WO2011080826A1 - 防炎性レーヨン繊維及びその製造方法、並びに防炎性繊維構造物 - Google Patents
防炎性レーヨン繊維及びその製造方法、並びに防炎性繊維構造物 Download PDFInfo
- Publication number
- WO2011080826A1 WO2011080826A1 PCT/JP2009/071771 JP2009071771W WO2011080826A1 WO 2011080826 A1 WO2011080826 A1 WO 2011080826A1 JP 2009071771 W JP2009071771 W JP 2009071771W WO 2011080826 A1 WO2011080826 A1 WO 2011080826A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- fiber
- sodium
- rayon fiber
- flameproof
- mass
- Prior art date
Links
- 239000000835 fiber Substances 0.000 title claims abstract description 259
- 229920000297 Rayon Polymers 0.000 title claims abstract description 163
- 239000002964 rayon Substances 0.000 title claims abstract description 127
- 238000000034 method Methods 0.000 title claims description 23
- 238000004519 manufacturing process Methods 0.000 title description 10
- 230000008569 process Effects 0.000 title description 6
- 239000011734 sodium Substances 0.000 claims abstract description 92
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 88
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 88
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 31
- 239000010703 silicon Substances 0.000 claims abstract description 31
- 239000000243 solution Substances 0.000 claims abstract description 31
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 22
- -1 silicic acid compound Chemical class 0.000 claims abstract description 20
- 238000009987 spinning Methods 0.000 claims abstract description 17
- 238000009991 scouring Methods 0.000 claims abstract description 16
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 14
- 150000001340 alkali metals Chemical class 0.000 claims abstract description 14
- 238000002441 X-ray diffraction Methods 0.000 claims abstract description 6
- 238000012805 post-processing Methods 0.000 claims description 31
- 230000003139 buffering effect Effects 0.000 claims description 25
- 239000004745 nonwoven fabric Substances 0.000 claims description 15
- 239000011550 stock solution Substances 0.000 claims description 12
- 238000005259 measurement Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 8
- 238000012360 testing method Methods 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 20
- 239000007853 buffer solution Substances 0.000 abstract description 11
- 239000007864 aqueous solution Substances 0.000 description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 26
- 229910001868 water Inorganic materials 0.000 description 26
- 239000004115 Sodium Silicate Substances 0.000 description 20
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 20
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 20
- 229910052911 sodium silicate Inorganic materials 0.000 description 20
- 239000000872 buffer Substances 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 18
- 238000005406 washing Methods 0.000 description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 16
- 229920002678 cellulose Polymers 0.000 description 16
- 239000001913 cellulose Substances 0.000 description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- 238000011282 treatment Methods 0.000 description 15
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 11
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 10
- 229910000403 monosodium phosphate Inorganic materials 0.000 description 10
- 235000019799 monosodium phosphate Nutrition 0.000 description 10
- 235000017557 sodium bicarbonate Nutrition 0.000 description 10
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 10
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 10
- 159000000000 sodium salts Chemical class 0.000 description 10
- 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 description 8
- 229920000742 Cotton Polymers 0.000 description 8
- 239000003063 flame retardant Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 239000000377 silicon dioxide Substances 0.000 description 8
- 229920003043 Cellulose fiber Polymers 0.000 description 7
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 7
- 239000004744 fabric Substances 0.000 description 7
- 239000011521 glass Substances 0.000 description 7
- 229910052938 sodium sulfate Inorganic materials 0.000 description 7
- 235000011152 sodium sulphate Nutrition 0.000 description 7
- 229910004298 SiO 2 Inorganic materials 0.000 description 6
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 238000004380 ashing Methods 0.000 description 5
- 238000002485 combustion reaction Methods 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 229920000728 polyester Polymers 0.000 description 4
- 238000004876 x-ray fluorescence Methods 0.000 description 4
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000002265 prevention Effects 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- 229910001415 sodium ion Inorganic materials 0.000 description 3
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 3
- 229910001948 sodium oxide Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000002759 woven fabric Substances 0.000 description 3
- 239000004677 Nylon Substances 0.000 description 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000004760 aramid Substances 0.000 description 2
- 229920006231 aramid fiber Polymers 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 238000004061 bleaching Methods 0.000 description 2
- 235000019504 cigarettes Nutrition 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229920001778 nylon Polymers 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000004080 punching Methods 0.000 description 2
- 125000005624 silicic acid group Chemical group 0.000 description 2
- 235000002639 sodium chloride Nutrition 0.000 description 2
- 150000003388 sodium compounds Chemical class 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 229920002972 Acrylic fiber Polymers 0.000 description 1
- 206010029350 Neurotoxicity Diseases 0.000 description 1
- 241000208125 Nicotiana Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 206010044221 Toxic encephalopathy Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 1
- 229920003235 aromatic polyamide Polymers 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000009960 carding Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 239000000567 combustion gas Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- JEVCWSUVFOYBFI-UHFFFAOYSA-N cyanyl Chemical compound N#[C] JEVCWSUVFOYBFI-UHFFFAOYSA-N 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005108 dry cleaning Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- HJUFTIJOISQSKQ-UHFFFAOYSA-N fenoxycarb Chemical compound C1=CC(OCCNC(=O)OCC)=CC=C1OC1=CC=CC=C1 HJUFTIJOISQSKQ-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002366 halogen compounds Chemical class 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000009940 knitting Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000007135 neurotoxicity Effects 0.000 description 1
- 231100000228 neurotoxicity Toxicity 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000013094 purity test Methods 0.000 description 1
- 239000004627 regenerated cellulose Substances 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910001388 sodium aluminate Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- PVGBHEUCHKGFQP-UHFFFAOYSA-N sodium;n-[5-amino-2-(4-aminophenyl)sulfonylphenyl]sulfonylacetamide Chemical compound [Na+].CC(=O)NS(=O)(=O)C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=C1 PVGBHEUCHKGFQP-UHFFFAOYSA-N 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Images
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
- 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
Definitions
- the present invention relates to a flameproof rayon fiber, a method for producing the same, and a flameproof fiber structure.
- Patent Document 1 proposes mixing viscose and silicate soda and spinning in a bath containing sulfuric acid to fiberize the composite fiber.
- Patent Document 2 proposes a cellulose fiber in which sodium silicate is mixed with viscose, sodium aluminate is used in a scouring process, and aluminum is contained.
- Patent Document 3 proposes a cellulose fiber in which sodium silicate is mixed with viscose, an alkali solution containing Mg is brought into contact in a scouring step or a post-processing step, and Mg is contained therein.
- the cellulose fiber disclosed in Patent Document 1 is simply a composite of cellulose and silicic acid, and when exposed to high temperatures, a glassy skeleton is formed, but it cannot inhibit the decomposition of cellulose and is difficult. It is necessary to further improve the flammability.
- the cellulose fiber currently disclosed by patent document 2 contains aluminum, since the possibility that aluminum has neurotoxicity is suggested, the further improvement is needed from the surface of safety
- the cellulose fiber currently disclosed by patent document 3 is exposed to high temperature, while forming a vitreous frame
- the work of Mg processing may be complicated.
- the present invention provides a flameproof rayon fiber that is excellent in flame resistance and flame retardancy, a method for producing the same, and a flameproof fiber structure.
- the flameproof rayon fiber of the present invention contains silicon and sodium components in the rayon fiber.
- the rayon fiber has a property that glassy material remains when burned at 800 ° C, and the glassy material softens at 800 ° C.
- the silicon content is in the range of 5 to 30% by mass and the sodium content is in the range of 0.1 to 3% by mass.
- the method for producing a flameproof rayon fiber comprises the steps of preparing a viscose stock solution, and adding a silicate compound containing an alkali metal to the viscose stock solution by adding a solution containing a silicate compound containing an alkali metal.
- the flameproof fiber structure of the present invention contains at least 30% by mass of the flameproof rayon fiber.
- the flameproof rayon fiber of the present invention exhibits excellent flameproof performance and self-extinguishing properties (flame retardant) by containing components of silicon and sodium in the rayon fiber.
- flameproof rayon fiber of the present invention is non-halogen, the generated gas when temporarily burned has no harmful substances such as cyan and halogen compounds.
