EP2473657A1 - Fire-retardant cellulose fiber, use thereof, and method for the production thereof - Google Patents
Fire-retardant cellulose fiber, use thereof, and method for the production thereofInfo
- Publication number
- EP2473657A1 EP2473657A1 EP10754846A EP10754846A EP2473657A1 EP 2473657 A1 EP2473657 A1 EP 2473657A1 EP 10754846 A EP10754846 A EP 10754846A EP 10754846 A EP10754846 A EP 10754846A EP 2473657 A1 EP2473657 A1 EP 2473657A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- flame
- cellulose
- fibers
- fiber
- viscose
- 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.)
- Granted
Links
- 239000003063 flame retardant Substances 0.000 title claims abstract description 49
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- 229920003043 Cellulose fiber Polymers 0.000 title claims abstract description 6
- 238000000034 method Methods 0.000 title claims description 15
- 239000000835 fiber Substances 0.000 claims abstract description 92
- 239000004753 textile Substances 0.000 claims abstract description 23
- 239000004627 regenerated cellulose Substances 0.000 claims abstract description 5
- 229920000297 Rayon Polymers 0.000 claims description 42
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims description 40
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- 229920002678 cellulose Polymers 0.000 claims description 31
- 239000001913 cellulose Substances 0.000 claims description 31
- 238000009987 spinning Methods 0.000 claims description 26
- 229910052698 phosphorus Inorganic materials 0.000 claims description 23
- 239000011574 phosphorus Substances 0.000 claims description 23
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 17
- 239000006185 dispersion Substances 0.000 claims description 17
- 239000000126 substance Substances 0.000 claims description 16
- -1 phosphorus compound Chemical class 0.000 claims description 13
- 239000000049 pigment Substances 0.000 claims description 13
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 10
- YJWLZUOMOYYHGA-UHFFFAOYSA-N 2-[(5,5-dimethyl-1,3,2-dioxaphosphinan-2-yl)oxy]-5,5-dimethyl-1,3,2-dioxaphosphinane Chemical compound O1CC(C)(C)COP1OP1OCC(C)(C)CO1 YJWLZUOMOYYHGA-UHFFFAOYSA-N 0.000 claims description 8
- 239000003607 modifier Substances 0.000 claims description 8
- 229920000728 polyester Polymers 0.000 claims description 7
- 239000003513 alkali Substances 0.000 claims description 6
- 239000004744 fabric Substances 0.000 claims description 6
- 239000002270 dispersing agent Substances 0.000 claims description 5
- 150000002903 organophosphorus compounds Chemical class 0.000 claims description 5
- 150000001298 alcohols Chemical class 0.000 claims description 4
- 150000002170 ethers Chemical class 0.000 claims description 4
- 229920000151 polyglycol Polymers 0.000 claims description 4
- 239000010695 polyglycol Substances 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- 125000003545 alkoxy group Chemical group 0.000 claims description 3
- 239000004359 castor oil Substances 0.000 claims description 3
- 235000019438 castor oil Nutrition 0.000 claims description 3
- 238000009826 distribution Methods 0.000 claims description 3
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 3
- 229920000847 nonoxynol Polymers 0.000 claims description 3
- 235000021317 phosphate Nutrition 0.000 claims description 3
- 229920005646 polycarboxylate Polymers 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 12
- 239000000203 mixture Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 6
- BWGNESOTFCXPMA-UHFFFAOYSA-N Dihydrogen disulfide Chemical compound SS BWGNESOTFCXPMA-UHFFFAOYSA-N 0.000 description 5
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 229910052938 sodium sulfate Inorganic materials 0.000 description 5
- 235000011152 sodium sulphate Nutrition 0.000 description 5
- 239000004952 Polyamide Substances 0.000 description 4
- 239000004693 Polybenzimidazole Substances 0.000 description 4
- 239000004734 Polyphenylene sulfide Substances 0.000 description 4
- 229920003235 aromatic polyamide Polymers 0.000 description 4
- 229920002647 polyamide Polymers 0.000 description 4
- 229920002480 polybenzimidazole Polymers 0.000 description 4
