KR101226166B1 - Method for producing the electrically polyester conductive fiber - Google Patents
Method for producing the electrically polyester conductive fiber Download PDFInfo
- Publication number
- KR101226166B1 KR101226166B1 KR1020120063624A KR20120063624A KR101226166B1 KR 101226166 B1 KR101226166 B1 KR 101226166B1 KR 1020120063624 A KR1020120063624 A KR 1020120063624A KR 20120063624 A KR20120063624 A KR 20120063624A KR 101226166 B1 KR101226166 B1 KR 101226166B1
- Authority
- KR
- South Korea
- Prior art keywords
- agent
- polyester fiber
- conductivity
- fiber
- minutes
- Prior art date
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- 239000000835 fiber Substances 0.000 title claims abstract description 103
- 229920000728 polyester Polymers 0.000 title claims abstract description 78
- 238000004519 manufacturing process Methods 0.000 title description 2
- 238000000034 method Methods 0.000 claims abstract description 46
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000007822 coupling agent Substances 0.000 claims abstract description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 15
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 14
- 230000007062 hydrolysis Effects 0.000 claims abstract description 14
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 14
- 238000007670 refining Methods 0.000 claims abstract description 13
- 239000002736 nonionic surfactant Substances 0.000 claims abstract description 10
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 9
- 239000000839 emulsion Substances 0.000 claims abstract description 9
- 239000012535 impurity Substances 0.000 claims abstract description 9
- 230000009467 reduction Effects 0.000 claims abstract description 9
- 239000003002 pH adjusting agent Substances 0.000 claims abstract description 7
- 239000003381 stabilizer Substances 0.000 claims abstract description 7
- 235000011121 sodium hydroxide Nutrition 0.000 claims abstract description 6
- 150000003464 sulfur compounds Chemical class 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 24
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 24
- 239000010949 copper Substances 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 19
- 230000004048 modification Effects 0.000 claims description 15
- 238000012986 modification Methods 0.000 claims description 15
- 239000003513 alkali Substances 0.000 claims description 14
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 12
- 239000003054 catalyst Substances 0.000 claims description 12
- 229910052802 copper Inorganic materials 0.000 claims description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 9
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 9
- 239000003623 enhancer Substances 0.000 claims description 8
- 230000007797 corrosion Effects 0.000 claims description 6
- 238000005260 corrosion Methods 0.000 claims description 6
- 235000019253 formic acid Nutrition 0.000 claims description 6
- 230000002940 repellent Effects 0.000 claims description 6
- 239000005871 repellent Substances 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 239000003093 cationic surfactant Substances 0.000 claims description 5
- 239000008139 complexing agent Substances 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 5
- 239000003349 gelling agent Substances 0.000 claims description 5
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 5
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 5
- 239000002216 antistatic agent Substances 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 4
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 4
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 4
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 4
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 3
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 3
- 239000004902 Softening Agent Substances 0.000 claims description 3
- 239000003963 antioxidant agent Substances 0.000 claims description 3
- 230000003078 antioxidant effect Effects 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 230000001804 emulsifying effect Effects 0.000 claims description 3
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical group CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 claims description 3
- 230000003301 hydrolyzing effect Effects 0.000 claims description 3
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims description 3
- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical group CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 229960001763 zinc sulfate Drugs 0.000 claims description 3
- 239000003112 inhibitor Substances 0.000 claims description 2
- 239000012744 reinforcing agent Substances 0.000 claims description 2
- 239000011686 zinc sulphate Substances 0.000 claims description 2
- 235000009529 zinc sulphate Nutrition 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims 1
- 239000005749 Copper compound Substances 0.000 abstract description 3
- 150000001880 copper compounds Chemical class 0.000 abstract description 3
- 238000001879 gelation Methods 0.000 abstract description 2
- 238000005406 washing Methods 0.000 abstract description 2
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- 238000006722 reduction reaction Methods 0.000 description 12
- 235000013351 cheese Nutrition 0.000 description 10
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- 238000006297 dehydration reaction Methods 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 description 7
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 238000002407 reforming Methods 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 230000003068 static effect Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 230000000536 complexating effect Effects 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 4
- 235000019345 sodium thiosulphate Nutrition 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- ZNBNBTIDJSKEAM-UHFFFAOYSA-N 4-[7-hydroxy-2-[5-[5-[6-hydroxy-6-(hydroxymethyl)-3,5-dimethyloxan-2-yl]-3-methyloxolan-2-yl]-5-methyloxolan-2-yl]-2,8-dimethyl-1,10-dioxaspiro[4.5]decan-9-yl]-2-methyl-3-propanoyloxypentanoic acid Chemical group C1C(O)C(C)C(C(C)C(OC(=O)CC)C(C)C(O)=O)OC11OC(C)(C2OC(C)(CC2)C2C(CC(O2)C2C(CC(C)C(O)(CO)O2)C)C)CC1 ZNBNBTIDJSKEAM-UHFFFAOYSA-N 0.000 description 3
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 description 3
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 3
- -1 auxiliaries Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 3
- 238000004043 dyeing Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 229910000378 hydroxylammonium sulfate Inorganic materials 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 229910052763 palladium Inorganic materials 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 229920002972 Acrylic fiber Polymers 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 229910001431 copper ion Inorganic materials 0.000 description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 2
- 229910000366 copper(II) sulfate Inorganic materials 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- 235000010855 food raising agent Nutrition 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000003449 preventive effect Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- YPNVIBVEFVRZPJ-UHFFFAOYSA-L silver sulfate Chemical compound [Ag+].[Ag+].[O-]S([O-])(=O)=O YPNVIBVEFVRZPJ-UHFFFAOYSA-L 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000001509 sodium citrate Substances 0.000 description 2
- 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 2
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical group CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- ONLPKGMCOFNAJA-UHFFFAOYSA-N 3-methoxysilylpropane-1-thiol Chemical compound CO[SiH2]CCCS ONLPKGMCOFNAJA-UHFFFAOYSA-N 0.000 description 1
- DCQBZYNUSLHVJC-UHFFFAOYSA-N 3-triethoxysilylpropane-1-thiol Chemical compound CCO[Si](OCC)(OCC)CCCS DCQBZYNUSLHVJC-UHFFFAOYSA-N 0.000 description 1
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical group C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- 229910017920 NH3OH Inorganic materials 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 229910004878 Na2S2O4 Inorganic materials 0.000 description 1
- 229910004879 Na2S2O5 Inorganic materials 0.000 description 1
- 229910021205 NaH2PO2 Inorganic materials 0.000 description 1
- 229910008051 Si-OH Inorganic materials 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 229910006358 Si—OH Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
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- 230000002159 abnormal effect Effects 0.000 description 1
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- 239000000853 adhesive Substances 0.000 description 1
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- 150000001298 alcohols Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- RJTANRZEWTUVMA-UHFFFAOYSA-N boron;n-methylmethanamine Chemical compound [B].CNC RJTANRZEWTUVMA-UHFFFAOYSA-N 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 description 1
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 229960003280 cupric chloride Drugs 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000004332 deodorization Methods 0.000 description 1
- DGLRDKLJZLEJCY-UHFFFAOYSA-L disodium hydrogenphosphate dodecahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].OP([O-])([O-])=O DGLRDKLJZLEJCY-UHFFFAOYSA-L 0.000 description 1
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- 239000004744 fabric Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000005338 heat storage Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002883 imidazolyl group Chemical group 0.000 description 1
- 239000012770 industrial material Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
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- 229910021645 metal ion Inorganic materials 0.000 description 1
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- INJVFBCDVXYHGQ-UHFFFAOYSA-N n'-(3-triethoxysilylpropyl)ethane-1,2-diamine Chemical compound CCO[Si](OCC)(OCC)CCCNCCN INJVFBCDVXYHGQ-UHFFFAOYSA-N 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 description 1
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- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 description 1
- JVBXVOWTABLYPX-UHFFFAOYSA-L sodium dithionite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])=O JVBXVOWTABLYPX-UHFFFAOYSA-L 0.000 description 1
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- 235000010262 sodium metabisulphite Nutrition 0.000 description 1
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- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
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- 239000002344 surface layer Substances 0.000 description 1
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- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- SDVHRXOTTYYKRY-UHFFFAOYSA-J tetrasodium;dioxido-oxo-phosphonato-$l^{5}-phosphane Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)P([O-])([O-])=O SDVHRXOTTYYKRY-UHFFFAOYSA-J 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
- D06M11/42—Oxides or hydroxides of copper, silver or gold
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/01—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with hydrogen, water or heavy water; with hydrides of metals or complexes thereof; with boranes, diboranes, silanes, disilanes, phosphines, diphosphines, stibines, distibines, arsines, or diarsines or complexes thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
- D10B2331/04—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyesters, e.g. polyethylene terephthalate [PET]
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2401/00—Physical properties
- D10B2401/16—Physical properties antistatic; conductive
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- Engineering & Computer Science (AREA)
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Abstract
Description
본 발명은 폴리에스터(polyester) 섬유에 화학적에너지 차(화학적 환원법)를 이용하여 부도체인 폴리에스터 섬유에 금속(Cu)화하여 전도성을 부여하는 방법에 관한 것으로서, 보다 상세하게는 폴리에스터 섬유를 실란계 커플링제와 구리화합물의 결합력을 높이는 반응제로 개질하는 섬유개질처리 후 화학적환원법에 의해 전도성을 부여하는, 폴리에스터 섬유의 전도성 부여 방법에 관한 것이다. The present invention relates to a method of imparting conductivity by metalizing (Cu) a polyester fiber, which is an insulator, by using a chemical energy difference (chemical reduction method) to a polyester fiber, and more particularly, a silane fiber The present invention relates to a method for imparting conductivity of a polyester fiber to impart conductivity by a chemical reduction method after a fiber reforming treatment to be modified with a reactive agent that enhances the bonding strength between the system coupling agent and the copper compound.
