CN115819934A - Light-color heat-generating and heat-accumulating fiber master batch and preparation method thereof - Google Patents
Light-color heat-generating and heat-accumulating fiber master batch and preparation method thereof Download PDFInfo
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- CN115819934A CN115819934A CN202211614981.XA CN202211614981A CN115819934A CN 115819934 A CN115819934 A CN 115819934A CN 202211614981 A CN202211614981 A CN 202211614981A CN 115819934 A CN115819934 A CN 115819934A
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- heat
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- light
- tungsten bronze
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- 239000000835 fiber Substances 0.000 title claims abstract description 63
- 239000004594 Masterbatch (MB) Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims description 16
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 75
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 75
- 239000010937 tungsten Substances 0.000 claims abstract description 75
- 239000000843 powder Substances 0.000 claims abstract description 44
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 43
- 239000000194 fatty acid Substances 0.000 claims abstract description 43
- 229930195729 fatty acid Natural products 0.000 claims abstract description 43
- 150000004665 fatty acids Chemical class 0.000 claims abstract description 39
- 229910000906 Bronze Inorganic materials 0.000 claims abstract description 31
- 239000010974 bronze Substances 0.000 claims abstract description 31
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000000919 ceramic Substances 0.000 claims abstract description 30
- 239000002131 composite material Substances 0.000 claims abstract description 30
- 229920000642 polymer Polymers 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000013329 compounding Methods 0.000 claims abstract description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 46
- 239000010410 layer Substances 0.000 claims description 27
- 238000001354 calcination Methods 0.000 claims description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- 238000002844 melting Methods 0.000 claims description 13
- 230000008018 melting Effects 0.000 claims description 13
- 229910052792 caesium Inorganic materials 0.000 claims description 12
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 claims description 12
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- 239000002243 precursor Substances 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 5
- 239000012792 core layer Substances 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 150000004671 saturated fatty acids Chemical class 0.000 claims description 4
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 4
- 125000004432 carbon atom Chemical group C* 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910052691 Erbium Inorganic materials 0.000 claims description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 2
- 229910052779 Neodymium Inorganic materials 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- 238000005520 cutting process Methods 0.000 claims description 2
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 claims description 2
- 238000001125 extrusion Methods 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 2
- 229910052744 lithium Inorganic materials 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 229910052701 rubidium Inorganic materials 0.000 claims description 2
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 abstract description 53
- 230000000694 effects Effects 0.000 abstract description 46
- 238000005338 heat storage Methods 0.000 abstract description 32
- 239000004744 fabric Substances 0.000 abstract description 9
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 description 22
- 230000020169 heat generation Effects 0.000 description 15
- 239000000463 material Substances 0.000 description 15
- 238000005406 washing Methods 0.000 description 13
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 11
- -1 polyethylene Polymers 0.000 description 11
- VHYFNPMBLIVWCW-UHFFFAOYSA-N 4-Dimethylaminopyridine Chemical compound CN(C)C1=CC=NC=C1 VHYFNPMBLIVWCW-UHFFFAOYSA-N 0.000 description 10
- QOSSAOTZNIDXMA-UHFFFAOYSA-N Dicylcohexylcarbodiimide Chemical compound C1CCCCC1N=C=NC1CCCCC1 QOSSAOTZNIDXMA-UHFFFAOYSA-N 0.000 description 10
- OHUPZDRTZNMIJI-UHFFFAOYSA-N [Cs].[W] Chemical compound [Cs].[W] OHUPZDRTZNMIJI-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 9
- 238000003860 storage Methods 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 8
- 239000013078 crystal Substances 0.000 description 8
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- 239000000377 silicon dioxide Substances 0.000 description 7
- 239000004094 surface-active agent Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- TWJNQYPJQDRXPH-UHFFFAOYSA-N 2-cyanobenzohydrazide Chemical compound NNC(=O)C1=CC=CC=C1C#N TWJNQYPJQDRXPH-UHFFFAOYSA-N 0.000 description 6
