US 1996753 A
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Patented g 35 y y I I UNIT D STATES PATENT OFFICE YVAR'N AND ME'rn'on on PRE- lv PARING THE SAME' V I Camille Dreyfus, New York, N. ,Y., and William Y Whitehead; Cumberland; .MdaFassignors to Celanese Corporation of America,;a corpora?- tiontof De lawarev No Drawing: Application June 16,, 1928, i ;Serial No. 286,070 I 1 5Claims. (01.18-54) a I This invention relates to the preparation of formate, cellulose-propionate and cellulose butyartificial yarns andparticularly' yarns-made of rate while examples of cellulose ethers are methyl Containing organic derivativesfof cellulose cellulose, ethyl cellulose and ,benzyl cellulose. Such as iq l e acetate from solutions contain- However, because'of the superior results obtained 5 ingthe same. by its use, we prefer cellulose acetate whichrrnay E 6 Anobject of ouriinventionis to prepare yarns or may not be solublep m p c fically containing organic derivativesjofrcellulose, parwe prefer to use. an acetime soluble cellulose aceticularly cellulose acetate, which yarns are'eastatehav'ing anacetylwalue of 52.5% to 56%; and c J ilywettedj bywater, whereby fabri d of preferably 5 l x5%', but thisinvention is not limited 10 the same. may be readily scoured, dyed and/or 0 the used u cellulose acetategive an other desired finishing treatment. h l we d n t lim t u selves toa sp oific A further objectrof our.inventionis toprepare o t Solvent o b used r c we artificial yarns containing organic derivatives have'found th t acetone ar b of'cellulos'e such as cellulose acetate, which yarns 's s' tj I l The r la ve 1011:?913 16 may besubjectedtofurthertextilelo er t gs b tile substancexadded tether-spinning solution as knitting or weavin'g'without the "additien f may beanypsuitable substance that. is miscible c lubricants, o 'with the-additionsjofilesslubricants with thecvqlatile Solvent d in e ar n xi hi than have heretoforei'been used; I Spinning 559111121011, a which s 9 Q l b i A furtherobjectfof our invention is td'piii re t is cap i ii ns l ithit e 20 artificial" yarns containing organic" derivatives organiffderivatives 9 19 0 w W- 2 5 jects of ouninventionswillappear fromthe jfol ducedfromsuch solutionsfmay be more, readily of f cellulose and" particularly cellulose acetate, paring I H which'yarns produce. lesssnarlinglin textile:operhave found that r ativ -Volat e al- 'ations and which do not break as readily in looms 9011015 are n t y Suited 9 hi r s W as prior, artificialiyarnsof mistyped-[Other obe found? particularly ithat ht s s ethylene glycol or diethylene glycol give eminently lowingjdetailed' des ipti p v satisfactoryresults," Likewise we havefound'thatci I In thepi' paratidh' ofartifi ia1 f m on glycerol and diacetone alcohol are very us'eful in i garlic. derivatives. of cellulose such; as cellulose ithisvpmcess" A n cont-aming i acetate,lthemostZgenerally usedniethod'involves @1 9 groups ehia e ke on c m w the spinningof solutions of the sarne iniayolatile s fl v u e F h mo lithe-rs 9 m .solv ent into an. evaporative atmosphere; asinthe "relatively Q t F i J Such. as the a dry spinning procession-into a'precipitating bath of glycol d f iof which h m j as in the wet spinning process. M .ethylgther of ethylepe 9 mentioned we have found the surprisingsfactthatfia are suitable foruse n th1srnvent1on; 'I 'he term v v ,atively: nonvolatile substance is added to the freIQftIVEIY non'vqlame t i q as us-ed m f stunningsolution containing the organic derivalispeclfica'twn and m the 019111.115 1s p d tive sofi cellulose, which" substance soluble in i iggq' i igg g igs ggg 52 33 632 ggz water or any other scouring ncy, yarns. proorganic derivatiyesyinlfaivolatfle solvent ov ingthese substances is evaporated at atemper; I 3 g? fgi gifis giig gfifii zg g fi ll l ailre which is suificient to volatilize the volatile 'tio nsis-notgenerally'required 8 open -9 thgse substance mmamlargaily I f d t1l1z ed, and are present in the y arn to.1rnpa r the: o 11, 810001 8,1106 W]. 0111 lIlVell. 1011, prepare c i 14- 'amsolution containingthe. organic derivatives of The amountbtrelativgly non volatfle subs e cellulosecin a volatile-solvent, to. which" solution a is soluble in wa t g aa t th vis: also added a" relativelynon-volatile substance spinning solution, may be varied within wide lur'i t 'WhlCh' is. miscible "Wlth "the? solution, and which t d 'ndingpp'onthe nature ofithe substan ces' m y readlly removed from theyam used andthe resultsrequired? Generallywe have ab q fq e f m' QY y scouring n found that'if the organicderivatives of cellulose M ter or anyo a e scouringzagency; are dissolved in solventmixtures containing from;
Theorganic derivative of cellulose used for l to 30% of the relatively non-volatile substance, making the yarn may be any suitable organic excellent results are obtained. "Theternfierature' esters or ethers of-cellulosei Examples of organic *of the-spinningmay also be 'vari ed in'a ccordance "55 Testers of-cllulose are cellulose-acetate,'-cellmose with-the -natureofth'e- -volatile solventfused'filie accordancewith our process is self lubricated and therefore further lubrication for textile operations nature of the relatively non-volatile substances used, and the relative proportion of non-volatile substances to volatile solvent.
