % strain. The strength and elongation at break «ground in the usual units (g / den or f>) and printed out

dry samples of the Faaer measured. *

Am suitable for the production of the Faaer vegetables of the invention ο

netea polypropylene let hochkriotallln what off in sharp and ° * marked Röntgend iugrammen is expressed, and aoll pros ^m sugswelae a stiffness of more than 8437 kg / cni or

BATHROOM OFiIGlNAL

120,000 pounds / square inch (determined on test rods in accordance with ASTM test standard J) ^ 747). The polypropylene can do anything high molecular weight polymer with a Sobmelz index (determined according to ASTIi-PrUfnor "1958" -1238-57 ", part 9, p. 38) from 0.1 to 200 »preferably 0.5 to 50. In the preferred range products with significantly better elastic properties are obtained «

Xa (n) Di «" intrinsic viscosity ¹¹ is defined as - , where c is the

c ConsantratioD in Sraasm (0.1Q) of the polymer in 100 ml of des Löaungeaittela (Secahyäronaphthulin) and (n) _r the relative ViseoBität »deb. the ratio of 3or low flow rate of the polymer material and the solvent, in each case at 130 ° C., by means of a viscometer. Horaalerw @ lse an antioxidant (0.2 #) is added to both the polymer solution and the solvent »

The essence of the invention lies in the creation of a fiber made of polypropylene, not any particular process for making such a fiber. However, there are generally three critical points to be observed in the manufacture of the fiber, which for the sake of clarity and simplicity are specifically described below in The following are described on the fiber.

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(1) Spinnbadingubgcn

The Auepreeeune of the Paser should take place under such conditions that a y-orientation or latent potential / -Orientation is obtained. The variables in the spinning process are set in such a way that the Viaeoeität of the Polynerlsatsohnelse when squeezing;) from the spinneret and the deep

ooeitat of the fiber in the transition from the molten to the fixed state in the thread run can be regulated · With any } e camouflages conditions related to the type of polymer. SninndUsen dimensions, spinneret opening and polymer throughput becomes the y or latent y «orientation by regulating the Temperature and Jufwickelgeech speed achieved. the Temperature is a function of the temperature of the molten one Polycerisatee before pressing, the expressing speed, the three-dimensional shape of the spinneret and the degree of cooling or Brhltsung on the spinneret by must sugefünrte Warm or absorbent air. The right temperature control at The formation of the foot can be supported by using a cooling air quench.

(2) Orientation

The Imser should be oriented in a degree, the one Orientation angles of 10 to 55 ° are obtained by setting the spin stretching under appropriate suction corner conditions

(i.e. unfolding speed / calculated speed

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The polymer gate exit from the outlet opening) urtf or or the extension of the solidified fibers is selected accordingly. DIq stretching can be done in any appropriate condition, but the stretch ratio must not exceed 2.5. Preferred products are made without stretching.

O) heat treatment

This stage is important to making good stress deformation recoveries to develop in polypropylene. In the case of a paser that is produced under optimal spin conditions (bö that you do not need a separate stretching step), mtn can be used at Temperatures of 105 to 160 ° C achieve valuable products. In order to achieve better products, one should with a Working temperature from 130 to 140 ° »

If the fiber had an orientation angle between 10 and 55 ° before the heat treatment, this treatment results in a fiber with a y-orientation. su a heat-stable orientation angle of 10 to ⁰

The Paser is, εiah during treatment is preferably in a state that is free to shrink in the vie, wherein the degree of 3urcb treatment caused relaxation (shrinkage) is usually i varying from 1 50th 909808/0793

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The duration of treatment is not critical and can range from 0.6.

last up to 24 hours. The heating can be carried out in a separate stage, such as in an oven or autoclave, or continuously .

