DE1435610A1 - Artificial thread and manufacture of the same - Google Patents

Description

Ε »I. DU PONI DE NEMOUES AND COMPANY 10th and Market Streets» Wilmington 98 ₈ Delaware, VaSt, A »

Kunstfadan and making the same

The invention relates to fabric yarns, particularly improved composite crimped yarns, and the manufacture of the same

In the development course of Sextilkunstfaoerindustrie has taken great trouble "fiber to achieve, in which the known benefits of synthetic fibers such as light maintainability, durability and improved mechanical properties retained, remain _s but which at the same time necessary to achieve aesthetically extraordinarily attractive textiles Have properties that are characteristic of goods made of wool, for example *

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Woollens have © in © good © VolutBinosität and Beekkraft and are equipped with a "" rerhältnismässig low shrinkage Eertigmaehen avai © h ₉ which is very desirable in economic terms, "Wool Products have also excellent elastic properties, such Streökbarkeit, elasticity b © i ZiasasHaeBdrüökrag IMD - Jerkiness and a pleasant grip on the surface. Sehlie-seliish is the surface yob W © llwar © n © rsKsaerbar % seifest Ka © 3a äerart stai'ken Defor = · laatioaen like 'I @ sdrü © kuag or appearances το »Pressglanss lets ice Easily create a n © u working © surface by dampening the Was® fe®f © weh't © t ₉ or simply letting it relax in the damp “air”

Ee are versehiedesi © paths ¥ ®rges © lilag © n been, 'where the m ^ tars 3Sigeraart © H won Wool Products obtained © IIaE © but, in kaiEiera case are those Kunstpr © dlukt © in actual Sisin © than more than yoursr © b @ rfläQhli © h © n Besshacity- according to kind "bets ¹ respected ■ - ■

One has ¥ ®rg @ s © hlag® », sur der W®t <& i © n - synthetic fibers ® ± me β l © _no - fiber» of this kind in conditions or? .. Hachb @ handlu »iig © n Sound of a 'single .... component g> conjugal sialic symbols

of properties

-to be granted
special spinning = w © l @ h ©, on which _: Quers © hni-tt, threads unterohie.dli? » , © the. by To =

909807/0730

Λ ~ 4ϋ? / 408

Arm spinning of two or more fabrics ku a composite thread _P d. ho a thread was made, which the grain = »

components in a awf regarding the thread cross-section eccentric arrangement contains If the two components of a Yerbundfadens have a much different shrinkage causes the different Very vaccination of erspon "nenen and stretched components © ine Ripple ₀

Before it was proposed to produce curled composite threads from synthetically formed polymers, which are capable of changing the amount of crimp when exposed to a swelling agent and to take on the original crimp again when the swelling agent is no longer effective. For the sake of simplicity, this self-sufficiency is referred to as "reversible crimping" and is expressed in a "sieve winding" of the thread upon both application and removal of the swelling agent Kum. 3) The level of this irreversibility of puckering is shown by the ability (5 ^ r threads of yarn in the textile goods, B ± eh under #era Einflur-ji clnna Qiielmittel such as water (and cbeniHlla get removal of the same) in the ¹ goods or { '! Jt'ehöiiti to move afrsr trotsciera with removal of the QueXlnittala, as by OirocLiienp in animal goods the origin "Hch ¹ ·, ripple again iUiHtmehmen", goods which ^{contain this thread "3} ·; ·) _r obtain" to ö -Around the swelling treatment a star! to full heat declaration force and maintain this or

909807/0730

they even accept it even more if they are repeatedly subjected to such treatments _o If the shrinkage during finishing or finishing is low, yarns in such threads have a relatively open structure, so that the goods show unusual elastic properties »

It has wiffifäg jeiosji found that the high degree of curling in the fibers, which is required for the production of yarns trad goods with good oluminosity ₉ good elasticity with compression, good pulp preparation on finishing treatments mad good recovery of Pregsglanss ", is generally required by one high Kj; äUfjir # lfr @ quensi (or crimping often = k © it) is accompanied »This high crimping frequency leads to a harsh, scratchy (Ja'iff von Wijrk == and woven goods and ? M difficulties" in batch processing, what how « which results in a bad iFleiühmäseigkeit and a high Gf ar η.

The inventor α Big puts a crimped composite thread at the disposal of the © In © gcmüg «jiid high sensitivity to noise has _P um (Sine gti -?;: I Krlioluiag before * vej: di © hteud τ / acting forces and the Äusbildimg © inser good ¥ olmminosity and opacity in the Vi'are to he leg _r miä shows a degree of ripple , tier la the V / are © in <sn augQUQlitmn vrollasrtigen & riff results »

90980.7 / 07 30

A-4Q7 / 4O8

It also provides a method aur to reduce the degree of curl of a composite thread while a given The degree of pucker reversibility is retained.

The synthetic thread according to the invention is characterized by 10 to 18 helical crimps / 2 1/2 cm (1 inch) extended length and an equilibrium a crimp reversibility from 25 to 50 #.

In the method gemäas the invention, two fiber-forming materials are simultaneously jsu a composite yarn spun and thereby _s which give rise to a rapid erection of the fiber structure under conditions pressed into a spin cell "The composite yarn can be due to the eccentric relationship zwischen'seinen components and the composition thereof, to curl when shrinking from the straight state and has the property of curling reversibility.

According to a preferred embodiment, the polymers are Components so angsoxdnet that the edge of the bandage thread, which has the low shrinkage component, for Center of the spinning cell, and the thread edge, which has the higher-shrinking component, is directed towards the circumference of the spinning cell.