대부분의 합성섬유와 일부 천연섬유는 섬유간의 마찰이나, 섬유와 피부간의 마찰에 의하여 정전기가 발생되어 대전됨은 이미 알려진 사실로, 이러한 정전기 발생은 피복의 착용에서뿐만 아니라 산업 현장에서도 큰 문제를 발생시키는 것으로 알려져 있다.It is known that most synthetic fibers and some natural fibers are charged by static electricity due to friction between fibers or friction between fibers and skin. Such generation of static electricity causes a great problem not only in the wearing of the coating but also in the industrial field. Known.
따라서, 이러한 섬유의 정전기 발생문제를 해소하기 위하여 후처리 공정에서 대전 방지제 처리를 하거나, 섬유 자체에 도전성을 부여하는 방법 등이 개발되고 있다.Therefore, in order to solve the static electricity generation problem of the fiber, a method for treating the antistatic agent in the post-treatment process, or imparting conductivity to the fiber itself has been developed.
섬유 자체에 도전성을 부여하기 위한 방법 중 한 가지로 아크릴로니트릴 반복단위를 갖는 아크릴섬유에 도전성이 우수한 도전성 황화구리 나노미립자 조성물을 석출반응 시켜서 우수한 체적저항을 갖는 도전성 아크릴섬유를 제조하는 방법은 이미 다수 안출되어 사용되고 있다.As a method for imparting conductivity to the fiber itself, a method of preparing a conductive acrylic fiber having excellent volume resistance by precipitating a conductive copper sulfide nanoparticle composition having excellent conductivity to an acrylic fiber having an acrylonitrile repeating unit has already been performed. Many have been devised and used.
종래에 폴리에스터(POLYESTER) 섬유에 전도성을 부여하는 방법은 폴리에스터(POLYESTER) 직물을 고가의 귀금속인 팔라듐 촉매와 귀금속 환원반응 증가제, 활성제 등을 처리하여 전자기기의 전자파 차폐용으로 많이 사용되고 있다.Conventionally, a method of imparting conductivity to polyester fibers has been widely used for shielding electromagnetic waves by treating polyester fabrics with expensive noble metals such as palladium catalysts, noble metal reduction reactions, and activators. .
그러나, 이러한 종래의 고가의 귀금속인 팔라듐 촉매를 사용하는 방법은 Cheese 염색기에 적용하기에는 너무 고가라는 가격적인 부분과, 고가의 촉매제의 재활용이 어려워서 현장에서 외면 받았다(염화팔라듐(PdCl2) 10g/l 15만 원). However, the conventional method of using a high priced precious metal palladium catalyst has been neglected in the field because it is too expensive to apply to a cheese dyeing machine, and it is difficult to recycle expensive catalysts (palladium chloride (PdCl 2) 10g / l 15 Ten thousand won).
따라서, 고가의 귀금속인 팔라듐 촉매를 사용하지 아니한 방법으로서, 폴리에스터 섬유에 전도성을 부여할 수 있는 방법에 대한 연구가 필요한 실정이다. Therefore, as a method of not using an expensive noble metal palladium catalyst, research on a method for imparting conductivity to a polyester fiber is required.
본 발명은 상기의 문제점을 해결하기 위한 것으로서, 본 발명의 목적은 Cheese 염색기를 이용하여, 정련, 알카리 감량, 표면 개질, 전도성 부여, 탈수 및 건조단계를 거침으로써, 섬유+커플링제+황화구리가 화학적, 물리적으로 강력하게 결합(밀착)되도록 하여, 우수한 전도성을 지니는 폴리에스터 섬유의 전도성 부여 방법을 제공하는 것이다. The present invention is to solve the above problems, an object of the present invention is to use a cheese dyeing machine, through the refining, alkali reduction, surface modification, conductivity provision, dehydration and drying step, fiber + coupling agent + copper sulfide It is to provide a method for imparting conductivity of a polyester fiber having excellent conductivity by allowing it to be bonded (adherently) chemically and physically.
본 발명의 목적은 이상에서 언급한 목적으로 제한되지 않으며, 언급되지 않은 또다른 목적들은 아래의 기재로부터 명확하게 이해될 수 있을 것이다.The object of the present invention is not limited to the above-mentioned object, and other objects which are not mentioned will be clearly understood from the following description.
본 발명은 상기의 목적을 달성하기 위한 것으로서, 본 발명의 폴리에스터 섬유의 전도성 부여방법은, 폴리에스터 섬유에 부착된 불순물을 제거하는 정련단계;폴리에스터 섬유를 알카리 가수분해제인 가성소다 수용액에서 온도 50~65℃, 25~50분간 처리한 후, 염산용액으로 중화 후 수세하는, 폴리에스터 섬유 표면에 대한 알카리 감량단계; 물을 용매로 하여 실란계 커플링제, 알코올류 겔화 방지제, 가수분해 촉매제, 보조제를 첨가하여 80~105℃로 서서히 승온하면서 120~200분 처리하여, 폴리에스터 섬유를 개질하는 개질 단계; 동(Cu)화합물, 환원제, 안정제, 착화 및 PH 조정제, 황화합물을 첨가하여 35~65℃에서 200~400분 처리하여, 폴리에스터 섬유에 구리로 전도성을 부여하는 전도성 부여 단계; 및 상기 전도성이 부여된 폴리에스터 섬유를 함수율 25~35%가 되도록 탈수시키고, 열을 가하여 건조시키는 탈수 및 건조 단계;를 포함한다. The present invention is to achieve the above object, the method of imparting the conductivity of the polyester fiber of the present invention, refining step of removing impurities attached to the polyester fiber; temperature of the polyester fiber in an aqueous solution of caustic soda which is an alkali hydrolyzing agent An alkali reduction step for the surface of the polyester fiber, which is treated with 50 to 65 ° C. for 25 to 50 minutes and then neutralized with hydrochloric acid solution and washed with water; A reforming step of modifying the polyester fiber by adding a silane coupling agent, an alcohol gelling agent, a hydrolysis catalyst, and an auxiliary agent to water for 120 to 200 minutes while gradually raising the temperature to 80 to 105 ° C using water as a solvent; Adding a copper (Cu) compound, a reducing agent, a stabilizer, a complexing agent and a PH adjusting agent, and a sulfur compound to treat 200 to 400 minutes at 35 to 65 ° C. to impart conductivity to the polyester fiber with copper; And dewatering and drying the polyester fibers to which the conductivity is imparted so as to have a water content of 25 to 35%, and drying by applying heat.
바람직한 실시예에 따르면, 상기 정련단계에서 저기포성 비이온성계면활성제가 사용된다. According to a preferred embodiment, a low foaming nonionic surfactant is used in the refining step.
바람직한 실시예에 따르면, 상기 알카리 감량 단계에서 양이온성 계면활성제를 추가로 포함한다. According to a preferred embodiment, the cationic surfactant is further included in the alkali reduction step.
바람직한 실시예에 따르면, 상기 개질 단계에서, 분산효과를 증대시키기 위해서 첨가제로서 비이온성 계면 활성제를 첨가한다. According to a preferred embodiment, in the modification step, a nonionic surfactant is added as an additive to increase the dispersing effect.