The following examples illustrate specific embodiments of the invention A uafiihrungü. In the drawings:

Flg. 1 In a schematic representation, a Faperrupinn- and -behändlungaroreinrichtung suitable for the production of the fiber according to the Er.firii.ung "

Fig. 2 in side view and in a veröeaerten Haaustab, sun part in the Yertikalechnitt, a spinning and quenching device suitable for the herotellun ^ the fiber gentiba the Brfixidunc, Fig. 2a a section on line 2a-2a of Flg. 2, Pig » 3 Stress-strain curves of broken fibers according to Examples 1, 2 and 3,

Fig. 4 shows two stress-strain curves showing different behavior of a Paser in guessing and other cycles on a test device for the springback,

Fig. 5 In. Graphic representation of a rüntjenciia ^ ramn, which explains the type of orientation, which is characteristic of polypropylene, and on which the shaped patterns are built up , and

6 shows, in graphical representation, an X-ray diagram which explains the "normal" orientation which is characteristic of the polypropylene in previously known molded structures .

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~ 11 -. - ^F

BATH ORIGINAL

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JLJL

Crystalline Pclyi ropylf η (Ochmelaindex 0.7, intrinsic viscosity? »7 ^>" ProiTöJc "of Hercules JErowder Co ,, Wilmington, Del., Y ₀ St.A») wif <ί. 1 as a melt of 289 ° C through a spinneret 9 ion 238 ° C (measured on the surface), the solidified P ^ dengut is operated via the feed rollers 3 and 4 at 41 m / min are, and then guided over the stretching rollers 5 and 6, which run at the same speed, and wound up on a conveyor 7. The spinneret 9 has 34 outlets from O _f 3S on the Surchmeoiier to _s which are offset in a pike of 25 × 4 × 4 × 8, as in *% § «1 all ^ emain at A and in Figs. 2 and 2ft shown in detail, is arranged perpendicular to the surface of the iJpimidUfle 9 a Abaciireckvorrichtune which has a tube 10 x 19f1 ffici outer diameter with one x number of iiksjh ^ rn of 1.6 mm length, which the air against the '''linden of the * 11 is provided in which the tube Zylinderkemraex, the F ^ align with the exception d # r denlauf facing wall. On the wall facing the Fadon run, the chamber is provided with a 20 ° near sieve 12. Pressed through the tube 10, BUf meets the fixed walls of the roller 11 and is connected to the thread path through the sieve wall 12 facing the powder path

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deflected towards the tube 10 is supplied with air at a rate of 51 l / min. Dee wound up in the tense fora on the pack of 7 Fadengut has a total titre of 1409 the »an orientation angle of 22 °, the γ orientation and a y intensity ratio · - nle of 1.5

The physical properties of a sample of this padding material in the erect state without further treatment are given in Table I under IA. A large sample of this thread material is sewn onto the strand and treated in an air oven for 10 units at 135 ° C, so that the fiber would have a stable orientation angle of 20 °, the γ-orientation and a Y-intensity ratio of 3, It is an example of the preferred embodiment of the Krfindunc ₍ and its physical properties are listed in Table I under IB, where the initial modulus for each sample is the strength and the requirement for a stress-strain test of zero strain The stress-strain curves of samples IA and IB are shown in Fig. 3. Sample IA has a yield ratio of 7.2, sample IB of 9-1.

BATH ORIGINAL

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1H

Samples IA and 13 si \> d identiach except daoa IB is heiauentapannt. Table I shows that both samples, with the exception of the fire odor, have similar properties. Sample IB has an excellent TR25 ^of ^ 2 fit. Sample IA, on the other hand, has a very bad 5? $ »It is surprising that the helo relaxation can lead to such a drastic change in the springback»

The same polymer as above is pressed out through a spinneret with 3 outlet openings of 0.51 μm diameter, the thread material is quenched with air as above, which is supplied at 28 l / min, wound up at 430 d / ΙΙχπ »and then as above Heisssatspannt, The thread obtained has the γ-orientation, a väraestabilen orientation angle of 14 ° and the physical properties according to Table I (sample IC). This Fadeiigut illustrates a preferred, specific Ausführungsforo of the invention and has after 25 elongation (in aweiten cycle bestinot) auäfezeiohnete a resilience (94 $>) °

In the present example, the fiber is not stretched and the orientation through the spinning conditions causes «sample IA clearly shows that the Paoer according to the invention DOOh is not obtained if only the orientation angle

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in this area reads »der Orientierungswinkel muse also be aerostable in connection with the high springback with the other good physical properties to get » which are characteristic of the fiber geraäoe of the invention.

