DE1494598A1 - Process for the production of staple fibers from regenerated cellulose - Google Patents

Description

DLe iVri'ii ".dung relates to" staple fibers ana gel; looser.renerate fibers with high fluid strength and improved cardability, which are at least relatively non-fibrillatable, as well as a method for producing such staple fibers.

Yes, high '..' awfosti.rkeit according to the ötand of Jec: .nik are not afflicted with a number of parts that de.-en ilut ^ appl ^ confine. Many of them are brittle and fibrillated and were further found to have poor cardiarity. An excessive one The amount of fiber remains on the card and is therefore lost for further processing.

The invention is referred to below, for example, under explained on the attached drawings:

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J ¹ L-. 1 ! .St eL?: E aiu / rn - .: 'ν I -j .jv ·. r> ht fji>: -. * r. ·. · ο. ".,: r ·:. -π; \; Π :: 1er 7LXT ^ c: do.-; 'tu;:," first i. .on, nor erf'L ¹ .; ^r - £ j · & »■ ·; - jn <3r. j: i.: ern uua re er.eriercer 'Je ^ lvioae:.! ■ · ■ ·. r '.? ■' * - ■ \ ''! J "i veit.

j'iQ ert'lr "" n .j ü ...- Ό · ^ ι · - ocjteLL-o :. ^';; i.'eri j re ^ .. eri-ir.'...? , ur 0e.LUJ.Oi39 teöi'J / 'ji. uir.er.! .c: .32i;,' u "fo3 i.;. ^- 31 ^ aK.oau I of .eri. ■ -stens 1" unu aj.1 - ;. ". a vn i ι lh. D'i-i ^v " .ner I ;: ¹ : riL -.- xt -t'i; i * i_. Lien M *;. ; er ro.! u *; iv *: io: .t : 'l r: .1 i ^ r; ^ r un-i v / ei3t e L: io S-iQiJ - .: · ...! ir.., a: j.; or ν; n: .Lc .. · · o; .r · _Ιβ 1-5 on. - »le r ': iaer: j jir. i da-iurol'i -e.ienr.rwiu.ir.et, -r ... ;;; .! oseLian eir.yü ni ·? drirt; r. "Kreiii ^ e L-Bela-iuri.- si'airtcr"; \: .v-siaen, ie 2in aer .rti -en factor, the κ-leii.er aio ζ, έ.5 i'.r fibers niü 1.5 Dei-ier ur.u one L ^:: n, Te from 39 | 7 no. is. -iie eri'inaur.-u.-emüFji; Herreatell ton fibers can be present within a broad denier; rD9reiohe3 and Unr-j :, - range, such as 1 to> denier and etv / a 3-v t> io about 51 mm length »

A special ler.irai uer erfindun ^ ö.; Enäsa manufactured fibers consists in that dis-seloe :: esüglion der Ilawfe.g ^ igkeit, der Schrucipfoharicteristika una aer de ^ nfkhiirkeit and elongation both in the wet as well as in the condition of the hem wool are similar. On G-runu these characteristic Ilerknale can These fibers are used instead of La-.irjv.'clle for many textile purposes or diesel: s can be used in G-eni3ch with Bauiav / olle ' will. The new fibers also have the appropriate ones Properties of other textile fibers made from viscose rayon in terms of gloss, smoothness and grip.

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^ .UG these fibers hf; r - es1 e; "! Te Tex ii lr-iii teriaii en icünreE αν, eh njui.i; .i.iüc ... 3 Zuau:.: ^ ndivu / .sn uec Ie :: 'i 1' Ut.ia in I.e i. ^ ei.ric- * un.- viri / itttilü ra-: r: i; iiter '"'. 'err.H a -eüBweise be stabilized.