- ⁵ ~ '"" see ORIGINAL

909807/0730

A-407/408 '■. ■ ·' ■ "■ ''"

A further embodiment is used for the polymer 'which provides the homo thread with a lower shrinkage' · _s a spinning solution of lower concentration than for the other polymer · = * "component"''"·

ErgeDen i under the conditions which a rapid Aufrictotiiäi gram of the fiber structure _s siad high gas = - and cell ntempe rat acids -, - höh © .ßasstro'mu'ngsgeschwiiS'digkeiten- -and: low SpinngesQhwin · * = digkeiteri. to understand. These Beiliagaagea lead to a low solvent residual gelialt of the yarn during dry spinning. When driving according to the invention, a solvent = Hestgahalt in the range of 13 "to 25 $ for a single thread = 8 denier in the original state "received (equal to 'O ₉ 85 part: ₉ where .te: s the fiber = -""bsw.I'adeiigev / ieht in? for 1", ö km. "means)"; The solvent solids content _s "obtained in ⁵ other 'KTtern, can easily be seen from the I ¹ Ig. 8' in. Which 'the. the curve shifted against this curve - 2 the preferred ^1; Solvent = icing content for the various Padentitef figs. '^;' ^: ""''· ·· ■ ·. ■ - <: · ■ ·

Die.feäuselrevereibllität vder forests according to the invention v? Ird, following ", test determined s - · ν - --... * - .... ^ v ₅

■ A-407/408

A single thread is separated from the thread or cable of the stretched, non-relaxed threads. A 7 * 6 cm long piece of the thread is io attached to the opposite sides of a rectangular copper wire frame in a slack between the ends of the 30th The frame and thread are then boiled for 15 Mira to develop the curl. The crimped yarn is then in a piece Speaialbetrachtungshalter did so by eetl''igt the ends as with tape or glue J * _s that an about 10 $ IGEX slack is present and the yarn length between the clamped ends approximately 6.4 cm "beträßt The thread and position holder are then placed vertically in a plugged test tube which contains a dehydrating agent. The tube is kept overnight (18 to 24 hours) in a vertical position at 70.degree then brought to the cleared temperature (about 25 ^Ö ) "Man Ifisfät 50 min. cool down", and then counts the total number of curls in the thread between the fixed ends. In the case of a kieser count, all curls are ignored removed from the glass, filled the glass with water and stored vertically for β hours at 70 ° C. Then oil 2 × the crimps in the wet thread as above. These conditions are repeated as often as is necessary to obtain reproducible results.

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A-407 / 408-:

tion in the Krauselsahl / 2 1/2 cm extended length of 25 ° dry to 70 ° wet is calculated from the following equation = nets

the ripple ^ J ^^^! ^ * ase), _χ

Number of crimps egg exlitat ₍₂₅ Ö _troofcen) .

On the other hand, you can also work with the actual change in the number of frills / 2 1/2 cm extended length from 25 ° dry to 80 ° wet, expressed as / S frill / inch, and calculate as follows?

Equilibrium curl = number of frills / 2 i / 2 cm / V frill 1 / inch. ^ Μ ^ ΣΜ ^ λ ^^ ^ aua ^ e he stretches X

100

Under "extended length" is the length of a thread or Yarn "at such a tension κu understand that the crimps are pulled out and an essentially straight thread or a substantially straight yarn is obtained. All curl numbers ■ relate to the extended length "·

Another very important property of the threads according to the ",

Invention consists in its ability to "self" from condensation

to recover. This property is determined here as follows. ι * ■ "* ■■■

90 # 807 / Q730

143561Ö

1 = 407/408

Curled leaden is cut to a length of 5 »1 om, carded by hand and pellets weighing 0.120 g are made. The pellets are placed in a cylinder (bore 1.5 cm in diameter) under a freely sliding piston which _{exerts a pressure of 70 93} kg / cm for 2 minutes. The height of the pellet is measured under the pressure. Pressed pellets of the same fiber are removed from the cylinder and (Ί) ä in dry air overnight allowed to recover and then placed (2) for 5 min, to the action of steam from Atmoaphärendruck. The height of the pellets recovered after treatments (I) and (2) is measured and the recovery from compaction is calculated:

Amount of the recovering- ^ Amount of the together .-- üruoiung *> ^ i ^^ 'i - ^^^^^^ Q ^' t ^^ f ^ Xetr ' ^{x ιυυ}

The invention is explained below with reference to the Dry spinning «! of polymers of acrylonitrile in dimethylformamide in a special Trookenspinnssellerityp "described The practice, the device and the method are of course included the invention wide changes s

One works with a closed spinning cell, the one has a cylindrical cell, over which a "spinning head lies" The cell is vaporizing with a means of circulation

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1-407 / 408 - ■ ' ^: . :

effective medium through, the cell "which it through, the spinning head" enters around the threadline * a means which shower the solution, squeezes the spinneret into the head, and provided a means _t -which let the sam dtircu. subtracts the bottoms of the cell; O-

The head tempera-door is clio (temperature of the gas "when" exiting the GöBh, eiS! V6rriö} itiins tind irox the entry into the spinning cell

Spirinaelleiiwanc! ·, .. ■. . '

In the drawings, s "■."

Hg ο 1 a «» .Mittelctuersölinitt ■ by © ine spinneret arrangement die-bei cer Hersteir.in _; j; cl ^ r TerauiiaiäfleB geaiaäs the

.? ig »IA art eiwei 'Darstslli ag ei.iCi;?. Part iron Kg 1 in large te w "Masfistafe ßliiBe ^ / ieiteu eggs Spi:.. Anäüse an d ^A he Off · = _..

kickaöffnußgj, -. - .- ■■ -. . - - -.