A special peculiarity in the behavior of the elastic polypropylenes according to the invention is explained in FIG. 4 on the basis of both stress-strain curves. D'ieec curves have been made on a lirobe beetinut which was produced like sample IB and is essentially identical to it. They 1 robe is expanded in the first cycle to 50. i 'stretch and then allowed to recover at standard conditions, üie is then clamped to the "wide cycle back into the tester and extended to sum Bruon. As shown in FIG. 4 aeißt, the fiber, however, results in the first cycle a Hachgiebigkeitsverhältnis of 5 _f 6, in the second cycle the considerably higher '..ert of 13.3. In the 0 »third and in the following cycles the fiber behaves as in the ο second cycle if the fiber is relaxed in the

When water boils, it returns to a form in which it 01

ο first a behavior as in the above mentioned first cycle and et then the spreading time as in the above-mentioned second cycle. Dleees behavior is more or less strongly for the ^poly: propylene gemäsn the invention characteristic and provides the reason for this is to relate the RUckfederungewerto on the second cycle. Other polypropylenes of the invention

Hahaieno could hold iiica similar to vi'j.

BAD ORiGiNAU

Tabel

sample Total ~
. stretch
hold up-
nis Heisa-
un-
span
nuffg IA IX te ine IB 1X 3a. - IC TX 3a HA 2X 3g 113 4X 3a no 5X 3a HIA IX 3a IHB 2X Yes HIC 3X 3a. HID 4X 3a IHE 5X 3a HIF 6X 3a

Orientation WisikgL Art

22 ^V

20 * 14 <25 ⁽ 13 «12 ⁽ 180 * W 13 ^{ 11 * 14 ⁽ 14 ⁽

57 92 94

.normal 78

normal 63

no 58

γ S6

normal 7o

normal 66

normal 60

normal 57

Fe-

Btiß-

kelt, fi / den

1.3 1.1 1.9

4.9

5.5

Phyeikaliache Sigenaehaften ürucn- Anrange- caaerdehmodul titer, nung, g / den

650
620
455
215
45
27

10,
8.4
10.3
10.5

SC?

41 43

15th

21

13th

to

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Table I states, for example, for samples IA and IB Wb «te de · IBL · - of 57 and 92 #», these values being valid for the second cycle. Based on the erotic cycle, TR ₂ ^ of samples IA and IB is 50 to 90 <£. The values obtained in the third and subsequent cycles agree with those of the second tone.

Pig. 5 shows a graphical representation of an X-ray diagram of the fiber, the tension of which is 3-strain and S-curve in Pig. 4 is shown. This diagram clearly shows the γ-Orientierune and is for the Iolypropylene from which the fiber e ^e "nuées the dung iat constructed characteristic.

B i a p 1 e 1 2

This example illustrates the effect of stretching the Faeer, which in view of a good elastic behavior in the preferred area of a springback of j and “or rather torsuce welee is not stretched at all. However, no special coating is allowed, although if the draw ratio is too high, the fiber with Y-orientation and the extraordinary springback will no longer be retained according to the invention. A stretching ratio of up to 2.5 is acceptable, even if it is not preferred. ^ "^ r ^ $"

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The procedure d-ea example 1 is repeated with the / banding * that the thread material from the feed rollers with 41 m / min, is continued and the stretching rollers are operated at higher speeds to achieve various stretching characteristics mentioned below.

The sample HA according to Table I is a fiber that is stretched twice in air from room temperature, the sample HB is a fiber that is attached to a metal rod (not shown in FIG. 1) with a diameter of 2 1/2 co., Which is between ' the feed rollers 3 and 4 uod the Streok rollers 5 and 6 is arranged "at 100 ° C and in a 360 ⁰ -TMole is stretched four times, and sample HQ a fiber that is stretched on a metal rod from 60 ° C to five times has been. Each fiber is "hot-relaxed" by heating it to 135 ° C for 10 minutes in the de-energized state, and then determining its physical properties.