- TUNFSRHWOTWDNC-UHFFFAOYSA-N Myristic acid Natural products CCCCCCCCCCCCCC(O)=O TUNFSRHWOTWDNC-UHFFFAOYSA-N 0.000 description 6
- 235000021360 Myristic acid Nutrition 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- WJYAJBDKANFOID-UHFFFAOYSA-N 2-(dodecylamino)propanoic acid Chemical compound CCCCCCCCCCCCNC(C)C(O)=O WJYAJBDKANFOID-UHFFFAOYSA-N 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 229920000139 polyethylene terephthalate Polymers 0.000 description 5
- 239000005020 polyethylene terephthalate Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- WBEHKXQILJKFIN-UHFFFAOYSA-N 2-amino-2-methyltetradecanoic acid Chemical compound CCCCCCCCCCCCC(C)(N)C(O)=O WBEHKXQILJKFIN-UHFFFAOYSA-N 0.000 description 4
- 239000002202 Polyethylene glycol Substances 0.000 description 4
- 125000000217 alkyl group Chemical group 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 4
- 229920001223 polyethylene glycol Polymers 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- 125000005472 straight-chain saturated fatty acid group Chemical group 0.000 description 4
- 238000000967 suction filtration Methods 0.000 description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 4
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 description 4
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 229960003237 betaine Drugs 0.000 description 3
- FJDQFPXHSGXQBY-UHFFFAOYSA-L caesium carbonate Chemical compound [Cs+].[Cs+].[O-]C([O-])=O FJDQFPXHSGXQBY-UHFFFAOYSA-L 0.000 description 3
- 229910000024 caesium carbonate Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000011858 nanopowder Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 238000009987 spinning Methods 0.000 description 3
- 239000002344 surface layer Substances 0.000 description 3
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 3
- YJCJVMMDTBEITC-UHFFFAOYSA-N 10-hydroxycapric acid Chemical compound OCCCCCCCCCC(O)=O YJCJVMMDTBEITC-UHFFFAOYSA-N 0.000 description 2
- 239000005635 Caprylic acid (CAS 124-07-2) Substances 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910000420 cerium oxide Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- FBUKVWPVBMHYJY-UHFFFAOYSA-N nonanoic acid Chemical compound CCCCCCCCC(O)=O FBUKVWPVBMHYJY-UHFFFAOYSA-N 0.000 description 2
- RZJRJXONCZWCBN-UHFFFAOYSA-N octadecane Chemical compound CCCCCCCCCCCCCCCCCC RZJRJXONCZWCBN-UHFFFAOYSA-N 0.000 description 2
- 229960002446 octanoic acid Drugs 0.000 description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- 229910001887 tin oxide Inorganic materials 0.000 description 2
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 2
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- ZWGSXIDHYSLQGT-UHFFFAOYSA-N 3-hydroxypropyl dimethyl phosphate Chemical compound P(=O)(OCCCO)(OC)OC ZWGSXIDHYSLQGT-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 239000005632 Capric acid (CAS 334-48-5) Substances 0.000 description 1
- 235000021314 Palmitic acid Nutrition 0.000 description 1
- 239000005643 Pelargonic acid Substances 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- KOPBYBDAPCDYFK-UHFFFAOYSA-N caesium oxide Chemical compound [O-2].[Cs+].[Cs+] KOPBYBDAPCDYFK-UHFFFAOYSA-N 0.000 description 1
- 229910001942 caesium oxide Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 229910000423 chromium oxide Inorganic materials 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 239000002060 nanoflake Substances 0.000 description 1
- 239000002057 nanoflower Substances 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- 229940038384 octadecane Drugs 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 239000012782 phase change material Substances 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920001230 polyarylate Polymers 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- SKRWFPLZQAAQSU-UHFFFAOYSA-N stibanylidynetin;hydrate Chemical compound O.[Sn].[Sb] SKRWFPLZQAAQSU-UHFFFAOYSA-N 0.000 description 1
- 229940117986 sulfobetaine Drugs 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000005382 thermal cycling Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The application relates to a light-color heat-generating and heat-accumulating fiber master batch, which comprises the following raw materials in parts by weight: 1-50 parts of ceramic composite powder and 50-100 parts of polymer carrier; the ceramic composite powder is prepared by compounding tungsten bronze, mesoporous oxide and fatty acid; the heating and heat storage fiber master batch disclosed by the invention has an excellent heating and heat storage effect, and when the heating and heat storage fiber master batch is used in fibers or fabrics with the heating and heat storage effect, the heating and heat storage stability is good, the fiber color is light, and the heating and heat storage fiber master batch can be used in fabrics with high requirements on color.
