CN114990880B - 一种导电液晶聚芳酯纤维及其制备方法 - Google Patents
一种导电液晶聚芳酯纤维及其制备方法 Download PDFInfo
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- CN114990880B CN114990880B CN202210582115.0A CN202210582115A CN114990880B CN 114990880 B CN114990880 B CN 114990880B CN 202210582115 A CN202210582115 A CN 202210582115A CN 114990880 B CN114990880 B CN 114990880B
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- polyarylate
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- 239000000835 fiber Substances 0.000 title claims abstract description 151
- 239000004973 liquid crystal related substance Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 229920001230 polyarylate Polymers 0.000 claims abstract description 90
- 238000007747 plating Methods 0.000 claims abstract description 47
- 238000000034 method Methods 0.000 claims abstract description 28
- 229910052751 metal Inorganic materials 0.000 claims abstract description 27
- 239000002184 metal Substances 0.000 claims abstract description 27
- 238000005530 etching Methods 0.000 claims abstract description 20
- 239000000126 substance Substances 0.000 claims abstract description 20
- 230000004913 activation Effects 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 79
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 51
- 238000001035 drying Methods 0.000 claims description 37
- 150000001875 compounds Chemical class 0.000 claims description 34
- 238000003756 stirring Methods 0.000 claims description 29
- 238000004140 cleaning Methods 0.000 claims description 27
- 239000011259 mixed solution Substances 0.000 claims description 26
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 14
- 239000001509 sodium citrate Substances 0.000 claims description 14
- 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 claims description 14
- 230000003213 activating effect Effects 0.000 claims description 13
- 230000004048 modification Effects 0.000 claims description 13
- 238000012986 modification Methods 0.000 claims description 13
- 238000007788 roughening Methods 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 12
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 10
- 239000003638 chemical reducing agent Substances 0.000 claims description 9
- 150000003839 salts Chemical class 0.000 claims description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical class NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 8
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 claims description 8
- 229920000768 polyamine Polymers 0.000 claims description 8
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 6
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 6
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims description 5
- 125000003277 amino group Chemical group 0.000 claims description 5
- 229960001149 dopamine hydrochloride Drugs 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 4