- 229920000069 polyphenylene sulfide Polymers 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 210000002268 wool Anatomy 0.000 description 4
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 4
- 229960001763 zinc sulfate Drugs 0.000 description 4
- 229910000368 zinc sulfate Inorganic materials 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 229920002972 Acrylic fiber Polymers 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 2
- 229920000433 Lyocell Polymers 0.000 description 2
- 229920002821 Modacrylic Polymers 0.000 description 2
- 239000004962 Polyamide-imide Substances 0.000 description 2
- 229920001108 Polyimide P84 Polymers 0.000 description 2
- PQYJRMFWJJONBO-UHFFFAOYSA-N Tris(2,3-dibromopropyl) phosphate Chemical class BrCC(Br)COP(=O)(OCC(Br)CBr)OCC(Br)CBr PQYJRMFWJJONBO-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 238000010348 incorporation Methods 0.000 description 2
- 239000004951 kermel Substances 0.000 description 2
- 238000009940 knitting Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229920006277 melamine fiber Polymers 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000004745 nonwoven fabric Substances 0.000 description 2
- 238000012803 optimization experiment Methods 0.000 description 2
- 229920002239 polyacrylonitrile Polymers 0.000 description 2
- 229920002312 polyamide-imide Polymers 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- COWMHTOCXHIQHS-UHFFFAOYSA-N 1,2-dichloro-3-[chloro(2,3-dichloropropoxy)phosphoryl]oxypropane Chemical compound ClCC(Cl)COP(Cl)(=O)OCC(Cl)CCl COWMHTOCXHIQHS-UHFFFAOYSA-N 0.000 description 1
- GAUFKBQSTGCCOC-UHFFFAOYSA-N 2-[(5,5-dimethyl-2-sulfanylidene-1,3,2$l^{5}-dioxaphosphinan-2-yl)oxy]-5,5-dimethyl-2-sulfanylidene-1,3,2$l^{5}-dioxaphosphinane Chemical compound O1CC(C)(C)COP1(=S)OP1(=S)OCC(C)(C)CO1 GAUFKBQSTGCCOC-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 101100165186 Caenorhabditis elegans bath-34 gene Proteins 0.000 description 1
- 240000000731 Fagus sylvatica Species 0.000 description 1
- 235000010099 Fagus sylvatica Nutrition 0.000 description 1
- ZCQWOFVYLHDMMC-UHFFFAOYSA-N Oxazole Chemical compound C1=COC=N1 ZCQWOFVYLHDMMC-UHFFFAOYSA-N 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000005708 Sodium hypochlorite Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 150000001555 benzenes Chemical class 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- ZOOODBUHSVUZEM-UHFFFAOYSA-N ethoxymethanedithioic acid Chemical compound CCOC(S)=S ZOOODBUHSVUZEM-UHFFFAOYSA-N 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- JLYXXMFPNIAWKQ-GNIYUCBRSA-N gamma-hexachlorocyclohexane Chemical compound Cl[C@H]1[C@H](Cl)[C@@H](Cl)[C@@H](Cl)[C@H](Cl)[C@H]1Cl JLYXXMFPNIAWKQ-GNIYUCBRSA-N 0.000 description 1
- CAYGQBVSOZLICD-UHFFFAOYSA-N hexabromobenzene Chemical compound BrC1=C(Br)C(Br)=C(Br)C(Br)=C1Br CAYGQBVSOZLICD-UHFFFAOYSA-N 0.000 description 1
- 229920006253 high performance fiber Polymers 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229960002809 lindane Drugs 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 230000000051 modifying effect Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 150000003021 phthalic acid derivatives Chemical class 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- PJNLXXROLSYGPE-UHFFFAOYSA-N tris(1-bromo-3-chloropropan-2-yl) phosphate Chemical compound ClCC(CBr)OP(=O)(OC(CCl)CBr)OC(CCl)CBr PJNLXXROLSYGPE-UHFFFAOYSA-N 0.000 description 1
- 238000009941 weaving 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
-
- 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
-
- 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
-
- 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
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2913—Rod, strand, filament or fiber
- Y10T428/2933—Coated or with bond, impregnation or core
Definitions
- the present invention provides flame-retarded cellulosic regenerated fibers having improved functional properties for textile
- Fibers by the viscose process are mainly known today as cellulosic regenerated fibers and are produced worldwide for standard applications in the textile and nonwovens sector with a single fiber titer of between 0.8 and 16 dtex.