Description
Technical Field
The invention relates to the field of C09C1/00, in particular to a light-color heat-emitting and heat-storing fiber master batch and a preparation method thereof.
Background
Inorganic heating materials such as antimony tin oxide, indium tin oxide and tungsten bronze nano materials are widely applied to the field of textile fibers, wherein the tungsten bronze nano materials are functional compounds with oxygen octahedron special structures, have low-temperature superconductivity and strong absorption capacity on near infrared light, have strong absorption effect on infrared bands larger than 1100nm, and have absorption rate as high as 55%. However, the inorganic exothermic material has a problem when applied in the field of chemical fiber: for example, 1, the heat storage and warm keeping effects are not enough; 2. the addition of the inorganic heating material deepens the color of the fiber, and limits the application of the fiber in clothes with higher requirements on color; 3. when the internal functional material is subjected to phase change of solid-liquid conversion, the risk of leakage is easily caused, and the heat storage performance is reduced; 4. intolerance to ultraviolet radiation, etc. It is of practical significance to solve the above problems and widen the application of inorganic heating materials in the chemical fiber field.
CN108950717A discloses a light-absorbing and heat-generating fiber and a spinning process thereof, wherein inorganic heat-generating particles and carbon black particles are used in the technology to improve the light-absorbing and heat-generating functions of the fiber, but the materials are dark in color, the application of the prepared fiber in light-colored clothes is limited, and in addition, the stability of the powder in the fiber is not good; chinese patent CN110067038A uses polyvinyl butyral doped with cesium tungsten bronze as a shell layer to wrap octadecane, and prepares the nano intelligent fiber through electrostatic spinning, although the phase change latent heat of the material is high, the cesium tungsten bronze is irradiated by ultraviolet light for a long time, the heat generation and storage effect of the material is reduced, and the leakage of the internal phase change material can be caused.
Disclosure of Invention
In order to solve the technical problems, the invention firstly provides a light-color heat-generating and heat-storing fiber master batch; the master batch comprises the following raw materials in parts by weight: 1-50 parts of ceramic composite powder and 50-100 parts of polymer carrier; the ceramic composite powder is prepared by compounding tungsten bronze, mesoporous oxide and fatty acid.
Further, the polymer carrier is selected from at least one of polyethylene, polypropylene, polyamide, polyethylene terephthalate, polybutylene terephthalate and polyarylate.
Furthermore, the ceramic composite powder has a three-layer structure, and the core layer has a general formula of M x WO 3 The middle layer of the tungsten bronze is mesoporous oxide, and the outer layer of the tungsten bronze is fatty acid.
Further, the general formula is M x WO 3 The tungsten bronze of (a) is in a nano-scale, and the nano-shape includes, but is not limited to, any one of a nano-fiber shape, a nano-tree shape, a nano-rod shape, a nano-flower shape, a nano-flake shape, a nano-sphere shape, and the like.
Preferably, the tungsten bronze is nano-platelet; preferably, the nano flaky tungsten bronze is 3 to 35nm in width, 15 to 200nm in length and 2 to 25nm in thickness.
Further, the M x WO 3 Wherein M is selected from any one of rare earth metal elements, alkali metals and alkaline earth metal elements, and x is 0.01-0.5.