- 150000001414 amino alcohols Chemical class 0.000 claims description 4
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims description 4
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims description 4
- 229910021645 metal ion Inorganic materials 0.000 claims description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 4
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 claims description 4
- 229920002554 vinyl polymer Polymers 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 claims description 2
- HXKKHQJGJAFBHI-UHFFFAOYSA-N 1-aminopropan-2-ol Chemical compound CC(O)CN HXKKHQJGJAFBHI-UHFFFAOYSA-N 0.000 claims description 2
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 2
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 2
- 239000001263 FEMA 3042 Substances 0.000 claims description 2
- WTDRDQBEARUVNC-LURJTMIESA-N L-DOPA Chemical compound OC(=O)[C@@H](N)CC1=CC=C(O)C(O)=C1 WTDRDQBEARUVNC-LURJTMIESA-N 0.000 claims description 2
- OUYCCCASQSFEME-QMMMGPOBSA-N L-tyrosine Chemical compound OC(=O)[C@@H](N)CC1=CC=C(O)C=C1 OUYCCCASQSFEME-QMMMGPOBSA-N 0.000 claims description 2
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 claims description 2
- 239000005708 Sodium hypochlorite Substances 0.000 claims description 2
- QVYARBLCAHCSFJ-UHFFFAOYSA-N butane-1,1-diamine Chemical compound CCCC(N)N QVYARBLCAHCSFJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- 238000010668 complexation reaction Methods 0.000 claims description 2
- 229960003638 dopamine Drugs 0.000 claims description 2
- 235000004515 gallic acid Nutrition 0.000 claims description 2
- 229940074391 gallic acid Drugs 0.000 claims description 2
- SYECJBOWSGTPLU-UHFFFAOYSA-N hexane-1,1-diamine Chemical compound CCCCCC(N)N SYECJBOWSGTPLU-UHFFFAOYSA-N 0.000 claims description 2
- 229940102253 isopropanolamine Drugs 0.000 claims description 2
- 238000006011 modification reaction Methods 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 2
- 238000006116 polymerization reaction Methods 0.000 claims description 2
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 2
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 2
- 235000015523 tannic acid Nutrition 0.000 claims description 2
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 claims description 2
- 229940033123 tannic acid Drugs 0.000 claims description 2
- 229920002258 tannic acid Polymers 0.000 claims description 2
- OUYCCCASQSFEME-UHFFFAOYSA-N tyrosine Natural products OC(=O)C(N)CC1=CC=C(O)C=C1 OUYCCCASQSFEME-UHFFFAOYSA-N 0.000 claims description 2
- KPZGRMZPZLOPBS-UHFFFAOYSA-N 1,3-dichloro-2,2-bis(chloromethyl)propane Chemical compound ClCC(CCl)(CCl)CCl KPZGRMZPZLOPBS-UHFFFAOYSA-N 0.000 claims 1
- RJTANRZEWTUVMA-UHFFFAOYSA-N boron;n-methylmethanamine Chemical compound [B].CNC RJTANRZEWTUVMA-UHFFFAOYSA-N 0.000 claims 1