ELruii Ie; I am for Tex ui. .Li:; veoi: .e made of Kunatseide fibers i..it B -. ':::. Wool einva— i.; O ii'. ^:: IU:, T, is the eruetliche loss, about I'o / "in the rieehuniseien j ^ ^ esti ness of the I-inistseide-ii ^ .fien di-.rr. rewecen, - .. a: aiaae-iex; aer iiulien liatriumUydroxyd- "el; · iiaiun, '·: under- \, .. x'i'en .-. erüen, the i'.ir one Γ-ercerize before ^; α ι .-.' Οχϊ-kirnen and is applied- .. On the basis of this er ^ el-li uhen? esci.- and the dchviiei'igireiten, .lie them :: s ^ ei .ieir ..materialien Jii-.e-'iGionale btabilitüt ri; mediate, the Kunatseidepalt is the previousi—.; en size; .isclie from liauiiv / olle and the previously known Lunstseidef & sern citu .iiaxir.al about '>0', * esp. Lriinkt woi ^ den · .- ». On the other hand, leads a learning. Loss of Eerrei '' f ^ stig, since only 10 'tis 1 ^^. <pus: .in eriaöfjlicho die! '' äiiigiceit the Te ^ tiij made from the ^ aser ..: ut dißiensional by means of physical working methods of the textile material uu stabilize the anv.eniun.c of 'Jei-iisciien from cotton and other new types Fibers with an artificial silk content of 10.0 or less to about 70 to 75 "".

The JTaISf es / cness used here is an average one Resistance to hatred and represents the load in & ramn per denier of the iaser represent the 2üm stretches of completely soaked fiber divided by 5 ^ ά its length by. 0.05 is required * The

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The ability to stretch or stretch represents the amount of stretching, as it is generally expressed as a percentage of the fiber length at the point where the fiber breaks. Measurements of wet strength and elongation or dexin ability can be carried out in the usual way using the her - / - om:.: Lichen Instron Tensile Tester as a «t-ts tear tester. The nasal strength of the synthetic viscous fibers according to the invention amounts to about 10 to 20. This is η -r less ;; less than the wet strength of cotton fibers, and thus the fibers stretch to about the same extent as cotton during the day; ens una üppretierens the woven textile fabric. This property also trürrt to the fact that üer content of the rayon in ie 'isciien cotton rayon New York Convention on YO-15f> eri.ü:.. May be it. Jieeer Factor steiit a Uaü for the Peotig- _; : eii of the fibers are faithful to a stretch or stretch when they are subjected to tensile stress. The elongation or glue capacity of the fibers is generally in a range from B to 22 p when wet and amounts to about 9 to 15 m. conditioned condition,

Made entirely from such viscose art & eide fibers Textiles have a residual shrinkage or shrinkage after repeated "ashes about 5>" or less, and Again, this is about the same Baiiüiv / olltextilien have. The residual shrinkage of a woven; Textile goods can be reduced by about $ 2.2 ^ that it is subjected to a pressure treatment in the warp thread alignment. The wet of shrinking

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is similar to the rest of the shrinking for de- talking cotton fabrics · made from such fibers Textile materials have about the same resistance to ice in the direction of the thread in the wet state, as is the case with Cotton is. the same pointers, but a tensile strength in the warp thread direction in the conditioned state, the etv / a 25 $ better than the corresponding tree-covered textiles

Previously known rayon fibers with a high tear and wet strength indicate excessive fibrillation. I am very essential Feature of the fibers produced according to the invention is their very low fibrillation, about the same as with conventional types of textiles from Reyon.

Fibrillation is the splitting or peeling off of pieces of fiber to understand. The parts of the fibrils either break completely away or peel away from the circumference of the fibers in in a similar way to peeling a banana. The fibrillation increases the size and the mechanical The strength of the fibers is reduced, and this also gives the fibers a frayed appearance. The fibers that contain lightly fibrillating fibers and are colored seem to have lighter shades in those To discolor areas that contain such fibers, due to the light refraction or light scattering effect of the fibrillated fibers. This can be especially true of

identify materials of dark colors »

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Ua3 AubDais a fibrillation3 of the fibers can be increased by the fiI-ter8i _r er.auaften or the j'liaenaaal of .asser when using a C3suii.:ir.th fiber ^ ewichtes he ::. I n-jeit after the fibers in an ..incher or percussion r: it 'ir.i-xii "er." ien 1' ¹ IU ^ a have slept for a certain period of time. jJieae r'lieüszahl, from the in Besenreibun .: and claims gas, smelled v / ird _r be— 3ti:.;: t x.an by the fact that uan 4 g fibers in ^ ü ( ^; - .asner in the , sctiiugwer-: brings in and the mixture flies in for 20 minutes. The raser filters out the aurac broken fibriils, divided into two parts, are removed and grounded for 3 seconds, the sieved fibers and water are placed in a 3-phase HF filter, which contains a filter plate made of ösint-artet is marketed by Ace G-xass Qv.uanj Yincland, Hew Jersey, USA and is listed in ier publication "Hydro Cellulose. Father Flow! lumber" by OA Battista, JA Ho-.smen and Sidney Co ^ ick in Industrial and Engineering Chemistry, Volume 45, page 2107, September 1953.

