US3007766A - Production of viscose rayon - Google Patents
Production of viscose rayon Download PDFInfo
- Publication number
- US3007766A US3007766A US781491A US78149158A US3007766A US 3007766 A US3007766 A US 3007766A US 781491 A US781491 A US 781491A US 78149158 A US78149158 A US 78149158A US 3007766 A US3007766 A US 3007766A
- Authority
- US
- United States
- Prior art keywords
- viscose
- threads
- bath
- grams per
- strength
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 229920000297 Rayon Polymers 0.000 title claims description 44
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 238000000034 method Methods 0.000 claims description 18
- 239000000835 fiber Substances 0.000 claims description 15
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 13
- 230000008569 process Effects 0.000 claims description 13
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 13
- 235000011152 sodium sulphate Nutrition 0.000 claims description 13
- 150000001412 amines Chemical class 0.000 claims description 12
- -1 ALKALI METAL SALT Chemical class 0.000 claims description 10
- 229910052783 alkali metal Inorganic materials 0.000 claims description 10
- 239000003607 modifier Substances 0.000 claims description 6
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 4
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 4
- 239000011260 aqueous acid Substances 0.000 claims description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 19
- 235000002639 sodium chloride Nutrition 0.000 description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 14
- 239000002964 rayon Substances 0.000 description 13
- 239000002253 acid Substances 0.000 description 12
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 8
- 229910000368 zinc sulfate Inorganic materials 0.000 description 8
- 229960001763 zinc sulfate Drugs 0.000 description 8
- 229920002678 cellulose Polymers 0.000 description 7
- 235000010980 cellulose Nutrition 0.000 description 7
- 238000009987 spinning Methods 0.000 description 6
- 239000001913 cellulose Substances 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 235000019864 coconut oil Nutrition 0.000 description 4
- 239000003240 coconut oil Substances 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 235000011151 potassium sulphates Nutrition 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical class OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920000768 polyamine Polymers 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 150000003856 quaternary ammonium compounds Chemical class 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- GKQHIYSTBXDYNQ-UHFFFAOYSA-M 1-dodecylpyridin-1-ium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+]1=CC=CC=C1 GKQHIYSTBXDYNQ-UHFFFAOYSA-M 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 239000007832 Na2SO4 Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- ZOOODBUHSVUZEM-UHFFFAOYSA-N ethoxymethanedithioic acid Chemical compound CCOC(S)=S ZOOODBUHSVUZEM-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000006259 organic additive Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- 230000005070 ripening Effects 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000012991 xanthate Substances 0.000 description 1
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
- D01F2/08—Composition of the spinning solution or the bath
- D01F2/10—Addition to the spinning solution or spinning bath of substances which exert their effect equally well in either
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S264/00—Plastic and nonmetallic article shaping or treating: processes
- Y10S264/27—Process of spinning viscose where viscose has high degree of polymerization
Definitions
- This invention relates to the production of rayon threads and fibers and more particularly to the production of such threads and fibers having low elongation values and high strength values.
- the threads or fibers having such low elongation values and high strength values find particular use in rubber products.
- modulus M 1OO times break strength (grams/ den.):-elongation percent.
- An additional object of the present invention is to provide a simple and economical process for manufacturing rayon blends and fibers of low elongation values and high strength values.
- rayon threads and fibers of low elongation values and high breaking strength and therefore high moduli can be obtained by adding to the viscose rayon solution a watersoluble alkali metal salt of a strong acid. Up to 50 grams/ kg. of such a salt may be added.
- modifier in the viscose such as an ethoxylated amine or similar agent such as ethoxylated fatty acids or alcohols, polyethylene glycols, amines, polyamines, quaternary ammonium compounds,
- the modifier may be present to the extent of 0.3 to 3.0 grams/kg. of viscose.
- the preferred method of accomplishing this invention is to add the alkali metal salt to the caustic soda dissolving solution for the cellulose Xanthate.
- the thus obtained viscose after it has been filtered, deaerated, and finally ripened in the known manner, is spun into a spin bath containing sulfuric acid, zinc sulfate and sodium sulfate.
- the thread or fiber is then passed into an intermediate bath containing sulfuric acid, Zinc sulfate, sodium sulfate and preferably formaldehyde, and finally into a second acid bath containing sulfuric acid, zinc sulfate, sodium sulfate and preferably formaldehyde in different concentrations than used in either the first acid bath or the intermediate bath. Thereafter the thread or fiber thus obtained is simultaneously stretched and dried.
- the alkali metal salt of the strong acid may be any one of the following which have been found to accomplish the objects of this invention: sodium sulfate, sodium chloride, potassium sulfate, potassium chloride, sodium nitrate or potassium nitrate.