- flame-retardant finish of viscose fibers various chemicals are described in the literature. Above all, flame retardants based on halogens, silicon and phosphorus are used.
- the patent US2678330 describes the use of a bis (2,3-dichloropropyl) chlorophosphonate for this purpose.
- the publication GB1158231 mentions the use of a tris (1-bromo-3-chloro-2-propyl) phosphate.
- the patent FR2138400 describes the use of liquid polybromobenzenes and more preferably hexabromobenzene. Since liquid flame retardants are only embedded in the structure of the fiber but do not bind to the cellulose component, the migration of these chemicals from the fiber is significantly higher than with solid substances. Especially after repeated drying at high temperatures (e.g., in the tunnel dryer), the flame retardancy of the fiber can be significantly reduced.
- the Soviet patent SU661047 also describes the use of halogenated compounds such as hexachlorocyclohexane, halogenated benzenes and tris (dibromo-propyl) phosphate.
- halogenated flame retardants was in recent years due to ecological Concerns greatly reduced and does not represent a sustainable solution for future developments.
- Tris (dibromo-propyl) phosphate for example, even led by the Oeko-Tex® community as a prohibited flame retardant.
- Viscose fibers whose flame retardant effect relies on the use of silicates - described e.g. in the patents W09313249 or CN1847476 - are ecologically harmless, but by no means meet the
- Patent EP0836634 describes a flame-retarded regenerated fiber made by the lyocell process which would theoretically meet the above requirements. The production of there
- Dispersions for the flame-retardant finish of viscose fibers are Dispersions for the flame-retardant finish of viscose fibers.
- EP1882760 also describes the preparation of flame-retardant
- Viscose fibers using flame retardant dispersions based on a 2,2'-oxybis [5,5-dimethyl-1, 3,2-dioxaphosphorinan] 2,2'disulfide There is described as an important feature of the invention that the particle size may be a maximum of 10 pm and that the spinning mass must therefore be cleaned before spinning through filters with a maximum mesh size of 10 pm. However, it has been found that this criterion is not sufficient to produce fibers that describe the one described here
- Particle size of 10 pm may be for viscose filaments, i. H.
- Endless filaments sufficient, but far from meeting the requirements of modern staple fiber production with fiber finenesses of about 1 to 4 dtex; a 1, 3 dtex fiber has a diameter of about 10 pm.
- Standard viscose fibers are now widely used in light-weight fashion textiles.
- the low strength, especially when wet, the high elongation and the high surface shrinkage put the use of viscose but limits.
- these textile properties do not permit use in segments which require frequent washing (especially in industrial washes) of the textiles.
- a measure of the washability is the area shrinkage.
- BISFA wet modulus measured according to the regulations of BISFA and therefore hereafter called BISFA wet modulus (BISFA, Testing Methods Viscose, Modal, Lyocell and Acetate Staple Fibers and Tows, 2004 Edition).
- the fibers described in the prior art, or commercially available are all made by standard viscose methods. Although they show comparatively good mechanical fiber data for flame-retardant viscose fibers, since the phosphorus contents are very low.
- Synthetic high performance fibers such as (aromatic) polyamides, aramids, polyimides and the like are already commonly used for such products.
- these fibers have a low wearing comfort, since they are not able to absorb moisture sufficiently.