바람직한 실시예에 따르면, 상기 개질 단계에서, 알코올류 겔화 방지제는 상기 커플링제가 메톡시 실란류의 경우에는 메탄올이 사용되고 상기 커플링제가 에톡시 실란류의 경우에는 에탄올이 사용되며, 상기 가수분해 촉매제는 염산(HCl), 아세트산(CH3COOH), 개미산(HCOOH), 및 옥살산(C2H2O4)으로 이루어진 군으로부터 선택된 1종 이상이 사용되며, 상기 보조제는 이소프로필알코올(IPA), 폴리알킬암모늄, 및 알칸올아민으로 이루어진 군으로부터 선택된 1종 이상이 사용된다. According to a preferred embodiment, in the reforming step, the anti-gelling agent for alcohols is methanol when the coupling agent is methoxy silanes and ethanol is used when the coupling agent is ethoxy silanes. Is at least one selected from the group consisting of hydrochloric acid (HCl), acetic acid (CH3COOH), formic acid (HCOOH), and oxalic acid (C2H2O4), the auxiliary agent is isopropyl alcohol (IPA), polyalkylammonium, and alkanol At least one selected from the group consisting of amines is used.
바람직한 실시예에 따르면, 상기 전도성 부여 단계에서, 질산은, 황산은, 및 염화은으로 이루어진 군으로부터 1종 이상 선택되는 내구성 강화제를 추가로 포함한다. According to a preferred embodiment, in the imparting conductivity, the silver nitrate further includes a durability enhancer selected from the group consisting of silver sulfate and silver chloride.
바람직한 실시예에 따르면, 상기 전도성 부여 단계에서, 황산니켈(NiSO4.6H2O), 황산아연(ZnSO4, 및 황산망간(MnSO4)으로 이루어진 군으로부터 1종 이상 선택되는 내식성 강화제를 추가로 포함한다. According to a preferred embodiment, in the imparting conductivity, at least one corrosion resistance enhancer selected from the group consisting of nickel sulfate (NiSO4.6H 2 O), zinc sulfate (ZnSO 4, and manganese sulfate (MnSO 4) is further included.
바람직한 실시예에 따르면, 상기 전도성 부여 단계 이후에, 촉감개선제, 발수제, 발유제, 기모향상제, 방청제, 유연평활제, 대전방지제, 코팅제, 및 산화방지제로 이루어진 군으로부터 1종 이상이 선택된 기능성유제를 이용하여 폴리에스터 섬유에 유제처리하는 유제처리 단계를 추가로 포함한다.
According to a preferred embodiment, after the conductivity imparting step, at least one functional oil selected from the group consisting of tactile improver, water repellent, oil repellent, brush raising agent, rust preventive agent, softening agent, antistatic agent, coating agent, and antioxidant And an emulsion treatment step of emulsifying the polyester fibers.
본 발명의 폴리에스터 섬유의 전도성 부여방법에 따르면, 폴리에스터 필라멘트를 Cheese 형태로, 용이한 방법으로, 원가를 낮추면서 전도성 섬유를 대량생산(10~1,000kg/Batch) 할 수 있다. According to the method of imparting the conductivity of the polyester fiber of the present invention, the polyester filament in the cheese form, in an easy way, it is possible to mass-produce (10 ~ 1,000kg / Batch) the conductive fiber while lowering the cost.
가장 보편화되고 다양한 용도로 사용되고 있는 POLYESTER 섬유의 다양한 기능(성질)을 이용한 전도성 섬유의 다양한 이용이 가능하고, 정전기로 인한 전기적 장해, 역학장애, 방전장해를 방지하고, 구리가 갖고 있는 전자파 차폐, 항균, 방취, 축열 기능을 활용한 산업용 자재, 의류, 기능성 생활용품에 적용이 용이해져서 고부가가치화가 가능할 것으로 기대된다. It is possible to use a variety of conductive fibers using various functions (properties) of POLYESTER fiber which is the most common and used for various purposes, and to prevent electric, mechanical and electrical discharges caused by static electricity, electromagnetic shielding and antibacterial of copper It is expected to be able to be added to industrial materials, clothing, and functional household goods utilizing deodorization and heat storage functions, thereby enabling high added value.
본 발명에 따르면, 폴리에스터 필라멘트 표면을 화학적으로 부식시켜서 표면적을 커게 하고, 주름, 줄, 요철을 생성시킨다. 또한, 섬유개질용 커플링제, 보조제, 첨가제를 사용하여 화학적 물리적 결합력을 증대시키고, 개질된 폴리에스터 섬유에 화학적환원으로 황화구리를 석출(Coating)시킨 다음 기능성 유제를 처리하여 건조공정에서 열(습열→건열)에 의하여 폴리에스터섬유+커플링제+황화구리가 화학적, 물리적으로 강력하게 결합(밀착)되도록 하여, 폴리에스터(polyester)의 우수한 물성을 이용한 전도성 섬유를 제공할 수 있다.
According to the present invention, the surface of the polyester filament is chemically corroded to increase the surface area and produce wrinkles, strings, and irregularities. In addition, by using a coupling agent, auxiliaries, and additives for fiber modification, the chemical physical bonding strength is increased, and copper sulfide is deposited on the modified polyester fiber by chemical reduction, followed by treatment with a functional emulsion to heat (wet heat) in the drying process. → dry heat) allows the polyester fiber + coupling agent + copper sulfide to be bonded (adherently) chemically and physically, thereby providing a conductive fiber using the excellent physical properties of polyester.
도 1은 본 발명의 바람직한 실시예에 따른, 폴리에스터 섬유의 전도성 부여방법의 순서도. 1 is a flow chart of a method for imparting conductivity of a polyester fiber according to a preferred embodiment of the present invention.
이하에서는 첨부된 도면을 참조로 하여, 본 발명의 폴리에스터 섬유의 전도성 부여방법을 보다 상세히 설명하기로 한다. Hereinafter, with reference to the accompanying drawings, it will be described in more detail the method for providing conductivity of the polyester fiber of the present invention.
도 1은 본 발명의 바람직한 실시예에 따른, 폴리에스터 섬유의 전도성 부여방법의 순서도이다. 1 is a flowchart of a method for imparting conductivity of a polyester fiber according to a preferred embodiment of the present invention.
본 발명의 폴리에스터 섬유의 전도성 부여방법은 기본적으로 유제 및 불순물을 제거하는 정련단계, 폴리에스터 섬유 표면에 대한 알칼리 감량단계, 실란 커플링제, 겔화방지제, 가수분해촉진제, 보조제를 첨가하여 폴리에스터 섬유를 개질하는 개질화 단계, 폴리에스터 섬유에 전도성을 부여하는 전도성 부여단계, 탈수 건조단계를 포함한다. The method of imparting conductivity of the polyester fiber of the present invention basically includes a refining step of removing oil and impurities, an alkali weight reduction step on the surface of the polyester fiber, a silane coupling agent, an antigelling agent, a hydrolysis accelerator, and an auxiliary agent to add the polyester fiber. A reforming step of modifying a, imparting conductivity to impart conductivity to the polyester fiber, and a dehydration drying step.
본 발명의 폴리에스터 섬유의 전도성 부여방법은 정압장치가 부착된 Cheese/Loose 겸용 염색기를 사용하여 실시하는 것이 효율적인 면에서 바람직하다.The method for imparting conductivity of the polyester fiber of the present invention is preferably carried out using a cheese / Loose combined dyeing machine equipped with a static pressure device in terms of efficiency.
제품 생산(정련~전도성부여)공정에서 가동과 동시에 2.0kg/㎠ 압력을 물 또는 Air로써 유지시키면서 용액순환을 In→Out, Out→In으로 3~10분씩 교대로 운전하여 아래와 같은 효과를 얻게 된다. Simultaneously operate the solution circulation from In → Out and Out → In 3 to 10 minutes while maintaining 2.0kg / ㎠ pressure as water or air at the same time as operating in product production (refining ~ conductive imparting) process. .
첫째, Cheese(염색콘)의 필라멘트 또는 실의 변형을 방지한다. 2.0kg/㎠ 압력이 피염물(폴리에스터 섬유) 전체에 미치고 있음으로 Pump수압에 의한 변형이 없다. (Pump 압력 : 0.4~0.7kg/㎠ 바람직함). Pump에 의한 용액의 과대유량은 피염물의 사층 붕괴의 원인이 된다. First, it prevents deformation of the filament or yarn of the cheese. There is no deformation by Pump water pressure because 2.0kg / cm 2 pressure is applied to the whole tainted material (polyester fiber). (Pump pressure: 0.4 ~ 0.7kg / ㎠ is preferred). Excessive flow of the solution by the pump causes the dead layer to collapse.