- the alkali metal salts of phosphoric acid have been found to give a lower moduli than the above listed salts.
- the salts of weak acids are ineffective and will not accomplish the objects of this invention.
- Tables II and III illustrate the effect of using various quantities of sodium sulfate and sodium chloride, respectively, in the process of this invention. These salts were added, together with 1.5 grams of an ethoxylated coconut oil amine of a molecular weight of about 1100 per kilogram of viscose.
- alkali metal salt may be added in proportions of 350 grams/kg. of viscose.
- ethoxylated fatty acids ethoxylated fatty alcohols
- polyethylene glycols amines
- polyamines polyamines
- quaternary ammonium compounds or their exthoxylated derivatives
- These addition agents may be added in proportion of 0.3 to 3.0 grams/ kg. of viscose with the preferred proportion being 1.5 grams/ kg.
- This viscose following filtering, deaeration, and ripening in the known manner, is spun with a gamma number of about 48 and a viscosity by the ball-falling test of 93 seconds.
- a spinning nozzle having 1000 orifices of a diameter of 60 microns each is used to obtain a titre of 1650 denier.
- the spun thread runs from the spinning nozzle through a horizontally disposed tube of a length of 50 cm. and an internal diameter of 20 mm, which tube is submerged in an acid spinning bath. This bath is maintained at 48 C. and contains 4.3% sulfuric acid, 13.0% sodium sulfate, and 6.0% zinc sulfate.
- the spun thread leaves the tube and passes over a guide roller to a godet rotating at 19 m./ min.
- the thread is caused to travel four times around this godet by a grooved roller arranged below it.
- This grooved roller is submerged in a so-called intermediate bath containing 22 grams/kg. sulfuric acid, grams/kg. sodium sulfate, 38 grams/ kg. zinc sulfate, and 18 grams/kg. formaldehyde and maintained at 30 C. The above proportions are expressed in grams per kilogram of bath solution.
- This second acid bath contains 15 grams/kg. sulfuric acid and small amounts of sodium sulfate, zinc sulfate and formaldehyde. The proportion of the sulfuric acid is based on the total bath composition.
- the trajectory length of this second acid bath is 140 cm.
- the thread passes from this second acid bath around a third godet rotating at 35.8 rn./min., into a slowly rotating bucket.
- the mass of threads While remaining in this bucket is deacidified, desulfurized and sized by any methods known in the art. Thereafter, the thread is removed from the bucket and stretched 11% in a final stretching assembly While being simultaneously dried.
- the thread produced by this method is indicated in Table II as No. 6.
- the thread has a very desirable high breaking strength, low elongation value and therefore a high modulus.
- cellulose of any origin may be used, such as linters, high-grade celluloses, and standard rayon celluloses. It is possible to vary the cellulose content or the cellulose/caustic ratio without departing from the scope of this invention.
- the viscose solutions obtained by the process of this invention are spun with a gamma number between 56 and 35 into acid baths which contain preferably more than 20 grams/ kg. of zinc sulfate.
- the spinning baths may contain viscose and/or spinning auxiliaries such a lauryl pyridinium chloride, or other surface-active agents.
- a process for the production of high strength vis- M 100 S divided by E wherein M is the modulus, S is the dry strength in grams per denier, and E is the dry elongation, which comprises extruding viscose containing about 3.0 to 50 grams per kilogram of viscose, of an alkali metal salt of the class consisting of sodium sulfate and potassium sulfate, about 0.3 to 3.0 grams per kilogram of viscose, of a modifier of the class consisting of polyethylene glycols, ethoxylated amines and their quaternized derivatives, into an aqueous acid zinc-containing spin bath, passing the thus produced threads to an intermediate bath containing taining formaldehyde, and finally collecting the same.