Iflgo 2 in the section nash. L.irde 2-2 of the Fig. 1 details of the

Head of the ilückplätta ,, ..

3 im -Söhulti aaoh ϊ, Χινίβ 3-3 tob "Pig .. 1 Details of the Boctena. The .backplate ,. ' . ■ .. ".- ... ..

to- ■:. "*

9O98Ö7 / Q730

ΛΑ

A-407 / 4-03

Fig * 4 i ^v i the Pig .. 1 corresponding view a spinneret anoidnung, with which p.ieh composite threads on three concentric circles, can be spun _t

¥ ± g, f> VLb 7 in greatly enlarged sections perpendicular to PadenaohiH-- typical .gen £ .as the invention by dry spinning generated Päden, wolcd a component hatched "eats to ..Ie Irennuiiis awiachen the components zn show ™ and

1 & -8 JLY; ο enclosed graphical representation (with the Löü'-tigiii'-lttel-Ues'ugehall in percent as ordinate and the exi? {;> uiίο if; η IPs-Uenlittsr in! Denier a, ls Absaissen values) ο

iü ipiiT / idüyer.bod &nplat'e 2, which holds a rice from Ausittsöfft: ur- _t ;? a 5 ei. · ", .vi d via retaining rings 12, H and a boIi = .Ii i '* l au der . _Rüolr%> l tie 1 held "plate between the spin ^ and is Rückpl- tie \ is a spacer as the -'an.'α i f --- iir-iaechiiiße-?.. i'iah 4 fs "B. with 200 stitches / 2 1/2 cm; under Indruoic Hie Rück ;: latte 1 contains awei ring chambers 8.9"which; : - and the filtration system are connected (ni'lt ö ^ iigezei clmet). voi the Rir.gkammer 9 lead guide bores' 1 Kuju back room 7 u?.: d in front of the annular chamber, 8 guide bores 10 itin fc. ngxauit 6. The spaces 6, 7 are covered by the wall 5 which is above the opening 3 and the screen 4 is kept at a distance from the spinning mat 2 so that the screen 4 is kept at a distance

11
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A-4Ö7 / 408. - ■■; ■

the flowing spinning materials freely and against each other can _{pass through the openings 3 through the annular spaces 6- s} 7. The meshes of the screen 4 are fine enough to allow the spinning material 3 to pass through the openings 3, which is shown in FIG. 1A shows.

FIG. 2 shows four guide bores W ₉ 11 at the same distance from one another within the chambers 8 and 9 6, respectively

Fig. 5 shows the concentric inner and outer spaces = annular spaces 6s, 7 and the 'fine-meshed sieve 4? a part in the cut -

The Bstrieb the obenbeßchriebenen Torrichtung lead in by the invention is easy · = ₀ aii understand the inner Ringkamraer 9 and the ausseien Ringlcaiamer 8 of the back plate are fed geeorxcierte textile fibers; the first-mentioned spinning material flows from the chamber 9 through the Iieitböhrungen

11 into the inner ßingraum 7 and from there through the "'Si ^ b- 4

and the opening 3 to form a Te ils the composite thread, while the second-mentioned spun material au by the Leitb.ohrung 10 the ausseien annular chamber 6 and then through the screen 4, and "the outside of the Austrittsoffuung 5 to form the other ropes of the composite yarn» e

^{Under the basic vision "intrinsic visGoaity 11} " denoted by the symbol (n), the value of ln (n) is an def

ORIGINAL BATHROOM

A-407/408

1436610/13

Sefenitiatelle with the ordinate aeh.se (ie for c equals 0) in a graphic representation of ln (n) _r / e (quadratic values) and c (g / 100 cnr solution; abscess values) to understand »; (n) _r is a symbol for relative viscosity, i.e. ' H. the ratio of the flow times of a polymer solution and the solvent in a viscometer. In, the logarithm is zat base e, that is, the natural logarithm. All measurements on polymers that contain acrylonitrile bound in the polymer molecule are carried out on solutions in dimethylformamide at 25 °.

For s ρ ie 1 1

This example explains the preferred product and the predicted processes according to the invention.

A 2% solution of a polyacrylonitrile (basic viscosity 1.955 containing 27 milliequivalents of acid groups / kg of polymer, determined titrimetrically in a solution in dimethylformamide - hereinafter referred to as polymer "A") is 47 g / min. the Kingkaramer 9 of the Pig device. 1 supplied. It then fits into the annular space 7 and so as part of a composite thread outwards into the spinning cell (22.9 cm diameter, 4 * 5 nt length), since it is directed towards the center of the spinning cell. Simultaneously, a 27 $ ig® solution of a mixed polymer of 96 percent is. ° ß> acrylonitrile and 4 wt. ^ Styrenesulfonic in

. _13th

90980T / 6730

14356tO

A-.407 / 408 '' ■

Jiimetiiylformaraid (G round viscosity 1 ₈ 54ι containing 240 milliequivalents of acid / kg of polymer determined analytically; hereinafter referred to as polymer "B") at 47 g / min »fed to the annular space 8. The material then flows through the annular space 6 and, as the other component of a composite thread, is pressed out in such a way that it is directed towards the spinning wall "A mixture of carbon dioxide and nitrogen gas is circulated through the cell at a rate of 25.9 kg / hour. Temperatures of 105, -315- or * 180 ° for the spinning solutions _s head and cell. The resulting 14 ° composite filaments existing product is wound up at 183 m / min. | it contains 19 dimethylformamide and 1.0 ^σ β> water, based on its Sroeken = weight *