둘째, 용액의 순환이 일정하게 됨으로 반응도 고르게 일어나 사고방지, 품질이 좋게 된다.Second, because the circulation of the solution is constant, the reaction occurs evenly, preventing accidents and improving quality.
셋째, 원심 Pump의 단점인 공동현상(온도가 높을 때 액체→기체로 변하여 Pump수압이 저하되는 현상)을 정압장치를 이용하면 비등점을 높여줌으로 온도변화에 따라 Pump수압이 일정하게 유지됨으로 균일한 품질을 생산할 수 있다. Third, the common phenomenon, which is the disadvantage of centrifugal pumps (when the temperature is high, changes from liquid to gas to decrease the pump water pressure), the constant pressure increases the boiling point. Can produce
넷째, 공정종료 후 사층이 일정하게 유지되어 후공정인 Re-Winder 작업이 용이하고 생산성이 증가한다. Fourth, the four floors are kept constant after the end of the process, making it easier to work as a post-process re-inder and increasing productivity.
다음으로, 본 발명의 폴리에스터 섬유의 전도성 부여방법의 각 단계에 대해서 보다 구체적으로 설명하기로 한다. Next, each step of the method for imparting conductivity of the polyester fiber of the present invention will be described in more detail.
먼저, 폴리에스터 섬유에 부착된 불순물을 제거하는 정련단계를 거친다. 정련단계는 폴리에스터 섬유에 부착된 불순물을 제거하는 단계이다. 정련단계는 피염물(필라멘트)에 부착된 유제 및 원사가공~준비작업 과정에서 부착된 불순물을 제거하는 공정으로, 바람직하게는 (저기포성) 비이온성계면활성제이 사용된다. 비이온성계면활성제의 사용량은 1~2g/l, 온도 60± 5℃, 처리시간 30분으로 한다. First, a refining step is performed to remove impurities attached to the polyester fibers. The refining step is a step of removing impurities attached to the polyester fiber. The refining step is a process of removing the oil adhered to the chlorine (filament) and the impurities attached in the process of preparing and preparing the yarn, preferably a (low foaming) nonionic surfactant. The amount of nonionic surfactant used is 1 to 2 g / l, temperature 60 ± 5 ℃, and treatment time is 30 minutes.
정련단계를 거친 폴리에스터 섬유에 대해서, 폴리에스터 섬유 표면에 알칼리 감량 단계를 거친다. For the polyester fiber subjected to the refining step, an alkali weight loss step is performed on the polyester fiber surface.
폴리에스터 섬유를 알칼리 가수분해를 통해 부드러운 드레이프성을 부여하는 것을 '감량가공' 또는 '알카리 감량가공' 이라고 한다. 일반적으로 합성 폴리에스터 섬유의 단면은 원형이고, 표면은 매끈하여 커플링제의 결합력(밀착력)이 약하게 되기 때문에 Polyester 필라멘트 표면을 가성소다(알칼리 가수분해제), 양이온성 계면활성제(분산력 강화)를 사용하여 섬유의 알칼리 가수분해를 용이하게 하여 섬유표면에 요철을 생성시켜 표면적이 커지고 차후 공정을 거친 후 제품 상태에서 결합(밀착, 접착)력을 증대시킨다. Giving soft drape property through alkali hydrolysis of polyester fiber is called 'reduced' or 'alkali reduced'. Generally, synthetic polyester fibers have a circular cross section, and the surface is smooth, so that the bonding strength (cohesion) of the coupling agent is weak, so that the surface of the polyester filament is made of caustic soda (alkaline hydrolysing agent) and cationic surfactant (dispersion strengthening). This facilitates alkali hydrolysis of the fiber, creating unevenness on the fiber surface, increasing the surface area and increasing the bonding (adhesion, adhesion) force in the product state after subsequent processing.
Polyester 필라멘트 감량은 가성소다 20~80g/l, 양이온성 계면활성제 1~3g/l의 수용액에서 온도 80~100℃, 60~100분 처리 후, 염산 0.007~0.020g/l 용액으로 중화하고 수세한다. Polyester filament weight loss is neutralized and washed with a solution of 0.007 ~ 0.020g / l hydrochloric acid after treatment at temperature of 80 ~ 100 ℃ for 60 ~ 100 minutes in aqueous solution of 20 ~ 80g / l caustic soda and 1 ~ 3g / l cationic surfactant .
한편, 지나친 감량은 폴리에스터 섬유의 물성을 약화시키고, 미흡한 감량은 결합력 효과를 약화시킬 수 있음으로 주의해야 한다. 본 발명에서 Polyester 감량율은 4~10% 가 이상적이다. 즉, 10% 이상의 과도한 감량은 폴리에스터 섬유 고유의 물성을 저하시키며, 3% 미만의 감량은 물리적 결합력의 증가효과가 미미하여 감량의 효과를 발생시키지 못한다. On the other hand, it should be noted that excessive weight loss weakens the physical properties of the polyester fiber, and insufficient weight loss may weaken the effect of the bonding force. In the present invention, polyester loss ratio is ideally 4 ~ 10%. That is, excessive weight loss of more than 10% lowers the inherent physical properties of the polyester fiber, and weight loss of less than 3% does not cause an effect of weight loss due to a slight increase in physical bonding force.
다음으로, 물을 용매로 하여, 실란계 커플링제, 알코올류 겔화 방지제, 가수분해 촉매제, 보조제를 첨가하여 35~80℃로 서서히 승온하면서 120~200분 처리하여, 폴리에스터 섬유를 개질하는 개질 단계를 거친다. 폴리에스터 섬유의 개질화는 고분자물질인 섬유(유기질)와 금속이온(무기질) 간의 결합력을 향상시키기 위해서 수행된다. Next, a reforming step of modifying the polyester fiber by treating with 120 to 200 minutes while gradually raising the temperature to 35 to 80 ℃ by adding a silane coupling agent, an alcohol gelling agent, a hydrolysis catalyst, an auxiliary agent using water as a solvent. Go through. Modification of the polyester fiber is carried out to improve the binding force between the high molecular fiber (organic) and metal ions (inorganic).
폴리에스터 섬유개질 처리에 사용하는 커플링제로서는 실란계 커플링제, 티탄계커플링제, 알루미늄계 커플링제, 지르코늄계 커플링제가 있는데 이들을 1종 또는 2종을 병용할 수도 있으나, 본 발명의 폴리에스터 섬유에 처리하는 커플링제로서는 실란계 커플링제를 사용하는 것이 바람직하다. 실란계 커플링제 중에서 비닐기, 아미노기, 머캅토기, 이미다졸기 등의 관능기를 분자 중에 갖는 것이 바람직하며, 아미노프로필트리에톡시 실란, 아미노에틸아미노프로필트리에톡시 실란, 머캅토프로필트리메톡시 실란, 또는 머캅토프로필트리에톡시 실란 등을 사용할 수 있다. 실란계 커플링제의 사용량은 5~40g/l 이 바람직하다. Coupling agents used in the polyester fiber modification treatment include a silane coupling agent, a titanium coupling agent, an aluminum coupling agent, and a zirconium coupling agent. Although these may be used alone or in combination, the polyester fiber of the present invention It is preferable to use a silane coupling agent as the coupling agent to be treated. It is preferable to have functional groups, such as a vinyl group, an amino group, a mercapto group, and an imidazole group, in a molecule | numerator among a silane coupling agent, and it is aminopropyl triethoxy silane, aminoethylaminopropyl triethoxy silane, mercaptopropyl trimethoxy silane. Or mercaptopropyltriethoxy silane can be used. As for the usage-amount of a silane coupling agent, 5-40 g / l is preferable.
겔화 방지제는 커플링제의 용해를 돕고 Gel화를 방지하기 위한 것으로서, 알코올류 겔화 방지제가 바람직하게 사용된다. 알코올류 겔화방지제에 커플링제를 서서히 가하면서 충분히 교반해 주는 것이 좋다. 알코올류 겔화 방지제는 5~20g/l이 사용되며, 메톡시 실란류에는 메탄올을 사용하고, 에톡시 실란류에는 에탄올을 사용하는 것이 교차반응을 방지하게 되어 바람직하다. The antigelling agent is used to assist the dissolution of the coupling agent and to prevent gelation, and alcohol antigelling agents are preferably used. It is good to stir thoroughly, adding a coupling agent to alcohol-type antigelling agent gradually. 5-20 g / l of alcohol gelling inhibitor is used, methanol is used for methoxy silanes, and ethanol is used for ethoxy silanes, and it is preferable to prevent cross reaction.