The sintered grass filter has an average pore size of about 40 Lixiron, a laircrjnesser of about 32 mm and a thickness of 1.6

After the fibers have been applied to the filter, they are allowed to sit down until a fiber cove has formed on the filter disc. A pressure equal to 60 .mu.m Hg is applied to the lower side of the filter disc, allowing the liquid to pass through the

fibrous cake and the sintered glass plate flow,

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_ ₇ _ 14i4Sfi

while this negative pressure is maintained, the time required for 100 ml of water to pass through the cake and the sintered cake is measured Asnlatte is required. This number in seconds represents the so-called i ^ lieas ^ aiil. Fibers produced here that are relatively non-brilliant, have a flow number of less than 25 .

The staple fiber made from regenerated cellulose produced in this way has a ^tt Kre '.. pel-Belaüui; Thread factor "of less than 'jfZo on. This is a louse .Faktor for cie rasermenre that sieii on the Lurdierungszj'linder during a r.orr.alen Kardierun. svor ^ ^ .un it ansa .irielt! and for the iextilverarbeitunr get lost. ..

The liier used krenpel-Beladungsi'Eiktor is so bestiunt, daii a staple fiber made of regenerated cellulose advises l _r 5 denier UNAE ~ ^ a is 39.7 mm of a höiv-üunliehen .tiiiten 1 m uir.lau- fenden carding flat top , uie rzi'c Jraht is drowned out, EUi. is led. The urahtsai :! amounts to 1υϋ'ε. the cylinder and to 110 ^f s on the Pilettro. : .. el and plat. The staple fiber is fed to the freshly cleaned carding cylinder by means of a storage container working with a taciiel roller in a quantity of 2.27 kg per 20 minutes. The carding machine is operated for 20 minutes and the fibers that have gathered on the circular cylinder are removed by means of a purste. The load factor is now the weight of that removed from the Kremvelnylinean. Fiber multiplied by 100

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and divides dun :: J ^ s (iewicnt of the fibers suggested by the χ-rerupel, ie 2 _t 2 ^r ( k ^ _o When using finer denier values and ebeiualla longer, the circle: pel loadun _t / sfuktor will be proportional i--; rüEaer oil der Krei.ij el load factor for staple fibers made of regenerated cellulose with l _t -j denier and a length of 39.7 vs.

All staple fibers according to the invention are all produced by spinning a viscose containing an aminoviscose additive or spinning agent into a sulfuric acid spinning bath containing a little acid and little salt, which is also Contains zinc sulphate. The amino additive is chosen so that it chemically urates with sulfur and zinc during the spinning process to form a zinc-sulfur compound or complex that is insoluble in neutral and alkaline solutions. ., ie additives used to carry out the process according to the invention can ζ. B. Monoamines such as Dime thy lamin and diethylamine, diamines such as /.ethylenediamine and other polyamines such as diethylenetriamine. The iunino-Zusatzniittel can narrow.-In relatively small, such as above the Oellulosegewicht ale either alone or in combination with other viscose additives, such as condensation products of ethylene oxide and applied phenol and related PoIyoxyäthylenglykolen 1 to 4/0 ·

The viscose used according to the invention generally contains 4 to 9% cellulose, 5 to 10 $ sodium hydroxide and 30 up to $ 38 carbon disulfide based on the weight of cellulose. The Sodium Chloride Salt Point of the ViskoBe can range from 7 to