- the prior art merely discloses
- this object could be achieved by a flame-retardant regenerated cellulose fiber for textile applications, which as a flame-retardant substance, a spun, particulate,
- Phosphorus compound preferably contains an organophosphorus compound and has a use value between 6 and 35, preferably between 8 and 35 and particularly preferably between 10 and 35.
- Such a fiber could be produced for the first time by a modified viscose process according to the invention.
- This flame retardant substance preferably has one
- organophosphorus compound 2,2'-oxybis [5,5-dimethyl-1,3,2-dioxaphosphorinan] 2,2'-disulfide (Formula I) is preferably used.
- This substance is among others under the trade names Exolit and Sandoflam in
- the fiber according to the invention contains at least 2.8%, preferably between 3.2% and 6.0%, particularly preferably between 3.5% and 6.0% phosphorus, in each case based on cellulose.
- a flame-retarded fiber of the invention having a BISFA wet modulus B m of greater than or equal to 0.5 x (V " T) x 10 ⁇ at an elongation of 5% in the wet state, where T is the denier of a single fiber , expressed in dtex, B m is expressed in cN / tex.
- the fiber according to the invention is present as a staple fiber, d. H. it becomes uniform throughout the manufacturing process
- Usual cutting lengths for staple fibers for the textile sector are between about 20 and 150 mm. Only such a uniform length of all Fibers allow easy processing on today's in the textile chain usual machines with high productivity.
- the present invention also provides the use of the fiber according to the invention for the production of a game.
- a yarn is characterized by yarns made of fibers, which were previously available, by a significantly higher strength. Order for the respective
- such yarn according to the invention in addition to the fibers according to the invention may also contain fibers of other origin, for example wool, flame-retardant wool, para- and meta-aramids, polybenzimidazole (PBI), p-phenyl-2,6-Bezobisoxazol (PBO ), Polyimide (P84®), polyamideimide (Kermel®), modacrylic, polyamides, flame-retarded polyamides, flame-retarded acrylic fibers, melamine fibers, polyesters, flame-retardant polyesters, polyphenylene sulfide (PPS), polytetrafluoroethylene (PTFE), glass fibers, cotton, silk,
- fibers of other origin for example wool, flame-retardant wool, para- and meta-aramids, polybenzimidazole (PBI), p-phenyl-2,6-Bezobisoxazol (PBO ), Polyimide (P84®), polyamideimide (Kermel®
- PANOX® oxidized thermally stabilized polyacrylonitrile
- this fabric may also contain other fibers, for example and in particular wool,
- PPS Polyphenylene sulfide
- PTFE polytetrafluoroethylene
- PANOX® fibers Polyacrylonitrile (PANOX®) fibers and electrically conductive fibers, and mixtures of these fibers.
- the sheet is preferably a woven, knitted or knitted fabric, but may in principle also be a nonwoven. Also for high quality nonwovens is the use of fibers with high BISFA wet modulus and high strength crucial.
- the mixture of the fibers according to the invention with the other fibers is either by mixing before yarn production, the so-called
- the fiber according to the invention can be replaced by an inventive
- Endless filaments have been known in principle for many years and, for example, described in detail by K. Götze, Chemiefasern nach den Viskoseclar, 1967.
- the textile properties of the resulting fibers and filaments are significantly affected by many parameters.
- limits are set for many influencing factors by the design of the existing production plants, which can not be exceeded for technical or economic reasons, so that any variations of the parameters are often not possible and therefore the expert would not have caused this.
- the spinning parameters must be adjusted accordingly due to the Zudöstechnik the flame-retardant FR-pigment.
- the invention therefore also provides a process for producing a flame retarded regenerated cellulose fiber for textile applications by spinning a viscose with a content of 4 to 7% cellulose, 5 to 10% NaOH, 36 to 42% (based on cellulose) carbon disulfide and 1 to 5% (based on cellulose) of a modifier in a spin bath, stripping off the coagulated filaments, using a viscose whose spin gamma value is 50 to 68, preferably 55 to 58, and whose Spinning viscosity is 50 to 120 falling seconds; and that the
- the final discharge takes place from the spinning bath at a speed between 5 and 60 m / min and
- a pigmented organophosphorus compound is spun in the form of a pigment dispersion.
