US3419652A - Process for producing highly crimped fibers - Google Patents
Process for producing highly crimped fibers Download PDFInfo
- Publication number
- US3419652A US3419652A US393784A US39378464A US3419652A US 3419652 A US3419652 A US 3419652A US 393784 A US393784 A US 393784A US 39378464 A US39378464 A US 39378464A US 3419652 A US3419652 A US 3419652A
- Authority
- US
- United States
- Prior art keywords
- fibers
- percent
- bath
- temperature
- sulfuric acid
- 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
- 239000000835 fiber Substances 0.000 title description 117
- 238000000034 method Methods 0.000 title description 49
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 119
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 87
- 230000001112 coagulating effect Effects 0.000 description 62
- 229920000297 Rayon Polymers 0.000 description 55
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 34
- 229910000368 zinc sulfate Inorganic materials 0.000 description 34
- 229960001763 zinc sulfate Drugs 0.000 description 34
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 27
- 229910052938 sodium sulfate Inorganic materials 0.000 description 27
- 235000011152 sodium sulphate Nutrition 0.000 description 27
- 229920002678 cellulose Polymers 0.000 description 26
- 239000001913 cellulose Substances 0.000 description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 239000003513 alkali Substances 0.000 description 16
- 238000002788 crimping Methods 0.000 description 16
- 230000018109 developmental process Effects 0.000 description 16
- 150000003839 salts Chemical class 0.000 description 16
- 238000007670 refining Methods 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 241000700143 Castor fiber Species 0.000 description 9
- 239000000243 solution Substances 0.000 description 8
- 238000009987 spinning Methods 0.000 description 7
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 6
- 235000011121 sodium hydroxide Nutrition 0.000 description 6
- 206010016807 Fluid retention Diseases 0.000 description 5
- 229920001407 Modal (textile) Polymers 0.000 description 5
- 239000002253 acid Substances 0.000 description 5
- 238000006116 polymerization reaction Methods 0.000 description 5
- 230000008929 regeneration Effects 0.000 description 4
- 238000011069 regeneration method Methods 0.000 description 4
- 239000003929 acidic solution Substances 0.000 description 3
- 230000032683 aging Effects 0.000 description 3
- 238000004043 dyeing Methods 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000011260 aqueous acid Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- QGJOPFRUJISHPQ-NJFSPNSNSA-N carbon disulfide-14c Chemical compound S=[14C]=S QGJOPFRUJISHPQ-NJFSPNSNSA-N 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 230000002040 relaxant effect Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- IRHVLQMEQPABHG-ZLYSWTFPSA-N (3r,4r,5r,6r,7r,8r,9s,10r,13r,14r,17r)-3,4,6,7-tetrahydroxy-17-[(1s)-1-[(2s,4s)-6-hydroxy-4-propan-2-yloxan-2-yl]ethyl]-10,13-dimethyl-1,2,3,4,5,6,7,8,9,11,12,14,16,17-tetradecahydrocyclopenta[a]phenanthren-15-one Chemical compound C1[C@H](C(C)C)CC(O)O[C@@H]1[C@@H](C)[C@@H]1[C@@]2(C)CC[C@@H]3[C@@]4(C)CC[C@@H](O)[C@H](O)[C@@H]4[C@@H](O)[C@H](O)[C@H]3[C@H]2C(=O)C1 IRHVLQMEQPABHG-ZLYSWTFPSA-N 0.000 description 1
- SMNDYUVBFMFKNZ-UHFFFAOYSA-N 2-furoic acid Chemical compound OC(=O)C1=CC=CO1 SMNDYUVBFMFKNZ-UHFFFAOYSA-N 0.000 description 1
- STOOUUMSJPLRNI-UHFFFAOYSA-N 5-amino-4-hydroxy-3-[[4-[4-[(4-hydroxyphenyl)diazenyl]phenyl]phenyl]diazenyl]-6-[(4-nitrophenyl)diazenyl]naphthalene-2,7-disulfonic acid Chemical compound OS(=O)(=O)C1=CC2=CC(S(O)(=O)=O)=C(N=NC=3C=CC(=CC=3)C=3C=CC(=CC=3)N=NC=3C=CC(O)=CC=3)C(O)=C2C(N)=C1N=NC1=CC=C([N+]([O-])=O)C=C1 STOOUUMSJPLRNI-UHFFFAOYSA-N 0.000 description 1