Sample HA is a fiber according to the invention, which however does not belong to the preferred embodiments and, as shown in Table I, has a TR25 ^of 82,56, which corresponds to the lower limit of the springback of the fiber according _{to the direction.} However, if you increase the stretching ratio,

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with other essential conditions remaining unchanged, the fiber no longer has a γ-orientation and TH ₂ C falls far below the minimum of 82 * (cf. HB and HC in Table I). One must therefore carefully impose restrictions on the conventional practice of stretching to increase strength and initial modulus in order to. the pasers of the invention so come

Fig. 3 shows part of the stress-strain curves of the IYobe η HA »HB and HC. ^ robe HA has a compliance everhaltnls voo 5.2, while the curves of the two 'other specimens in each case a very low V / ert of the compliance β ratios « demonstrate. The contrast between the curves of samples HB and ΙΪΟ on the one hand and HA on the other hand is very clear.

6 shows a graphic representation of an X-ray a fiber that is largely the counterpart of fiber HB. Ee shows no γ-orientation and shows one Y intensity parameter of only 0.02. The HA fiber of others » on the other hand shows the γ-orientation and a γ-Intensltätsve never from 1.6.

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ίο

Q- (J 31 Be io pi e 1 3

The procedure of example 1 is repeated with the modification, dnsis nan uses a spinneret that has an outlet = Has an opening of 0.76 mra, the Abachreckluft with 54 l / Hin. feeds and all four rollers operate at the same speed eo that the thread material in the spun state with 198 «/ Min. is wound up. Dae ereponnene Ilonofil (IUA in table I) has a liter of 108 den and an orientation angle la ereponnen state of about 180 ° (wae shows an almost completely unoriented structure), but knows one latent γ-orientation.

Part of the flute, β-stretch and s-curve of the pad is in «■>«

Fig. 3 is shown as IIIA. The compliance ratio * "* ■ of 16.5 lies outside the range of the Paser ^ em of the invention · <$

After the above, one divides in the spun state * present thread material is produced, the drafting rollers eo that a double stretching takes place in the air, and Deactivates the product (IHB in Table I). share the product are then in the air additionally on Goaamtstreokverhfiltniuae of 3 »4, 5 and 6 (samples IHC, IIIü, IIIν b «w. IHF) stretched. It 'intgen diagrams of samples 311G through IHF

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have no γ-Qrientie r \ in &. A microphotometer curve of samples IIIC and HID gives γ-intensity ratios of only 0.20 and 0.12, respectively.

None of the samples IHB bio IHF in the spun state has a TR ₂ 5 ^{that reaches 50 Ji. A} portion of each sample is made into a strand and heated for 10 minutes at 135 ° C., with the TR ₂₅ values according to Table III being obtained. The sample HIB ■ divides; a faeer according to the invention with a very good M ₂₅ of £ 86. None of the samples IIIC to IHP are in accordance with the invention, and the heat relaxation is also unequal su- ^ Ιη, ς? Improvement of the springback leads (see table where> over d * e fR ₂ c eotar the sample IHC well below the UInI- ▼ op 82 K! Redeems. Indeed, the sample is subject to HIC

at 25 pounds of elongation a permanent elongation »which by more than. I "is greater than that of the Paser IIIB 72, which drastically

Welue explains the loss of elastic behavior »der when stretching the riser 3 times instead of 2 times.

IHe sample IHB has a compliance β ratio between the limits 2 and 15 and a stress at 5 ','·> elongation between the limits 0.1 and 0.6 g / den.

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Example 4

This example explains that in order to achieve the parameters of the invention, not only is the thermal relaxation required, but that a heat-stable orientation angle and a TR25 ^{must also be achieved within the} scope of the invention. Furthermore, a drastic thermal stress (150 C, Table II) can also be harmful.

Strands of the Paser HIB from Example 3 (made from the stretched, not yet heat-treated fiber) are heated in an air oven for 10 minutes to various temperatures in a tension-free air. Table II shows the springback of 25 '£ elongation (TRgc) in a wide cycle.

tab Hurry II * TR ₂₅ Treatment temperature,
⁰ C 42
5u, 2
76.0
84.2
87.9
75.1 ■ ^; i "Bp
110
120
130
140
"1·
150

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Bets pi e 1

This example explains the production of five fibers (VA to VE n-ch Table III), all of which are examples of preferred embodiments of the invention. These fibers have excellent springbacks of at least ' B? Ϊ the γ-orientation and heat-stable orientation angles from 10 to 21 °. The fibers of the present example are not stretched «