- a process according to claim 7 in which the threads after having been collected and purified are dried under tension.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Artificial Filaments (AREA)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DEV13660A DE1052054B (de) | 1958-01-04 | 1958-01-04 | Verfahren zur Herstellung von Faeden oder Fasern mit niedriger Dehnung und hoher Festigkeit durch Verspinnen einer Viskose |
Publications (1)
Publication Number | Publication Date |
---|---|
US3007766A true US3007766A (en) | 1961-11-07 |
Family
ID=7574297
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US781491A Expired - Lifetime US3007766A (en) | 1958-01-04 | 1958-12-19 | Production of viscose rayon |
Country Status (7)
Country | Link |
---|---|
US (1) | US3007766A (en)) |
BE (1) | BE574151A (en)) |
CH (1) | CH411220A (en)) |
DE (1) | DE1052054B (en)) |
FR (1) | FR1211235A (en)) |
GB (1) | GB864821A (en)) |
NL (2) | NL107735C (en)) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3351696A (en) * | 1960-04-22 | 1967-11-07 | Cta Cie Ind De Textiles Artifi | Method for producing regenerated cellulose products |
US3364290A (en) * | 1962-10-30 | 1968-01-16 | American Enka Corp | High tenacity rayon yarn production |
US4182735A (en) * | 1978-05-25 | 1980-01-08 | International Paper Company | Production of high crimp, high strength, hollow rayon fibers |
US4242411A (en) * | 1978-05-25 | 1980-12-30 | International Paper Company | High crimp, high strength, hollow rayon fibers |
US5482776A (en) * | 1988-10-05 | 1996-01-09 | Asahi Kasei Kogyo Kabushiki Kaisha | Viscose rayon fiber having superior appearance |
CN105780173A (zh) * | 2014-12-04 | 2016-07-20 | 财团法人纺织产业综合研究所 | 纤维的制备方法与纺丝粘液 |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE19754314A1 (de) * | 1997-12-08 | 1999-06-10 | Henkel Kgaa | Hilfsmittel für die Herstellung von Cellulosefasern |
Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2439039A (en) * | 1944-09-26 | 1948-04-06 | American Viscose Corp | Process of producing medullated artificial filaments |
US2452130A (en) * | 1943-12-17 | 1948-10-26 | American Enka Corp | Method of spinning high tenacity viscose rayon |
US2572217A (en) * | 1950-01-23 | 1951-10-23 | American Enka Corp | Manufacture of viscose rayon |
US2787517A (en) * | 1953-02-10 | 1957-04-02 | American Enka Corp | Manufacture of artificial viscose products |
US2852334A (en) * | 1954-11-03 | 1958-09-16 | American Viscose Corp | Method of producing viscose rayon |
US2852333A (en) * | 1954-05-21 | 1958-09-16 | Du Pont | Viscose spinning process |
US2937070A (en) * | 1955-08-02 | 1960-05-17 | Du Pont | Viscose process |
-
0
- NL NL234167D patent/NL234167A/xx unknown
- NL NL107735D patent/NL107735C/xx active
-
1958
- 1958-01-04 DE DEV13660A patent/DE1052054B/de active Pending
- 1958-12-03 CH CH6687158A patent/CH411220A/de unknown
- 1958-12-17 FR FR1211235D patent/FR1211235A/fr not_active Expired
- 1958-12-19 US US781491A patent/US3007766A/en not_active Expired - Lifetime
- 1958-12-22 BE BE574151A patent/BE574151A/fr unknown
- 1958-12-30 GB GB42047/58A patent/GB864821A/en not_active Expired
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2452130A (en) * | 1943-12-17 | 1948-10-26 | American Enka Corp | Method of spinning high tenacity viscose rayon |
US2439039A (en) * | 1944-09-26 | 1948-04-06 | American Viscose Corp | Process of producing medullated artificial filaments |
US2572217A (en) * | 1950-01-23 | 1951-10-23 | American Enka Corp | Manufacture of viscose rayon |
US2787517A (en) * | 1953-02-10 | 1957-04-02 | American Enka Corp | Manufacture of artificial viscose products |
US2852333A (en) * | 1954-05-21 | 1958-09-16 | Du Pont | Viscose spinning process |
US2852334A (en) * | 1954-11-03 | 1958-09-16 | American Viscose Corp | Method of producing viscose rayon |
US2937070A (en) * | 1955-08-02 | 1960-05-17 | Du Pont | Viscose process |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3351696A (en) * | 1960-04-22 | 1967-11-07 | Cta Cie Ind De Textiles Artifi | Method for producing regenerated cellulose products |
US3364290A (en) * | 1962-10-30 | 1968-01-16 | American Enka Corp | High tenacity rayon yarn production |
US4182735A (en) * | 1978-05-25 | 1980-01-08 | International Paper Company | Production of high crimp, high strength, hollow rayon fibers |
US4242411A (en) * | 1978-05-25 | 1980-12-30 | International Paper Company | High crimp, high strength, hollow rayon fibers |
US5482776A (en) * | 1988-10-05 | 1996-01-09 | Asahi Kasei Kogyo Kabushiki Kaisha | Viscose rayon fiber having superior appearance |
CN105780173A (zh) * | 2014-12-04 | 2016-07-20 | 财团法人纺织产业综合研究所 | 纤维的制备方法与纺丝粘液 |
Also Published As
Publication number | Publication date |
---|---|
CH411220A (de) | 1966-04-15 |
FR1211235A (fr) | 1960-03-15 |
NL234167A (en)) | 1900-01-01 |
NL107735C (en)) | 1900-01-01 |
DE1052054B (de) | 1959-03-05 |
GB864821A (en) | 1961-04-06 |
BE574151A (fr) | 1959-04-16 |
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