- the flameproof rayon fiber of the present invention is mainly composed of rayon, and can be buried in the soil and decomposed.
- FIG. 1 is a photomicrograph showing the ashing state at 800 ° C. of the flameproof rayon fiber of one example of the present invention.
- FIG. 2 is a photomicrograph showing the ashing state at 800 ° C. of the flameproof rayon fiber according to another embodiment of the present invention.
- FIG. 3 is a photomicrograph showing the ashing state at 800 ° C. of the flameproof rayon fiber of the comparative example.
- FIG. 4 is a photomicrograph showing the ashing state at 800 ° C. of the flameproof rayon fiber of another comparative example.
- the flameproof property in the present invention means a flame barrier property and means a characteristic obtained by leaving a glassy skeleton. Specifically, even when a flame is applied, the afterflame time is short and the carbonized area is small. This performance is useful, for example, as a property of burning a cigarette and burning it even if the cigarette fire falls on a bed sheet.
- flame retardancy refers to a property that is self-extinguishing and that the fiber itself is difficult to burn. Specifically, it refers to the characteristic of self-extinguishing without flashing even when defibrated cotton is ignited.
- the flameproof rayon fiber of the present invention contains silicon and sodium components in the rayon fiber.
- the rayon fiber of the present invention softens at a temperature lower than 1000 ° C., for example, a tobacco fire temperature of about 800 ° C., has biodegradability, and other components excluding the rayon component are compounds containing silicon and sodium (mainly silicic acid). Sodium) is formed, so that it can be a rayon fiber with a low environmental load.
- the rayon fiber is a fiber obtained by coagulating and regenerating viscose obtained by xanthogenizing cellulose and diluting and dissolving with a dilute alkali, and is not particularly limited by materials such as cellulose and its production method.
- the flameproof rayon fiber contains silicon and sodium in the fiber, so that it forms a soda glass structure upon combustion, has a low softening point, and the glass softens quickly at a high temperature such as about 800 ° C. Presumed to inhibit degradation.
- a high temperature such as about 800 ° C. Presumed to inhibit degradation.
- the combustion of cellulose continues because combustion gas generated by heat is flammable, but by forming a soda glass structure during combustion, the decomposition of cellulose is inhibited and the combustion is suppressed and self-extinguishes. It will be.
- the silicon content of the flameproof rayon fiber is 5 to 30% by mass, preferably 8 to 23% by mass, more preferably 13 to 19% by mass as measured by X-ray fluorescence analysis. It is a range.
- the strength and texture of the rayon fiber are maintained by keeping the silicon content in the above range.
- the sodium content of the flameproof rayon fiber is 0.1 to 3% by mass, preferably 0.15 to 1.5% by mass, more preferably when measured by fluorescent X-ray analysis.
- the range is 0.2 to 1.0% by mass.
- the flameproof rayon fiber having better flameproofing and self-extinguishing properties can be obtained by setting the sodium content within the above range.
- the ratio of the silicon content to the sodium content and the silicon / sodium mass ratio are preferably 10 or more and less than 90.
- the silicon / sodium mass ratio is a parameter indicating the ease of softening of the fiber. The lower the silicon / sodium mass ratio, the more the flameproof rayon fiber becomes soda vitrified inside the fiber when it is burned. Easier to self-extinguish (flame retardant).
- a more preferable silicon / sodium mass ratio is 15 to 70.
- sodium silicate xNa 2 ⁇ ySiO 2 ⁇ zH 2 O, where x is from 1 to 5, y ⁇ x, z is 1 to 3
- the mass ratio of silicon / sodium is 10 or more, since the glass is softened while leaving a glassy skeleton, good flameproofing and flame retardancy can be obtained.
- the presence of sodium in the flameproof rayon fiber may be at least partially contained in the rayon fiber, and the other may be attached to the surface of the rayon fiber. Whether or not sodium is present in the rayon fiber (inside the fiber) can be confirmed by washing with water.
- the silicon and the sodium compound are not particularly limited depending on the state, and may be uniformly mixed in the fiber, or may be present in a compatible or incompatible state.
- a part of the sodium may be present as a sodium compound such as sodium silicate, and the other may be contained as a sodium salt such as sodium oxide or sodium hydroxide.
- the ash content of the flameproof rayon fiber is preferably in the range of 10 to 50% by mass, more preferably in the range of 15 to 40% by mass, and particularly preferably in the range of 25 to 38% by mass.
- the ash content is an inorganic substance that incinerates an organic substance at a high temperature and remains as a residue later.
- the flameproof property of the flameproof rayon fiber tends to be lowered.
- the ash content exceeds 50% by mass, the strength of the flameproof rayon fiber tends to be lowered or the texture tends to be impaired.
- the conventional rayon that does not use a flame retardant is used. It tends to be difficult to obtain the same texture as the fiber.
- the flameproof rayon fiber of the present invention by setting the ash content of the flameproof rayon fiber of the present invention within the above range, the flameproof rayon fiber having good flameproofness and good texture can be obtained.
- the ash content of the flameproof rayon fiber is measured according to JIS L 1015 8.20, and the flameproof rayon fiber is 850 ° C. with respect to the absolutely dry mass of the flameproof rayon fiber. It is shown in mass% of the mass of the component remaining when it is burned. The same applies to the following.
- the flameproof rayon fiber preferably has a LOI value of 31 or more, more preferably 32 or more, as measured according to JIS L 1091 E method (oxygen index method test) (E-1). preferable.
- the flameproof rayon fiber preferably has a LOI value of 23 or more, more preferably 24 or more in nonwoven fabric measurement (E-2) according to JIS L 1091 E method (oxygen index method test). It is.
- the rayon fiber of the present invention is preferable because it has a flame retardancy while having a flameproof property because the LOI value satisfies the above range.
- the flameproof rayon fiber has an L value (whiteness) of preferably 40 to 90, more preferably 44 to 86, and particularly preferably 48 to 70.
- the L value is an index of whiteness when white is set to 100 and black is set to 0. The larger the value is, the more white the color becomes.
- the L value of 100 is white, but the whiteness of ordinary rayon fiber is about 92 to 95, and it does not become pure white due to the effect of the change in the hue of cellulose during heating. It tends to be difficult to produce.
- the L value is less than 40, the hue tends to deteriorate when the product is produced, and the value of the product tends to decrease.
- the flameproof rayon fiber is not particularly limited by its fineness, and generally has a fineness in the range of 1 to 17 dtex, preferably in the range of 1.7 to 10 dtex. If the fineness is less than 1 dtex, the strength of the rayon fiber tends to decrease, and if the fineness exceeds 17 dtex, the fiber diameter tends to be too thick and coarse.
- the flameproof rayon fiber is not particularly limited by the fiber length, and can be used as a filament or a staple. The fiber length can be set freely, and can be used for non-woven fabric or spun yarn if it is 20 to 200 mm. Long fiber bundles can be used without being cut after scouring.
- the fiber cross section of the flameproof rayon fiber is not particularly limited by its shape, and can be appropriately selected depending on the intended use.
- shapes such as a circular shape, an irregular shape, a hollow shape, and a flat shape are exemplified.
- the flameproof rayon fiber of the present invention retains useful physical properties generally possessed by rayon, which is regenerated cellulose, such as biodegradability, water absorption, hygroscopicity, antistatic properties, thermal stability, and the like.
- the rayon which is the main component of the flameproof rayon fiber of the present invention, has biodegradability and is decomposed in 1 to 3 months, for example, by being embedded in soil. Further, other components excluding rayon are compounds mainly containing silicic acid and sodium (mainly sodium silicate). Therefore, the flameproof rayon fiber of the present invention is a fiber with a low environmental load.
- the flameproof rayon fiber of the present invention can be obtained as follows. First, a silicic acid compound containing an alkali metal in a viscose stock solution, for example, sodium silicate (Na 2 O.nSiO 2 .xH 2 O, where n is 1 to 3, x is 10 to 20) is added to contain an alkali metal. Silica compound-added viscose liquid (hereinafter, also simply referred to as viscose liquid), the viscose liquid is extruded from a nozzle in a spinning bath containing sulfuric acid (H 2 SO 4 ), spun, and treated with a silicate compound Fabricate the fiber.