Further, said M x WO 3 Wherein M is selected from any one of lanthanum, neodymium, erbium, lithium, sodium, potassium, rubidium and cesium.
In a preferred embodiment, M is cesium; the cesium tungsten bronze nano powder has large atomic radius, and the formed cesium tungsten bronze nano powder has more surface defects, so that the cesium tungsten bronze nano powder has strong infrared absorption capacity.
Further, x is 0.1 to 0.33; the doping of M causes more defects in the crystal and on the crystal surface, the content of current carriers is increased, the infrared shielding performance is improved along with the doping, when the doping amount of M is increased, the heating effect of the ceramic composite powder can be improved, but when the doping amount is excessive, a part of M exists in the oxidation state of the M, effective doping is not formed, and the photoinduced heating performance is reduced.
Further, the method adopts the steps of mixing an M source, a tungsten source and tungsten trioxide and then calcining to prepare the compound with the general formula M x WO 3 The tungsten bronze of (1).
Preferably, the general formula is M x WO 3 The preparation method of the tungsten bronze comprises any one of the following methods:
the method comprises the following steps: the ratio of the amount of the substances is 1: uniformly mixing 2-100 parts of M and tungsten (W), and keeping the temperature for 1-10 hours at the calcining temperature of 400-1000 ℃ to obtain tungsten bronze powder;
the second method comprises the following steps: dispersing a tungsten source and tungsten trioxide in a hydrogen peroxide solution to obtain sol, adding an M source accounting for 0.01-0.5 time of the tungsten substance, stirring, and drying to obtain a precursor; grinding the powder, and calcining the powder for 1 to 10 hours at the temperature of between 400 and 1000 ℃ to obtain the tungsten bronze powder.
Furthermore, the calcination temperature of the first method and the second method is 400-850 ℃, and the calcination time is 1.5-8h.
Preferably, the calcining temperature of the first method and the second method is 550-700 ℃, and the calcining time is 1.5-8h; the application finds that: when the calcination temperature is too low, the growth of cesium-doped crystal grains is slow, but when the calcination temperature is too high, the atomic arrangement and the doping of cesium ions are biased to a disordered state, the number of lattice defects and oxygen vacancies is too large, the crystal grain size is increased, the agglomeration phenomenon occurs, the heating effect is reduced, the visible light transmittance of the material is also reduced, and the color of a fiber product prepared from the master batch is deepened.
Further, the thickness of the intermediate layer is less than or equal to 25nm.
Further, the thickness of the intermediate layer is 5-25nm.
Preferably, the thickness of the intermediate layer is 5-10nm.
Further, the mesoporous oxide is selected from at least one of alumina, magnesia, titania, tungsten oxide, chromium oxide, tin oxide, cobalt oxide, iron oxide, indium oxide, cerium oxide, and silicon oxide.
Further, the mesoporous oxide is at least one of cerium oxide, aluminum oxide, silicon oxide and tin oxide.
Preferably, the mesoporous oxide is silicon oxide and aluminum oxide. The application discovers that the mesoporous silica and the mesoporous alumina are coated in a composite mode, heat can be quickly transferred to surface fatty acid after the nano tungsten bronze generates heat, the heating and heat storage efficiency is accelerated, on the other hand, the whiteness of fiber master batches can be improved, and downstream application is widened.
Further, the fatty acid is selected from at least one of linear saturated fatty acid, linear unsaturated fatty acid, branched saturated fatty acid and branched unsaturated fatty acid.
Preferably, the fatty acid is a straight-chain saturated fatty acid, and the number of carbon atoms is 8-18; the present application found that when the fatty acid is a linear saturated fatty acid having 8 to 18 carbon atoms, the heat-absorbing and heat-generating effect of the heat-accumulative base particles is more excellent, presumably because: the-COOH end of the straight-chain saturated fatty acid is grafted on the middle layer, and the long paraffin end is distributed on the outer side of the heating powder, so that the heating powder has hydrophobic and oleophylic properties, and has good dispersibility and compatibility in a polymer carrier; when the molecular chain is too long, the mobility and dispersibility of the material in the polymer carrier are poor, and the heat generation and storage effects are reduced.