- SGHZXLIDFTYFHQ-UHFFFAOYSA-L Brilliant Blue Chemical compound [Na+].[Na+].C=1C=C(C(=C2C=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C=2C(=CC=CC=2)S([O-])(=O)=O)C=CC=1N(CC)CC1=CC=CC(S([O-])(=O)=O)=C1 SGHZXLIDFTYFHQ-UHFFFAOYSA-L 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- BPHHNXJPFPEJOF-UHFFFAOYSA-J chembl296966 Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]S(=O)(=O)C1=CC(S([O-])(=O)=O)=C(N)C2=C(O)C(N=NC3=CC=C(C=C3OC)C=3C=C(C(=CC=3)N=NC=3C(=C4C(N)=C(C=C(C4=CC=3)S([O-])(=O)=O)S([O-])(=O)=O)O)OC)=CC=C21 BPHHNXJPFPEJOF-UHFFFAOYSA-J 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- ZOOODBUHSVUZEM-UHFFFAOYSA-N ethoxymethanedithioic acid Chemical compound CCOC(S)=S ZOOODBUHSVUZEM-UHFFFAOYSA-N 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012991 xanthate Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc 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
-
- 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
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/02—Chemical after-treatment of artificial filaments or the like during manufacture of cellulose, cellulose derivatives, or proteins
Definitions
- ABSTRACT OF THE DISCLOSURE A process for producing highly crimped viscose fibers which includes extruding a viscose containing at least 4% cellulose, and having a viscosity of from 100 to 1000 poises and a salt point of at least 16, into a coagulating bath containing zinc sulfate, formaldehyde and a small amount of sulfuric acid, stretching the thus formed fibers in an aqueous bath at a temperature of from 66 to 88 C. under substantially tensionless conditions, and relaxing the stretched fibers in an aqueous bath at a temperature of from 30 to 70 C.
- This invention relates to highly crimped viscose fibers having good dimensional stability and nonuniform crosssectional structure and to a process for producing the fibers.
- high-wet-modulus fibers which have improved dimensional stability. These fibers are produced generally by extruding a viscose of high viscosity and of high gamma value into a coagulating bath of low acid and low salt content. Since coagulation of viscose is slow under these conditions, the cross section of the fibers is circular and the cross-sectional structure is uniform. As in the case of conventional crimped viscose fibers, it is possible to give polynosic fibers some extent of crimp by stretching the fibers as they emerge from a coagulating bath, cutting to staple length and then relaxing the fibers in an aqueous bath.
- the percentage crimp thus obtained is generally less than 5 percent and it is difficult to make it more than 6 percent. Moreover the crimp of these fibers is lost by applying only a small load and the crimp cannot be re covered by removing the load. Accordingly it is essentially impossible for polynosic fibers to be used as crimped fibers.
- a viscose which contains 4 weight percent of cellulose, and has a viscosity of from 100 to 1000 poises and a salt index (salt point) of more than 16 is extruded into a coagulating bath containing from 0.05 to 0.5 g./l. of zinc sulfate, from 10 to 250 g./l. of sodium sulfate and from 6 to 20 g./l. of formaldehyde and sulfuric acid having such a concentration as defined in the following formulas, the fibers thus formed are Withdrawn from said bath and stretched in a bath of water or diluted aqueous acid solution at a temperature from 60 C.
- the fibers produced by the present invention have remarkably superior crimp characteristics. For example, they can have more than 12 crimps per inch, more than 9 percent crimp and more than percent of crimp elasticity. Crimp stability is better than that of conventional crimped viscose staple fibers. Crimp recovery in Water is also superior. These superior properties are due to the nonuniform structure of fiber cross section. It is surprising that fibers produced at the extremely slow coagulating conditions of viscose as in the present invention show the same nonuniform cross-sectional structure as those produced by the so called conjugate spinning process. As hereinafter described, such advantages can only be gained by a specified combination of various conditions of the viscose, coagulating bath, stretching bath and crimping bath, all of which are significant points of the present invention.
