US3632722A - Rayon process - Google Patents

Rayon process Download PDF

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Publication number
US3632722A
US3632722A US795681*A US3632722DA US3632722A US 3632722 A US3632722 A US 3632722A US 3632722D A US3632722D A US 3632722DA US 3632722 A US3632722 A US 3632722A
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Prior art keywords
fibers
bath
stretching
acid
treated
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US795681*A
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English (en)
Inventor
Takashi Asaeda
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Tachikawa Research Institute
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Tachikawa Research Institute
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Classifications

    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose

Definitions

  • the application discloses a process for producing highly polymerized viscose rayon filaments having high loop and knot tenacity. Fibers of high viscosity are spun into a low acid concentration bath and before fixing in a hot acid bath are stretched either in air or in a separate bath. After stretching the fibers are introduced into a separate bath which is substantially neutral and has a temperature of from to 40 C. As a modification, a second separate bath is employed into which the fibers are introduced after the first mentioned separate bath and his bath has a temperature of from 30 to 80 C. and has a pH of 8 to 10.5.
  • Such a fact may depend on the fact that in the high polymerization-low acid process strain is apt to result within the fibers and the strain is more easily fixed in the fibres in comparison with that which occurs in conventional viscose processes.
  • Our applied process is characterized by the fact that the spun thread is treated, between its stretching stage and heat-setting stage, by water, a diluted solution of acid or weak alkaline neutral-salt or weak alkaline acidsalt whose pH is in the range from 1.4 to 10.5, being selected in conformity with the degree of development of the inner structure of the thread.
  • the object of our invention is to provide improved fiber of highly polymerized rayon filament having high loop and knot tenacity without any deterioration of its so-called polynosic characteristics (hereinafter referred to as improving-effect).
  • the spun threads immediately after leaving the spinning bath have a double layer structure whose inner layer consists of non-decomposed cellulose xanthate, the outer one consisting of regenerated cellulose with extremely low degree of coagulation. Therefore, the development of fiber structure is attained mainly outside the spinning bath, and yet its progress is very slow because the acid content of the liquor attached to the filaments is very low.
  • the spun thread is stretched immediately after leaving the spinning bath in order to increase the tenacity of the fibers. Therefore, in the high polymerization-low acid process, the stretching is applied at a relatively early stage of fiber formation, and the development of the fiber structure, that is, the hydrogen bonding, occurs mainly after the stretching stage.
  • the essential points of our process exist in that, firstly the spun threads must be relaxed before the heat-setting stage and, secondly, the condition of the relaxing liquor should be determined in conformity with the degree of development of the fiber structure during the treatment.
  • the fiber structure changes from the stretching stage to the heat-setting stage. Therefore, the suitable conditions of the relaxing liquor must be chosen corresponding to its stage of the treatment. Practically speaking, the relaxing liquor must have such an intensity that it can relax the amorphous regions only but has no influence upon the crystal regions.
  • the relaxing intensity is too low for the fiber structure, then the desired improvement will not occur and, if it is too high, then although the improvement is sufficient, the crystal regions may be disturbed, and various defects, for instance, the decreasing of the polynosic characteristics or the formation of sticky fibers will result.
  • the stages of fiber developments after the spinning bath and prior to the heat-setting stage are threefold, viz fiber condition during the stretching stage and immediately after the stretching and after travelling a certain distance in the air after stretching.
  • the threads must be treated by a diluted acid liquor whose pH-value is more than 1.27 in order to obtain the desired improvement.
  • the acid concentration of the treating liquor should be lower than that of the liquor previously attached to the fibers. Then the acid concentration in the surrounding liquor of the fibers is lowered, and the fiber structure which have already developed corresponding to the liquor attached to the fibers shall be relaxed, and accordingly the strain which is to occur at the stretching is limited.
  • the treating-liquor in this case must be acidic, and water or an alkaline liquor is too strong for the relaxation of the fiber structure, and accordingly the formation of the sticky-fibers or the deterioration of the polynosic characteristics may be caused.
  • Table 2 a treating liquor that will not change the y-value of the threads should be used. This case is shown in Example 1.
  • the threads must be treated by using water or a solution whose pH-value is 7 or thereabouts containing extremely small quantity of acids, alkalis, or salts. By the said treatment only the amorphous regions are relaxed and the desired improvement will be obtained.