- MUJIDPITZJWBSW-UHFFFAOYSA-N palladium(2+) Chemical compound [Pd+2] MUJIDPITZJWBSW-UHFFFAOYSA-N 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 14
- 238000000151 deposition Methods 0.000 abstract description 6
- 230000008021 deposition Effects 0.000 abstract description 6
- 239000011248 coating agent Substances 0.000 abstract description 5
- 238000000576 coating method Methods 0.000 abstract description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 4
- 238000007385 chemical modification Methods 0.000 abstract description 4
- 229910052802 copper Inorganic materials 0.000 abstract description 4
- 239000010949 copper Substances 0.000 abstract description 4
- 239000002131 composite material Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract 1
- 239000008367 deionised water Substances 0.000 description 27
- 229910021641 deionized water Inorganic materials 0.000 description 27
- 238000002791 soaking Methods 0.000 description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 27
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 22
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 16
- 230000000536 complexating effect Effects 0.000 description 14
- 230000009467 reduction Effects 0.000 description 13
- 230000001105 regulatory effect Effects 0.000 description 11
- 229910052759 nickel Inorganic materials 0.000 description 10
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 10
- 239000007853 buffer solution Substances 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 101150003085 Pdcl gene Proteins 0.000 description 7
- 238000007772 electroless plating Methods 0.000 description 7
- 239000004744 fabric Substances 0.000 description 7
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 description 6
- -1 amine compounds Chemical class 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- YPTUAQWMBNZZRN-UHFFFAOYSA-N dimethylaminoboron Chemical compound [B]N(C)C YPTUAQWMBNZZRN-UHFFFAOYSA-N 0.000 description 6
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 description 5
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 5
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 5
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 125000001424 substituent group Chemical group 0.000 description 4
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 3
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 2
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229910001431 copper ion Inorganic materials 0.000 description 2
- 229910000365 copper sulfate Inorganic materials 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
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 239000012286 potassium permanganate Substances 0.000 description 2
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- KGYLMXMMQNTWEM-UHFFFAOYSA-J tetrachloropalladium Chemical compound Cl[Pd](Cl)(Cl)Cl KGYLMXMMQNTWEM-UHFFFAOYSA-J 0.000 description 2