- a silicic acid compound containing an alkali metal in a viscose stock solution for example, sodium silicate (Na 2 O.nSiO 2 .xH 2 O, where n is 1 to 3, x is 10 to 20) is added to contain an alkali metal.
- Silica compound-added viscose liquid hereinafter
- the silicate compound containing the alkali metal in the viscose liquid such as sodium silicate (Na 2 O.nSiO 2 .xH 2 O, where n is 1 to 3, x is 10 to 20) is the sulfuric acid. Reacts with (H 2 SO 4 ) to convert to silicon dioxide (SiO 2 , but polymer). Thereafter, the fiber to be treated is treated with a solution having a buffering action containing sodium having a pH in the range of 4 to 11 in the scouring step or the post-processing step to obtain the flameproof rayon fiber of the present invention. Obtainable. By this treatment, silicon and sodium react to form a compound. This compound containing silicon and sodium is presumed to have the following structure in the rayon fiber.
- silicic acid forms a layered structure, and sodium exists in the form of sodium oxide between the layers of the unit structure. Silicic acid and sodium oxide are bonded by sharing some oxygen part, sodium gel is produced, sodium silicate (xNa 2 O ⁇ ySiO 2 ⁇ zH 2 O, where x is from 1 to 5, y ⁇ x, z is 1 to 3) is presumed to form.
- sodium silicate xNa 2 O ⁇ ySiO 2 ⁇ zH 2 O, where x is from 1 to 5, y ⁇ x, z is 1 to 3
- the sulfur content passes through a scouring process. Must be removed. Since sodium remaining in the fiber is also removed from the system in the scouring process, sodium is not bonded to silicic acid in the fiber.
- a general acidic spinning bath containing sulfuric acid may be used.
- H 2 SO 4 is 110 to 170 g / liter
- ZnSO 4 is 10 to 30 g / liter
- Na 2 SO 4 is 150 to 350 g / liter.
- a Mueller bath containing 1 liter can be used.
- the temperature of the spinning bath is generally 45 to 65 ° C.
- the viscose stock solution may have a general composition.
- a viscose stock solution containing 5 to 15% by mass of cellulose, 5 to 10% by mass of NaOH, and 1 to 5% by mass of CS 2 is used. be able to.
- the silicic acid compound containing an alkali metal is preferably in the range of 10 to 100% by mass, more preferably 25 to 70% in terms of silicon dioxide (SiO 2 ), based on the mass of cellulose contained in the viscose stock solution. It is the range of mass%. Since the silicic acid compound containing an alkali metal in the viscose liquid reacts with the sulfuric acid (H 2 SO 4 ) and is converted into silicon dioxide (SiO 2 , but polymer), silicon dioxide (SiO 2 ) Conversion. By containing silicon dioxide within the above range, the strength and texture of the fiber can be maintained, and rayon fibers having good flameproofing properties when treated with a solution containing sodium can be produced.
- silicate compound containing the alkali metal examples include sodium silicate.
- the step of adding a silicate compound containing an alkali metal such as sodium silicate may be performed by mixing an aqueous solution of a silicate compound containing an alkali metal into a general viscose stock solution.
- the addition ratio of the sodium silicate is preferably in the range of 10 to 100% by mass, more preferably in the range of 15 to 80% by mass, particularly preferably in the range of 30 to 70% in terms of SiO 2 with respect to the cellulose of the viscose stock solution. It is the range of mass%.
- the amount of sodium silicate within the above range, the amount of silicon dioxide contained in the fiber to be treated can be adjusted to an amount suitable for the flameproof rayon fiber of the present invention described above.
- sodium silicate for example, sodium silicate No. 3 (JIS K 1408) can be used.
- the fiber to be treated containing the silicon component obtained in the spinning step is treated with a buffering solution containing sodium having a pH in the range of 4 to 11, Silicon and sodium are reacted to form a compound containing silicon and sodium.
- a compound containing silicon and sodium is presumed to form sodium silicate.
- a post-processing step after the treatment there is a treatment of immersing the fiber to be treated in a solution having a buffering action containing sodium.
- the bath ratio may be appropriately selected according to the buffering solution containing sodium to be used.
- the mass of the fiber to be treated / the mass of the solution is in the range of 1/10 to 1/1000. is there.
- the bath temperature is in the range of 0 to 100 ° C. and the dipping time is about 30 seconds, and good processing is possible, and the range of 20 to 300 seconds is preferable.
- the solution having a buffering action containing sodium may have a pH in the range of 4 to 11, preferably in the range of 6 to 10, more preferably in the range of pH 7 to 8.6, particularly preferably pH 7.3. Is in the range of ⁇ 8.6. If the pH is less than 4, sodium does not enter the fiber and self-extinguishing properties cannot be obtained. On the other hand, if it exceeds pH 11, the silicic acid content in the fiber is eluted, the ash content after processing is low, and as a result, flameproofing properties are hardly obtained.
- the solution having a buffering action containing sodium is preferably an aqueous solution having a pH in the range of 4 to 11.
- the “solution having a buffering action containing sodium” means any solution having a buffering action, ie, a solution containing sodium in the buffer and having a pH in the range of 4 to 11. Such a form may be sufficient.
- a buffer solution comprising a water-soluble sodium salt having no buffering action and a sodium salt having a buffering action
- a buffer solution comprising a sodium salt having a buffering action a water-soluble sodium salt having no buffering action and a drug having a buffering action
- a buffer solution containing a weak acid or a weak salt can be used.
- a buffer solution composed of a sodium salt having a buffering action is preferable.
- the water-soluble sodium salt having no buffering action for example, sodium chloride, sodium sulfate, sodium nitrate and the like can be used.
- sodium salt having a buffering action examples include sodium hydrogen carbonate (sodium bicarbonate), sodium carbonate, disodium hydrogen phosphate, sodium dihydrogen phosphate, sodium citrate and the like.
- sodium bicarbonate sodium carbonate
- disodium hydrogen phosphate sodium dihydrogen phosphate
- sodium citrate sodium citrate
- weakly alkaline sodium carbonate and sodium bicarbonate buffer are more preferable from the viewpoint of use in which the phosphorus component is not desired or from the viewpoint of pH.
- These sodium salts may be used in combination of one or more.
- the content of sodium salt in the solution containing a buffer containing sodium is defined by the sodium ion concentration.
- concentration of sodium ions in the solution having a buffering action containing sodium is preferably in the range of 500 to 10,000 mg / L, more preferably in the range of 1,000 to 8,000 mg / L.
- the content of the flameproof rayon fiber is preferably 30% by mass or more, and more preferably 60 to 80% by mass.
- a flameproof fiber structure excellent in flameproofing and flame retardancy can be obtained.
- Other fibers used in the flameproof fiber structure are not particularly limited.
- binder fibers such as low melting point polyester fibers, flame retardant acrylic fibers such as “Kanekaron” (manufactured by Kaneka Corporation) (moda acrylic), and the like.
- Incombustible fibers such as aramid fibers (aromatic polyamide), and the like.
- the flameproof rayon fiber of the present invention is a rayon fiber having good flameproofness and flame retardancy.
- a rayon fiber having a good texture and having dry cleaning resistance and biodegradability is obtained.
- the flameproof rayon fiber of the present invention is processed into a woven fabric, a knitted fabric, a nonwoven fabric, etc., for example, disaster prevention articles, kitchen fan filters, sheets, pillow covers, bedding mats, bedding covers, fire screens, interior goods ( Carpet, chair upholstery, curtain, wallpaper base fabric, wall material, etc.) and vehicle interior materials (mat, lining fabric, etc.).
- Example 1 Production of viscose solution A viscose stock solution containing 8.5% by mass of cellulose, 5.7% by mass of sodium hydroxide, and 2.6% by mass of carbon disulfide was prepared. Next, a mixed solution of No. 3 sodium silicate, sodium hydroxide and water is added to the prepared viscose stock solution, and the composition of the viscose solution becomes 7.2 mass% cellulose and 7.4 mass% sodium hydroxide. Thus, a sodium silicate-added viscose solution was obtained. The addition rate of sodium silicate was 50% by mass with respect to the cellulose mass in terms of SiO 2 .