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- 9

12, and for some purposes ViüKose with a salt point of 2 to 17 can be used. The viscose is spun into a spinning bath with a low acid and salt content, which contains 5 to 10% sulfuric acid, 9 to 20% sodium sulphate and up to 9% and preferably 2.5 to 7% zinc sulphate. The spin bath has a temperature of 10 to 4O ⁰ C. * The formed fiber is drawn out of the spin bath system and to 80 to, preferably-125 to $ 160, while the same by an e! "verdüBn'tea ^ acidic Kaskadenbad is pulled comprising about 3 $, sulfuric acid, sodium sulfate, and 1.5 # 5 '> zinc sulphate at a temperature of 85 to 100 ⁰ C vpn contains stretched. The spin speed is 20 to 40 m / min. The freshly spun and drawn fibers are then cut into the length of staple fibers and before drying, and preferably immediately before cutting, they are treated with a dilute acid of suitable concentration, temperature and for a long enough time to remove all reaction products or complexes of the aminoviscosis additive mixture and of the sulfur and zinc present in the spinning process. The acid <fcan & sohsreic acid, hydrochloric acid, or any other organic or other organic acid which is used in the case of the intended

Procedure «ftd turn
rock acid eel time from 15.

is applicable. For example, "B" is the An-It & j ^ solution from 0.2 to 1.4 wt. # Schweeratur of 96 ° 0 and suitable for a treatment. The acid solution and the dissolved lasers peeled off, the same

_f like 4iae | i BIe

·. ■■ .; , -ti

BATH OR101MAL.,

^; vi ^ f ^.ul:; · Ϊ?

-ίο- U94598

and desulphurisation, and then in a conventional manner dried.

The method of manufacturing the invention. so-called fibers from regenerated cellulose can be used in conventional equipment be carried out as z.3. iiagramre-shaped in the attached drawing is reproduced. Here, a low acid and rinsing bath is indicated by the reference symbol 2 Sa. '"Gehultes reproduced, in which a spinneret 2 is arranged to which the viscose is fed through line 4. The fibers formed in the bath are v / ground to a Beekvor- Direction supplied, äie a pair of inevitably driven shoulders or forging rollers 6 and 7 has. The corner roller 7 is driven at a faster speed than the rear roller 6, so do the pasers during the passage between do justice to the same in the desired manner. The fibers are a cascade bath of dilute acid at high temperature subjected in the Irog 8, while the same are guided between the forging rollers, whereby aie regeneration of the Cellulose is practically brought to an end. The fibers then pass over the rope rolls in the form of a bundle or rope 9 to the cutting device 10 where the fibers are cut into short pieces, as indicated by the reference .11 is reproduced. The cut fibers will then be used Dropped into an Irog or Zone 12, where the J? aee3 * £ t with a by the spray device 15 dispensed dilute acid "Concentration and temperature" of this kind are treated with sulÄage

that the present is insoluble in alkali and water

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int vez'oinaung or .Kor · / lex eic nt and through the Flue pipe 14 en \ ti * err. c wr.-rden is, jJie äta, sir:.: then he becomes in the usual white. ^ ev.aac ^ .en, bleached, desoü.efeit and re-dries. Ea korr.en here herkörjr.liohe 7orr \ .- 'atun ^ en in .Inwenaung who are not capable of Vienna: e e ei. are.

The following examples are used for further explanation the ürfindun ^:

example 1

j3s i / ird viscose ourcii die i5e.:a,ndlun ₍ -j from Ze l.lstofiplat ten (high a-cellulose content and type of viscose) with IT- trium hydroxide, .Terschnitseln der Erl: L: .. i.tenen ^ liialicellulose, /.anthOi'-eriierung UNU dissolve the alkali cellulose in a Hatriumiiydroxydlösung prepared the thus herfosteilte viscose contains cellulose 65ε, 7 / "Kaüriurahydroxyd and 34 $ Schwefelkoulenstoff be" o s _c to the Öellulosesewieht in these:.. -iiusxiihruiv'sbeispiel belauft specific to , the ratio of cellulose: sodium hydroxide of 1.0: 1.17 * the viscose is then aged in the conventional ffeise for 12 hours at 18 ⁰ C. the viscose at the time of spinning comprises a Sal-ztestwert of sodium chloride of 8.0. a falling ball viscosity of 60 to 75 seconds and a total sulfur content of 1.6 to 1.7 $. The xanthate sulfur amounts to 1.1 to 1.2> £. During the mixing process, the Viscose 3,3 $ dirnethylamine and 1,7yö Polyoxyätiiylenglykoläther des Pheno Is, which contains an average of 15 ethylene oxide units per mole of phenol, incorporated. The Dim & tliylauiin. And '<&<& £ ■ Pkeaoläther can be used in the manufacture. , :: ίγ-. : ... -: -12-

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the Viy.rse sui ^ eI-υ ■■■!, ■ "öii places are added.