본 발명에서 실란 커플링제의 주 용매로 물을 사용하는 것이 경제적이다. In the present invention, it is economical to use water as the main solvent of the silane coupling agent.
가수분해 촉매제는 커플링제의 가수분해를 촉진하기 위하여 염산(HCl), 아세트산(CH3COOH), 개미산(HCOOH), 및 옥살산(C2H2O4)으로 이루어진 군으로부터 선택된 1종 이상이 사용할 수 있다. 가수분해 촉매제를 사용하는 것은 커플링제의 가수분해가 좋을수록, 후공정의 작업이 원활하고 품질이 좋아지기 때문이다. 반면에 용해성이 나쁘면 커플링제의 분자간의 거리가 가깝게 되고, 자기축합반응이 쉽게 일어나 불량의 원인이 된다. 실란 커플링제 가수분해 촉매제의 사용량은 약 0.0005~0.001g/l 이 사용된다. 일반적인 실란 커플링제의 용해는 약산성인 pH 3~5가 적합하며 용액의 안정성이 보장되나, 그 밖의 영역에서는 축합반응으로 겔(Gel)화되기 쉽고, 겔(Gel)화 되면 커플링제로서의 기능을 제대로 발휘할 수 없게 됨으로 주의가 필요하다. 관능기로 아미노기를 갖는 커플링제는 pH 7~10 이 적당하다.The hydrolysis catalyst may be used by one or more selected from the group consisting of hydrochloric acid (HCl), acetic acid (CH3COOH), formic acid (HCOOH), and oxalic acid (C2H2O4) to promote hydrolysis of the coupling agent. The reason why the hydrolysis catalyst is used is that the better the hydrolysis of the coupling agent, the smoother the work in the post process and the better the quality. On the other hand, when the solubility is poor, the distance between molecules of the coupling agent is close, and the self-condensation reaction easily occurs, which causes defects. The amount of the silane coupling agent hydrolysis catalyst used is about 0.0005 ~ 0.001 g / l. In general, the dissolution of the silane coupling agent is suitable for pH 3 ~ 5, which is weakly acidic, and the stability of the solution is guaranteed, but in other areas, it is easy to gel by condensation reaction, and when gelled, it functions properly as a coupling agent. Attention is needed because it becomes infeasible. PH 7-10 are suitable for the coupling agent which has an amino group as a functional group.
보조제는 고분자물질인 섬유 및 무기질 간의 결합력(Bonding)을 증가시켜 내구성을 향상시키기 위해서 사용된다. 상기 보조제는 이소프로필알코올(IPA), 폴리알킬암모늄, 및 알칸올아민으로 이루어진 군으로부터 선택된 1종 이상을 사용될 수 있다. 보조제 사용량은 5~30g/l 이 바람직하다. Auxiliaries are used to increase the bonding strength between the fibers and the inorganic material (Bonding) to improve the durability. The auxiliary agent may be used one or more selected from the group consisting of isopropyl alcohol (IPA), polyalkylammonium, and alkanolamine. The amount of adjuvant is preferably 5 to 30 g / l.
섬유 개질 단계에서 선택적으로 계면활성제를 첨가제로서 사용할 수 있는 데, 이는 분산효과, 용액순환을 용이하게 하기 위하여 계면활성제를 선택적으로 사용할 수 있다. 계면활성제는 비이온성 계면활성제가 좋고, 사용량은 임계미셀농도가 적합하다. Surfactants may optionally be used as additives in the fiber modification step, which may optionally be used to facilitate dispersion and solution circulation. The surfactant is preferably a nonionic surfactant, and the amount of use thereof is appropriate for the critical micelle concentration.
개질화 단계에서 조제들의 용해 순서에 대해 설명하면, 먼저 총사용 물 양의 1/3에 아세트산(가수분해 촉매제)을 투입하여 순환시켜 놓는다. 다음으로 별도의 PE 용기에 Gel화 방지제를 투입하고, 실란 커플링제를 서서히 가하면서 5분 이상 교반하여 아세트산이 투입된 상기 용액에 투입한다. 보조제 IPA, 폴리알킬암모늄, 및/또는 알칸올아민을 투입, 필요시 첨가제인 비이온성 계면활성제를 투입하고 30±5℃, 20±5분간 순환시킨다. 정련을 한 필라멘트 Carrier(폴리에스터 섬유)를 장착하고, 액비 1:15~1:20, pH 3~5로 조정하여 용액순환 Pump를 가동하여 정압(2.0kg/㎠)을 유지하고, 용액은 3~10분 간격으로 In→Out, Out→In으로 교대로 순환시키며 80~105℃로 서서히 승온하여 120~200분 처리하고 온수 및 냉수로 충분히 수세하여 미 반응물을 제거한다.The dissolution order of the preparations in the reforming step is first circulated by adding acetic acid (hydrolysis catalyst) to 1/3 of the total amount of water used. Next, the gelling agent is added to a separate PE container, and the mixture is stirred for 5 minutes or more while gradually adding the silane coupling agent to the solution into which acetic acid is added. Auxiliaries IPA, polyalkylammonium, and / or alkanolamine are added, and if necessary, an additive, a nonionic surfactant, is added and circulated for 30 ± 5 ° C. and 20 ± 5 minutes. Equipped with refined filament carrier (polyester fiber), adjusted to liquid ratio 1: 15 ~ 1: 20, pH 3 ~ 5 to operate solution circulation pump to maintain constant pressure (2.0kg / ㎠), Circulate alternately from In to Out and Out to In at intervals of ~ 10 minutes, slowly warm up to 80 to 105 ° C, process for 120 to 200 minutes, and wash with hot and cold water to remove unreacted material.
그런 후, 전도성을 부여하기 전에 탈수하여 전도성을 부여하거나, 80~100℃에서 2~3시간 건조하여 전도성을 부여할 수도 있다. Then, before giving conductivity, dehydration may be performed to give conductivity, or drying may be performed at 80 to 100 ° C. for 2 to 3 hours to give conductivity.
다음으로, 개질화된 폴리에스터 섬유에 대해서, 동(Cu)화합물, 환원제, 안정제, 착화 및 PH 조정제, 황화합물을 첨가하여 35~65℃에서 200~400분 처리하여, 폴리에스터 섬유에 구리로 전도성을 부여하는 전도성 부여 단계를 거친다. 즉, 개질된 섬유를 화학적환원법(화학적에너지 차)에 의해 전도성을 부여하게 된다. Next, for the modified polyester fiber, copper (Cu) compound, reducing agent, stabilizer, complexing and PH adjusting agent, sulfur compound was added and treated at 35-65 ° C. for 200-400 minutes to conduct conductive copper to polyester fiber. The conductivity is passed through the step of giving. In other words, the modified fibers are given conductivity by chemical reduction (chemical energy difference).
동(Cu)화합물은 구리 이온원으로서, 황산제2구리(CuSO4.5H2O), 질산제2구리[Cu(NO3)2], 염화제2구리 (CuCl2. 2H2O), 아세트산구리[Cu(CH3COO)2] 등 1종 또는 2종을 사용할 수 있다. 동(Cu) 화합물 사용량은 10~30g/l 이다.Copper (Cu) is a copper ion source, cupric sulfate (CuSO4.5H2O), cupric nitrate [Cu (NO3) 2], cupric chloride (CuCl2H2O), copper acetate [Cu (CH3COO) 2] etc. can be used 1 type or 2 types. The amount of copper (Cu) compound is 10 to 30 g / l.
환원제는 황산히드록실아민[(NH3OH)2SO4], 염산히드록실아민(NH2OH.HCl), 구연산나트륨[(CH2COONa)2.2H2O], 차아인산염(NaH2PO2), 포름알데히드(HCHO), 디메틸아민보란[(CH3)2HNBH3], 하이포인산나트륨(NaH2PO2), 티오황산나트륨(Na2S2O3), 수소화붕소나트륨(NaBH4)을 이용할 수 있다. 환원제 사용량은 10~30g/l이다. The reducing agent is hydroxylamine sulfate [(NH3OH) 2SO4], hydroxylamine hydrochloride (NH2OH.HCl), sodium citrate [(CH2COONa) 2.2H2O], hypophosphite (NaH2PO2), formaldehyde (HCHO), dimethylamineborane [( CH 3) 2 HNBH 3], sodium hypophosphate (NaH 2 PO 2), sodium thiosulfate (Na 2 S 2 O 3), and sodium borohydride (NaBH 4). The amount of reducing agent is 10-30 g / l.