Further, the fatty acid includes, but is not limited to, at least one of palmitic acid, stearic acid, caprylic acid, pelargonic acid, capric acid, myristic acid, 15-hydroxydecanoic acid, 10-hydroxydecanoic acid, and the like.
Preferably, the fatty acid is selected from at least one of caprylic acid, n-capric acid, 15-hydroxydecanoic acid.
Preferably, the fatty acid is chemically grafted in the middle layer mesoporesThe thickness of the fatty acid layer on the surface of the oxide is 5-30nm, and the grafting density of the fatty acid is 0.2-0.9g/cm 3 (ii) a The graft density = (weight of post-graft-weight of pre-graft)/surface area of the object.
Further, the thickness of the fatty acid layer is 10-20nm, and the grafting density of the fatty acid is 0.3-0.65g/cm 3 The present application found in the study: when the grafting amount of the fatty acid is too small, the heat-conducting property of the resin is improved, and the heat storage capacity of the material is reduced; when the grafting density of the fatty acid is too high, heat transmission is possibly hindered, so that the heat generation and storage capacity of the material is reduced; the heating and heat storage performance of the heating ceramic powder is improved by controlling the synergistic effect of the fatty acid, the compounded mesoporous oxide and the nano tungsten bronze.
Further, the preparation method of the ceramic heating powder comprises the following steps: (1) preparing tungsten bronze powder; (2) Dispersing a mesoporous oxide source and a surfactant in deionized water, and adjusting the pH of the solution to 7.5-9.2 by using ammonia water to obtain a mixed solution; according to the mesoporous oxide source: the tungsten bronze powder is 0.5-3:1, adding the tungsten bronze powder into the solution in a mass ratio, stirring and reacting for 3-8h, performing suction filtration, washing, drying and crushing to obtain a precursor, heating the precursor to 300-700 ℃, and calcining for 0.5-2h to obtain mesoporous oxide coated tungsten bronze powder; (3) Adding the tungsten bronze powder coated with the fatty acid and the mesoporous oxide into redistilled tetrahydrofuran, stirring for 20-40 minutes, adding N, N' -dicyclohexylcarbodiimide and 4-dimethylaminopyridine under the protection of nitrogen, condensing, refluxing and stirring at 65-80 ℃, reacting for 48-72 hours, filtering, and drying.
Further, in the step (2), the concentration of the mesoporous oxide source in the deionized water is 0.01-0.15mol/L.
Further, the mass ratio of the mesoporous oxide source to the surfactant is 2-14:1; preferably 6 to 10:1.
further, the surfactant is at least one selected from polyethylene glycol, dodecyl aminopropionic acid, alkyl dimethyl betaine (with the number of alkyl groups of 12-16), dodecyl ethoxy sulfobetaine, dodecyl sulfopropyl betaine and alkyl dimethyl hydroxypropyl phosphate betaine (with the number of alkyl groups of 12-16).
In a preferred embodiment, the mesoporous oxide sources are a silicon source and an aluminum source.
In a preferred embodiment, the mass ratio of the silicon source to the aluminum source is 1:5-9.
Further, the silicon source is selected from at least one of sodium silicate, methyl orthosilicate, ethyl orthosilicate, aminopropyl triethoxysilane and methyl trimethoxysilane.
Further, the aluminum source is selected from at least one of aluminum nitrate, aluminum sulfate, sodium metaaluminate and aluminum alkoxide.
Further, the mass of the fatty acid in the step (3) is 30-80% of that of the tungsten bronze powder coated by the mesoporous oxide; preferably 50 to 70%.
Further, the mass of the N, N' -dicyclohexylcarbodiimide is 1-2 times of that of the fatty acid; preferably 1.2 to 1.5 times.