- the sodium silicate-added viscose liquid was spun at a spinning speed of 50 m / min and a draw rate of 50% by a two-bath tension spinning method to obtain a fiber having a fineness of about 3.3 dtex.
- the composition of the first bath (spinning bath) was 115 g / liter of sulfuric acid, 15 g / liter of zinc sulfate, 350 g / liter of sodium sulfate, and the temperature was 48 ° C.
- the temperature of the second bath (hot water bath) was 85 ° C.
- the sodium silicate-added viscose liquid was extruded from a nozzle to produce a rayon long fiber bundle (treated fiber) containing silicon.
- Example 2 In the post-processing, Example 1 was used except that an aqueous solution (bath temperature 50 ° C., pH 7.79) containing 0.34% by mass of sodium sulfate and 0.1% by mass of sodium bicarbonate was used as the sodium-based buffer. In the same manner as described above, a flameproof rayon fiber c (hereinafter referred to as fiber c) of Example 2 was produced.
- aqueous solution bath temperature 50 ° C., pH 7.79
- fiber c flameproof rayon fiber c
- Example 3 In the post-processing, Example 1 was used except that an aqueous solution (bath temperature 50 ° C., pH 7.93) containing 0.17% by mass of sodium sulfate and 0.3% by mass of sodium bicarbonate was used as a sodium-based buffer. In the same manner as described above, flameproof rayon fiber d of Example 3 (hereinafter referred to as fiber d) was produced.
- aqueous solution bath temperature 50 ° C., pH 7.93
- fiber d flameproof rayon fiber d of Example 3
- Example 4 In the post-processing, Example 1 was used except that an aqueous solution (bath temperature 50 ° C., pH 7.31) containing 0.41% by mass of sodium sulfate and 0.01% by mass of sodium bicarbonate was used as a sodium-based buffer. In the same manner as described above, flameproof rayon fiber e (hereinafter referred to as fiber e) of Example 4 was produced.
- aqueous solution bath temperature 50 ° C., pH 7.31
- fiber e flameproof rayon fiber e
- Example 5 In post-processing, Example 5 was performed in the same manner as Example 1 except that an aqueous solution containing 0.1% by mass of sodium hydrogen carbonate (bath temperature 50 ° C., pH 8.40) was used as the sodium-based buffer. Flameproof rayon fiber f (hereinafter referred to as fiber f) was produced.
- Example 6 In the post-processing, Example 6 was performed in the same manner as Example 1 except that an aqueous solution containing 0.5% by mass of sodium hydrogen carbonate (bath temperature 50 ° C., pH 8.42) was used as the sodium-based buffer. Flameproof rayon fiber g (hereinafter referred to as fiber g) was produced.
- Example 7 In the post-processing, Example 7 was carried out in the same manner as Example 1 except that an aqueous solution containing 1.0% by mass of sodium bicarbonate (bath temperature 50 ° C., pH 8.43) was used as the sodium-based buffer. Flameproof rayon fiber h (hereinafter referred to as fiber h) was produced.
- Example 8 In the post-processing, an example was prepared in the same manner as in Example 1 except that an aqueous solution containing 0.5% by mass of sodium dihydrogen phosphate (bath temperature 50 ° C., pH 4.69) was used as the sodium-based buffer. 8 flameproof rayon fiber i (hereinafter referred to as fiber i) was produced.
- Example 9 In the post-processing, an example was prepared in the same manner as in Example 1, except that an aqueous solution (bath temperature 50 ° C., pH 4.53) containing 1.0% by mass of sodium dihydrogen phosphate was used as the sodium-based buffer. 9 flameproof rayon fiber j (hereinafter referred to as fiber j) was produced.
- Example 10 In the post-processing, an example was prepared in the same manner as in Example 1, except that an aqueous solution containing 3.0% by mass of sodium dihydrogen phosphate (bath temperature 50 ° C., pH 4.24) was used as the sodium-based buffer.
- Ten flameproof rayon fibers k (hereinafter referred to as fibers k) were produced.
- Example 11 In the post-processing, the prevention of Example 11 was carried out in the same manner as Example 1 except that an aqueous solution containing 0.5% by mass of sodium carbonate (bath temperature 50 ° C., pH 10.86) was used as the sodium-based buffer. Flamed rayon fiber 1 (hereinafter referred to as fiber 1) was produced.
- Example 12 was the same as Example 1 except that an aqueous solution containing 0.5% by mass of disodium hydrogen phosphate (bath temperature 50 ° C., pH 8.70) was used as a sodium-based buffer in post-processing. Flame retardant rayon fiber m (hereinafter referred to as fiber m) was produced.
- Example 13 was the same as Example 1 except that an aqueous solution containing 1.0% by mass of disodium hydrogen phosphate (bath temperature 50 ° C., pH 8.76) was used as a sodium-based buffer in post-processing. Flame retardant rayon fiber n (hereinafter referred to as fiber n) was produced.
- Example 14 In the post-processing, Example 14 was carried out in the same manner as in Example 1 except that an aqueous solution containing 3.0% by mass of disodium hydrogen phosphate (bath temperature 50 ° C., pH 8.79) was used as the sodium-based buffer. Flame retardant rayon fiber o (hereinafter referred to as fiber o) was produced.
- Example 15 In post-processing, an aqueous solution (bath temperature 50) containing 0.2M disodium hydrogen phosphate and 0.2M sodium dihydrogen phosphate in a ratio (volume ratio) of 94.7: 5.3 as a sodium-based buffer solution.
- a flameproof rayon fiber p (hereinafter referred to as fiber p) of Example 15 was produced in the same manner as in Example 1 except that ° C and pH 8.3) were used.
- Example 16 In post-processing, an aqueous solution (bath temperature 50) containing 0.2 M disodium hydrogen phosphate and 0.2 M sodium dihydrogen phosphate in a ratio (volume ratio) of 91.5: 8.5 as a sodium-based buffer solution.
- a flameproof rayon fiber q (hereinafter referred to as fiber q) of Example 16 was produced in the same manner as in Example 1 except that [° C., pH 8.0) was used.
- Example 17 In the post-processing, an aqueous solution (bath temperature 50 ° C., pH 7.7) containing 0.2 M disodium hydrogen phosphate and 0.2 M sodium dihydrogen phosphate in a ratio of 81:19 (volume ratio) as a sodium-based buffer.
- a flameproof rayon fiber r (hereinafter referred to as fiber r) of Example 17 was produced in the same manner as Example 1 except that 6) was used.
- Example 18 In the post-processing, as a sodium-based buffer solution, an aqueous solution containing 0.2 M disodium hydrogen phosphate and 0.2 M sodium dihydrogen phosphate in a ratio (volume ratio) of 61:39 (bath temperature 50 ° C., pH 7. Except that 2) was used, flameproof rayon fiber s (hereinafter referred to as fiber s) of Example 18 was produced in the same manner as Example 1.
- Example 19 In the post-processing, as a sodium-based buffer solution, an aqueous solution containing 0.2 M disodium hydrogen phosphate and 0.2 M sodium dihydrogen phosphate in a ratio (volume ratio) of 37.5: 62.5 (bath temperature 50 ° C., A flameproof rayon fiber t (hereinafter referred to as fiber t) of Example 19 was produced in the same manner as in Example 1 except that pH 6.8) was used.
- Example 20 In the post-processing, as a sodium-based buffer solution, an aqueous solution containing 0.2 M disodium hydrogen phosphate and 0.2 M sodium dihydrogen phosphate in a ratio (volume ratio) of 18.5: 81.5 (bath temperature 50 ° C., A flameproof rayon fiber u (hereinafter referred to as fiber u) of Example 20 was produced in the same manner as in Example 1 except that pH 6.3) was used.
- Comparative Example 1 A flameproof rayon fiber a (hereinafter referred to as fiber a) of Comparative Example 1 was produced in the same manner as in Example 1 except that the fiber to be treated was not post-processed with an aqueous solution containing sodium. .