Yarns produced by the dry spinning of solutions of organic derivatives as above described,
retain a large percentage of. the relatively nonvolatile substances added, and sinee these substances are soluble in water, the yarn or the fabric from'which the. yarn is, formed may be readilyi" wetted by water.- This is of great, advantage in such as.winding,twisting, knitting and 'weaving'is not absolutely required with these'yarns. Moreover, these yarns produce less snarling when twisted and less breaking in the loom thanprior yarns, which is obviously a great advantage.
Although the yarns made in accordance with our- 'invention-are weaker than prior yarns while .they'still contain :the relatively non-volatile sub-. stances that have been addedto the spinning solutionj theyare of 'sumcient strength towithstand the strains to whichfthey are subjected in ordinarytextile operations. However, after they are thoroughly scoured, which scouring may bedone onthe yarns priorto making theminto fabric, but
which is; preferably done after they areformed into fabrics, theyarns have strength atleast equal to that of yarns formed from solutionsnotcontaining these relatively non-volatile substances, and in many. cases they are'actually stronger.
Inorder', furtherto illustrate our inventionibut without in anyway limiting ourselves thereby, the
following specific examples are given.
g Exemplar We take. a cellulose acetate having an acetyl .value of 54.5% andaviscosity of 20 as determined on an Oswald Viscosimeter with. a solution'ioffi grams of cellulose" acetateand- IOOgrams of acetone, the visco'sity of glycerol being called 100.) cellulose acetateznormally has 'arnoisture .content. of 5% and maybe used directly in our process. However, if desired,. the cellulose acetate may be placed in a vacumn drier where it is dried at an'elevated temperature under a vacuum of 2 5.f of mercury.I (i e. 5"" of mercury absolute pressure) untilits moisture content is reduced below 1%. The cellulose acetate is then dissolved in a mixture containing from 1to.5% of diethylene glycol and from 99. to 95% of acetone, in
amounts sufficient to. form a solution containing substantially 25%01": celluloseacetate. The solution 'isthen'filtered, andspun in a dry spinning machine wherein thesolvent is evaporated'off at a temperature'ofz55 to (3., the. thread thus formed:'being gathered up and wound or reeled.
. 'Ilheyarhi-prddnced,in manner displays a remarkable increase in ability to being. wetted by wate This is indicated by tl efactj that if a fabric made of this yam'j s placed-on the surface r water, it sinksin l5j seconds, whereas fabric made from yarn which-hasbeen formed from solutions not containing the diethlene glycol does 'lnot sink in water until after 60. seconds.- The yarn is' self lubricated and may be subjected to .textilefoperations, without further lubrication. :A erih varna i cbu e i w crto r move: th
diethylene. glycolywhich present therein and I then dried, the yarn shows an ability to regain moisture of about 8% of itsweight as against about 5% of its weight for a yarn formed in accordance with the prior practices. When this yarn is highly twisted and made; up j into crepe of is level and otherwise satisfactory,a result which was not obtainable by lthe use of yarnmade by priorprocesses.