- Fibers produced according to the present invention not only have superior crimp characteristics but also have exceedingly superior mechanical properties. This is, tenacity, elongation and wet modulus of the fibers are about the same as those of the latest known polynosic fibers. Dry
- the fibers produced by the present invention have good dimensional stablity and can stand repeated washing. Knot strength and abrasion resistance are also excellent. Water retention is about 70 percent. This value is about the same or slightly higher than that of latest polynosic fibers and it is a sufiicient value for water resistance and dimensional stability. The fact is that the fibers of the present invention are not low in water retention dyeing properties.
- the skin layer is biassed, the core is exposed to the outside and the fiber cross sectional structure is as nonuniform as that of the so-called conjugate spinning fibers.
- the present fibers have good spinability to yarn and can be used in a wide variety of fabrics with or without synthetic or cotton fibers. Fabrics converted from the present fibers have comfortable hand, high slip-resistance, high dimensional stability and superior mechanical properties.
- a process having similarity to the present invention is I disclosed in Japanese Patent No. 452,141.
- This process relates to producing fibers having dry tenacity of more than 5 g./d., wet tenacity of more than 4 g./d., water retention of less than 55 percent and circular cross-sectional structure by extruding a viscose containing cellulose of a high degree of polymerization, having high viscosity and high gamma value into a coagulating bath of relatively low acid concentration containing formaldehyde and subsequently subjecting the extruded fibers to a high extent of stretch in a hot aqueous bath.
- the present invention relates to a process for producing highly crimped fibers having nonuniform crosssectional structure using a specified viscose, coagulating bath and stretching conditions. It is impossible to produce the highly crimped fibers of the present invention by use of the method of the Japanese patent.
- the cellulose concentration in the viscose is more than 4 percent by weight. When it is lower than 4 percent, development of crimps is not satisfactory.
- Preferable cellulose concentration is from 6 to 10 percent by weight.
- the alkali concentration in the viscose is preferably from 2 to 8 percent by weight and more preferably from 3 to 6 percent by Weight.
- the ratio of alkali to cellulose is particularly preferable when it is in the range of from 0.521 to 0.7: 1.
- the viscosity of the viscose must be in the range of from 100 to 1000 poises. Beyond this range, development of crimps is not satisfactory. Most preferably, the viscosity is from 200 to 700 poises.
- the salt index of the viscose to be used in spinning must be higher than 16. With a value less than 16, satisfactory crimp development cannot be obtained. Most preferably, the salt index is from to 23.
- the coagulating bath must contain sulfuric acid, sodium sulfate, Zinc sulfate and formaldehyde.
- the concentration of sulfuric acid is calculated in accordance with the concentration of alkali in the viscose.
- the sulfuric acid concentration must be in the following range:
- concentration lower than the above-defined range development of crimps is not satisfactory and spinning operations are difiicult.
- concentration higher than that range deveolpment of crimps become impossible.
- the concentration of sodium sulfate must be from 10 to 250 g./l., preferably from 50 to g./l. for fibers having deniers of 2 or less than 2 and preferably from to g./l. for fibers having deniers of more than 2.
- the concentration of zinc sulfate must be from 0.05 to 0.5 g./l. When the coagulating bath contains less than 0.0 5 g./l. of zinc sulfate or it does not contain zinc sulfate at all, the development of crimps becomes insufficient and When the bath contains higher than 0.5 g./l. of Zinc sulfate extruded fibers stick together and thus, crimps can not be developed.
- the concentration of zinc sulfate is from 0.1 to 0.3 g./l. It is possible to replace Zinc sulfate with cadmium, sulfate or nickel sulfate but ammonium sulfate or magnesium sulfate is not effective.
- the formaldehyde concentration must be from 6 to 20 g./l. At concentrations lower than 6 g./ 1., develop- Inent of crimps is not sufficient and at concentrations higher than 20 g./l., crimp development becomes insufficient. Most preferably, the concentration of formaldehyde is from8 to 15 g./l.
- the temperature of coagulating bath is preferably from 15 C. to 25 C.
- the length of immersion in the coagulating bath is suitably in the range of from 20 cm. to 60 cm. Fibers emerging from the coagulating bath can not develop sufficient crimps unless they are stretched under conditions of high gamma value.
- the gamma value of the viscose to be spun is 78
- the gamma value of fibers emerging from the coagulating bath is from 60 to 75 to be most suitable.
- the preferred gamma value of fibers emerging from the coagulating bath for the development of crimps is in the range of 60 to 80.
- Fibers emerging from the coagulating bath are subjected to stretching in an aqueous stretching bath.