- Comparative Example 2 Commercially available rayon fiber (Shandong Helon Co., LTD, “HELON”, hereinafter simply referred to as HELON) was used as Comparative Example 2.
- Example 3 the flameproof rayon fiber v of Comparative Example 3 (hereinafter, referred to as “Example 1”) was used in the same manner as in Example 1 except that an aqueous solution containing 3% by mass of sodium sulfate (bath temperature 50 ° C., pH 7.8) was used. Fiber v)).
- Ash content was measured according to JIS L 1015 8.20. Specifically, the mass of a component remaining when a fiber having a mass of 1 g was burned in an electric furnace at 850 ° C. for 2 hours was measured to obtain an ash content. In addition, ash content is the mass% of the mass of the component which remain
- the water absorption test method (knitting basket method) in the purity test method of absorbent cotton for Japanese pharmacy method was applied to perform the water washing treatment. Specifically, 2 g of fibers are precisely weighed and packed into a container. As the container, a cylindrical cage of 8 cm in height and approximately 5 cm in diameter processed with enameled wire is used. After the fibers were uniformly placed in the container, the sample was immersed in 25 ° C. ion exchange water for 3 minutes, then taken out from the container, centrifuged and dehydrated, and then dried with a dryer to obtain a sample after washing with water.
- D evaluation is a result of observation with a general rayon fiber. It is.
- a typical rayon fiber is a rayon fiber manufactured by a general manufacturing method in which sodium silicate is not added to viscose and no post-treatment is performed using an aqueous solution containing sodium.
- the whiteness (L value) was measured as follows according to JIS L 1015 8.17 C method (Hunter method). 20 g of the fiber opened through the carding machine was placed in a constant temperature blast dryer (“FC-612” manufactured by ADVANTEC) set at a temperature of 190 ° C. and subjected to heat treatment for 5 minutes to prepare a sample. The whiteness was measured using a whiteness meter “ZE-2000” manufactured by Nippon Denshoku Industries Co., Ltd. The sample 20g prepared in a container attached to the measuring instrument is packed, and the direction of the sample is changed, and the color measurement is performed four times (L, a, b). The average of the four measurements (L value) was taken as the whiteness of the fiber.
- the LOI value is determined according to JIS L 1091 E method (oxygen index method test) using an oxygen index flammability tester (ON-1 type) manufactured by Toyo Rika Kogyo Co., Ltd. No.) or non-woven fabric (E-2) was attached to a support and measured.
- the test piece was produced as follows.
- E-1 test piece (from strand): 1 g of sample cotton is opened and the fiber length is adjusted to 20 to 30 cm, and then one end is fixed and twisted from the other end. Specifically, twisting is performed while pulling, and the twisting is stopped immediately before the bump is formed. Then, it is folded in half from the center to produce a strand having a length of about 110 mm and a width of about 6 mm.
- E-2 test piece (non-woven fabric): 30% by mass of low melting point polyester fiber (“4080” manufactured by Unitika Ltd., fineness 4.4 dtex, fiber length 51 mm) and 70% by mass of flameproof rayon fiber were mixed. Then, a card web is produced using a card machine, and is overlaid so that the basis weight is 300 g / m 2 . Thereafter, the card web is placed on a punching plate using a constant temperature blast dryer (ADVANTEC “FC-612”) set at a temperature of 180 ° C., and a nylon mesh is placed on the web, resulting in 20 g / cm 2. Put a weight like this and set it in a constant temperature air dryer. After leaving as it is for 10 minutes, it is taken out from the constant temperature air dryer, and a nonwoven fabric having a length of 150 mm and a width of 60 mm is produced.
- ADVANTEC “FC-612” constant temperature blast dryer
- the flameproof rayon fibers of the examples have a LOI value of 31 or more measured by this (E-1 method) measurement, and a LOI value of 24 measured by the nonwoven fabric (E-2 method) measurement. It is above and is excellent in a flame retardance.
- FIGS. 1 to 4 micrographs showing the incineration state at 800 ° C. of the flameproof rayon fibers of Examples 2 and 5 and Comparative Examples 1 and 2 are shown in FIGS. 1 to 4, respectively.
- the fiber of the comparative example was not softened and bubbles could not be observed, but the fiber of the example was softened and bubbles could be observed. That is, the fibers of the examples form a soda glass structure when burned, the softening point becomes low, and the glass softens quickly at high temperatures, thereby inhibiting the decomposition of cellulose.
- the fiber e tended to have a slightly low flame retardancy because there were few components having a buffering action in the aqueous solution used for post-processing.
- the fiber f had a low sodium ion concentration in the aqueous solution used for post-processing, the flame retardancy tended to be slightly low.
- the fibers i, j, k had a low flame retardancy because the pH of the aqueous solution used for post-processing was low.
- the aqueous solution used for the post-processing contains sodium but does not contain a drug having a buffering action, that is, it is not a buffer solution containing sodium. It was not obtained. This is considered because sodium does not exist inside the fiber.
- the fibers b to h showed almost no decrease in ash even after washing with water. Since the properties are not substantially changed, sodium is considered to remain inside the fibers in the flameproof rayon fibers of the examples.
- the fibers i, j, and k had high whiteness, that is, the fibers Although the whiteness is maintained, the flame retardancy tends to be slightly low, and the fiber l has low whiteness, that is, the fiber is colored, and the flame retardancy is high, but the product value is lowered depending on the application. there were.
- the fibers of the other examples maintained high flame retardancy and product value.
- X-ray fluorescence analysis was performed by theoretical calculation using the FP method using an X-ray fluorescence analyzer “LAB CENTER XRF-1700” manufactured by Shimadzu Corporation. The outline and measurement conditions of this measuring apparatus are as follows.
- the fibers b, f and g and the fiber g after the water washing treatment contain silicon and sodium components and form sodium silicate.
- the fiber g was washed with water. From the result of the fiber g after the water washing treatment in Table 3, it can be seen that the amount of sodium of 0.1% by mass or more is maintained even with water washing. It can also be seen from the result of fiber g after the water washing treatment that at least a part of sodium is present in the fiber.
- the fibers b, f, g, the fibers g after washing with water (Example), and the HELON (Comparative Example) when the Si / Na mass ratio is seen, it is particularly good when the mass ratio is less than 90. It was confirmed that flammability was obtained.
- a flameproof nonwoven fabric was prepared using each sample cotton of fibers b, g, l and m (Example) and fibers a and HELON (Comparative Example). 30% by mass of low-melting polyester fiber ("4080" manufactured by Unitika Ltd., fineness 4.4dtex, fiber length 51mm) and 70% by mass of sample cotton are mixed to produce a card web using a card machine. The layers were superposed so as to be 300 g / m 2 .
- the card web is placed on a punching plate, a nylon mesh is placed on the web, and 20 g / cm 2 is placed there. Such a weight was placed and set in the dryer. The low melting point polyester fiber was melted by leaving it for 10 minutes as it was to bond the fibers together. Thereafter, the nonwoven fabric was taken out from the dryer to obtain a flameproof nonwoven fabric.
- the flameproof nonwoven fabric containing the fibers b, g, l, and m of Examples showed good flame retardancy.
- the present invention can provide a flameproof rayon fiber that has good flameproofness for preventing flames and has flame retardancy (self-extinguishing property), and a method for producing the same.
- the rayon fiber which is the main component of the present invention is biodegradable and the other components are compounds mainly containing silicon and sodium, it is possible to provide a flameproof rayon fiber with little environmental load.
- it can be used as a material to replace glass fiber, asbestos, aramid fiber, etc. that have been used in conventional flameproof products.
- the flameproof rayon fiber of the present invention is processed into a woven fabric, a knitted fabric, a nonwoven fabric, etc., for example, disaster prevention articles, kitchen fan filters, sheets, pillow covers, bedding mats, bedding covers, fire screens, interior goods ( Carpet, chair upholstery, curtain, wallpaper base fabric, wall material, etc.) and vehicle interior materials (mat, lining fabric, etc.).