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 229920001410 Microfiber Polymers 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 206010042674 Swelling Diseases 0.000 description 1
- 239000004974 Thermotropic liquid crystal Substances 0.000 description 1
- 208000034953 Twin anemia-polycythemia sequence Diseases 0.000 description 1
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000009990 desizing Methods 0.000 description 1
- 229910052805 deuterium Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012943 hotmelt Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000000155 isotopic effect Effects 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 239000003658 microfiber Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000008363 phosphate buffer Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920005594 polymer fiber Polymers 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Classifications
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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
- D06M11/83—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 metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
- C23C18/28—Sensitising or activating
- C23C18/30—Activating or accelerating or sensitising with palladium or other noble metal
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
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- 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
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/152—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen having a hydroxy group bound to a carbon atom of a six-membered aromatic ring
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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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/325—Amines
- D06M13/328—Amines the amino group being bound to an acyclic or cycloaliphatic carbon atom
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Abstract
本发明公开了一种导电液晶聚芳酯纤维及其制备方法。本发明的制备方法采用先物理刻蚀后化学修饰的化学镀前处理工艺,修饰改性纤维表面,使纤维表面附着活性基团,经活化后通过化学镀工艺在LCP纤维表面化学镀镍或铜,制备导电LCP复合纤维,提升金属镀层与纤维的结合力,提高LCP纤维的导电性,生产效率高,且经济环保。本发明的导电液晶聚芳酯纤维采用上述的制备方法制备获得,其中金属镀层与纤维表面的结合稳定性好、镀层沉积均匀,整体导电液晶聚芳酯纤维具有良好的导电性能。
Description
技术领域
本发明涉及聚芳酯纤维制造技术领域,具体涉及一种导电液晶聚芳酯纤维及其制备方法。
背景技术
热致液晶聚芳酯(liquid crystalline polymer—LCP)是一种通过酯基连接的芳环高分子工程塑料,其纤维产品是采用热熔纺丝加工而成,纺丝过程高分子链高度取向形成有序微纤致密结构,化学药品和气体难以渗入,耐酸耐碱性极佳。这些特点赋予了聚芳酯纤维的优异力学强度、耐辐射、耐化学品、耐蠕变等特性,广泛应用于国防军工、航空航天、个体防护、绳索电缆等特种领域。
实际上,LCP纤维高取向的刚性链构象也会导致其在金属化学镀前处理粗化过程显得非常有难度,不易进行化学刻蚀改性,现有的高性能聚合物纤维的化学镀工艺并不适用于LCP纤维的金属化,镀膜在LCP表面的沉积不均匀、结合力低,且化学镀的LCP纤维导电性能差。
而传统聚碳酸酯、ABS塑料化学镀工艺中所采用的高锰酸钾或高浓度碱溶液对LCP处理仅起物理粗化作用,也就是可以对LPC表面进行物理刻蚀形成粗糙结构,但不能极化材料表面并形成极性基团,因此不能改善材料表面的亲水性。如中国专利CN110983306 B公开的LCP塑料的镀前表面粗化方法,包括膨胀剂膨润处理、高锰酸钾微蚀处理及酸性溶液中和处理三个步骤;中国专利申请CN 112647065A公开的LCP器件化学镀前表面粗化方法,具体是将LCP材料放入通有臭氧的过硫酸钾粗化液中,在超声波作用下进行粗化处理。但是,这些方法仅适用于LCP膜等塑料器件,并不适用于LCP纤维的粗化,且这些方法在进行表面粗化处理所采用的溶液均对环境不友好。