350 thread bundles of the type obtained in the above manner with a total titre of 382,000 deniers are combined to form a cable and the rest in water baths of 95 °, ϊ / elche Extract dimethylformamide, stretched to 4 times its original length (i.e. with a reek ratio of 4)> The stretched and unstressed wet cable is mechanically raised in a stuffer box, 6 to 7 bone curls ^. 1/2 cm extended length at · a storage chamber temperature of ■ 50 ° crimped »The crimped cable is then stacked

- 14

Δ-4Ο7 / 4Ο8

cut from 7.9 cm »The cut stacked goods become loose arranged in a bowl, 15 min. in a convection oven at 132 to 155 ° dried «The dried stacked material has a mechanically weak crimp of 6 to 7 crimps / 2 i / 2 cm plus 6 to 8 helical crimps / 2 1/2 cm on »

The stacked material produced in this way develops 16 helical crimps / 2 1/2 cm extended length when cooked in Wasaex free of inhibiting forces. The helically crimped fibers thus obtained have an 'equilibrium' crimp reversibility of 40 $> and a Z ^ Crimps / 2 1/2 cm ve;. 6 _f 4 crimps / 2 1/2 cia. La. - all mechanical crimping is essentially STäfex: it «The stacked goods have a strength of 2.2 g / 3en and a yruol stretch of 40 i ° and a thread count of 5.0 den (O _f 34 t <$: see) after boiling and drying ο

The properties of the product according to the invention according to Example 1 are shown in Table 3 with the egg adhesions of other composite fibers. The fiber according to Example 1 meets the requirements of the X'orliegeriden invention, since it has a high level of curl reversibility (irrelevant curl reversibility of 25 % or more) in connection with a low curl intensity (10 Mb 18 krüusftl / 2 \ / z cm more extended

909807/073 0

A-407/408.

Length) has, Me in the table I for others, not after the fibers produced according to the invention ¥ ¥ erte aeigen that a reduction in the ripple of one Reduction of pucker reversibility is accompanied »

Another important improvement of this property is the recovery from compression after steaming, which shows the clearest comparison of the Fourth (Table I) for the sample first with those _y for sample 2 4 and 5 "

A measurement of the force of the crimp development, whereby single threads are tensioned on an Instrom = tester to O ₉ OI5 g / den j then stretched out at 90 ° and the percentage tension is measured which is developed again during drying, results in the following

Sample Kraft der Krause 1 development, fo

f. 20th

, 2 5

3 20

4 0

5 0

The product of Example 1 is continued with a basic Dyestuff colored by placing it in a ^ parb liquor of 50 °

-. 16 - _-'.....
90984f / G73p ^

A-4O7 / 4Q8 '"■..

dives, in a period of 15 min. then heated to boiling tract 50 min. keeps on eggs boiling point * bflot As Par te an aqueous' solution is used which _s

Astraaon-Red 6B 1 "A

Acetic acid. Λ f> sodium laurel! Sulfate 2 i *

contains. The ratio of liquor to fiber is kept at 50 s 1. The fiber looks like a bright red hue _o

is a fiber _s by spinning the Folyacrylnitrillögung (homopolymer) is made of Example 1 to einkomponen "term Fäöen? colored in an appropriate fleet "colors them in ei / aem sehwachen ₉ ungleiciamä ^3S iS ^en pale pink hue.

It is surprising that the terbund fiber results in deep, relatively luminous shades _o

Similar results are obtained with other basic dyes.

From staple fibers corresponding to samples 1 to 5 of table I, will spare similar yarns (60 tex, 355 Z ~ Dre *

""''" .. 'SAD OR) GIMM Ö6""

A-4Q7 / 40S

hungen / m _p wool system) and knitted fabrics. The volume (on ^J / g) <5 goods with a similar structure (rows of rows / 2 1/2 cm times Aachen's tabchen / 2 1/2 cm equals 200 "with ß-item number 60 tex), the result of weight and thickness (determined by means of a kolbenartigcn Dickeraessers, the won on the product a pressure _fl 5 8 g / om "exercises.) is nachstehend- specified along with statements about the handle of the goods"

Sample - Yöluminosity _ "handle

1 13 fine wool-like, elastic

2 ■ 10 V _t - harachig, -

5 13. "," Very harsh,. "' ^:

4th 11 soft, moderately airy;,

■ .- 5 ' ^: 9 .. soft, thin

Me Yorteile dea inventive product (1) are open = visibly

la -

attempt SompoRRJuts 1 (η) component ^! ? a 2 in} b e Ils 1 Siter _s
the Ripple
2 1/2 cm ⁺ ' Ripple
Equilibrium
reversitoi-
Iitat " % Erho
lung,
steam-
Taeh * 2.0 ¹ «- ■ Horizontal bar
behaved- 1
_(E Ex 1 AH
) 1.5 AS / SSA
96/4 S J) Λ » ++ 3 15th 40
# 375 2 AN / HA / SSA
93.6 / 1 / 0.4 2 ₉ O
2.0 AS / SSA ■ 2.0
2.0 210 4.0 * £
^ » 20th 22nd 215 3
. 4th AS
AS / SSA
98.5 / 1 * 5 AI / SSA
93 / ^
Aff / SSA
97-2 / 2.8 1 ₉ 5
7th 150 4.0 6th 30th
10 Ί9
18th 360
145 co
O
co
00 5 AN / MA / SSA
97 / 2.3 / 0.7 AS / ÜA / SSA
96.0 / 2.3 / 1, 318
70 8th
8th 3 10 19th ■ 140 §Y 60 4.5

+) extended long

++) Different longevity due to the coiled polymer
and the mixed polymer in milliequiTalents acid / kg polymer

AN acrylonitrile MA aoryl acid methyl ester SSA p-styrenesul, fonaic acid

B.elsj iel 3. . ■■ - "''. ■ _

This example illustrates the preferred location of the two Components in the spinning cell «. . . . -. ".-.