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Artificial Filaments (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
Description
(1)ビスコース液の製造
セルロースを8.5質量%、水酸化ナトリウムを5.7質量%及び二硫化炭素を2.6質量%含むビスコース原液を作製した。次いで、作製したビスコース原液中に、3号珪酸ソーダと水酸化ナトリウムと水の混合溶液を添加し、ビスコース液の組成がセルロース7.2質量%、水酸化ナトリウム7.4質量%になるように調整して、珪酸ソーダ添加ビスコース液を得た。珪酸ソーダの添加率はSiO2に換算して、セルロース質量に対して50質量%であった。
(2)紡糸
前記珪酸ソーダ添加ビスコース液を、二浴緊張紡糸法により紡糸速度50m/min、延伸率50%で紡糸して、繊度が約3.3dtexの繊維を得た。第一浴(紡糸浴)の組成は、硫酸115g/リットル、硫酸亜鉛15g/リットル、硫酸ナトリウム350g/リットルであり、温度は48℃とした。第二浴(熱水浴)の温度は85℃とした。前記珪酸ソーダ添加ビスコース液をノズルより押し出して、珪素を含むレーヨン長繊維束(被処理繊維)を作製した。
(3)精練
前記長繊維束を、カッターを用いて繊維長51mmにカッティングして精練処理を行った。精練工程は、熱水処理、漂白、酸洗い、水洗の順で実施した。圧縮ローラーで余分な水分を除いて、60℃の恒温乾燥機で7時間乾燥させた。このようにして得られた被処理繊維の物性は、繊度:3.3dtex、乾強度(cN/dtex):1.4、湿強度(cN/dtex):0.8、乾伸度(%):25、湿伸度(%):20であった。
(4)後加工
ナトリウムを含む緩衝作用を有する溶液(以下、ナトリウム系緩衝液という。)として、硫酸ナトリウム0.38質量%と、炭酸水素ナトリウム0.05質量%を含む水溶液(浴温度50℃、pH7.76)を用い、この水溶液中に前記乾燥させた被処理繊維を30秒間浸漬させた。このとき浴比は、被処理繊維の質量と前記水溶液の質量とが1:20となる割合とした。次に、前記被処理繊維を水洗し、遠心脱水した。最後に、105℃の恒温乾燥機で30分乾燥させ、実施例1の防炎性レーヨン繊維b(以下、繊維bという。)を得た。
後加工において、ナトリウム系緩衝液として、硫酸ナトリウムを0.34質量%、炭酸水素ナトリウムを0.1質量%含む水溶液(浴温度50℃、pH7.79)を用いたこと以外は、実施例1と同様にして、実施例2の防炎性レーヨン繊維c(以下、繊維cという。)を製造した。
後加工において、ナトリウム系緩衝液として、硫酸ナトリウムを0.17質量%、炭酸水素ナトリウムを0.3質量%含む水溶液(浴温度50℃、pH7.93)を用いたこと以外は、実施例1と同様にして、実施例3の防炎性レーヨン繊維d(以下、繊維dという。)を製造した。
後加工において、ナトリウム系緩衝液として、硫酸ナトリウムを0.41質量%、炭酸水素ナトリウムを0.01質量%含む水溶液(浴温度50℃、pH7.31)を用いたこと以外は、実施例1と同様にして、実施例4の防炎性レーヨン繊維e(以下、繊維eという。)を製造した。
後加工において、ナトリウム系緩衝液として、炭酸水素ナトリウムを0.1質量%含む水溶液(浴温度50℃、pH8.40)を用いたこと以外は、実施例1と同様にして、実施例5の防炎性レーヨン繊維f(以下、繊維fという。)を製造した。
後加工において、ナトリウム系緩衝液として、炭酸水素ナトリウムを0.5質量%含む水溶液(浴温度50℃、pH8.42)を用いたこと以外は、実施例1と同様にして、実施例6の防炎性レーヨン繊維g(以下、繊維gという。)を製造した。
後加工において、ナトリウム系緩衝液として、炭酸水素ナトリウムを1.0質量%含む水溶液(浴温度50℃、pH8.43)を用いたこと以外は、実施例1と同様にして、実施例7の防炎性レーヨン繊維h(以下、繊維hという。)を製造した。
後加工において、ナトリウム系緩衝液として、リン酸二水素ナトリウムを0.5質量%含む水溶液(浴温度50℃、pH4.69)を用いたこと以外は、実施例1と同様にして、実施例8の防炎性レーヨン繊維i(以下、繊維iという。)を製造した。
後加工において、ナトリウム系緩衝液として、リン酸二水素ナトリウムを1.0質量%含む水溶液(浴温度50℃、pH4.53)を用いたこと以外は、実施例1と同様にして、実施例9の防炎性レーヨン繊維j(以下、繊維jという。)を製造した。
後加工において、ナトリウム系緩衝液として、リン酸二水素ナトリウムを3.0質量%含む水溶液(浴温度50℃、pH4.24)を用いたこと以外は、実施例1と同様にして、実施例10の防炎性レーヨン繊維k(以下、繊維kという。)を製造した。
後加工において、ナトリウム系緩衝液として、炭酸ナトリウムを0.5質量%含む水溶液(浴温度50℃、pH10.86)を用いたこと以外は、実施例1と同様にして、実施例11の防炎性レーヨン繊維l(以下、繊維lという。)を製造した。
後加工において、ナトリウム系緩衝液として、リン酸水素二ナトリウム0.5質量%含む水溶液(浴温度50℃、pH8.70)を用いたこと以外は、実施例1と同様にして、実施例12の防炎性レーヨン繊維m(以下、繊維mという。)を製造した。
後加工において、ナトリウム系緩衝液として、リン酸水素二ナトリウム1.0質量%含む水溶液(浴温度50℃、pH8.76)を用いたこと以外は、実施例1と同様にして、実施例13の防炎性レーヨン繊維n(以下、繊維nという。)を製造した。
後加工において、ナトリウム系緩衝液として、リン酸水素二ナトリウム3.0質量%含む水溶液(浴温度50℃、pH8.79)を用いたこと以外は、実施例1と同様にして、実施例14の防炎性レーヨン繊維o(以下、繊維oという。)を製造した。
後加工において、ナトリウム系緩衝液として、0.2Mのリン酸水素二ナトリウムと0.2Mのリン酸二水素ナトリウムを94.7:5.3の割合(体積比)で含む水溶液(浴温度50℃、pH8.3)を用いたこと以外は、実施例1と同様にして、実施例15の防炎性レーヨン繊維p(以下、繊維pという。)を製造した。
後加工において、ナトリウム系緩衝液として、0.2Mのリン酸水素二ナトリウムと0.2Mのリン酸二水素ナトリウムを91.5:8.5の割合(体積比)で含む水溶液(浴温度50℃、pH8.0)を用いたこと以外は、実施例1と同様にして、実施例16の防炎性レーヨン繊維q(以下、繊維qという。)を製造した。
後加工において、ナトリウム系緩衝液として、0.2Mのリン酸水素二ナトリウムと0.2Mのリン酸二水素ナトリウムを81:19(体積比)の割合で含む水溶液(浴温度50℃、pH7.6)を用いたこと以外は、実施例1と同様にして、実施例17の防炎性レーヨン繊維r(以下、繊維rという。)を製造した。
後加工において、ナトリウム系緩衝液として、0.2Mのリン酸水素二ナトリウムと0.2Mのリン酸二水素ナトリウムを61:39の割合(体積比)で含む水溶液(浴温度50℃、pH7.2)を用いたこと以外は、実施例1と同様にして、実施例18の防炎性レーヨン繊維s(以下、繊維sという。)を製造した。
後加工において、ナトリウム系緩衝液として、リン酸水素二ナトリウム0.2Mとリン酸二水素ナトリウム0.2Mを37.5:62.5の割合(体積比)で含む水溶液(浴温度50℃、pH6.8)を用いたこと以外は、実施例1と同様にして、実施例19の防炎性レーヨン繊維t(以下、繊維tという。)を製造した。
後加工において、ナトリウム系緩衝液として、リン酸水素二ナトリウム0.2Mとリン酸二水素ナトリウム0.2Mを18.5:81.5の割合(体積比)で含む水溶液(浴温度50℃、pH6.3)を用いたこと以外は、実施例1と同様にして、実施例20の防炎性レーヨン繊維u(以下、繊維uという。)を製造した。
被処理繊維に対し、ナトリウムを含む水溶液による後加工を行わなかったこと以外は、実施例1と同様にして、比較例1の防炎性レーヨン繊維a(以下、繊維aという。)を製造した。
市販品のレーヨン繊維(Shandong Helon Co.,LTD製“HELON”、以下において、単にHELONという。)を比較例2として用いた。
後加工において、硫酸ナトリウムを3質量%含む水溶液(浴温度50℃、pH7.8)を用いたこと以外は、実施例1と同様にして、比較例3の防炎性レーヨン繊維v(以下、繊維vという。)を製造した。
(1)灰分
灰分は、JIS L 1015 8.20 に準じて測定した。具体的には、質量1gの繊維を、850℃の電気炉で2時間燃焼させたときに残る成分の質量を測定し、灰分を求めた。なお、灰分は、前記繊維の質量から水分を除いた質量に対して、燃焼させたときに残る成分の質量の質量%である。また、以下のように水洗処理した後の繊維を用いて、同様に灰分を求めた。
日本薬局法脱脂綿の純度試験方法にある吸水量試験方法(編みカゴ法)を適用し水洗処理を行った。具体的には、繊維2gを精秤し、容器に詰め込む。容器はエナメル線で加工した高さ8cm径約5cmφの円筒のかごを使用する。容器に均一に繊維を入れたのち、25℃のイオン交換水に3分間浸漬した後に容器より取り出し、遠心脱水し、その後乾燥機で乾燥したものを水洗処理後のサンプルとした。
板状に広げた繊維に、その2cm下方からディスポライターの炎(炎の長さ2.5cm)を直接あてた時の様子を観察した。炎は繊維塊に対して垂直にあてた。なお、評価用サンプル(繊維塊)は、原綿1~2gをカード機で開繊してウェブとし、これを塊状にして作製した。また、繊維を前記のように水洗処理した後に、同様に炎をあて、その様子も観察した。観察結果に基いて、難燃性は、以下のような4段階で評価した。