The viscose. Is. Vorui .telo! Extrusion of the same by üi'f— "now .ren with one." -, aviii.e. he of u, O6j5i3 ran into a spinning bath, spun in .. ,,, a 1.5 denier, 1 ^, 000 yarn. The spinning bath contains 1 $ sulfuric acid, 11 / ° sodium sulfate and 4? B Zinc sulphate and is kept at a temperature of about po C. The threads are passed out of the iiau,; eκoijen _f over a first forging roll, through a hot, second iSad, over a second forging roll, then.; Ea ? ii ..;. ieit and subjected to Kach.Behandlung the second bathroom v.ird by diluting a leiles the spinning bath manufactured and enthUlt etv / a '$ for sulfuric acid, such as * \ _t 5 ° / ° zinc sulfate and about 5> » Natriumsulfat'und is maintained at a temperature of about 95 ⁰ C, ./ährend of passing Trittes the threads durcn the iiei & se bath are the same stretched about 140) £. the spinning speed neläuft to about 25 m / min. the fibers are then in ota ] elf fibers with a length of 39 # 7 are now cut and, before drying, the action of a dilute 1 oleic sulfuric acid solution at 96 ⁰ G 15 Subjected for minutes in order to remove the zinc dimethyldithiocarbamate formed by the reaction of the demethylarain-viecose additive and the sulfur and zinc. The dilute acid containing the dissolved product is drawn off and the removal of the remaining compound or complex during the subsequent liquid treatments is completed before the fibers are dried. The fibers are then usually washed in the ice, coated, bleached and dried. In the following xt.belle the physical properties of eier c ^ Auen wieuervege Jen are: —13—

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Table I.

H94598

strength

wet 3 »40 g / denier

conditioned 5.00 g / denier

strain

wet $ 17

conditioned 15 *

Cross-sectional swelling 45.1 * 0

ilaas strength at 5 $ elongation 15

Haaste stiffness factor 20.0, Waaser flow number 9.85

Single fiber bend 115,000 cycles

Cross-sectional skin around 30 ^

Fibrillation _c . no

The rigidity factor is the folding strength in grams per Denier divided by the percentage elongation when wet "

The single-fiber bend is achieved by means of a Test Inc., Arcweld Building, Grove City, Pennsylvania, USA measures the resistance of individual fibers to fatigue when bending »

In this device, a fiber is attached to a reciprocating moving component and passes over a carefully polished rod that has an edge that is abrg * -folded to a diameter of 0.13 mm. The other end of the thread is secured in this case on a small weight · Once, the device a reciprocating movement is imparted to the yarn is _t pulled over the edge of the bar, "the number of individual movement to gears to break ate thread is aurgezeichnet. As indicated in the table above, 10 threads and the number are subjected to this test

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of the work cycles reproduced as soon as the b. of 10 pasers breaks. This is entrusted as the lit'el value. The corresponding test for the Einfiser-Bi- ^ enabel ^; ; .ui't see 69,000 cycles for cotton. Diise Prüivmr stands in direct relation to the wear and tear equipment of textile materials made from these special fibers. The testing methods for the fibers are described in Lefferdink and Briar's paper, "Interpretation of Fiber Properties", published by Textile Research Journal, Volume 29, June 1959.

The fibrillation is measured by exposing the fibers to the action of a striking tool with rotating blades for 20 minutes _; ; subjected and the same are then examined under the microscope.