  • the desired improving-effect is obtained by treating the threads using an alkaline solution whose pH-value is 8 to 10.5.
  • the neutral salts or acid salts, whose aqueous solutions are alkaline are suitable as treating agents.
  • acid salts as sodium bicarbonate or disodium hydrogen phosphate exhibit an excellent improving-effect in a certein concentration range Without causing any damage to the polynosic characteristics of the fibers.
  • the pH- value of the solutions of such acid salts is nearly constant irrespective of their concentration, as shown in Table 4.
  • the relaxing-ability has no relation to their concentration, because the relaxingability depends mainly on the concentration of the hydroxyl ions (pH-value).
  • the presence of the salts is antagonistic to the relaxing action of the relaxing action of the hydroxyl ions hereinafter referred to as the salt-effect.
  • the range of relaxing effect is rather limited up to in the relatively lower-ordered regions where the strains are accumulated.
  • the formation of the sticky fibers is also restrained in proportion to the salt concentration.
  • caustic soda solution or ammonia water indicates a high pH-value even in low concentration, and with these agents the suitable pH-value for the relaxing treating can be attained at extremely low concentration, so that the salt-eifect can not be expected from such caustic alkalis. Therefore, damage to the polynosic characteristics occur under conditions where strain is eliminated from the fibers. For that reason, caustic alkalis are not desirable in the process.
  • sodium carbonate or sodium silicate presents some danger on account of their fairly strong alkali content although they are neutral salts. But it is not so unfavorable as caustic alkalis.
  • Example 6 The process employing the multi-step treatments at succeeding time periods is also possible.
  • Example 6 The process using the two-step treatment is shown in Example 6, and that of the three-step treatment is shown in Example 7.
  • R is an alkyl radical having more than twelve carbon atoms
  • R R and R are one of the following radicals, i.e. methyl, ethyl, hydroxymethyl, and hydroxyethyl radicals
  • X is halogen or sulphate radical.
  • the outer layer of regenerated cellulose makes a harder structure due to stretching in comparison with the corresponding structure of the conven tional viscose process.
  • This hard structure of the outer layer completely overcomes the contraction force of the inner layer which occurs as a result of the hot bath treatment. As a consequence, the contraction force of the inner layer produces a strain within the fibers.
  • EXAMPLE 4 A viscose having a high viscosity and a high 'y-value is EXAMPLE 1 spun in a low acid concentration bath. After the stretch- Viscose having a ball-falling viscosity of 420 sec. and 5 ing, the tow is cut t the r d length- T u fi s r -yalue of 63 is spun at 30 in a spinning bath cOntreated at various temperatures by a liquor containing 3 taining 17 g./l. of sulphurlc acid, 60 g./l. of sodium sulof NaHCOB, and am successively treated at phate, and 0.5 g./1. of zinc sulphate.
  • the spun threads are assin thm h h t b th t 3 /l f 1 led to the stretching device after passing through guides p g ug a f a con ammg Suand a drawing roller.
  • the concentration of sulphuric acid 10 P mud to fix the Inner structure of the fibersin a. liquor attached to the fibers at the entrance of the The results are shown in Table in comparison with stfetchlng dtfvlce 1S 11 (P the non-treated fibers. In this experiment, the influence Whlle bemg Stretched.
  • threads are treated by various 11qu1ds having the acid conr h d th tent shown in the 1st column of Table 2 and a temperam a mon to t e Stu y of e lmprovmg'efiect of ture shown in the 4th column of Table 2.
  • the results are a- Y these treatments the curled fibers are shown in Table 2 in comparison with the non-treated tained whose curl number is 9 to 10 per 2.5 cm. fibers.
  • a viscose same as Example 2 is spun at 30 C. in a spinning bath containing 18.5 g./l. of sulphuric acid, 60 g./l. of sodium sulphate, and 0.45 g./l. of zinc sulphate. After the stretching on the stretching device the threads are cut to desired length. The cut fibers are treated at 55 C. for 5 minutes by liquids containing various quantities of Na HPO and are successively treated at 85 C. passing through a hot acid containing 3 g./l. of sulphuric acid to fix the inner structure of the fibers.
  • EXAMPLE 7 A viscose having a ball-falling viscosity of 450 sec. and a y-value of 72 is spun at 31 C. in a spinning bath containing 18.4 g./l. of sulphuric acid, 60 g./l. of sodium sulphate, and 0.4 g./l. of zinc sulphate.
  • the tow is treated on the stretching device at 16 C. by a liquor containing 3.1 g./l. sulphuric acid and 0.3 g./l. of dimethyl stearyl B-hydroxyethyl ammonium chloride, and are successively treated by an aqueous liquor containing 0.5 g./l. of the above-mentioned surface active agent.
  • the cut fibers are treated at 40 C. for 2 minutes by a liquor containing 3 g./l. of Na HOP and are immediately treated at 90 C. on passing through a hot acid bath to fix the inner structure of the fibers.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Artificial Filaments (AREA)
  • Air Transport Of Granular Materials (AREA)
US795681*A 1964-11-02 1969-01-31 Rayon process Expired - Lifetime US3632722A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP6184164 1964-11-02