发明内容
本发明的目的是为了解决LCP纤维化学镀过程中存在表面预处理工艺不环保、沉积不均匀、结合力低、导电性能改善不明显等问题,提供了一种导电液晶聚芳酯纤维的制备方法。该制备方法采用先物理刻蚀后化学修饰的化学镀前处理工艺,经活化后通过化学镀工艺在LCP纤维表面化学镀镍或铜,制备导电LCP复合纤维,提升金属镀层与纤维的结合力,提高LCP纤维的导电性。
本发明的另一目的在于提供一种导电液晶聚芳酯纤维,该导电液晶聚芳酯纤维由上述制备方法制得。
本发明的目的通过如下技术方案实现。
一种导电液晶聚芳酯纤维的制备方法,其特征在于,包括如下步骤:
S1、将聚芳酯纤维洗涤处理,干燥;
S2、将洗涤处理后的聚芳酯纤维在蚀刻液中刻蚀粗化,取出,清洗、干燥;
S3、将刻蚀粗化后的聚芳酯纤维置于修饰液中进行表面修饰,取出,清洗、干燥;
S4、将经表面修饰后的聚芳酯纤维置于活化液中活化,取出,清洗、干燥;
S5、将活化后的聚芳酯纤维置于镀液中进行化学镀,取出,清洗、干燥,获得导电液晶聚芳酯纤维。
优选的,S1中,所述洗涤处理为脱浆洗涤,具体的,将所述聚芳酯纤维浸泡于丙酮溶液中6~12小时,浸泡温度为常温,再用无水乙醇和去离子水反复清洗干净,去除纤维表面的杂质。
优选的,S1中,所述干燥是在60~80℃真空干燥6~12小时。
优选的,S2中,所述蚀刻液为浓度1~20mol/L金属碱性氢氧化物和浓度1~15mol/L增溶剂的混合溶液;所述刻蚀粗化的时间为5~60分钟。
更优选的,所述金属碱性氢氧化物包括氢氧化钠、氢氧化钾和氢氧化锂中的一种以上;
和/或,所述增溶剂包括尿素和氨基醇类衍生物中的一种以上,所述氨基醇类衍生物包括2-羟基乙胺和异丙醇胺中的一种以上。
更优选的,所述蚀刻液为浓度5~15mol/L金属碱性氢氧化物和浓度1~10mol/L增溶剂的混合溶液。
更优选的,所述刻蚀粗化的时间为10~30分钟。
优选的,S3中,所述修饰液为含酚羟基和胺基化合物的溶液,且能自身氧化聚合反应沉积于纤维表面;或者,所述修饰液为含酚羟基化合物与含胺基化合物的混合物溶液,且能通过化学反应生成膜沉积于纤维表面;
所述表面修饰的反应在室温、pH值7~10、60~600r/min搅拌条件下进行。
更优选的,所述修饰液为含酚羟基和胺基化合物的溶液,且浓度为0.005~0.05mol/L。
更优选的,所述修饰液为含酚羟基化合物与含胺基化合物的混合物溶液,所述含酚羟基化合物的浓度为0.005~0.05mol/L。
更进一步优选的,所述含酚羟基化合物与含胺基化合物的摩尔浓度比为1:4~4:1,更优选为1:1。
更优选的,上述任一项所述的导电液晶聚芳酯纤维的制备方法,所述含酚羟基和胺基化合物包括多巴胺、多巴胺盐酸盐、多巴和酪氨酸中的一种以上;
和/或,所述含酚羟基化合物包括单宁酸、没食子酸或邻苯二酚;和/或,所述含胺基化合物包括长链烷烃多胺类化合物或多乙烯基多胺化合物。
更进一步优选的,所述的长链烷烃多胺类化合物包括丁二胺和己二胺中的一种以上,所述的多乙烯基多胺化合物包括乙二胺、二乙烯三胺、三乙烯四胺和四乙烯五胺中的一种以上。
更优选的,所述PH值采用缓冲溶液调节;所述缓冲溶液包括磷酸盐缓冲液PBS、Tris-盐酸缓冲液或TAPS缓冲液。
更优选的,所述表面修饰的反应在pH=8.5的条件下进行。
优选的,S4中,所述活化液为金属盐活化液,且所述活化为采用所述还原剂在纤维表面络合金属离子;所述金属盐活化液的浓度为0.001~0.005mol/L;所述活化的络合温度为30~50℃,时间为5~30min。
更优选的,所述金属盐活化液的金属盐包括硝酸银、氯化钯或四氯合钯(II)酸;和/或,所述还原剂包括次氯酸钠、柠檬酸钠和二甲胺基甲硼烷(DMAB)中的一种以上,所述还原剂可将所述金属盐活化液中的金属盐离子还原附着于纤维表面。
更优选的,所述还原剂的浓度为0.01~0.05mol/L。
优选的,S5中,所述镀液为化学镀金属盐溶液;所述化学镀为利用还原剂将所述化学镀金属盐溶液中的化学镀金属盐离子还原沉积在纤维表面,所述化学镀金属盐离子为导电性金属的盐离子。
更优选的,所述化学镀金属盐离子包括金属镍离子或铜离子,具体的,利用还原反应,在LCP纤维表面将金属镍离子或铜离子还原沉积以进行镀镍或镀铜。
一种导电液晶聚芳酯纤维,按照任一项所述的制备方法制备获得。
与现有技术相比,本发明具有如下优点和有益效果:
本发明采用先物理刻蚀后化学修饰的化学镀前处理工艺,其中以含酚羟基及胺基化合修饰处理纤维表面,修饰改性纤维表面,使纤维表面附着活性基团,解决了物理刻蚀不能在聚芳酯纤维表面形成活性基团的难题,将大大提高金属镀层与纤维基材的结合力,提升纤维的导电率。
另外,化合物修饰后其酚羟基及胺基能与金属离子进行络合,经活化直接利用还原剂将金属离子原位还原在纤维表面形成催化中心,以替代传统化学镀工艺中使用的敏化工艺,再通过化学镀工艺在LCP纤维表面化学镀镍或铜,制备镀层沉积均匀且结合稳定性高的导电LCP复合纤维,生产效率高。且采用的表面处理溶液经济环保,使该制备方法具有广泛适用性,适用于其他惰性材料表面的化学镀工艺。
本发明的导电液晶聚芳酯纤维采用上述的制备方法制备获得,其中金属镀层与纤维表面的结合稳定性好、镀层沉积均匀,整体导电液晶聚芳酯纤维具有良好的导电性能。
附图说明
图1为未经KOH/2-羟基乙胺蚀刻液处理以及经KOH/2-羟基乙胺蚀刻液处理10分钟、30分钟后的纤维FTIR图。
具体实施方式
以下结合具体实施例对本发明的技术方案作进一步详细的描述,但本发明的保护范围及实施方式不限于此。本发明可以以许多不同的形式来实现,并不限于本文所描述的实施例。相反地,提供这些实施例的目的是使对本发明的公开内容的理解更加透彻全面。
并且,除非另有定义,本文所使用的所有的技术和科学术语与属于本发明的技术领域的技术人员通常理解的含义相同。本文中在本发明的说明书中所使用的术语只是为了描述具体的实施例的目的,不是旨在于限制本发明。
本文所使用的术语“和/或”包括一个或多个相关的所列项目的任意的和所有的组合。
应该理解,在本发明中使用的单数形式,如“一种”,包括复数指代,除非另有规定。此外,术语“包括”、“含有”、“具有”是开放性限定并非封闭式,即包括本发明所指明的内容,但并不排除其他方面的内容。换言之,所述术语也包括“基本上由…构成”、或“由…构成”。另外,说明书中的“及其组合”指的是列举的所有项目的任意组合形式。