AoT of the device according to Example 1 will be different polypropylene · ve: Spönnen, with the supply and Utreckalsen adjusts so that no stretching takes place and a tightly stretched ·· thread material is obtained. In all experiments one Similar to SpinndQee as in Example 1 with 34 holes of 0.30 op Diameter used, except for dor irobe V-C, for the ■ used on a spinneret with 30 holes 0.36 mm in diameter »those on a circle of 2 1/2 cm in diameter are arranged

For samples V-A and V-B, the polymer! Eat according to Example 1 For V-C, a polypropylene with a melt index of 15 (obtained by heating the polymer from Example 1 to)

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a screw press in the presence of tert-butyl hydroperoxide to 230 ° C and then. Addition of 0.1> 4,4'-butylidenebis- (6 ~ tert-butyl- »m-kresüi) used as a stabilizer).

The polymer according to Example 1 is extracted repeatedly with boiling n-heptane of the commercial grade until about 8 Gew.ji are extracted. The iTebe V-D is manufactured with the residue, ·.

sample V-E becomes a crystalline polypropylene with a jS: cl (m ^ lzindejic of 0.18 ("Escon" of En jay Go., Inc., 1 ^ West 51st Street, New Yorkj TT. Y., V.St.A.) are used.

Table III lists the physical properties of the relaxed fibers after 10 minutes of hot relaxation at 135 ° O>

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! Table IXI

Sample spinning conditions

V-E

VI-P

VI-G ⁺

VI-TT ⁺

VI-I
VI-J
VI-K ⁺

VI-M

VI-N
VI-O

Spinning-Ab- Atffdüsenschreck «wickiempemedium *. lung _t
ratur, l / min »· m / min,

⁰ C. ... ■ ν

Orientation angle type TE,

290
290

270
290
290

295

295
295

290
290
260

250
250

280
500

102
190

190

102

74

45

102

170
57,

170;

170

102:
102

125
138

91 y "
91.

165 "

32-

n- 91

.9 *

λ 25
274

224

¹⁶ pp

10-21 ° 14 ° 15 ° 11 °

10-21 ° 18 °

10-30 ° 10-21 °

10-21 ° 10-21 °

10-21 °

Y Y normal

Y Y

normal Y Y

"• .Υ ;. Y

Y normal

Physical Properties

Fractional initial Baserdehming ,. module, tit he,

ability, $> g / den

g / den

1.6 1.7

1.3 1.7 1.9

1.2 1.6 1.6

1.2 1.6 1.6

1.8 2.0

1.0

480 396

147 342

190

497 520

414

477 469 4-17

312 243

509

10 7.5

10 ..

12.3 11.5

10, Q-9.7

9.3 9.3,

, 7 13.0

12 13.6

4.4 12.5

Ϊ6.6

18.5 ^ 8.0

03.3

13.0

10.7

4.1 3.8

■ 7.4

ο
«Ο
co

^T 5 All these fibers have compliance ratios like 2 and i: \ tmd- ^ r yield
Stresses at 5 i » elongation between 0.1 and 0.8 g / den.

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Example 6

This example explains the production of ten fibers (samples VI-F to VI-O of Tobelle III) using various variables in the spinning process and the effect on the inherent fiber properties. In all cases, the polypropylene according to Example 1 is pressed out as a melt at 289 ° C. using the device according to FIG. 1, the support and stretching whales being set so that no stretching takes place and generally unstretched thread material is obtained. All fibers obtained are & egg? same warm relaxation »ie TO Min. in an Of @ n τοπ 135 ° C in a stress-free state, subjected«

The? A @ e? » Vt- ?, YX-G and VI-H are produced in an identical manner "old of the modification" that the deterrent air of 21 ° C old ÖöSöti speeds of 45, 102 baw. 170 l / min, is guided. The spinneret has 25 holes of 0.23 mm Duront & esser »which are arranged in a rectangular pattern. You Table XII se igt the significant increase in Küekfederisng, one with an increase d © r ^ aäohwindigkeit the cooling of the pressed fiber in remaining constant for the rest Bedingung® "receives" Di © Peeer VI-F is significantly aass®rhalb dee the Srfinaung "