안정제는 전도성 부여시 용액의 급격한 반응을 방지하여 안정된 상태를 유지하도록 하여 반응이 일정하게 고르게 진행되도록 한다. 즉, 생성되는 황화구리의 입자를 고르게 하고, 황화구리의 침전물 생성을 방지하는 역할을 한다. 안정제는 시안화합물, 티오요소[(NH2)2CS], 인산디나트륨(Na2HPO4.12H2O)등을 사용하고, 사용량은 10~40g/l 이다. The stabilizer prevents the rapid reaction of the solution when the conductivity is imparted to maintain a stable state so that the reaction proceeds evenly. That is, it serves to even out the particles of copper sulfide produced and to prevent the formation of precipitates of copper sulfide. The stabilizer is a cyanide compound, thiourea [(NH2) 2CS], disodium phosphate (Na2HPO4.12H2O), and the like. The amount is 10 to 40 g / l.
착화 및 pH 조정제는 EDTA, 구연산(C6H10O8), 주석산(C4H6O6), 탄산(H2CO3), 염산(HCl), 황산(H2SO4), 아세트산(CH3COOH) 등을 사용한다. 착화 및 pH 조정제의 사용량은 10~20g/l 이다. Complexing and pH adjusting agents use EDTA, citric acid (C6H10O8), tartaric acid (C4H6O6), carbonic acid (H2CO3), hydrochloric acid (HCl), sulfuric acid (H2SO4), acetic acid (CH3COOH) and the like. The use amount of complexing and pH adjusting agent is 10-20 g / l.
황(S)화합물은 섬유에 반응된 구리 이온을 황화구리로 고르게 분산 흡착시켜 전도성을 갖도록 한다. 아디티온산나트륨(Na2S2O4), 산성아황산나트륨(Na2S2O5), 티오황산나트륨(Na2S2O3), 론가리트(NaHSO2HCHO.2H2O), 아황산수소나트륨(NaHSO3) 등을 사용할 수 있다. 황화합물 사용량은 10~30g/l 이다.The sulfur (S) compound evenly disperses and adsorbs copper ions reacted with fibers with copper sulfide to have conductivity. Sodium adithionate (Na2S2O4), acidic sodium sulfite (Na2S2O5), sodium thiosulfate (Na2S2O3), rongarite (NaHSO2HCHO.2H2O), sodium hydrogen sulfite (NaHSO3), etc. can be used. Sulfur compound used is 10 ~ 30g / l.
전도성 부여 단계에서 선택적으로 내구성 강화제가 사용될 수 있다. 내구성 강화제는 질산은(AgNO3), 황산은(Ag2SO4), 및 염화은(AgCl)으로 이루어진 군으로부터 1종 이상을 선택하여 사용할 수 있고, 사용량은 0.10~0.50g/l이며, 내구성 및 내식성을 향상시키게 된다. Durability enhancers may optionally be used in the conductivity provision step. Durability enhancers can be used by selecting one or more from the group consisting of silver nitrate (AgNO3), silver sulfate (Ag2SO4), and silver chloride (AgCl), the amount of use is 0.10 ~ 0.50g / l, improves durability and corrosion resistance .
또한, 전도성 부여 단계에서 선택적으로 내식성 강화제가 사용될 수 있다. 내구성 강화제는 황산니켈(NiSO4.6H2O), 황산아연(ZnSO4), 황산망간(MnSO4)을 사용할 수 있고, 사용량은 0.10~0.50g/l 이며, 내식성 향상을 위해 사용된다. In addition, a corrosion resistance enhancer may optionally be used in the conductivity provision step. Durability enhancers may be used nickel sulfate (NiSO4.6H2O), zinc sulfate (ZnSO4), manganese sulfate (MnSO4), the amount is 0.10 ~ 0.50g / l, used to improve the corrosion resistance.
전도성 부여 단계에서 조제들의 용해 순서에 대해 설명하면, 조제들을 25~35℃에서 20~30분간 충분히 교반하여 용해한 후에, 피염물 Carrier(폴리에스터 섬유)를 장착하고, 액비를 1:15~1:20, pH 2.5~4.0으로 조정하여 용액순환 Pump를 가동하여 정압(2.0kg/㎠)을 유지하고, 용액은 3~10분 간격으로 In→Out, Out→In으로 교대로 순환시켜 반응을 고르게 하여 내외부의 이상반응을 방지하고 우수한 제품을 생산한다. 전도성부여 처리온도는 35~65℃에서 200~400분 처리한다. The dissolution order of the preparations in the step of imparting conductivity is described. After dissolving the preparations at 25 to 35 ° C. for 20 to 30 minutes, the salt solution Carrier (polyester fiber) is mounted and the liquid ratio is 1:15 to 1: 20, pH 2.5 ~ 4.0 to operate the solution circulation pump to maintain a constant pressure (2.0kg / ㎠), and the solution is circulated alternately by In → Out, Out → In every 3-10 minutes to evenly react Prevents abnormal reactions inside and outside and produces excellent products. Conductivity treatment temperature is 200 ~ 400 minutes at 35 ~ 65 ℃.
본 발명에서 폴리에스터 섬유에의 전도성 부여는 화학적환원법(화학적에너지 차)에 의한 전도성 부여 방법인데, 고분자재료(섬유)와 실란계 커플링제의 가수분해 된 Si-OH기가 금속염(구리염)과 결합하는 가교결합(화학적 흡착), 수소결합 등 다양한 형태로 섬유표면 층을 형성하게 되고, 특히 알카리 감량으로 형성된 섬유표면의 요철부분이 Anchor 효과로 우수한 밀착력을 발휘하게 되어 물리적인 강도개선과 전기적 성질, 내구성도 좋아지게 된다.In the present invention, the imparting conductivity to the polyester fiber is a method of imparting conductivity by chemical reduction method (chemical energy difference), and the hydrolyzed Si-OH group of the polymer material (fiber) and the silane coupling agent is combined with the metal salt (copper salt). The fiber surface layer is formed in various forms such as crosslinking (chemical adsorption), hydrogen bonding, and the like, and the uneven portion of the fiber surface formed by alkali reduction exhibits excellent adhesion due to the anchor effect, thereby improving physical strength and electrical properties, Durability is also improved.
다음으로, 촉감개선제, 발수제, 발유제, 기모향상제, 방청제, 유연평활제, 대전방지제, 코팅제, 및 산화방지제로 이루어진 군으로부터 1종 이상이 선택된 기능성유제를 이용하여 폴리에스터 섬유에 유제처리하는 유제처리 단계를 선택적으로 이용한다. 정련단계에서 전도성 부여 단계를 거친 폴리에스터 섬유를 소비자의 요구에 맞게 유제를 처리하여 해사성, 제편성, 제직성, 촉감, 기모성, 기능보호, 발수성, 발유성, 방청성 등의 기능을 보유하기 위하여 적절한 유지분을 갖도록 한다. 통상 제품상태의 유지분은 0.35~1.00 중량% 이며 사용목적에 따라 조정한다.Next, an emulsion for emulsifying the polyester fiber by using a functional oil agent selected from the group consisting of a tactile improver, a water repellent, an oil repellent, a raising agent, a rust preventive agent, a softening agent, an antistatic agent, a coating agent, and an antioxidant. Optionally use processing steps. The polyester fiber that has undergone conductivity in the refining stage is treated with emulsion to meet the needs of the consumer so that it possesses functions such as sea repellency, knitting, weaving, texture, brushing, function protection, water repellency, oil repellency, and rust resistance. Make sure you have the right amount of fat. Normal maintenance of product is 0.35 ~ 1.00 wt% and it is adjusted according to purpose of use.
다음으로, 상기 전도성이 부여된 폴리에스터 섬유를 함수율 25~35%가 되도록 탈수시키고, 열을 가하여 건조시키는 탈수 및 건조 단계를 거친다. Next, the conductive fiber is dehydrated to have a water content of 25 to 35%, and subjected to a dehydration and drying step by applying heat to dry the polyester fiber.
탈수는 일반적인 원심탈수기나 고압공기에 의한 Cheese 탈수기를 사용하면 된다. 주의할 점은 과도한 탈수는 유지분을 저하시키고, 미흡한 탈수는 유지분의 상승과 건조 시간 지연으로 에너지 낭비요인이 됨으로 사전 테스트를 하고, 탈수 시 중간점검(실측확인)하여야 좋다. 탈수 후 함수율은 25~35%가 바람직하다. Dehydration can be done using a general centrifugal dehydrator or a cheese dehydrator with high pressure air. It should be noted that excessive dehydration lowers the oil content, and insufficient dehydration is a waste of energy due to the rise of oil content and delay in drying time, and should be tested in advance. The water content after dehydration is preferably 25 to 35%.