(A) Using the device and the polymers of Example 1, a. 21% solution of the polymer 1 in dimethylformamide and a 27% solution of the polymer En ■ in dimethylformamide at the same time (with 98 or »98 g / min _o ) pressed out ₉ so that the polymers in the composite thread to the middle bsw. are directed towards the V / and the cell, one works with temperatures of 110, 330 or 180 * for solution, head and EeIIe ₀ Pas gas is passed through the cell at 36.6 kg / hour? the yarn (denier 8.8 to 1.0 tex _{e 8} as-spun) is 343 m / min "wound _o Combine 350 and cable stretched on the 4,5fäche (as in Example 1) o

(B) A further attempt is made identical to (A) with the The essential exception is that the position of the two polymer solutions is reversed so that the polymer A faces the outside of the spinning cell when it is pressed out ο. "" -..-; ". ■ ■ - ■ '■ -

The - both uat © r (a) and (B) obtained - products have 24 »9 bgWo 32 _e 0 Kraus ®l / 2 1/2. cm after: "Boiling in water and

909807/073

SM

A "4O7 / 4Q8

a G-leiehgewiehts-KräuselreTersibtlität 24 or »$ 21 to the yarns according to (A) and (B) contained in the spun form IISW 5 ₀ 29 ₉ 5 -. # Bimethylf oraasaid"'_; . . ,

When one-component filaments under the same conditions it spins and stretched _p-has the .Polymere '(B) the greater shrinkage (z _o B ₀ 24 $> over $ 22 for the polymer A) I

(C) The above spinning processes are repeated under otherwise identical conditions with the exception that the spinning speed is reduced to 183 m / min _D and the solutions are supplied at a lower speed (53 or 53 g / min for the solutions of the polymer A or »B) _{¥ obtained} by the same titer. The resulting stacked product ₈ in which the polymer A is on the inside of the thread run results in 13.7 crimps / 2 1/2 cm when boiled. The stacked material (D), however, which is obtained in the other experiment the reverse position of the polymers. _S, has 16.2 crimps / 2 1/2 em in the boiling off of _o The yarns (G) and (D) contained in the in the spinning obtained form 20.3 baw ».22.0 £ dimethylformamidο

This SpinnTersuehe show aueh _p that is obtained a lesser Krämselgrad at lower spinning speeds ο

909807 / Ü73

At s Lll_i__l

This example explains the meaning of the Spiüngesoliwindig =

ability to travel according to the invention.

Using the system and the procedure of the example, apply a 21 ^ 1 ^ 0 solution of the polymer A in dimethylformamide at 53 g / min wM a 2-8 # solution of the polymer "B in methyl formamide .mit . S3 -g / min. _o ■ =. Gl.e ± currently. as an exterior! - or internal component-. by ¥ erbundtaden .spun * - Man working with temperatures voxi 11-0 _? 330 and- 18Q ⁰ ..forLäamng _{; K} .Kopf tew ^ ZsIIe ,, The ßas- will fill. 36. ₈ 3. kg / 5 ^ unde passed through the cell ". And the yarn is wound up with T83 m / Mia". " laugh, stretch out. the,, 4.5-fold "cutting" .ad Txocknen as .. in example 1 esatwiökelt the stacked goods (Fagerititer 5 fen) -be ^: in the ^r "decoction. 1? ₉ 6 I & ä.ii

If so, -the ".above" SpinsiT@rs.ueli if everything else is the same. Conditions with the exception of “repeats ₉ that the speed of exercise is increased to 343 za / min. And the solution is correspondingly increased. Speed. Supplied.,. ^ Is obtained. a pile good (thread guide ^ ^ - .den) », which. a degree of crimp. when boiling 26.9 Krause 1/2 1/2 om results» The speeds, from 183 to 543 m / min _o result -. Yarns » , "which in the spun form. 22.4 . or 41 s 4 i>. contain dimethylformamide and a .'fäden · -fetter.: of 8 ₉ 8 or _{8 P} 8. Obviously work with higher spinning speeds when the threads are exposed to higher temperatures ο

90980f / Öf30

B JL $ -SP-1-g-1 J -

This example illustrates the critical effect of concentration of the polymer (which results in the lower shrinkage homofilament) in the spinning solution *

A similar device is used as in Example 1, but which has a spinning cell of 1? ₉ 8 em diameter and 4.3 ι length and a spinneret with outlet openings of 1.499 mm diameter, which contains 84 openings on 3 concentric circles.

A 21 _t 5% solution of the polymer A in dimethylformamide with 15? g / min ", the polymer solution during the pressing in dem.Aussen- and the inner = ·» supplied so that circle facing the center of the cell component forms "A 28 _P 5 $ i £ e solution of the polymer B in dimethylformamide is the ring · = Integrity 16 at 157 g / min «so that this polymer formed the component facing the spinous cell wall on the outer circle and inner circle, while the component facing the middle of the thread circle formed the component facing the middle of the thread circle. ! hurry led? the reaction is carried Aiit Tem = · peratirien of HG _P 345 or "195 ° for solution, or head" 2elle _o Bas Gern (linear density? _P 8 öoii) is 320 m / min "aufgewickelt-, _4-f fnch stretched gesclmitteti and dried , which is done as in example 1 o Babel throws a stack of goods with a thread count of 5 $ · 3Ώ

■ 23. 909807/0730

equal-held * where one. however, the concentration of the polymer Λ'QUf 23 _P 5 ^c f ° -increased '.