Publications (1)

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US3632722A true US3632722A (en) 1972-01-04

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US795681*A Expired - Lifetime US3632722A (en) 1964-11-02 1969-01-31 Rayon process
US795682*A Expired - Lifetime US3632723A (en) 1964-11-02 1969-01-31 Viscose rayon process
US795680*A Expired - Lifetime US3632721A (en) 1964-11-02 1969-01-31 Process for improvement on viscose rayon filaments

Family Applications After (2)

Application Number Title Priority Date Filing Date
US795682*A Expired - Lifetime US3632723A (en) 1964-11-02 1969-01-31 Viscose rayon process
US795680*A Expired - Lifetime US3632721A (en) 1964-11-02 1969-01-31 Process for improvement on viscose rayon filaments

Country Status (10)

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US (3) US3632722A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
AT (1) AT283578B (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
BE (1) BE671154A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
CH (1) CH497555A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
DK (1) DK120608B (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
ES (1) ES319358A1 (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
FI (1) FI43216B (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
GB (1) GB1082899A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
NL (1) NL6514182A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
NO (1) NO117649B (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070184079A1 (en) * 2000-04-05 2007-08-09 The Cupron Corporation Antimicrobial and antiviral polymeric materials
US20080241530A1 (en) * 2007-03-28 2008-10-02 The Cupron Corporation Antimicrobial, Antifungal and Antiviral Rayon Fibers
US20080311165A1 (en) * 2004-11-07 2008-12-18 The Cupron Corporation Copper Containing Materials for Treating Wounds, Burns and Other Skin Conditions
US20090010969A1 (en) * 2004-11-09 2009-01-08 The Cupron Corporation Methods And Materials For Skin Care

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107999508A (zh) * 2017-11-07 2018-05-08 宜宾丝丽雅股份有限公司 一种粘胶废渣处理方法

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070184079A1 (en) * 2000-04-05 2007-08-09 The Cupron Corporation Antimicrobial and antiviral polymeric materials
US9439437B2 (en) 2000-04-05 2016-09-13 Cupron Inc. Antimicrobial and antiviral polymeric materials
US20080311165A1 (en) * 2004-11-07 2008-12-18 The Cupron Corporation Copper Containing Materials for Treating Wounds, Burns and Other Skin Conditions
US20090010969A1 (en) * 2004-11-09 2009-01-08 The Cupron Corporation Methods And Materials For Skin Care
US9403041B2 (en) 2004-11-09 2016-08-02 Cupron Inc. Methods and materials for skin care
US9931283B2 (en) 2004-11-09 2018-04-03 Cupron Inc. Methods and materials for skin care
US20080241530A1 (en) * 2007-03-28 2008-10-02 The Cupron Corporation Antimicrobial, Antifungal and Antiviral Rayon Fibers
US8741197B2 (en) * 2007-03-28 2014-06-03 Cupron Inc. Antimicrobial, antifungal and antiviral rayon fibers

Also Published As

Publication number Publication date
GB1082899A (en) 1967-09-13
ES319358A1 (es) 1966-04-16
US3632723A (en) 1972-01-04
AT283578B (de) 1970-08-10
CH497555A (de) 1970-10-15
BE671154A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html) 1966-02-14
FI43216B (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html) 1970-11-02
NO117649B (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html) 1969-09-08
US3632721A (en) 1972-01-04
NL6514182A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html) 1966-05-03
DE1494757A1 (de) 1969-12-11
DK120608B (da) 1971-06-21

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