在本说明书中,可由本领域技术人员选择基团及其取代基以提供稳定的结构部分和化合物。当通过从左向右书写的常规化学式描述取代基时,该取代基也同样包括从右向左书写结构式时所得到的在化学上等同的取代基。
本说明书所用的章节标题仅用于组织文章的目的,而不应被解释为对所述主题的限制。本申请中引用的所有文献或文献部分包括但不限于专利、专利申请、文章、书籍、操作手册和论文,均通过引用方式整体并入本文。
除非另有规定,本文使用的所有技术术语和科学术语具有要求保护主题所属领域的标准含义。倘若对于某术语存在多个定义,则以本文定义为准。
除非另有说明,本发明采用质谱、元素分析的传统方法,如傅氏转换红外线光谱(FTIR)分析,各步骤和条件可参照本领域常规的操作步骤和条件。
除非另有指明,本发明采用分析化学、有机合成化学和光学的标准命名及标准实验室步骤和技术。在某些情况下,标准技术被用于化学合成、化学分析。
本发明的化合物可以在一个或多个构成该化合物的原子上包含非天然比例的原子同位素。例如,可用放射性同位素标记化合物,比如氘(2H)。本发明的化合物的所有同位素组成的变换,无论放射性与否,都包括在本发明的范围之内。
在不违背本领域常识的基础上,上述各优选条件,可任意组合,即得本发明各较佳实例。
以下实施例中,采用的聚芳酯纤维原料来源为:市售的纤维长丝束。
实施例1
本实施例的导电液晶聚芳酯纤维为镀铜导电液晶聚芳酯纤维,具体制备步骤如下:
(1)将聚芳酯纤维布放入丙酮溶液中,在常温条件下浸泡12小时,使用无水乙醇和去离子水反复清洗干净,然后在60℃下干燥2小时,待用;
(2)配制浓度为9mol/L的KOH和浓度为4mol/L的2-羟基乙胺混合溶液200ml,取50ml混合溶液于培养皿中,将步骤(1)清洗干燥后的聚芳酯纤维浸泡于培养皿中,浸泡30分钟后,取出,去离子水清洗并在60℃下干燥;
(3)配制浓度为0.01mol/L的多巴胺盐酸盐溶液500ml,采用Tris-HCl缓冲液调节PH值至8.5;取300ml溶液置于特制的烧杯中,烧杯中间布置有丝网,将步骤(2)刻蚀的聚芳酯纤维浸泡于烧杯中的丝网下面,以300转/分的搅拌速度机械搅拌24小时,搅拌温度为室温;搅拌结束后取出,用去离子水清洗,并在40℃下干燥;
(4)配制浓度为0.001mol/L的PdCl2溶液100ml,将步骤(2)清洗干燥后的聚芳酯纤维浸泡于其中络合10分钟,络合温度40℃;之后加入浓度为0.05mol/L的柠檬酸钠还原10分钟,还原温度40℃;
(5)配制质量分数为10g/L的5水硫酸铜、质量分数为40g/L的酒石酸钾钠四水合物、质量分数为4g/L的六水合氯化镍、质量分数5g/L的二甲胺基甲硼烷(DMAB)化学镀液300ml,调节镀液PH值为8.0;将步骤(4)活化后的聚芳酯纤维置于镀液中,50℃下搅拌20分钟;取出,去离子水清洗,干燥,得到镀铜导电液晶聚芳酯纤维。
采用数字式万用表测试上述制得的镀铜导电聚芳酯纤维的线电阻值为2.5Ω/cm。
实施例2
本实施例的导电液晶聚芳酯纤维为镀镍导电液晶聚芳酯纤维,具体制备步骤如下:
(1)将聚芳酯纤维布放入丙酮溶液中,在常温条件下浸泡12小时,使用无水乙醇和去离子水反复清洗干净,然后在60℃下干燥2小时,待用;
(2)配制浓度为9mol/L的KOH和浓度为4mol/L的2-羟基乙胺混合溶液200ml,取50ml混合溶液于培养皿中,将步骤(1)清洗干燥后的聚芳酯纤维浸泡于培养皿中,浸泡10分钟后,取出,去离子水清洗并在60℃下干燥;
请参阅图1所示,采用KOH/2-羟基乙胺混合溶液对LCP纤维进行10分钟修饰处理后,通过FTIR检测分析,与未经KOH/2-羟基乙胺蚀刻液处理的LCP纤维相比,发现处理后的LCP纤维的FTIR谱峰变化不大,没有明显的吸湿性基团谱峰出现,表明采用KOH/2-羟基乙胺蚀刻液粗化LCP纤维仅起到表面物理粗糙作用,不能形成极性基团。
(3)配制浓度为0.01mol/L的多巴胺盐酸盐溶液500ml,采用Tris-HCl缓冲液调节PH值至8.5;取300ml溶液置于特制的烧杯中,烧杯中间布置有丝网,将步骤(2)刻蚀的聚芳酯纤维浸泡于烧杯中的丝网下面,以300转/分的搅拌速度机械搅拌24小时,搅拌温度为室温;搅拌结束后取出,用去离子水清洗,并在40℃下干燥;
(4)配制浓度为0.001mol/L的PdCl2溶液100ml,将步骤(2)清洗干燥后的聚芳酯纤维浸泡于其中络合10分钟,络合温度40℃;之后倒入浓度为0.05mol/L的柠檬酸钠还原10分钟,还原温度40℃;
(5)配制质量分数为30g/L的硫酸镍、质量分数为20g/L的柠檬酸钠、质量分数为25g/L的次磷酸钠、质量分数为2mg/L的硫脲混合镀液,调节镀液PH值为7,在80℃下搅拌20分钟;取出,去离子水清洗,干燥,得到镀镍导电液晶聚芳酯纤维。
采用数字式万用表测试上述制得的镀镍导电聚芳酯纤维的线电阻值为11.3Ω/cm。
实施例3
本实施例的导电液晶聚芳酯纤维为镀镍导电液晶聚芳酯纤维,具体制备步骤如下:
(1)将聚芳酯纤维布放入丙酮溶液中,在常温条件下浸泡12小时,使用无水乙醇和去离子水反复清洗干净,然后在60℃下干燥2小时,待用;
(2)配制浓度为9mol/L的KOH和浓度为4mol/L的2-羟基乙胺混合溶液200ml,取50ml混合溶液于培养皿中,将步骤1清洗干燥后的聚芳酯纤维浸泡于培养皿中,浸泡30分钟后,取出去离子水清洗并在60℃下干燥;
请参阅图1所示,采用KOH/2-羟基乙胺混合溶液对LCP纤维进行30分钟修饰处理后,通过FTIR检测分析,与未经KOH/2-羟基乙胺蚀刻液处理的LCP纤维相比,发现处理后的LCP纤维的FTIR谱峰变化不大,没有明显的吸湿性基团谱峰出现,表明采用KOH/2-羟基乙胺蚀刻液粗化LCP纤维仅起到表面物理粗糙作用,不能形成极性基团。
(3)配制浓度为0.01mol/L的多巴胺盐酸盐溶液500ml,采用Tris-HCl缓冲液调节PH值至8.5;取300ml溶液置于特制的烧杯中,烧杯中间布置有丝网,将步骤(2)刻蚀的聚芳酯纤维浸泡于烧杯中的丝网下面,以300转/分的搅拌速度机械搅拌24小时,搅拌温度为室温;搅拌结束后取出,用去离子水清洗,并在40℃下干燥;
(4)配制浓度为0.001mol/L的PdCl2溶液100ml,将步骤2清洗干燥后的聚芳酯纤维浸泡于其中络合10分钟,络合温度40℃;之后倒入浓度为0.05mol/L的柠檬酸钠还原10分钟,还原温度40℃;
(5)配制质量分数为30g/L的硫酸镍、质量分数为20g/L的柠檬酸钠、质量分数为25g/L的次磷酸钠、质量分数为2mg/L的硫脲混合镀液,调节镀液PH值为6~7,在80℃下搅拌10分钟;取出,去离子水清洗,干燥,得到镀镍导电液晶聚芳酯纤维。