- a viscose is used, to which the modifier is added only shortly before the spinning of the viscose.
- Cellulosic molecules bound carbon disulfide molecules.
- Spinning gamma value is determined according to Zellcheming leaflet draft by R. Stahn [1958] or leaflet III / F 2.
- the term "falling ball” is understood to mean the viscosity determined by the falling ball method; it is expressed in terms of bullet seconds. The determination is given in K. Götze, Chemiefasern [1951], p. 175.
- the flame retardant phosphorus compound which is prepared as a pigment, according to the invention, the viscose spinning solution in the form of a
- Pigment dispersion added.
- the finished fiber contains at least 2.6%, preferably between 3.2% and 6.0%, more preferably between 3.5% and 6.0% phosphorus, based on cellulose.
- a flame retardant which is particularly suitable for the purposes of the present invention is
- Organophosphorus compound 2,2'-oxybis [5,5-dimethyl-1,3,2-dioxaphosphorinane] 2,2'-disulphide is an important component of the pigment dispersion.
- the quality of the pigment dispersion has a significant influence on the fiber properties. This is determined by the average and maximum particle size of the pigments, the concentration of the dispersion in use, d. H. during the addition to the viscose spinning solution, as well as the type and amount of the dispersing aids.
- Fig. 2 shows a size distribution of a still suitable pigment dispersion.
- the pigment dispersion should contain between 10 and 50% of the flame retardant.
- the influence of the dispersant is not described as fully as it would be appropriate. Many chemicals that have a superbly stabilized
- Flame retardant provide, but have a negative impact on the spinning process, as they also have a modifying effect in the viscose, but not positively affect the fiber strength, in contrast to the modifiers used. As ideal
- Dispersants for the flame retardant dispersion for the production of the fibers according to the invention which do not adversely affect the fiber strength, have been found to be particularly those selected from the group consisting of containing modified polycarboxylates, water-soluble polyesters,
- the pigment dispersion should contain between 1, 5 and 13% of the dispersing aid.
- Alkylpolyglykoletherphosphorklareester 6 parts by weight of 2,2'-oxybis [5,5-dimethyl-1, 3,2-dioxaphosphorinan] 2,2'disulfide, 6 parts by weight of water and 0.55 parts by weight Alkylpolyglykoletherphosphorklareester be homogenized by means of a dissolver and in a stirred ball mill (Drais, type Perl Mill PML-V / H) with ZirkonoxidmahlSystemn at a temperature of 40-55 ° C.
- the alkali cellulose nonwoven was fiberized, aged and sulfided.
- the xanthate was dissolved with a dilute sodium hydroxide solution to a viscose with 5.6% cellulose, 6.8% NaOH and 39% CS 2 , based on cellulose.
- the viscose was filtered 4 times and vented. The viscose was 1 h before spinning 3%, based on cellulose, ethoxylated amine, a
- the nozzles used have a nozzle hole diameter of 60 ⁇ m.
- the spin bath contains 72 g / l sulfuric acid, 120 g / l sodium sulfate and 60 g / l zinc sulfate.
- the spinning bath temperature was 38 ° C.
- Regenerated plastic thread strand of pale yellow color was over a Galette (G 1) in a second bath, whose temperature was 95 ° C, out and stretched there between G 1 and a second galette (G 2) by 120%.
- the final discharge was 42 m / min.
- the tow was cut into stacks of 40 mm in length which were completely dissolved in dilute sulfuric acid
- the nozzles used have a Düsenioch preparer of 50 pm.
- the spin bath contains 73 g / l sulfuric acid, 120 g / l sodium sulfate and 58 g / l zinc sulfate.