- the temperature of the stretching bath must 'be from 60 C. to 88 C. If it is outside this range, suflicient crimps cannot be developed.
- a particularly preferred temperature of the stretching bath is from 70 C. to 83 C.
- a water bath may be used but an aqueous bath containing a low concentration of sulfuric acid is preferably used as the stretching bath.
- An aqueous bath containing sulfuric acid salts may also be used.
- a stretching bath having a sulfuric acid content of about 10 g./l. is most preferable. The percent stretch in the stretching bath is dependent upon the temperature of the stretching bath and the formaldehyde concentration in the coagulating bath.
- T C. is the temperature of the stretching bath
- F g./-l.
- Minimum stretch (percent) 2T-]-3.3F-96
- Maximum stretch (percent) 4T+6.6F 144
- Maximum stretch (percent) is preferably 3T+6.6F-128 for fibers having deniers of 2 or less than 2.
- the above two formulas have been empirically derived from many experimental results.
- the tension applied to the fibers in the stretching bath is not more than 0.2 g./d. and preferably, it is from 0.05 to 0.02 g./d. This is a significant point of the present invention.
- the stretching tension exceeds 0.2 g./d. it is impossible to produce fibers having non-uniform cross-sectional structure and accordingly it is impossible to develop crimps.
- the fibers stretched as described above are subjected to relaxation in an aqueous bath to develop crimps.
- the temperature of the relaxation bath must be in the range of from 30 C. to 70 C. Outside this range, development of crimps becomes insufiicient and properties of resulting fibers are poor.
- the temperature of the relaxation bath is from 40 C. to 60 C.
- the relaxation bath can be water for a diluted acidic aqueous bath.
- the fibers may be treated with a diluted acidic solution at a temperature higher than 70 C. to complete regeneration after development of crimps.
- the fibers may be cut to staple length after development of crimps but are preferably out before development of crimps.
- the crimped fibers obtained by the present invention are treated with from 2 to 4 percent by weight of a dilute aqueous sodium hydroxide solution at room temperature after completing regeneration, the crimp characteristics may be improved.
- this viscose was cooled, deaerated, ripened, and extruded through spinnerets at a viscosity of 250 poises, a salt index of 20 and a gamma value of 80 into a coagulating bath containing 14 -g./l. of sulfuric acid, 75 g./l. of sodium sulfate, 0.2 g./l. of zinc sulfate and 14 g./l. of formaldehyde at a temperature of 20 C.
- the length of bath immersion was 33 cm. and the gamma value of fibers emerging from the coagulating bath was 64.
- the fibers were stretched to 150 percent of their original length, namely to a stretch ratio of 2.50:1, in a second bath containing 10 g./l. of sulfuric acid at a temperature of 80 C., cut to staple and subjected to relaxation in a crimping bath containing 10 g./l. of sulfuric acid at a temperature of 50 C. to develop crimps.
- the crimped fibers were subjected to a convention-a1 refining process. The properties and characteristics of the resulting fibers were as follows.
- the resulting viscose was filtered, cooled, deaerated, ripened and extruded at a viscosity of 500 poises and a salt index of 20, into a coagulating bath containing 16 g./l. of sulfuric acid, 75 g./l. of sodium sulfate, 0.2 g./l. of zinc sulfate and 8 g./l. of formaldehyde at a temperature of 25 C.
- the length of bath immersion was 30 cm. and the gamma value of fibers emerging from the coagulating bath was 66.
- the fibers were cut to staple length and subjected to a stretching and relaxation treatment under the same conditions as in Example 1 to obtain crimped fibers.
- the properties and crimp characteristics of the resulting fibers were as follows.
- Fibers emerging from the coagulating bath were stretched percent in a second bath containing 10 g./l. of sulfuric acid at a temperature of 70 C., cut to staple and subjected to relaxation in a crimping :bath containing 10 g./l. of sulfuric acid at a temperature of 50 C. to develop crimps, and to a conventional refining process.
- the properties and crimp characteristics of resulting fibers were as follows.
- Skin dyeing was conducted in an aqueous solution containing 1 percent by weight of J apanol Brilliant Blue 6 BKX (C.I. Direct Blue 1) and 10 percent by weight of sodium chloride at a temperature of 100 C. for 30 minutes, followed by decoloration of the core and dehydration.