Basically obtained from the SpinMTersueh with a lower polymer _{concentration. When boiled, stacked goods result in 1.4 9} 5 'crimps / 2 1/2 CMg. the stacked goods. trying to use higher polymer

concentration on the other hand 1Yy4 ° ■ ■. . . ■■.

The lowering of the concentration-of 'dope the poly = mereh, -. Which provides the never drigersohrumpf end Homo thread, preferably rom an increase in the Gru'ndviscosität Polymei ⁱ en accompanied "to di © viscosity of. Spinning solution at the desired value- "to keep <> -. - -.

B ei 8 ρ ie 1. .β.

Under ¥ Erw @ ndusig der. Appendix, see example 5 , a 23 solution of the polymer A- ± m . Dimethylformaiaid with H? g / min _o -so. pressed out so that the polyamide in the outer edge of the threads of the cell wall is facing _p and © ine 28., 5% solution of the polymer B in "dimethylformamide at'147 g / min" so pressed out that it is in the outer ring of the threads in the middle , the cell trains · = Wandt isto the gas is' 37 _p O1 kg / hour through the ge = .A cell passes Man α working mit.Temperaturen Yon Ito ₉ .280 or "182 ° ■ g LöBUM-for, head -and- / Cell ο The yarn is _{wound up at 320 m / min o} = stretched 4 times, - cut ■ and dried, what how

• 909807/0730

Example 1 takes place, Van receives a staple fiber. (? Adentiter 3 den) »which after boiling in water 22, & - Krausel / 2 1/2 om. having

If insn the above spinning experiment is repeated under otherwise the same conditions with the exception that the head temperature is increased to -345 ° ■■ * the-3-den-Stapelfaeer .beim decoction 17 _B 4 · -.

Crimp / 2 1/2 sm on and. The dimethylformamide content of the spun yarn is reduced from 51 »9 to 25 #, - ·.

B e 1 ρ -P i e ΐ T '■' ■ '

This example illustrates the critical impact of the. Flow rate of the evaporating * medium, in of the spinning cell "- - .- _...-" ■

The two polymer solutions of example β are spun in the manner described there at temperatures tob 110, 345 baw »182 ° 'for "L'ö& ungg head and cell "'. The QaTn is wound up at 320 m / min '. In one case it is passed through the spinning gel at 29 »3 kg / hour, in a second case with 37» 01 kg / hour «Maeh 4faeher Eeckung," Drying and decoction as in Example 1 turns the first one into one Staple fiber (thread denier 3 "den) with T9 _S 7, KraUBel / 2 1/2 cm, while the second 'staple material (IPadentiteV 3" den)? "Which is spun at the higher ventilation daytime» only 1? ₉ Contains 4 crimps / 2 "1/2 cm. By using the higher gas flow rate, the content of the spinning

- 25 - "■

obtained yarn of dimethylformamide rom 29 ** 5 to 25; 5? _t

This example illustrates the critical table of cells · =

temperatureo. \, ■ .-,. ,. ■. · · ■

Hau works with the. Solutions ,, the device-and at the. Conditions .'des Example'5 (21.5% solution of the polymer A ₉ 28 ^: "5% solution of the polymer B *. Feed with Ί 57 -" baw "^ 57 g / min.) And the". gi © ielien spinning conditions, "but one.

Belling temperature "tone 17O ⁰ - composite threads are obtained which, according to 4fa" sher Reeteag . W & d "relaxation. 21 ₁ 0- frill 1/2 t / 2 cm

- "The application of a higher lellentemperatwr wan 195 ° feei otherwise ^: " same conditions, setat the Krausei intensely & B iQ ^ hnnnuissilenB to "14? 5 .ICräiis.el / 2 t / 2_.cm., down <, who ...

JjösusigsEiittel residual content "" of "the" two. © rapoisnenen yarns (Padentiter? _S 8 des) is .29 f tgeschät ^ l bsw. » ?. 24, 5 .. (geEehätgt () for 170 and 195 ° y ma .If a 'the' Bai game 1 _r with otherwise, ffl'e ich'en Bsding.iiag;... S _v, but below. . _Brhöhuag;.. d ^ r Zellöntemßeratur.auf - 210 ° repeated 9 "Börden threads 10 _r aohraubenf örmigen ... .. 'crimps / 2 1/2 em and eiwsr-.ßleiehgewiehtfc-Kräuselreversibili = - tat-won 30? 6--Preserved "Baa- O-arri contains ^ t in the ^; - e ^ epönkeead." State

2.6

9 Q -9 8 & Ψ / & ί SO ^: ". ' ■ '' ■ - ' ^Bm ORlGlMAL

A "407/408
Example 9

The procedure is as in Example 1, replacing the acrylonitrile homopolymer with a mixture of 94 parts of the aerylnitrile homopolymer and β parts of a copolymer of 96 % acrylonitrile and 4 $ syrolsulfonic acid, resulting in a total acidity of 45 milliequivalents in the mixed polymer of acid groups / kg of polymer is obtained "the sub-· = - eliminated longe halt between the blended polymers and the Misöhpolymeren is 195 milliequivalents / kg _o the closing = · lent obtained staple fiber has a denier of 2, 9 the" a strength of 2, 1 g / denier and an elongation of $ 31 and, after boiling, shows 15 helical crimps / 2 1/2 cm extended length? the equilibrium curl reversibility is 34 # »

The physical properties of the fiber of this example and those of Example 1 are considered to be essential considered equivalent. The fibers are subjected to circular knitting a subjective evaluation; in doing so, the aesthetic properties of the fibers are considered equivalent and very assessed as satisfactory »

Carded 2 = g samples of washed-out staple fibers are placed under differently long up to 4 hours in the following black Dye liquor (where the quantities refer to the fiber weight) subjected to a pot dyeing when boiling:

- 2? 909807/0730

14-356 ίΟ

Co Z ο -Baβie Yellow.11. 5 »06?