- Example 4 (comparative example) A fiber was made according to the teaching of CN 101037812. Since no information is given on the wet modulus in this publication, the conditions of the example with the highest wet strength (Example 2, 1, 52 cN / tex) of the obtained fiber were selected and
- the nozzles used have a nozzle hole diameter of 60 pm.
- the spin bath contains 15 g / l of sulfuric acid, 330 g / l of sodium sulfate and 45 g / l of zinc sulfate.
- a fiber was made according to CN1904156, with the process conditions specifically recommended there being set:
- the nozzles used have a nozzle hole diameter of 60 pm.
- the spinning bath contains 1 15 g / l sulfuric acid, 350 g / l sodium sulfate and 1 1 g / l Zinksulfati
- the spinning bath temperature was 49 ° C.
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AT0137109A AT508687A1 (en) | 2009-09-01 | 2009-09-01 | FLAME-RESTRICTED CELLULOSIC FIBER, THEIR USE AND METHOD FOR THE PRODUCTION THEREOF |
PCT/AT2010/000273 WO2011026159A1 (en) | 2009-09-01 | 2010-07-27 | Fire-retardant cellulose fiber, use thereof, and method for the production thereof |
Publications (2)
Publication Number | Publication Date |
---|---|
EP2473657A1 true EP2473657A1 (en) | 2012-07-11 |
EP2473657B1 EP2473657B1 (en) | 2014-04-30 |
Family
ID=42830479
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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EP10754846.3A Active EP2473657B1 (en) | 2009-09-01 | 2010-07-27 | Fire-retardant cellulose fiber, use thereof, and method for the production thereof |
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US (1) | US20120177919A1 (en) |
EP (1) | EP2473657B1 (en) |
CN (1) | CN102482800B (en) |
AT (1) | AT508687A1 (en) |
ES (1) | ES2487494T3 (en) |
TW (1) | TWI476309B (en) |
WO (1) | WO2011026159A1 (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP3476985A1 (en) | 2017-10-27 | 2019-05-01 | Lenzing Aktiengesellschaft | Fireproof cellulosic man-made fibres |
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DE102011101321A1 (en) * | 2011-05-12 | 2012-11-15 | Glanzstoff Bohemia S.R.O. | Flame-retardant cellulose regenerated filament fibers and process for its preparation |
AT511638B1 (en) | 2011-06-21 | 2016-06-15 | Glanzstoff Bohemia Sro | HIGHLY CELLULOSIC FILAMENT, ITS USE AND METHOD FOR THE PRODUCTION THEREOF |
AT511746B1 (en) * | 2011-08-10 | 2013-12-15 | Chemiefaser Lenzing Ag | ACTIVATED CARBON-CONTAINING CELLULOSIC MAN-MADE FIBER AND METHOD FOR THE PRODUCTION AND USE THEREOF |
TW201335450A (en) * | 2012-02-24 | 2013-09-01 | Acelon Chem & Fiber Corp | Manufacturing method for natural cellulose fiber having flame resistant function |
ES2569859T3 (en) * | 2012-05-14 | 2016-05-12 | Glanzstoff Bohemia S.R.O. | Regenerated cellulose fibers flame retardant and manufacturing process |
CN103668619B (en) * | 2012-09-14 | 2017-06-09 | 美利肯公司 | Yarn, textile material and the clothes containing it |
AT513426A1 (en) * | 2012-09-17 | 2014-04-15 | Chemiefaser Lenzing Ag | Spun-dyed modal fiber, its use and process for its preparation |
AT514469B1 (en) * | 2013-01-11 | 2015-04-15 | Chemiefaser Lenzing Ag | Flame retardant fabric for protective clothing and upholstery fabrics applications and its use |