采用数字式万用表测试上述制得的镀镍导电聚芳酯纤维的线电阻值为9.8Ω/cm。其中,相对于实施例2的镀镍导电聚芳酯纤维,步骤(2)中采用KOH/2-羟基乙胺混合溶液修饰处理时间相对更长,使相应的纤维粗化越好,化学镀后纤维的相应导电性也越好。
实施例4
本实施例的导电液晶聚芳酯纤维为镀镍导电液晶聚芳酯纤维,具体制备步骤如下:
(1)将聚芳酯纤维布放入丙酮溶液中,在常温条件下浸泡12小时,使用无水乙醇和去离子水反复清洗干净,然后在60℃下干燥2小时,待用;
(2)配制浓度为9mol/L的KOH和浓度为4mol/L的2-羟基乙胺混合溶液200ml,取50ml混合溶液于培养皿中,将步骤(1)清洗干燥后的聚芳酯纤维浸泡于培养皿中,浸泡10分钟后,取出去离子水清洗并在60℃下干燥;
(3)配制浓度为0.006mol/L四乙烯五胺与浓度为0.02mol/L的邻苯二酚混合液500ml,采用Tris-HCl缓冲液调节混合液PH值至8.5;取300ml混合液置于特制的烧杯中,烧杯中间布置有丝网,将步骤(2)刻蚀的聚芳酯纤维浸泡于烧杯中的丝网下面,以300转/分的搅拌速度机械搅拌24小时,搅拌温度为室温;搅拌结束后取出,用去离子水清洗,并在40℃下干燥;
(4)配制浓度为0.001mol/L的PdCl2溶液100ml,将步骤(2)清洗干燥后的聚芳酯纤维浸泡于其中络合10分钟,络合温度40℃;之后倒入浓度为0.05mol/L的柠檬酸钠还原10分钟,还原温度40℃;
(5)配制质量分数为30g/L的硫酸镍、质量分数为20g/L的柠檬酸钠、质量分数为25g/L的次磷酸钠、质量分数为2mg/L的硫脲混合镀液,调节镀液PH值为7,在80℃下搅拌20分钟;取出,去离子水清洗,干燥,得到镀镍导电液晶聚芳酯纤维。
采用数字式万用表测试上述制得的镀镍导电聚芳酯纤维的线电阻值为14.7Ω/cm。
对比例1
本对比例的导电液晶聚芳酯纤维为镀铜导电液晶聚芳酯纤维,具体制备步骤如下:
(1)将聚芳酯纤维布放入丙酮溶液中,在常温条件下浸泡12小时,使用无水乙醇和去离子水反复清洗干净,然后在60℃下干燥2小时,待用;
(2)配制浓度为9mol/L的KOH和浓度为4mol/L的2-羟基乙胺混合溶液200ml,取50ml混合溶液于培养皿中,将步骤(1)清洗干燥后的聚芳酯纤维浸泡于培养皿中,浸泡30分钟后,取出去离子水清洗并在60℃下干燥;
(3)配制浓度为0.001mol/L的PdCl2溶液100ml,将步骤(2)清洗干燥后的聚芳酯纤维浸泡于其中络合10分钟,络合温度40℃;之后倒入浓度为0.05mol/L的柠檬酸钠还原10分钟,还原温度40℃;
(4)配制质量分数为10g/L的5水硫酸铜、质量分数为40g/L的酒石酸钾钠四水合物、质量分数为4g/L的六水合氯化镍、质量分数5g/L为二甲胺基甲硼烷DMAB化学镀液300ml,调节镀液PH值为13;将步骤(4)活化后的聚芳酯纤维置于镀液中,50℃下搅拌20分钟;取出,去离子水清洗,干燥,得到镀铜导电液晶聚芳酯纤维。
采用数字式万用表测试上述制得的镀铜导电聚芳酯纤维的线电阻值为3.8Ω/cm。与实施例1相比,相应的镀铜导电聚芳酯纤维的线电阻值变大,导电性能减弱。
对比例2
本对比例的导电液晶聚芳酯纤维为镀镍导电液晶聚芳酯纤维,具体制备步骤如下:
(1)将聚芳酯纤维布放入丙酮溶液中,在常温条件下浸泡12小时,使用无水乙醇和去离子水反复清洗干净,然后在60℃下干燥2小时,待用;
(2)配制浓度为9mol/L的KOH和浓度为4mol/L的2-羟基乙胺混合溶液200ml,取50ml混合溶液于培养皿中,将步骤(1)清洗干燥后的聚芳酯纤维浸泡于培养皿中,浸泡10分钟后,取出去离子水清洗并在60℃下干燥;
(3)配制质量分数为0.2g/L的PdCl2溶液100ml,将步骤(2)清洗干燥后的聚芳酯纤维浸泡于其中络合10分钟,络合温度40℃;之后倒入质量分数为0.05mol/L的柠檬酸钠还原10分钟,还原温度40℃;
(4)配制质量分数为30g/L的硫酸镍、质量分数为20g/L的柠檬酸钠、质量分数为25g/L的次磷酸钠、质量分数为2mg/L的硫脲混合镀液,调节镀液PH值为7,在80℃下搅拌20分钟;取出,去离子水清洗,干燥,得到镀镍导电液晶聚芳酯纤维。
采用数字式万用表测试上述制得的镀镍导电聚芳酯纤维的线电阻值为15.6Ω/cm。与实施例2相比,相应的镀镍导电聚芳酯纤维的线电阻值变大,导电性能减弱。
对比例3
本对比例的导电液晶聚芳酯纤维为镀镍导电液晶聚芳酯纤维,具体制备步骤如下:
(1)将聚芳酯纤维布放入丙酮溶液中,在常温条件下浸泡12小时,使用无水乙醇和去离子水反复清洗干净,然后在60℃下干燥2小时,待用;
(2)配制浓度为9mol/L的KOH和浓度为4mol/L的2-羟基乙胺混合溶液200ml,取50ml混合溶液于培养皿中,将步骤(1)清洗干燥后的聚芳酯纤维浸泡于培养皿中,浸泡10分钟后,取出,去离子水清洗,并在60℃下干燥;
(3)配制浓度为0.005mol/L四乙烯五胺与浓度为0.01mol/L的邻苯二酚混合液500ml,采用Tris-HCl缓冲液调节混合液PH值至8.5;取300ml混合液置于特制的烧杯中,烧杯中间布置有丝网,将步骤(2)刻蚀的聚芳酯纤维浸泡于烧杯中的丝网下面,以300转/分的搅拌速度机械搅拌24小时,搅拌温度为室温;搅拌结束后取出,用去离子水清洗,并在40℃下干燥;
(4)配制浓度为0.001mol/L的PdCl2溶液100ml,将步骤(2)清洗干燥后的聚芳酯纤维浸泡于其中络合10分钟,络合温度40℃;之后倒入浓度为0.05mol/L的柠檬酸钠还原10分钟,还原温度40℃;
(5)配制质量分数为30g/L的硫酸镍、质量分数为20g/L的柠檬酸钠、质量分数为25g/L的次磷酸钠、质量分数为2mg/L的硫脲混合镀液,调节镀液PH值为7,在80℃下搅拌20分钟;取出,去离子水清洗,干燥,得到镀镍导电液晶聚芳酯纤维。
采用数字式万用表测试上述制得的镀镍导电聚芳酯纤维的线电阻值为16.9Ω/cm。与实施例2相比,相应的镀镍导电聚芳酯纤维的线电阻值变大,导电性能减弱。
以上所述实施例的各技术特征可以进行任意的组合,本说明书为使描述简洁,未对上述实施例中的各个技术特征所有可能的组合都进行描述。然而,只要这些技术特征的组合不存在矛盾,都应当认为是本说明书记载的范围。而且,以上所述实施例仅表达了本发明的几种实施方式,其描述较为具体和详细,但并不能因此而理解为对发明专利范围的限制。
应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。因此,本发明专利的保护范围应以所附权利要求为准。
Claims (4)
1.一种导电液晶聚芳酯纤维的制备方法,其特征在于,包括如下步骤:
S1、将聚芳酯纤维洗涤处理,干燥;
S2、将洗涤处理后的聚芳酯纤维在蚀刻液中刻蚀粗化,取出,清洗、干燥;