In the following Table II are additional examples of the Spinning conditions and the properties of the fibers obtained reproduced «

BAD ORIGIMAi

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ο
ο
to
co

- 15 -. Table II

co

ViBioae
5b CS ₂

Spinning bath

Ε _β ο; ·:, η denier

Fiber sheep

_Zerrei S ^en _Deiinui:

festirk. wet
wet ι: / Ί)

Wet strength! «; -

lie 3s te if ^neit "

Α-1
Α-2
Α-3
Α-4

B-1
Β-2
Β-3
Β-4

31
34
37

34

34
34
34
34

6.8
7.2

7.2

7.1
6.4
7.0
0.0

7.3

5.0
4.7

9.0 7.5

3.0

4.9
3.3
6.8
5.0

10.0 10.0

10.3 10.0 10.0 11.6 12.0 12.0 11.6

33
32
32
33
35
30th
30th
30th
30th

156
164
156
136
156
14 '.)
149
149
140

1.24 1.28 0.82 1,? ·! 1.14 1.56 1. 3H 1.46 1.39

17.3
14.4
14.0
13.1,

17.6
19.0

13, H 14.3 13.9 1 5.2 14.9 11.7 15.2 14.1 15.5

i -, 6

έ. ν,

Π, 6

3.7

23.5

12.9

20.0 1 <', ο

In the table below there are further examples of the physi · Kaliscnen jSi / jenschaften der Invention; o ^ eitäss produced Fibers vvieüergegeoenj

Table III

single fibers

Tear resistance
,--/Denier
Conditioned wet

Elongation at break conditions nafi

3.45 2 »03 5.41 2 , 22 5.54 2 , 14 5.39 2 , 06 3.50 2 , 05 3.51 1 , 7ö 2.15 1 , 16 5.16 1 , 97 2.99 1 , 68 2.91 , 01

9.2
9.1
9.15
9.60

9.27
10.8
12.4
11.1
12jO
12.3

8.4 '8.3 9.04 b, 40 8.56 11.1 12.3 11.4 11.8 11.3

In aer iOlgair-en Table IV are further examples of procedures i ".. r the production of the invention i'as reproduced;

Table IV s.-: c ae spinning bath Recken ^J / o

Spinning bath

^: G ->%% ierr.p. H ₂ SO ₄ ZnSO ₄ K

Iu ,1 ^ 5 8th , 15 6.02 1-5 1c , 0 35 7th , 71 6.02 1 -j 1 C- , ^ 16 , 41 5.91 1 y 1 '' _f 4 20th 7th , 71 6.07 13th 1 C , 5 ^ 7 »94 0.13 13th » ³ 27 U , 76 5.90 13th <*
I i , 0 25th 6th , 18 0.15 13th 10 , 7 t £ C 6th 5.97 13th 16 , 9 25th 7th Joo 0.00 13th 't5 25th 6th , 25 0.13 13th 14th 25th 8th , 25 6.00 15th 1': i5 6th , 75 0.02 15th

100 100

bO bO

85

cO

95

100

95 100

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Claims (1)

Pat en t ans prÜ ohe 1, Method of making Eegenera & celluloae-i fibers by splitting out an amine-modified viacosis into a Spinning bath containing sulfuric acid, sodium zinc sulfate low acid and salt content and subsequent flushing out, and then the fibers of an aqueous treatment liquid be subjected and dried to the soliessera, characterized by the3 that Viscose-2ussat? Agent is an aiain that contains sulfur and Zinc is insoluble in water and alkaline solutions The connection is formed and the fibers are thinned Acid solution dissolve and remove before drying the sulphurous and zinc compounds formed by the carbon fiber, treated. ^ 2, procedure according to claim l _t characterized by * ζ verifies that the additive is a manoamino viscose additive. 3, method naoh claim 1, characterized marked-ζ e i c h η e t that the additive is dimethylamine, the zinc dimethylidithioearbamate forms, 4 »Method according to claim 1 to 3, characterized in that dsüS the dilute acid solution Sulfuric acid solution is. 00 9 811/1 3 2 6 ORIGINAL BATHROOM Ϊ5. Staple fiber a: ts ΰβΐ- liosere ^ er.erat, da π η rchge> e η π :: eic t.'r. et, d, a33 ale: .oiie HaouCesti .'-. 'eit, voi ^; 2Us3v / eiue l'J: is 2O _f eir.e r'IIeas number less than 25 _f and with l, i? Denier and length of 39.7 mm each has a card load of less than 3%. BATH ORIGINAL 00981 1/1328