26 -

ftOeeoe / 0793

U35621

Q-631

Fibers VI-I, VI-J and VI-K are as above with the modification Manufactured because the spinneret had 40 holes of 0.23 now in diameter in a similar pattern to the spinneret used in Example 1 and the head of the quenching chamber 11 (yig. 2) calibrated 2 1/2 cm below the level of the surface of the spinneret 9, but with the air supply and the spinneret device changed according to table III «earth. This arrangement of the Abeohreckkammer is the fiber cooling to a certain degree delayed, and the Faeer VI-I lies well outside the range according to the invention. Even when using the same air supply (170 l / min.), At which the optimal fiber VI-H is obtained, only one fiber (VI-J) falls in the non-preferred one Scope of the invention at * The splint temperature must be on 260 ° C can be reduced in order to achieve a Faeer (VI-K), which see in addition to the desired elasticity of the Feser VI-R approaching

The effect of the angular velocity alone is explained by the fibers VI-Ii and VI-M, which are spun from a spinneret which has 34 holes of 0.30 mm diameter arranged in rows, the quenching chamber according to FIG. 1 being used. The higher winding speed when spinning the fiber VI-II leads to too rapid a cooling of the thread run, and as a result the TR ₂₅ falls from the 90-jG value of the fiber VI-L to 65 pounds . ^ '

- 27 - 9089Ü8 / 07S3

U35621

It

The fibers VI-N and VI-O explain the effect of a combination of variables in the spinning process. The fibers are spun in the same manner as fiber VI-L except for the spinning conditions (Table III). The fiber VI-N represents a preferred, specific embodiment of the invention, while the fiber VI-O, at which with a higher spinneret temperature, a lower quenching intensity and a lower spinning speed, ie conditions which tend to lengthen the cooling time, with a TR25 ^{of only} 55 ° is far outside the scope according to the invention and has no γ-orientation. ς ^ & Λ

B e 1 B ρ 1 el 7

Using a spinneret, make 3 holes of 0.76 mm in diameter has, according to the procedure of Example 1 is a Spun a bundle of threads, but to deter the air with 25 l / ml. feeds and the feed rollers 3 and 4 with 173 m / min, and the drafting rollers 5 and 6 with 241 m / min, operates « The three drawn filaments obtained are separated and wound onto separate packages. One of the packs is processed further in the present example and 30 MIn. heated to 130 ° C, the thread, since it is in the pack form is present, is under tension. It is usually preferable to heat the thread material in the de-tensioned state To let UQd shrink arbitrarily, but the so-called "goods relaxation" occurs in the present example and the

909803/0793

- · - 28 ™

IS

Attention to the maintenance of a certain shrinking capacity in that Thread is desirable here

The thread then becomes conical in the conventional manner The bobbin is opened and processed into a stocking on a 400-Radel single-feed seamless knitting machine at 173 rows / dm. and toe pieces employing commercially available 66 nylon yarn. Bas work takes place under the normal conditions for 66 nylon with the exception of a lower feed tension of 0.5 g · Bas stocking knitted fabric is trooken on a conventional metal mold for 15 minutes in air at 150 ° C, with a shrinkage of 14 # results in · Mach de «dry molding, the knitted fabric is washed out at 90 ° C, rinsed and dried«

The goods received in this way are of good quality and are » as shown by high tongue expansion values, in terms of stretchability, knitted hosiery made from normal polypropylene yarn as well 66 Hylon thread remarkably superior. It resists expansion deformation as well as the 66 nylon goods and lots better than the goods made of normal polypropylene «

The following table IV shows the strength and elongation of the yarn samples taken from the "knitted stocking and the values determined on the stocking in the manner described below. ^^ ^A -Song expansion values"

'. 29 - 90980 & / 0793

! 435621

Tabel

IV

Strength, g / den

(1) Stocking made in the 2.03 manner above

(&) Derived from 66-N2rlon-Öarn . put stocking

(3) Made of itolypropylene thread

normal orientation hll stocking

3.67

Stretching, tongue. $> expansion,

241

59
56

22 20

That from the finished, in the Gbenb @ sahrieb @ nen way The polypropylene yarn that has been preserved is made of stocking

and has a heat-stable orientation angle

from 10 to 3O ⁰ mä

genes of the invention

^ c

82 ^. 3Sb thus represents a fiber

The Zwngenausdehnwert® mentioned in table IY are beatimiat *, however, the inner diameter of the stocking s in dea Knts forms part obn0 Spasaniing (B ₀ ), with a tension of T g (D «) and with a tension ^ ß» 101 g ^ 1O1 ^ ^ ^fiS ^ · '^^ ^e Spasnung wiyä auf ·· _: the Strusapfismenseit® aiitfcels 2 1/2 χ 2 1/2 sqm large chaat aur linwirteuug broken, dis flexible with the hands' bars sit «di @ lhrer @ eit @ about-in Him -fathers.