- J apanol Brilliant Blue 6 BKX C.I. Direct Blue 1
- 10 percent by weight of sodium chloride at a temperature of 100 C. for 30 minutes
- Core dyeing was conducted in an aqueous solution containing 1 percent by weight of Solophenyl Fast Blue Green BL (C.I. Direct Green 27) and. 0.3 percent by Weight of sodium sulfate at room temperature for 5 hours, followed by washing with water.
- Solophenyl Fast Blue Green BL C.I. Direct Green 27
- EXAMPLE 4 Alkali cellulose produced by a conventional method was subjected to aging, added to 57 percent, based upon the weight of cellulose, of carbon disulfide, xanthated at a temperature of 26 C. for 2 hours and dissolved in an 1 aqueous caustic soda solution and water to obtain viscose containing 7 percent by weight of cellulose and 4 percent by weight of alkali.
- Fibers emerging from the coagulating bath were stretched 125 percent in a second bath containing 10 g./l. of sulfuric acid at a temperature of 70 C., out to staple length and subjected to relaxation in a crimping bath containing 10 g./l. of sulfuric acid at a temperature of 50 C. to develop crimps and to a conventional refining process.
- Crimp characteristics of the resulting fibers were as follows. As a control, fibers were produced by the same conditions as in Example 4 except that viscose ripened at 14 C. and having a salt index of 15 was used. The properties of the resulting fibers were very much the same as in Example 4. Crimp characteristics in both the cases were as follows.
- Viscose produced according to the same method as in Example 4 was extruded into a coagulating bath containing 18 g./l. of sulfuric acid, 125 g./l. of sodium sulfate, 0.2 g./l. of zinc sulfate and 10 g./l. of formaldehyde at a temperature of 20 C.
- Fibers emerging from the coagulating bath were stretched 175 percent in a second bath containing 10 g./l. of sulfuric acid at a temperature of 85 C., cut to staple length and subjected to relaxation in a crimping bath containing 10 g./l. of sulfuric acid at a temperature of 50 C. to develop crimps and to a conventional refining process.
- EXAMPLE 7 The same viscose as in Example 4 was extruded into a coagulating bath containing 18 g./l. of sulfuric acid, 50
- Fibers emerging from the coagulating bath were stretched 150 percent in a second bath containing 10 g./l. of sulfuric acid at a temperature of 80 C., out to staple length and subjected to relaxation in a crimping bath containing 10 g./l. of sulfuric acid at a temperature of 50 C. and to a conventional refining process.
- the properties and crimp characteristics of resulting fibers are shown in the following table.
- the properties and crimp characteristics of a control produced by the same method as in the present example except that the concentration of formaldehyde was 5 g./l. are also shown in the same table.
- Fibers emerging from the coagulating bath were stretched 150 percent in a second bath containing 10 g./l. of sulfuric acid at a temperature of 80 C., cut to staple length and subjected to relaxation in a crimping bath containing 10 g./l. of sulfuric acid at a temperature of C. to develop crimps and to a conventional refining process.
- the properties and crimp characteristics of the resulting fibers together with those of controls produced by the same conditions as in the present example except that sulfuric acid concentrations were 11 g./l. and 38 g./l. respectively, are shown in the following table.
- Viscose prepared under the same conditions as in Example 1 was extruded into a coagulating bath containing 16 g./l. of sulfuric acid, g./l. of sodium sulfate, 0.2 g./l. of zinc sulfate and 10 g./l. of formaldehyde at a temperature of 20 C. Fibers emerging from the coagulating bath, were stretched percent in a second bath containing 10 g./1. of sulfuric acid at a temperature of 70 C., cut to staple length and subjected. to relaxation in a crimping bath containing 10 g./l. of sulfuric acid at a temperature of 50 C. to develop crimps and to a conventional refining process.
- the properties and crimp characteristics of resulting fibers are shown in the following table.
- the properties and crimp characteristics of fibers crimped at a temperature higher or lower than those in the present example are added to the table. When the temperatures of the crimping bath is higher than 70 C., fibers stick together.
- Fibers emerging from the coagulating bath were stretched 150 percent in a second bath containing 10 g./l. of sulfuric acid at a temperature of 80 C. cut to staple length and subjected to relaxation in a crimping bath containing 10 g./l. of sulfuric acid at a temperature of 50 C. to develop crimps and to a conventional refining process. Sections prepared from the resulting fibers were skindyed as in Example 3. As controls, nonstretched fibers and fibers stretched by 350 percent were likewise skindyed.