CZ'Basic Red Ί3 ■ - _■: 15,04?

Basic Qrstnge of Example VIII

(w) of the USA patent

2,821,526. 4.32 f

CoIo Basic Green 4 '■. 1 "68?

"Long-chain.-alkyltrimethylammo ~ -

nlumbromid. . 5s-0 $>

'sodium sulfate. .. $ 12.5>

Na ir iuma e e ta t / E s s igs Kure.-Buf f e r

(pH β.5}. '. 0.5 $

The ratio of tone color fleite to fiber is 100; 1? the fibers are entered ",, after the liquor has been brought to the boil" ... ....

Sash the dye, become the fae-ern. in a 2 ^ .igen solution of a ■ iiichtionogenen © over £ läeheKakt: ven agent (!? condensation product von'.Poiyprepylenglykol uäd Aet iyl € i i © syd) 15 min> on boiling g @ Wäcken ,, rinsed ₉ {thrown. dried and for visual

Comparison, the quality of the color krer-.peltc

The luminosity and. The depth of the hue will increase over time. constant; better. »'Cross sections of these fibers according to Example 1 show that, in the. .! era th be: the hours of dyeing the säureModif-ied component the dye very quickly and unmodified · side (iloBroj / ölymeres) on their skin barrier in this period does not accept "_ Ber in der.nichtmodifielerfeen side present dye occurs; into it over the polymer polymer ßrensfläche in the 'composite barrel., After four hours

BAD ORIGINAL • - ■ - .28.-.- V-. - .. ■ -. "

909807/0730

t est ustellenj that the dye from the Pölymer-polymer Limit laugh her further into the niehtmodifi ed page penetrated and significant Anaeichen for skin coloration present ,, The fact j that the nichtmodifiaierte page at all any dye in this process takes ₉ is very surprising, as their great resistance to dye is well known »The four-hour dyeing provides deep, permanent = nism-moderately luminous black shades»

The fibers of the present example have a stronger dye penetration over the polymer-polymer ßrenäflache and a stronger slope to ring coloring o.- With the same long dyeing time, the fiber of this example @ia provides a more luminous black than the fiber of Example 1 *

The dyeings are repeated using dyes in quantities equivalent to 7 »3» H ₉ O to w »14» β $ i> based on the fiber weight. For the fibers aaefa. Example 1 is the highest © dye concentration required _? around at this coloring ». ' method brilliant, dumb, acceptable black hues can be obtained. Surprisingly, the fibers of the present example result in dye concentrations of. 7 »3 and 11 36 bright black shades ,. the dye concentration fön 14-9 ft β are equivalent in the other fiber _o of a single component existing, obtained from the polymer mixture threads (Ckssamtazidität 45 milliequivalents / kg) are colored in the above methods only slightly stu

9 09807/0 73Ü

Λ 4356 TO

Sin more convenient; un $ vilrtsöiiaftliefeer Feg- sm £ BrgeugtiHg der. Fibers of the present example contain "the acrylonitrile" = homopolymer with 10 fo or more, sucked & ut_ & 3 ± n _t & ewiQht _t of waste, the composite thread to be reduced. the «toe im. Spinning the fibers of this example, accrues » . And" then a solution of this amount. In -oeifObeii; - -bese & riebanen, W®.ise-mit einör! »Osting des -

sarai? .eii-.Miselipöl.fiQe3? ea z®.- i "

for the E? ^ ®eke of the invention suitable.PöXjmexQ see in all classes linear ¹ faaes-foililen & er polymers "which have a.: aolehe -Ifu'sli @ bkeit ;; thatnaaii them The two · gewälil-fen -Pölyffleren.jaüaseii .ü söhie4 -i-fl : - & ühmmp £ uMg uttä
der ¥@r.tesdfalen■-kräuselt .vmä

Each component © of the kE'äiiselrevei'griblea Y & ThunaSäää according to Erf / indang. can be, from many groups, addition polymexisates; choose a *; Pie .toeaötigt @ ^; reversible; Mtigeoaafleruiig de ^ Kbiaßöflent-ea throw- easily by- · -man-.den. "Sehalt- of the two 'polymers at -iosi groups

Such ionizable groups let go. easy to get, ¹ .by one example, acrylonitrile with. JSonomereii .'P & lymevie ± eTt _t ate Acid types » such as Carboa-« SuIf on- _p . © the. in the form of the salt or the free acid

Ζλ

Α-407/408 "

Outstandingly suitable for the purposes of the invention are the following sulfonated po £ ymerisierbare monomers and their salts, p-styrenesulfonic acid * ₉ methallylsulfonic acid, allyl = · sulf oic acid and 'Äthylensulf oic acid "

In a way that is obvious to Sen's professional, one can get the necessary Introducing ionizable groups into a polymeric component through quantities of two or more polymers »The Polymers should preferably be compatible o

One can, for the purposes of the present invention also work with other vinyl polymers as the Acrylnitrilpolymerieaten which, when eie not have as such the required reversible change in length is ₃ in the above manner changed by acidic or basic modifier so könnexi ₉ that the mixing polymers, the erforderliehe reversible Längenreränderung exhibit" .