¹⁰⁰ ORiGiMAL BATHROOM

U35621 Jf--

! The above examples are for explanation purposes only of the invention, generally comprising a polypropylene fiber jff orientation and a heat-stable orientation wijqjkel rdn 'IO fcie 30 ° includes

Xn the examples, Saharan lasers not falling within the scope of the invention are described together with their production, inter alia dl · effect τοπ show changes in various process conditions sa. Such do not fall within the scope of the invention falling fibers do not need to be state-of-the-art » but they can all be new. The most obvious stand ' de? Technology was allowed to "ground" from example 2 of Australian patent application 56 854, depending on which polypropylene yarn 3 »5faöh is treetoped» whereby the stretching ratio itself then it would be too high if one had other conditions according to the teaching of the present invention would apply * The example is like this In general, by changing or applying conditions that are not mentioned, one can fiber with the most diverse Properties and does not teach anything about Action without harm. Following the example is the yarn product "very voluminous", which also applies to the yarns of the invention, their preparation in the examples of the present application is not applicable. To reduce the volume of the faeern according to the examples of the present description would be more

A necessary «

- 51 -

909808/0793

As mentioned above, seigt Fig. 5 a graph showing a Rönügendiagramsa a polypropylene fiber with -f orientation in Rahman ö © r invention, and Fig. Β is a similar view for © ine polypropylene fiber, which does not fall within the erfindungegs & äesen Rahman and instead of a y- Orientation has a normal © orientation.

For the y-orientation the interferences 21 are characteristic, which in the representation according to Pig, 5 on the circle 22 (2Θ «H, O °)

lie below the azimuthal angle of more than 50 ° from the equator 23, there are no such interfexes on the ki * © i0 22 of the figure β. The orientation angle of the fiber is determined by the part of the interfereaz 24, which is centered on circles 25 (29 «16 _e 7 °). The higher crystallite orientation in comparison with Fig. Δ (13 °) is according to Pig. 5 (16 °) 2SU. The interferences 26, which are typical for all oriented polymakers, are of no interest here. The interferences 27, which lie on a circle 28 (20 = 28.6 °), are used in determining the intensity ratio. The diagram is divided symmetrically by the equator; the meridian extends through the middle of the bitegram and forms a right angle with the equator '.

Those skilled the difference is swischen the diffraction patterns of Figure 5 and 6 _o eye-catching and much more. the

... 32 BAD ORIGfWAL

. .. _: -. .909808 / 0703

U35621

Q-631 JS

Interference 21 according to rig. 5 are unusual and leave the unique crystalline structure of the polypropyl fiber according to the invention is immediately apparent.

The elastic fiber according to the invention possesses an extraordinarily favorable combination of properties, of which an elasticity previously unknown in polypropylene fibers is particularly outstanding. Example 7 shows the use of the Paser

according to the invention in hosiery. The fiber is suitable very good for purposes such as automotive upholstery, seat covers and the like, since the fibrous materials and fibrous materials obtained have an unusually good shape fidelity or shape retention exhibit. Pater's policy for non-woven fiber materials is also advantageous, as these in turn get a good shape accuracy or shape recovery.

Further embodiments are within the scope of the invention.

909608/0793

Claims (1)

Q-631 'Jjthxy Patan't an s pyjie he ίΐ oj BlastO! B @ re Polypropyl € nfä @ er _v kernteiohset duroh a y-Griaatiörurig and a wäraeetabil & n orientation angle from ΊΟ to 2 · fiber ma <slJ. Aigesprueli 1 »marked durcli oitiöii Orien- vtrn 10 big 21 ° and a y ~ Inteasitat ' of na @ k Aneprueh 2 »known without a spring suspension U $ $ gluing in the second and the following cycles at least 85 ^ β BATH 34 - 80980870793