- EXAMPLE 14 Viscose produced by the same conditions as in Example 4 was extruded into a coagulating bath containing 30 g./l. of sulfuric acid, 150 g./l. of sodium sulfate, 0.2 g./l. of zinc sulfate and 10 g./l. of formaldehyde at a temperature of 20 C. The fibers emerged from the coagulating bath were stretched 175 percent in a second bath containing 10 g./l.
- Example 4 Alkali cellulose produced by the same method as in Example 4 was aged, added to percent, based upon the Weight of cellulose, of carbon disulfide, xanthated for 2 hours at a temperature of 26 C. and dissolved in an aqueous caustic soda solution and water to give a viscose containing 8 percent by weight of cellulose and 4 percent by weight of alkali.
- the viscose was filtered, cooled, deaerateld, ripened rand extruded through spinnerets at a viscosity of 400 poises and a salt index of 20 g. into a coagulating bath containing 30 g./l.
- a process for producing highly crirnped viscose fibers which comprises extruding a viscose containing at least 4 percent cellulose, said viscose having a viscosity of from 100 to 1000 poises and a salt point of at least 16, into a coagulating bath containing from 0.05 to 0.5 g./l. zinc sulfate, from to 250 g./l. sodium sulfate, from 6 to g./l.
- F is the concentration of formaldehyde (g./l.) in the cogulating bath
- the coagulating bath contains from 0.05 to 0.4 g./l. of zinc sulfate, from 10 to 100 g./l. of sodium sulfate, from 6 to 15 g./l. of formaldehyde and a concentration of sulfuric acid of from 2A+4 to 3A+8.
- the coagulating bath contains from 0.1 to 0.3 g./l. of zinc sulfate, from 50 to g./l. of sodium sulfate, from 8 to 14 g./l. of formaldehyde and a concentration of sulfuric acid of from 2A+4 to 3A+ 8.
- the coagulating bath contains from 0.05 to 0.5 g./l. of zinc sulfate, from to 250 g./l. of sodium sulfate, from 6 to 20 g./l. of formaldehyde and a concentration of sulfuric acid of from 4A+4 to 7A+8.
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 |
---|---|---|---|
JP4783563 | 1963-09-10 |
Publications (1)
Publication Number | Publication Date |
---|---|
US3419652A true US3419652A (en) | 1968-12-31 |
Family
ID=12786401
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US393784A Expired - Lifetime US3419652A (en) | 1963-09-10 | 1964-09-01 | Process for producing highly crimped fibers |
Country Status (5)
Country | Link |
---|---|
US (1) | US3419652A (xx) |
BE (1) | BE652867A (xx) |
CH (1) | CH449842A (xx) |
DE (1) | DE1494674C3 (xx) |
GB (1) | GB1080671A (xx) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3487593A (en) * | 1966-11-03 | 1970-01-06 | Norton Co | Method for producing a stretchresistant coated abrasive product |
US3539679A (en) * | 1965-08-03 | 1970-11-10 | Mitsubishi Rayon Co | Process for producing polynosic fibers |
US3632468A (en) * | 1968-04-09 | 1972-01-04 | Rayonier Inc | High-crimp, high-strength rayon filaments and staple fibers and process for making same |
US3689622A (en) * | 1969-06-24 | 1972-09-05 | Mitsubishi Rayon Co | Method for producing highly crimped regenerated cellulose fibers by solvent stretching |
USRE31380E (en) * | 1975-11-07 | 1983-09-13 | Avtex Fibers Inc. | Rayon fibers containing starch |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3046083A (en) * | 1960-06-06 | 1962-07-24 | American Viscose Corp | Method for producing crimped rayon staple fiber |
US3107970A (en) * | 1960-10-04 | 1963-10-22 | Toho Rayon Kk | Process for the manufacture of high tenacity viscose rayon |
US3108849A (en) * | 1960-10-27 | 1963-10-29 | Mitsubishi Rayon Co | Process for producing viscose regenerated cellulose fibers |
US3109698A (en) * | 1962-04-02 | 1963-11-05 | Courtaulds North America Inc | Method for making high tenacity regenerated cellulose staple fiber |
US3226461A (en) * | 1962-02-27 | 1965-12-28 | Courtaulds North America Inc | Manufacture of regenerated cellulose fibers from viscose |