건조는 일반 열풍건조기나 고압치즈 건조기를 사용할 수 있으며, 에너지 절감 및 작업 의 용이성, 건조시간 단축 등의 면에서 고압 치즈 건조기가 이상적이다. 고압치즈 건조기는 공기의 밀도가 크게 되면 여기에 비례하여 열에너지도 크게 되는 성질을 이용한 것으로 5~6기압 정도의 열풍을 Cheese에 통과시켜 피염물에 함유된 수분을 콘덴서로 제거하고 다시 열풍을 통과시키는 과정을 반복하여 건조하는 장치이다. 기기에 부착된 습도계를 참조하여 피염물을 확인하여 관리하고 운전방법을 최적화 하여 에너지 낭비를 방지한다.
For drying, a general hot air dryer or a high pressure cheese dryer may be used. The high pressure cheese dryer is ideal for energy saving, ease of operation, and shortening of drying time. The high pressure cheese dryer uses the property that the heat energy increases in proportion to the density of the air. The hot air of about 5 to 6 atmospheres is passed through the cheese to remove the moisture contained in the chlorine with a condenser and then passes the hot air again. It is a device to dry the process repeatedly. Refer to the hygrometer attached to the equipment to check and manage the contaminants and to optimize the operation method to prevent energy waste.
다음으로, 구체적인 실시예를 예로 들어 본 발명의 화학적환원법에 의한 폴리에스터 섬유에 도전성을 부여하는 방법에 대해서 기술한다. 다만, 하기의 실시예는 본 발명의 바람직한 실시예일 뿐, 본 발명이 하기 실시예에 의해 한정되는 것은 아니다. Next, the specific example is given and the method to give electroconductivity to the polyester fiber by the chemical reduction method of this invention is described. However, the following examples are only preferred examples of the present invention, and the present invention is not limited by the following examples.
Polyester 70D/36F 필라멘트를 약 60℃ 온수에서 비이온성계면활성제 1.5g/l, 30분간 처리하여 유제 및 불순물을 제거하고 수세하였다. 알카리 감량은 Polyester 70D / 36F filament was treated with 1.5 g / l of nonionic surfactant for 30 minutes in hot water of about 60 ℃ to remove oil and impurities and washed with water. Alkaline weight loss
가성소다 20~80g/l, 양이온 계면활성제 1~3g/l, 온도 약 80℃에서 약 60분간 처리한 후, 염산 0.01g/l 용액으로 중화 후 수세를 하였다. Caustic soda was treated at 20 to 80 g / l, cationic surfactant 1 to 3 g / l at a temperature of about 80 ° C. for about 60 minutes, and then neutralized with hydrochloric acid 0.01 g / l solution and washed with water.
다음으로, 섬유개질은 γ-머캅토프로필메톡시실란 20g/l, 메탄올 15g/l, 아세트산 0.001g/l , 보조제인 IPA 12g/l, 폴리알킬암모늄 2g/l, 알칸올아민 10g/l 를 포함하는 욕비 1:20, pH 3~5 용액을 정압(2.0kg/㎠) 유지, 약 5분 간격으로 In→Out, Out→In으로 교대로 순환, 상온에서 90℃ 서서히 승온하여 180분 처리하고 온수 및 냉수로 충분히 수세하여 반응 잔류물을 제거하고 탈수하였다. Next, the fiber modification is γ-mercaptopropyl methoxysilane 20g / l, methanol 15g / l, acetic acid 0.001g / l, auxiliary IPA 12g / l, polyalkylammonium 2g / l, alkanolamine 10g / l Bath ratio 1:20, pH 3 ~ 5 solution containing a constant pressure (2.0kg / ㎠), maintaining the constant pressure (In → Out, Out → In circulating alternately at intervals of about 5 minutes, slowly heated to 90 ℃ at room temperature 180 minutes treatment Water washing with hot and cold water was sufficient to remove the reaction residue and dewatering.
개질된 폴리에스터(polyester) 필라멘트를 동(Cu)화합물인 황산제2구리 20g/l, 환원제 황산하이드록실아민 20g/l, 황화합물인 중아황산소다 5g/l, 착화 및 pH조정제 아세트산 15g/l, 안정제로 구연산나트륨 20g/l를 포함하는 약품용액을 30℃에서 약 25분간 충분히 교반하여 용해한 후에 피염물 Carrier를 장착하고, 액비를 1:15~1:20, pH 3~4으로 조정하여 용액순환 Pump를 가동하여 정압(2.0kg/㎠)유지, 약 10분 간격으로 In→Out, Out→In으로 교대로 순환 운전하였다. 처리온도는 약 50℃에서 240분 처리 후 온수 냉수로 충분히 수세하여 반응 잔류물을 제거하고 유제처리 탈수/건조하였다. 20 g / l cupric sulfate as a copper compound, 20 g / l as reducing agent hydroxylamine sulfate, 5 g / l as sodium bisulfite as sulfur compound, 15 g / l complexing and pH adjuster acetic acid, After dissolving the drug solution containing 20 g / l of sodium citrate as a stabilizer sufficiently for about 25 minutes at 30 ° C, dissolving the solution, the salt solution carrier was mounted, and the solution ratio was adjusted to 1:15 to 1:20 and pH 3 to 4 to circulate the solution. The pump was operated to maintain a constant pressure (2.0kg / ㎠) and cycled alternately from In to Out and Out to In at about 10 minute intervals. The treatment temperature was treated at about 50 ° C. for 240 minutes, washed with warm water and cold water to remove the reaction residue, and then dehydrated and dried.
실시예 1에서 제조된 제품에 대해서, 비저항, Cu 함량, 색상, 밀착 정도를 측정하여, 하기의 표1에 나타내었다. For the product prepared in Example 1, the specific resistance, Cu content, color, degree of adhesion were measured, and are shown in Table 1 below.
상기 실시예 1에서와 동일한 방법으로 실험을 실시하되, 섬유개질 후 약 90℃에서 2시간 건조하고, 상기 실시 예 1과 같은 방법으로 전도성을 부여하였다. The experiment was carried out in the same manner as in Example 1, but after the fiber modification was dried for 2 hours at about 90 ℃, the conductivity was given in the same manner as in Example 1.
분석결과는 표 1과 같고, 상기 실시 예 1에 비하여 섬유개질 후 2시간의 건조공정이 추가되었지만 결과가 실시 예 1과 유사한 것은 유제처리 후 건조공정에서 열에 의한 결합(밀착)력이 제품에 영향을 미치게 된다.The analysis results are shown in Table 1, and the drying process of 2 hours after the fiber modification was added as compared to Example 1, but the result is similar to that of Example 1, in which the bonding (adhesive) force by heat in the drying process after emulsion treatment affects the product. Get mad.
상기 실시예 1에서와 동일한 방법으로 실험을 실시하되, 전도성 부여 단계에서 환원제로 황산하이드록실아민 대신에 티오황산나트륨 20g/l를 사용하고, 내구성 강화제로 질산은(AgNO3) 0.2g/l을 추가로 사용하여 위 실시 예 1과 같은 방법으로 처리하였다. The experiment was conducted in the same manner as in Example 1, but 20 g / l of sodium thiosulfate was used instead of hydroxylamine sulfate as a reducing agent in the step of providing conductivity, and 0.2 g / l of silver nitrate (AgNO3) was further used as a durability enhancer. It was treated in the same manner as in Example 1.
분석결과는 표 1과 같고 고가의 희귀금속 사용으로 내구성이 좋아졌다.The analysis results are shown in Table 1 and the durability is improved by using expensive rare metals.
상기 실시예 1에서와 동일한 방법으로 실험을 실시하되, 내식성강화제로 황산니켈(NiSO4.6H2O) 5~15g/l를 추가하여 상기 실시 예 1과 같은 방법으로 처리하였다.The experiment was carried out in the same manner as in Example 1, but 5 to 15 g / l of nickel sulfate (NiSO4.6H 2 O) was added as a corrosion-resistant reinforcing agent and treated in the same manner as in Example 1.
분석결과는 표 1과 같다. The analysis results are shown in Table 1.
비교예Comparative example 1 One
알칼리 감량공정을 생략하고, 섬유개질 단계 중 보조제를 사용하지 않는 조건으로 하여 실시 예 1 과 같이 처리하였다. 분석결과는 표 1과 같이 비저항 상승, Cu함량 감소, 결합(밀착)력이 나쁘게 나타났다.The alkali reduction step was omitted and the treatment was carried out as in Example 1 under the condition that no auxiliary agent was used during the fiber modification step. As shown in Table 1, the increase in the resistivity, the Cu content decrease, and the bonding (adhesion) force were bad.