US10443153B2 (en) | 2014-03-11 | 2019-10-15 | Smartpolymer Gmbh | Flame-resistant molded cellulose bodies produced according to a direct dissolving method |
AT516414B1 (en) | 2014-10-28 | 2017-07-15 | Chemiefaser Lenzing Ag | Liquid-soaked non-woven fabric containing zinc oxide-containing cellulose fibers |
CN104988616A (en) * | 2015-05-28 | 2015-10-21 | 安徽省含山县顺天纺织有限公司 | Blending reprocessed cotton yarn capable of emitting anions and being good for health, and preparation method thereof. |
CN104988618A (en) * | 2015-05-29 | 2015-10-21 | 安徽省含山县顺天纺织有限公司 | Stretch-proofing mekralon blending reprocessed cotton yarn and preparation method thereof |
CN104963048A (en) * | 2015-05-29 | 2015-10-07 | 安徽省含山县顺天纺织有限公司 | Blending regeneration cotton yarn with ray proof efficacy and preparation method thereof |
CN105040207A (en) * | 2015-05-29 | 2015-11-11 | 安徽省含山县顺天纺织有限公司 | Industrial polypropylene fiber regenerated cotton blended yarn with flame retardance and preparing method thereof |
CN105586679A (en) * | 2016-01-26 | 2016-05-18 | 安徽省无为天成纺织有限公司 | Composite inflaming-retarding and high-temperature-resisting blended yarn for protective garment |
DE102016001910B4 (en) * | 2016-02-18 | 2019-10-10 | Viscose Faser Gmbh | A method of providing a pigment amount and using the amount of pigment provided therewith |
AT518061B1 (en) | 2016-04-28 | 2017-07-15 | Chemiefaser Lenzing Ag | Modified viscose fiber |
EP3260595B1 (en) | 2016-06-20 | 2018-05-09 | Viscose Faser GmbH | Method for obtaining highly fire-retarding synthetic fibres from textile scraps |
BR112020004363B1 (en) * | 2017-10-06 | 2024-04-30 | Lenzing Aktiengesellschaft | LYOCELL FLAME RETARDANT FILAMENT, ITS PRODUCTION PROCESS AND ITS USE, AND YARN, FABRIC OR TEXTILE PRODUCT |
US11905630B2 (en) | 2019-02-22 | 2024-02-20 | Jess Black Inc. | Fire-resistant double-faced fabric of knitted construction |
EP3754053A1 (en) | 2020-05-04 | 2020-12-23 | Lenzing Aktiengesellschaft | Spundyed cellulosic fiber |
CN114059208A (en) * | 2020-07-30 | 2022-02-18 | 湖南科力嘉纺织股份有限公司 | Easy abluent yarn for weaving |
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-
2009
- 2009-09-01 AT AT0137109A patent/AT508687A1/en not_active Application Discontinuation
-
2010
- 2010-07-27 EP EP10754846.3A patent/EP2473657B1/en active Active
- 2010-07-27 CN CN201080038900.5A patent/CN102482800B/en active Active
- 2010-07-27 WO PCT/AT2010/000273 patent/WO2011026159A1/en active Application Filing
- 2010-07-27 ES ES10754846.3T patent/ES2487494T3/en active Active
- 2010-07-27 US US13/392,987 patent/US20120177919A1/en not_active Abandoned
- 2010-08-05 TW TW099126093A patent/TWI476309B/en active
Non-Patent Citations (1)
Title |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP3476985A1 (en) | 2017-10-27 | 2019-05-01 | Lenzing Aktiengesellschaft | Fireproof cellulosic man-made fibres |
WO2019081617A1 (en) | 2017-10-27 | 2019-05-02 | Lenzing Aktiengesellschaft | Flame retardant cellulosic man-made fibres |
Also Published As
Publication number | Publication date |
---|---|
WO2011026159A1 (en) | 2011-03-10 |
CN102482800B (en) | 2015-04-22 |
ES2487494T3 (en) | 2014-08-21 |
AT508687A1 (en) | 2011-03-15 |
TW201129744A (en) | 2011-09-01 |
TWI476309B (en) | 2015-03-11 |
CN102482800A (en) | 2012-05-30 |
US20120177919A1 (en) | 2012-07-12 |
EP2473657B1 (en) | 2014-04-30 |
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