-
1964
- 1964-08-04 GB GB31515/64A patent/GB1080671A/en not_active Expired
- 1964-08-27 DE DE1494674A patent/DE1494674C3/de not_active Expired
- 1964-09-01 US US393784A patent/US3419652A/en not_active Expired - Lifetime
- 1964-09-09 CH CH1178564A patent/CH449842A/fr unknown
- 1964-09-09 BE BE652867D patent/BE652867A/xx unknown
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3046083A (en) * | 1960-06-06 | 1962-07-24 | American Viscose Corp | Method for producing crimped rayon staple fiber |
US3107970A (en) * | 1960-10-04 | 1963-10-22 | Toho Rayon Kk | Process for the manufacture of high tenacity viscose rayon |
US3108849A (en) * | 1960-10-27 | 1963-10-29 | Mitsubishi Rayon Co | Process for producing viscose regenerated cellulose fibers |
US3226461A (en) * | 1962-02-27 | 1965-12-28 | Courtaulds North America Inc | Manufacture of regenerated cellulose fibers from viscose |
US3109698A (en) * | 1962-04-02 | 1963-11-05 | Courtaulds North America Inc | Method for making high tenacity regenerated cellulose staple fiber |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3539679A (en) * | 1965-08-03 | 1970-11-10 | Mitsubishi Rayon Co | Process for producing polynosic fibers |
US3487593A (en) * | 1966-11-03 | 1970-01-06 | Norton Co | Method for producing a stretchresistant coated abrasive product |
US3632468A (en) * | 1968-04-09 | 1972-01-04 | Rayonier Inc | High-crimp, high-strength rayon filaments and staple fibers and process for making same |
US3689622A (en) * | 1969-06-24 | 1972-09-05 | Mitsubishi Rayon Co | Method for producing highly crimped regenerated cellulose fibers by solvent stretching |
USRE31380E (en) * | 1975-11-07 | 1983-09-13 | Avtex Fibers Inc. | Rayon fibers containing starch |
Also Published As
Publication number | Publication date |
---|---|
CH449842A (fr) | 1968-01-15 |
GB1080671A (en) | 1967-08-23 |
DE1494674C3 (de) | 1975-11-20 |
DE1494674A1 (de) | 1970-03-12 |
BE652867A (xx) | 1964-12-31 |
DE1494674B2 (de) | 1975-04-10 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
US2705184A (en) | Process for the production of rayon products | |
US2572936A (en) | Process for making crimped artificial filaments | |
US3720743A (en) | Process for producing high performance crimped rayon staple fiber | |
US5358679A (en) | Manufacture of regenerated cellulosic fiber by zinc free viscose process | |
US3419652A (en) | Process for producing highly crimped fibers | |
US3337671A (en) | Method of making regenerated cellulose filaments | |
US4364889A (en) | Process for preparing a cotton-like rayon fiber | |
US3108849A (en) | Process for producing viscose regenerated cellulose fibers | |
US3324216A (en) | Viscose spinning process | |
US2491938A (en) | Method of producing viscose filaments | |
US3352957A (en) | Process for spinning cellulosic fibers | |
US3107970A (en) | Process for the manufacture of high tenacity viscose rayon | |
US2841462A (en) | Production of all skin rayon | |
US3226461A (en) | Manufacture of regenerated cellulose fibers from viscose | |
US3351696A (en) | Method for producing regenerated cellulose products | |
US3574812A (en) | Process for producing polynosic fibers | |
US3109698A (en) | Method for making high tenacity regenerated cellulose staple fiber | |
US2114915A (en) | Process of spinning rayon and the bath used | |
US2347883A (en) | Production of cellulosic structures | |
US2347884A (en) | Method of producing cellulosic structures | |
US3494996A (en) | Method for producing high tenacity rayon | |
US2315560A (en) | Method for producing high strength and crimped staple fibers from viscose | |
US3340340A (en) | Manufacture of crimped viscose rayon fibres | |
US3097914A (en) | Process for the production of a ribbon filament yarn of regenerated cellulose | |
US2594496A (en) | Method of making artificial fibers or threads from viscose |