ErampleIl V Thecelluloseacetate such as described in Exhample I is dissolvedin a solvent mixture containing l' to 10% of diacetone' alcohol and 99 to 90% of fabricssuch as crepe .marocainJthe dyeing therei acetone-respectively, and preferably a solvent mix-,
-ture containing substantially 5% of diacetone alycqhcl and 95% of acetone. The concentration of the solution is such that preferably'it contains about'25% of the cellulose acetate. I The cellulose acetate and'the solventare mixed with thorough agitation for about 5 to 6 hours toobtain a sufficiently homogeneous solution, The solution is thenfiltered and spun in a dry spinning machine :25 Y
wherein the solvent is evaporated offatav temperature of 55 to C., andpreferably atsuch rate'that meters of filament or yarn are formed permin'ute. The thread or yarn thus formed isgathered up and wound or reeled. The
yarn produced in this manner contains diacetone alcohol whichhas not evaporated off at thespinning temperature, and displays all the desirable characteristics. of readiness 'to wetting, 'ease of -dyeing and selfilubrioating'properties as the yarn made in, accordance with Ex'ample I. This yarn afterjwashing in five changes of water'a't- 40 C. has a dry tenacity of 1.4. grams per denier 'as against a tenacity of 1.3 foryarnfprepared from solutions not containing the diacetone alcohol.
' It is ,to" be. understood that the foregoing: de-
taileddescription isgiven merely by way, of illustration and that many variations may be made therein'without departing from the spirit of this invention.
' v Having described our inventionwhatwe claim and desire'to secure: by Letters Patentis:
. 1. The method of' producing yarns containing organic 'derivatives of cellulose which com- 'prises spinning a solution of the organic derivatives of cellulose: ina mixture containing a. vola- "tile' solvent therefor and a relativelynon-volatile polyhydric alcohol that is anon-solvent for the organic derivatives of cellulose and is soluble in water. t t
2. Thej methodof producting yarns containing organicderivatives of cellulose which "comprises dry'spinning a solution of the organic derivatives of cellulosein'a mixture containing a volatile solvent therefor and a relatively nonvolatile polyhydric alcohol that is a non-solvent for-the organic derivatives of cellulose and is soluble in water. v
3. The method of producing yarns containing cellulose acetate which comprises dry spinning a solution of the cellulose acetate in a mixture atively non-volatile polyhydric alcohol that is a non-solvent for the cellulose acetate and is soluble in water;
.4. The method of producing yarns containing cellulosejacetate comprising dry spinning a solution of the cellulose acetate in amixture containing acetone and glycerol. l
5. Ina method of producing yarns containing cellulose acetate,-the step of dry spinning a so- 3 containing a volatile solvent therefor anda relalution of cellulose acetate in acetone which so cellulose acetate, the step of dry spinning a solution of cellulose acetate in acetone which solution also contains diethylene glycol.
7. Yarn containing organic derivatives of cellulose and a relatively non-volatile polyhydric alcohol'that is a non-solventfor the organic deriv'atives of cellulose and is soluble in water.
8. Yarn containing cellulose acetate and a relatively non-volatile polyhydric alcohol thatis a non-solvent for the cellulose acetate and is soluble in water. p
9. Yarn containing cellulose acetate and a glycol.
l0. Yarncontaining cellulose acetate and diethylene glycol. I V
11. The method (is producing yarns contain ing organic derivatives of cellulose, which comprises spinning a solution of the organic deriva, tive of cellulose ina medium containing a vola- 'tile solvent therefor and a proportion of from 1-30% of a relatively non-volatile polyhydric alcohol that is a non-solvent for the organic de- 12. The method of producing yarns containing cellulose acetate, whichcomprises dry s'pinningj; a solution of cellulose acetate in a medium'con taining a volatile solvent therefor 'andla prof v portion of from 1-30% of a relatively non-V012,;- 5 tile polyhydric alcohol that is a non-solve'ntfor I the cellulose acetate and issoluble in water. 1';
13. The method of producing yarns contain ing cellulose acetate, comprising dry-spinning a solution of cellulose acetate in a medium'con 10 f taining acetone and a proportion of from 1-30%; of a glycol. 14. The method of producing yarns containing cellulose acetate, comprising dry-spinning a solution of cellulose acetate in amediumicon taining acetone and a proportion of from 1-30% of diethylene glycol. j
g 15. The method of producing yarns contain-' ing cellulose acetate, comprising dry-spinning a solution of cellulose acetate in a medium contain- 0 ing acetone and a proportion of from 1-30% of glycerol.
WILLIAM WI-HTEHEAD. g