A:炎を近づけても炎が当たっている部分のみ燃焼の状態で、それ以上燃焼しない
B:炎を近づけたときに、綿のかたまり表面を若干走り、炎を離すと火が消える
C:炎を近づけたときに、綿のかたまり表面を火が走り、炎を離しても残炎がある
D:炎を近づけると燃え広がる
なお、上記において、D評価は一般的なレーヨン繊維にて観察した結果である。一般的なレーヨン繊維は、ビスコースに珪酸ソーダを添加せず、またナトリウムを含む水溶液を用いて後処理していない、一般的製造方法によって製造されたレーヨン繊維である。
白色度(L値)は、JIS L 1015 8.17 C法(ハンター法)に準じて、以下のように測定した。カード機を通して開繊した繊維20gを、温度190℃に設定した定温送風乾燥機(ADVANTEC製“FC-612”)に入れ、5分間熱処理を行い、試料を作製した。白色度の測定には、日本電色工業株式会社製白色度計“ZE-2000”を用いて測定した。測定器に付属の容器に作製した試料20gを詰めて、試料の向きを入れ替えて4回測色を行う(L,a,b)。その4回の測定値(L値)の平均を繊維の白色度とした。
LOI値は、JIS L 1091 E法(酸素指数法試験)に準じて、東洋理化工業業株式会社製酸素指数燃焼性試験機(ON-1型)を用いて、試験片としてこより(E-1号)又は不織布(E-2号)を支持具に取り付け測定した。試験片は、以下のとおり作製した。
繊維を既定の800℃に設定した電気炉内に放置し、灰化状態を顕微鏡(ニコン社製“ECLIPSE E600”、320倍)で観察し、軟化の有無及び気泡の有無を確認した。
繊維a、HELON(比較例)、繊維b、f及びg、並びに水洗い処理後の繊維g(実施例)の成分分析を、下記のように蛍光X線分析で行った。その結果を下記表3に示した。
蛍光X線分析は、島津製作所製蛍光X線分析装置“LAB CENTER XRF-1700”を用いて、FP法による理論計算により測定した。この測定装置の概略と測定条件は、次のとおりである。
(i)測定装置の概略
測定元素範囲 4Be~92U
X線管 4kw薄窓,Rhターゲット
分光素子 LiF,PET,Ge,TAP,SX
1次X線フィルタ 4種自動交換(Al,Ti,Ni,Zr)
視野制限絞り 5種自動交換(直径1,3,10,20,30mmφ)
検出器 シンチレーションカウンタ(重元素)、プロポーショナルカウンタ(軽元素)
(ii)測定条件
管電圧-管電流 40kw-95mA
繊維a、HELON(比較例)、繊維b、f及びg、並びに水洗い処理後の繊維g(実施例)のカットファイバーを用いて測定した。照射面は直径10mmφで厚み数mmに調整し、上方から照射して下方に透過させて測定した。
繊維b、g、l、m(実施例)及び繊維a、HELON(比較例)のそれぞれの試料綿を用いて、防炎性不織布を作製した。低融点ポリエステル繊維(ユニチカ(株)製“4080”、繊度4.4dtex、繊維長51mm)30質量%と、試料綿70質量%を混合し、カード機を用いてカードウェブを作製し、目付が300g/m2となるように重ね合わせた。次に、温度180℃に設定した定温送風乾燥機(ADVANTEC製“FC-612”)を用いて、上記カードウェブをパンチングプレートに置き、ウェブ上にナイロンメッシュを置き、そこに20g/cm2となるような重りを載せて、前記乾燥機内にセットした。そのまま10分間放置して低融点ポリエステル繊維を溶融させて繊維同士を接着させた。その後、前記乾燥機内から不織布を取り出して、防炎性不織布を得た。実施例の繊維b、g、l、mを含む防炎性不織布は、良好な難燃性を示した。
Claims (6)
- 防炎性を有するレーヨン繊維であって、
レーヨン繊維中に珪素とナトリウムの成分を含み、
前記レーヨン繊維は、800℃で燃焼したときにガラス質が残存し、ガラス質は800℃で軟化する性質を有しており、
前記レーヨン繊維を蛍光X線分析したとき、珪素の含有量は5~30質量%の範囲であり、ナトリウムの含有量は0.1~3質量%の範囲であることを特徴とする防炎性レーヨン繊維。 - 前記レーヨン繊維は、JIS L 1091 E法(酸素指数法試験)に準じた、こより(E-1号)測定において、LOI値が31以上、又は不織布(E-2号)測定において、LOI値が24以上である請求項1に記載の防炎性レーヨン繊維。
- 前記レーヨン繊維の灰分は10~50質量%の範囲である請求項1又は2に記載の防炎性レーヨン繊維。
- 前記レーヨン繊維における珪素とナトリウムの含有割合、珪素/ナトリウム質量比が10以上90未満の範囲である請求項1~3のいずれか1項に記載の防炎性レーヨン繊維。
- ビスコース原液を調製する工程と、
前記ビスコース原液中に、アルカリ金属を含む珪酸化合物を含有する溶液を添加してアルカリ金属を含む珪酸化合物添加ビスコース液とする工程と、
硫酸を含む紡糸浴に前記珪酸化合物添加ビスコース液をノズルより押し出して紡糸し、珪酸化合物を含む被処理繊維を作製する工程と、
前記被処理繊維に対して、精練工程又は後加工工程においてpHが4~11の範囲であるナトリウムを含む緩衝作用を有する溶液を用いて処理する工程とを含む防炎性レーヨン繊維の製造方法。 - 請求項1~4のいずれかに記載の防炎性レーヨン繊維を少なくとも30質量%含むことを特徴とする防炎性繊維構造物。
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN200980160918.XA CN102471939B (zh) | 2009-12-28 | 2009-12-28 | 防燃性人造丝纤维及其制造方法、以及防燃性纤维结构物 |
JP2010548695A JP4713695B1 (ja) | 2009-12-28 | 2009-12-28 | 防炎性レーヨン繊維及びその製造方法、並びに防炎性繊維構造物 |
PCT/JP2009/071771 WO2011080826A1 (ja) | 2009-12-28 | 2009-12-28 | 防炎性レーヨン繊維及びその製造方法、並びに防炎性繊維構造物 |
US13/258,979 US20120015185A1 (en) | 2009-12-28 | 2009-12-28 | Flameproof rayon fiber, method for manufacturing the same and flameproof fiber structure |
EP09852804.5A EP2463412A4 (en) | 2009-12-28 | 2009-12-28 | FLAME RETARDANT FIBER, METHOD FOR PRODUCING SAME, AND FIRE RETARDANT FIBER STRUCTURE |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
PCT/JP2009/071771 WO2011080826A1 (ja) | 2009-12-28 | 2009-12-28 | 防炎性レーヨン繊維及びその製造方法、並びに防炎性繊維構造物 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2011080826A1 true WO2011080826A1 (ja) | 2011-07-07 |
Family
ID=44226261
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP2009/071771 WO2011080826A1 (ja) | 2009-12-28 | 2009-12-28 | 防炎性レーヨン繊維及びその製造方法、並びに防炎性繊維構造物 |
Country Status (5)
Country | Link |
---|---|
US (1) | US20120015185A1 (ja) |
EP (1) | EP2463412A4 (ja) |
JP (1) | JP4713695B1 (ja) |
CN (1) | CN102471939B (ja) |
WO (1) | WO2011080826A1 (ja) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2016191020A (ja) * | 2015-03-31 | 2016-11-10 | ダイワボウホールディングス株式会社 | 難燃性複合成形用基材、ならびに難燃性複合成形体およびその製造方法 |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1064271A (en) | 1962-07-30 | 1967-04-05 | Fmc Corp | A method of making ablative, sinterable and sintered shaped structures and structures made thereby |
JP3179104B2 (ja) | 1991-12-31 | 2001-06-25 | ケミラ ファイブレス オイ | 二酸化ケイ素を含む製品およびその製造方法 |
JP2008501867A (ja) * | 2004-06-02 | 2008-01-24 | サテリ インターナショナル カンパニー リミテッド | ケイ酸塩含有繊維の製造法 |