하기의 표 1은 실시예 1 내지 4 및 비교예 1에서 측정된, 비저항, Cu함량, 밀착정도를 나타내었다. Table 1 below shows the specific resistance, Cu content, adhesion degree measured in Examples 1 to 4 and Comparative Example 1.
(Ω.㎝)Resistivity
(Ω.㎝)
<시험조건><Test Conditions>
비저항 : 온도(20±2℃), 습도(40±2%), Specific resistance: temperature (20 ± 2 ℃), humidity (40 ± 2%),
시험기기- WHEATSTONE BRIDGE(Fortable)Test Equipment-WHEATSTONE BRIDGE (Fortable)
Cu함량 : 섬유 중 Cu 함량 분석(습식분석법) Cu content: analysis of Cu content in the fiber (wet analysis method)
밀착정도 : 시험편(필라멘트 10cm, 무게 2g)을 50℃의 계면활성제 1g/l 용액에서 시험편을 반으로 접어서 200회 균일한 힘으로 문지른 후 세척하고 건조하여 정도에 따라 우수, 양호, 보통, 미흡, 불량으로 판정한다.
Adhesiveness: Fold the test piece (10cm filament, weight 2g) in 50g of 1g / l surfactant at 50 ℃, rub the test piece in half, rub it with 200 times uniform force, wash and dry it according to the degree of good, good, normal, poor, It is judged to be defective.
이상에서 본 발명의 실시예에 대하여 기재하였지만, 본 발명이 이에 한정되는 것은 아니고, 해당 기술 분야의 통상의 기술자는 상기 기재된 범위 및 하기의 특허청구범위에 기재된 본 발명의 사상 및 영역으로 부터 벗어나지 않은 범위 내에서는 본 발명을 다양하게 변경 및 수정시킬 수 있음을 인지할 수 있을 것이다.
While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims. It will be appreciated that various changes and modifications may be made therein without departing from the scope of the invention.
Claims (8)
폴리에스터 섬유를 알카리 가수분해제인 가성소다 수용액에서 온도 50~65℃, 25~50분간 처리한 후, 염산용액으로 중화 후 수세하는, 폴리에스터 섬유 표면에 대한 알카리 감량단계;
물을 용매로 하여, 실란계 커플링제, 알코올류 겔화 방지제, 가수분해 촉매제, 보조제 및 분산효과를 증대시키기 위해서 비이온성 계면 활성제를 첨가하여 80~105℃로 서서히 승온하면서 120~200분 처리하여, 폴리에스터 섬유를 개질하는 개질 단계;
동(Cu)화합물, 환원제, 안정제, 착화 및 PH 조정제, 황화합물을 첨가하여 35~65℃에서 200~400분 처리하여, 폴리에스터 섬유에 구리로 전도성을 부여하는 전도성 부여 단계; 및
상기 전도성이 부여된 폴리에스터 섬유를 함수율 25~35%가 되도록 탈수시키고, 열을 가하여 건조시키는 탈수 및 건조 단계;를 포함하는 것을 특징으로 하는 폴리에스터 섬유의 전도성 부여방법. Refining step of removing impurities attached to the polyester fiber;
An alkali reduction step for the surface of the polyester fiber, which is treated with polyester fiber in an aqueous solution of caustic soda which is an alkali hydrolyzing agent at a temperature of 50 to 65 ° C. for 25 to 50 minutes, and then neutralized with hydrochloric acid solution and washed with water;
Using water as a solvent, a silane coupling agent, an alcohol gelling agent, a hydrolysis catalyst, an auxiliary agent, and a nonionic surfactant were added to increase the dispersing effect, and then treated at 120 to 200 minutes while gradually warming to 80 to 105 ° C. A modification step of modifying the polyester fibers;
Adding a copper (Cu) compound, a reducing agent, a stabilizer, a complexing agent and a PH adjusting agent, and a sulfur compound to treat 200 to 400 minutes at 35 to 65 ° C. to impart conductivity to the polyester fiber with copper; And
And dehydrating and drying the polyester fibers to which the conductivity is imparted so as to have a water content of 25 to 35%, and drying by applying heat.
상기 정련단계에서 저기포성 비이온성계면활성제가 사용되는 것을 특징으로 하는 폴리에스터 섬유의 전도성 부여방법. The method of claim 1,
In the refining step, a low-bubble nonionic surfactant is used to impart conductivity of the polyester fiber, characterized in that used.
상기 알카리 감량 단계에서 양이온성 계면활성제를 추가로 포함하는 것을 특징으로 하는 폴리에스터 섬유의 전도성 부여방법. The method of claim 1,
The method of imparting conductivity of the polyester fiber, characterized in that it further comprises a cationic surfactant in the alkali reduction step.
상기 개질 단계에서,
알코올류 겔화 방지제는 상기 커플링제가 메톡시 실란류의 경우에는 메탄올이 사용되고 상기 커플링제가 에톡시 실란류의 경우에는 에탄올이 사용되며,
상기 가수분해 촉매제는 염산(HCl), 아세트산(CH3COOH), 개미산(HCOOH), 및 옥살산(C2H2O4)으로 이루어진 군으로부터 선택된 1종 이상이 사용되며,
상기 보조제는 이소프로필알코올(IPA), 폴리알킬암모늄, 및 알칸올아민으로 이루어진 군으로부터 선택된 1종 이상이 사용되는 것을 특징으로 하는 폴리에스터 섬유의 전도성 부여방법. The method of claim 1,
In the modification step,
Alcohol-gelling inhibitors include methanol when the coupling agent is methoxy silanes and ethanol when the coupling agent is ethoxy silanes.
The hydrolysis catalyst is one or more selected from the group consisting of hydrochloric acid (HCl), acetic acid (CH3COOH), formic acid (HCOOH), and oxalic acid (C2H2O4),
The auxiliary agent is a method for imparting conductivity of a polyester fiber, characterized in that at least one selected from the group consisting of isopropyl alcohol (IPA), polyalkylammonium, and alkanolamine is used.
상기 전도성 부여 단계에서,
질산은, 황산은, 및 염화은으로 이루어진 군으로부터 1종 이상 선택되는 내구성 강화제를 추가로 포함하는 것을 특징으로 하는 폴리에스터 섬유의 전도성 부여방법. The method of claim 1,
In the conductivity provision step,
Silver nitrate, sulfuric acid, silver chloride and silver chloride further comprises a durability enhancer selected from the group consisting of a method for imparting conductivity of the polyester fiber.
상기 전도성 부여 단계에서,
황산니켈(NiSO4.6H2O), 황산아연(ZnSO4, 및 황산망간(MnSO4)으로 이루어진 군으로부터 1종 이상 선택되는 내식성 강화제를 추가로 포함하는 것을 특징으로 하는 폴리에스터 섬유의 전도성 부여방법. The method of claim 1,
In the conductivity provision step,
Nickel sulfate (NiSO4.6H2O), zinc sulfate (ZnSO4, and manganese sulfate (MnSO4) at least one selected from the group consisting of corrosion-resistant reinforcing agent further comprises a method of imparting a conductivity of the polyester fiber.
상기 전도성 부여 단계 이후에,
촉감개선제, 발수제, 발유제, 기모향상제, 방청제, 유연평활제, 대전방지제, 코팅제, 및 산화방지제로 이루어진 군으로부터 1종 이상이 선택된 기능성유제를 이용하여 폴리에스터 섬유에 유제처리하는 유제처리 단계를 추가로 포함하는 것을 특징으로 하는 폴리에스터 섬유의 전도성 부여방법.
The method of claim 1,
After the imparting conductivity,
Emulsion treatment step of emulsifying polyester fiber using a functional oil agent selected from the group consisting of tactile improver, water repellent, oil repellent, brush raising, anti-rusting agent, softening agent, antistatic agent, coating agent, and antioxidant Conductive imparting method of the polyester fiber, characterized in that it further comprises.
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| JP2018514662A (en) * | 2015-03-27 | 2018-06-07 | 株式会社リテンド | Functional copper sulfide composition and functional fiber produced therefrom |
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| KR102152060B1 (en) | 2019-09-20 | 2020-09-04 | 조상진 | ESD safe mat and manufacturing method thereof |
| KR102264311B1 (en) * | 2020-12-14 | 2021-06-15 | 김근소 | Method for producing fiber with excellent conductivity and antioxidant |
| CN114105494A (en) * | 2021-10-22 | 2022-03-01 | 北京科技大学 | Coupling agent compounded ionic nickel palladium-free activation solution and method for preparing conductive basalt fiber |
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