The inclusion 1-15 i "beetimmter nonionic modifier in copolymers of acrylonitrile ^ reinforces the effect of any ionizable in the final Polymeren.vorliegender. Groups ο In general, it has been shown that the monomers effective in this respect are the same monomers which, when incorporated into an acrylonitrile polymer, increase the dyeability of fibers made from this polymer with dispersion dyes ^. - ' ^Ά '

.-. 31 - BATHROOM

909807/0730

% u The monomers which are more moderate with a view to increasing the effect of ionizable groups include acrylic acid = _{methyl ester 9} methyl methacrylate, methyl vinyl ketone, acrylamide ,; N = tert-o - = butyiacrylamide ₉ ? Inyl methoxyethyl ether _s methoxyethyl acrylate and vinyl acetate _e ■ _:

Inclusion of any of the above monomers enhances this. Effect of the ionizable groups on the reversible Längenveränderungin "in such small amounts, such as 1 io _r but in general 3" contained in dent-polymers-desirable to $ 10.

The composite yarn according to the invention are characterized-by the fact that at least one of the components ausρ equivalent at least 50 milligrams of a>ionlsierb'aren ß-ryipp @ / kg polymer contains "Yorzugswelse ₉ contains a component in addition to the content of - at least · 50 MilliäquiTaienifcen-, a substantial oberechuse of ionizable groups over the other component, if both components contain such groups: "It should be pointed out, however, that the nonionic monomers mentioned here, which increase the absorption capacity for disperse dyes, reduce the effect of the ionizable groups in the component proportion to the concentration of the - nlchtionogenen modifi ζ ation "means increase» Eo is therefore to achieve significant effects according to the invention desired, where appropriate, the content of non-ionic modifiers "to term into account"

90980770730

F-407A08

Yor ^ ugswelse working with a polyacrylonitrile (homopolymer) having a ßrundviscösität of 1, 5 to 2 x, 5 and a Mischpolymaren with a content of at least 95 f ° acrylonitrile · ■ and 1 to 5 $> an acid modified monomers (- acidity '95-350 meq / kg polymer) usd is particularly preferred with a Orundviseosität of 1 ₉ 0 to 2 _P 5 _Q is a poly · »acrylonitrile, and a' mixed polymer dos ÄcrylnitrilSf'das suif on * = ·" acid groups iii an acidity of 200 to 300 KUlli equivalents / kg polymer contains this preferred combination "yields". In the process conditions according to the invention, "a medium" high curling intensity (10 to 18 curls / 2 1/2 extended length), which leads to the goods at a comfortable grip t high ICräuselreTersibilität (Oleiehpewic-htekräuselreversibilität you 25 to 50 ^) _9, the gu a good rest and ferdiehtung (300 to 400 56 by! steam treatment) leads »eine'hohe bulkiness in articles such as Sweater "and good / stainability with basic dyes"

You can see the threads according to the invention for producing spun yarn using ^ but for some Änwendun% ο B "yarns, which are intended for the work of sweaters that little or no pilling ergeben-" has a look ^ found desirable in Srspinnen to give the yarn a high twist. One works expediently with a twisting factor of 2 "Q to 4" O _S as it does justice to the desired aesthetic properties ", the 2v" irn factor

909807/0730

H356TQ

A-407/4

with the twist (rotations / 2 _p 5 em) according to the following equation in relation to j. . - -

Turns / 2 1/2 em ~ twist factor χ | Cotton Count

The invention is', above .an-hand ypn * Mmetiiylfq ^ mamiö explains.e-rt, but you can search with. other .Iiögmigsmittela _{_arbeiten:} .how:.

'ietramethjrlensulföii.j, .ltiiy.lansartoo.nat _r .lüitrQiBethaii.-fasser · and; ■ their mixtures .with

BAb'OF «GINÄL ^: '" ^: ' ^:

Claims (3)

"It was 10 to 18 helical MRS / cm 2 1/2 fo comprise composite yarn having at least avrei troekengesponnenen fadeabildenden linear synthetic polymers in an eccentric arrangement, characterized in that (1 inch) length and a outstretched ßlGießgewiehts-KräuselreTersibilität of 25 to 50" 2ο filaments according to claim 1, characterized gekenrzeichnet _f that each of the Polyiaerkomponenten of polymers dea acrylonitrile is formed. 3. Threads according to claim 1 or 2 _f, characterized in that the solvent residue in the state received during spinning. is below the values given by curve 1 according to FIG. 8 of the drawing, 4 »Procedure cure production of peads according to claims 1 to 3 “is characterized by the fact that the thread-forming masses at the same time spun into a composite thread and under conditions be discharged into a spinning cell, which lead to a rapid erection of the fiber structure. 909807/0730. Method according to. Claim 4 _P by {■ Mkeimzelahnet _f that the thread-forming masses are spun in önloliev spatial position »that the component with lower shrinkage de .-: · Center of the spinning cell and the higher shrinking end K -.» <; Ipüneiiite <JU3ia ^ !! «Kurafang atigewandt ifatr. 6 »The method narh claim 4 or 5 <öadureh characterized _t ^ atJB the sjjinnlösg of the nitdrigörsiührsiührenden component with less Cor ^ teiatration a3 β the spinning of the other component e rings ce tzt wix i. 909807/0730