S3、将刻蚀粗化后的聚芳酯纤维置于修饰液中进行表面修饰,取出,清洗、干燥;
S4、将经表面修饰后的聚芳酯纤维置于活化液中活化,取出,清洗、干燥;
S5、将活化后的聚芳酯纤维置于镀液中进行化学镀,取出,清洗、干燥,获得导电液晶聚芳酯纤维;
S2中,所述蚀刻液为浓度1~20mol/L金属碱性氢氧化物和浓度1~15mol/L增溶剂的混合溶液;所述刻蚀粗化的时间为5~60分钟;所述金属碱性氢氧化物包括氢氧化钠、氢氧化钾和氢氧化锂中的一种以上;所述增溶剂包括尿素和氨基醇类衍生物中的一种以上,所述氨基醇类衍生物包括2-羟基乙胺和异丙醇胺中的一种以上;
S3中,所述修饰液为含酚羟基与胺基化合物的溶液,所述含酚羟基与胺基化合物的浓度为0.005~0.05mol/L,且能自身氧化聚合反应沉积于纤维表面;或者,所述修饰液为含酚羟基化合物与含胺基化合物的混合物溶液,所述含酚羟基化合物的浓度为0.005~0.05mol/L,所述含酚羟基化合物与含胺基化合物的摩尔浓度比为1:4~4:1,且能通过化学反应生成膜沉积于纤维表面;所述表面修饰的反应在室温、pH值7~10、60~600r/min搅拌条件下进行;
S4中,所述活化液为金属盐活化液,且所述活化为采用还原剂在纤维表面络合金属离子;所述金属盐活化液的浓度为0.001~0.005mol/L;所述活化的络合温度为30~50℃,时间为5~30min。
2.根据权利要求1所述的导电液晶聚芳酯纤维的制备方法,其特征在于,所述含酚羟基和胺基化合物包括多巴胺、多巴胺盐酸盐、多巴和酪氨酸中的一种以上,所述含酚羟基化合物包括单宁酸、没食子酸或邻苯二酚;所述含胺基化合物包括长链烷烃多胺类化合物或多乙烯基多胺化合物,所述的长链烷烃多胺类化合物包括丁二胺和己二胺中的一种以上,所述的多乙烯基多胺化合物包括二乙烯三胺、三乙烯四胺和四乙烯五胺中的一种以上。
3.根据权利要求1所述的导电液晶聚芳酯纤维的制备方法,其特征在于,所述金属盐活化液的金属盐包括硝酸银、氯化钯或四氯合钯(II)酸;所述还原剂包括次氯酸钠、柠檬酸钠和二甲胺基甲硼烷中的一种以上,所述还原剂的浓度为0.01~0.05mol/L。
4.一种导电液晶聚芳酯纤维,其特征在于,按照权利要求1-3任一项所述的制备方法制备获得。
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Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR20100023986A (ko) * | 2008-08-23 | 2010-03-05 | 김동현 | 전도성 섬유상의 금ㆍ은 도금방법 |
CN103221577A (zh) * | 2010-07-23 | 2013-07-24 | 希斯康先进材料股份有限公司 | 导电金属涂覆的纤维及其连续制备方法和使用方法 |
KR20140074708A (ko) * | 2012-12-10 | 2014-06-18 | 도레이케미칼 주식회사 | 투명 전기전도성 필름 및 이의 제조방법 |
KR20160067813A (ko) * | 2016-03-18 | 2016-06-14 | (주)오알켐 | 무전해 동도금법을 이용한 섬유 도금 방법 |
CN105821396A (zh) * | 2016-03-27 | 2016-08-03 | 华南理工大学 | 一种无钯化学镀铜的方法 |
CN106436306A (zh) * | 2016-06-14 | 2017-02-22 | 北京化工大学 | 一种纤维的表面改性方法 |
CN107354752A (zh) * | 2017-06-21 | 2017-11-17 | 北京化工大学 | 一种表面覆银f‑12导电纤维及其制备方法 |
CN110552193A (zh) * | 2018-05-31 | 2019-12-10 | 中国科学院化学研究所 | 一种改性超高分子量聚乙烯纤维、织物及其制备方法和应用 |
CN113956527A (zh) * | 2021-12-07 | 2022-01-21 | 深圳大学 | 一种表面金属化的液晶聚合物及其制备方法 |
-
2022
- 2022-05-26 CN CN202210582115.0A patent/CN114990880B/zh active Active
Patent Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR20100023986A (ko) * | 2008-08-23 | 2010-03-05 | 김동현 | 전도성 섬유상의 금ㆍ은 도금방법 |
CN103221577A (zh) * | 2010-07-23 | 2013-07-24 | 希斯康先进材料股份有限公司 | 导电金属涂覆的纤维及其连续制备方法和使用方法 |
KR20140074708A (ko) * | 2012-12-10 | 2014-06-18 | 도레이케미칼 주식회사 | 투명 전기전도성 필름 및 이의 제조방법 |
KR20160067813A (ko) * | 2016-03-18 | 2016-06-14 | (주)오알켐 | 무전해 동도금법을 이용한 섬유 도금 방법 |
CN105821396A (zh) * | 2016-03-27 | 2016-08-03 | 华南理工大学 | 一种无钯化学镀铜的方法 |
CN106436306A (zh) * | 2016-06-14 | 2017-02-22 | 北京化工大学 | 一种纤维的表面改性方法 |
CN107354752A (zh) * | 2017-06-21 | 2017-11-17 | 北京化工大学 | 一种表面覆银f‑12导电纤维及其制备方法 |
CN110552193A (zh) * | 2018-05-31 | 2019-12-10 | 中国科学院化学研究所 | 一种改性超高分子量聚乙烯纤维、织物及其制备方法和应用 |
CN113956527A (zh) * | 2021-12-07 | 2022-01-21 | 深圳大学 | 一种表面金属化的液晶聚合物及其制备方法 |
Non-Patent Citations (1)
Title |
---|
"热致液晶聚芳酯纤维表面改性及机理研究",刘冰倩,中国优秀硕士学位论文全文数据库工程科技I辑,第01期,第B016-544页;刘冰倩;中国优秀硕士学位论文全文数据库工程科技I辑(第1期);第B016-544页 * |
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