JP4094052B2 (ja) | 2005-08-26 | 2008-06-04 | 大和紡績株式会社 | 防炎性レーヨン繊維及びその製造方法 |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2373881A (en) * | 1940-04-27 | 1945-04-17 | Mathieson Alkali Works Inc | Rayon bleaching and scouring treatment |
US3565749A (en) * | 1967-02-27 | 1971-02-23 | Fmc Corp | High temperature resistant structures |
JPH03179104A (ja) * | 1989-12-06 | 1991-08-05 | Mitsubishi Heavy Ind Ltd | 蒸気タービン車室 |
JPH0494052A (ja) * | 1990-08-09 | 1992-03-26 | Matsushita Electron Corp | メタルハライドランプ |
CN1037458C (zh) * | 1994-02-03 | 1998-02-18 | 赵玉山 | 纤维素聚硅酸盐阻燃纤维及其生产方法 |
DE102004015138A1 (de) * | 2004-03-27 | 2005-10-27 | Mewa Textil-Service Ag & Co. Management Ohg | Gewebe |
CN101037812A (zh) * | 2007-04-06 | 2007-09-19 | 山东海龙股份有限公司 | 抗融阻燃粘胶纤维及其制备方法 |
-
2009
- 2009-12-28 WO PCT/JP2009/071771 patent/WO2011080826A1/ja active Application Filing
- 2009-12-28 US US13/258,979 patent/US20120015185A1/en not_active Abandoned
- 2009-12-28 JP JP2010548695A patent/JP4713695B1/ja not_active Expired - Fee Related
- 2009-12-28 CN CN200980160918.XA patent/CN102471939B/zh active Active
- 2009-12-28 EP EP09852804.5A patent/EP2463412A4/en not_active Withdrawn
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1064271A (en) | 1962-07-30 | 1967-04-05 | Fmc Corp | A method of making ablative, sinterable and sintered shaped structures and structures made thereby |
JP3179104B2 (ja) | 1991-12-31 | 2001-06-25 | ケミラ ファイブレス オイ | 二酸化ケイ素を含む製品およびその製造方法 |
JP2008501867A (ja) * | 2004-06-02 | 2008-01-24 | サテリ インターナショナル カンパニー リミテッド | ケイ酸塩含有繊維の製造法 |
JP4094052B2 (ja) | 2005-08-26 | 2008-06-04 | 大和紡績株式会社 | 防炎性レーヨン繊維及びその製造方法 |
Non-Patent Citations (1)
Title |
---|
See also references of EP2463412A4 |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2016191020A (ja) * | 2015-03-31 | 2016-11-10 | ダイワボウホールディングス株式会社 | 難燃性複合成形用基材、ならびに難燃性複合成形体およびその製造方法 |
Also Published As
Publication number | Publication date |
---|---|
EP2463412A1 (en) | 2012-06-13 |
US20120015185A1 (en) | 2012-01-19 |
JP4713695B1 (ja) | 2011-06-29 |
EP2463412A4 (en) | 2013-11-13 |
CN102471939B (zh) | 2013-06-19 |
CN102471939A (zh) | 2012-05-23 |
JPWO2011080826A1 (ja) | 2013-05-09 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP4094052B2 (ja) | 防炎性レーヨン繊維及びその製造方法 | |
AT502743B1 (de) | Cellulosischer formkörper, verfahren zu seiner herstellung und dessen verwendung | |
EP2098621B1 (en) | Fire retardant antiflux fiber and its production process | |
AU2011349082C1 (en) | Fireproof cellulosic man-made fibers | |
EP0619848B1 (en) | A product containing silicon dioxide and a method for its preparation | |
EP2488683B1 (en) | Flame barriers comprising flame-retardant lyocell fibers | |
US7776180B2 (en) | Process for preparing a flame retardant and glow resistant zinc free cellulose product | |
JP4713695B1 (ja) | 防炎性レーヨン繊維及びその製造方法、並びに防炎性繊維構造物 | |
JP4529146B2 (ja) | 高度難燃吸湿性繊維および繊維構造物 | |
CN105492464B (zh) | 具有抗燃性的纤维素基底及其相关生产方法 | |
JP2007291570A (ja) | 難燃性合成繊維、難燃繊維複合体およびそれを用いた炎遮断性バリア用不織布 | |
WO2006118009A1 (ja) | 難燃性寝具製品 | |
JP3797170B2 (ja) | アクリル系合成繊維及びその繊維複合体 | |
WO2016098952A1 (ko) | 다용도 기능성 위생 솜 및 이의 제조방법 | |
WO2023145820A1 (ja) | 防炎性レーヨン繊維、その製造方法、それを用いた紡績糸及び編地 | |
JP4346566B2 (ja) | 難燃性合成繊維および該難燃性合成繊維を用いた難燃性繊維複合体および該難燃性繊維複合体を用いた布張り家具製品 | |
CN103668522B (zh) | 一种非水溶性硅酸钙阻燃粘胶纤维的制备方法 | |
JP2007291571A (ja) | 難燃性合成繊維、難燃繊維複合体およびそれを用いた難燃性マットレス | |
CN111349993B (zh) | 一种耐酸的阻燃纱线及由其制得的耐酸的纺织品和服装 | |
Heidari et al. | Surface modification of hybrid fibres for fire protection | |
JPH05247812A (ja) | 難燃性ネップ入り紙状物及びその製造方法 | |
JPH04194053A (ja) | 難燃性布帛 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
WWE | Wipo information: entry into national phase |
Ref document number: 200980160918.X Country of ref document: CN |
|
WWE | Wipo information: entry into national phase |
Ref document number: 2010548695 Country of ref document: JP |
|
121 | Ep: the epo has been informed by wipo that ep was designated in this application |
Ref document number: 09852804 Country of ref document: EP Kind code of ref document: A1 |
|
WWE | Wipo information: entry into national phase |
Ref document number: 13258979 Country of ref document: US |
|
WWE | Wipo information: entry into national phase |
Ref document number: 2009852804 Country of ref document: EP |
|
NENP | Non-entry into the national phase |
Ref country code: DE |