Further, the mass of the 4-dimethylamino pyridine is 0.5-2% of that of the fatty acid.
Further, the preparation method of the heating and heat storage fiber master batch comprises the following steps: mixing the ceramic composite powder and a polymer carrier, putting the mixture into a double-screw extruder with a vacuumizing device, and performing melting, extrusion, cooling, bracing, traction and grain cutting.
Further, the melting temperature is 240-270 ℃, and the master batch size is as follows: 3mm plus or minus 1mm in length and 2.5mm plus or minus 1.5mm in diameter.
Furthermore, the master batch is used in the fiber or the fabric with the heating and heat storage functions.
Advantageous effects
1. The heating and heat storage fiber master batch disclosed by the invention has excellent heating and heat storage effects, and when the heating and heat storage fiber master batch is used in fibers or fabrics with the heating and heat storage effects, the heating and heat storage stability is good, and the heating and heat storage effects of the latter are still good after the latter are washed for many times.
2. According to the invention, the inorganic heating material nano tungsten bronze and the mesoporous oxide are combined, so that the color of the prepared heating heat storage fiber master batch and the color of the fiber thereof are lightened, and the fiber can be used in a use scene with higher color requirement; meanwhile, the nano tungsten bronze has excellent ultraviolet light stability, and the heating effect of the prepared heating heat storage fiber master batch is further stabilized.
3. The surface layer of the fiber is straight-chain saturated fatty acid, so that the fiber has a good heat storage effect, gives the heating and heat storage fiber master batch good hydrophobic and oleophilic properties, and increases the dispersibility of the fiber master batch in an organic system and the compatibility of the fiber master batch with the fiber.
4. The straight-chain saturated fatty acid is grafted on the middle layer through chemical action, so that the exudation phenomenon during phase change is avoided, the powder loss caused by washing can be effectively avoided, the heating ceramic powder has proper phase change temperature by limiting the length of a molecular chain, and the processed fiber has excellent comfort to human bodies.
Detailed Description
Examples
Example 1
The embodiment provides a light-color heat-generating and heat-storing fiber master batch, which comprises the following raw materials, by weight, 25 parts of ceramic composite powder and 75 parts of polyethylene terephthalate;
the preparation method of the ceramic composite powder comprises the following steps: (1) Mixing an alkali metal source (cesium carbonate), a tungsten source (tungstic acid) and tungsten trioxide, and calcining for 4.5 hours in vacuum at the temperature of 650 ℃, wherein the tungstic acid is used for obtaining tungsten bronze powder (the mass ratio of cesium to tungsten is 1; (2) Ethyl orthosilicate, aluminum nitrate and dodecyl amino propionic acid were mixed according to a ratio of 1:7:1 in deionized water (wherein, the ratio of the mesoporous oxide source to the dodecylaminopropionic acid is 8; according to the mesoporous oxide source: the tungsten bronze powder is 1.5:1, adding the tungsten bronze powder into the solution in a mass ratio of 5 hours, stirring and reacting for 5 hours, carrying out suction filtration, washing, drying and crushing to obtain a precursor, heating the precursor to 500 ℃ at a heating rate of 5 ℃/min, and calcining for 0.5 hour to obtain mesoporous oxide coated tungsten bronze powder; (3) Adding N-decanoic acid and mesoporous oxide coated tungsten bronze powder into redistilled tetrahydrofuran, stirring for 30 minutes, adding N, N' -dicyclohexylcarbodiimide (the mass of which is 1.4 times of that of myristic acid) and 4-dimethylaminopyridine (the mass of which is 1.2 percent of that of myristic acid) under the protection of nitrogen, condensing, refluxing and stirring for 48 hours at 75 ℃, and filtering and drying after the reaction is finished; wherein the mass of the n-decanoic acid is 60% of that of the mesoporous oxide coated cesium tungsten bronze powder.
The preparation method of the master batch comprises the following steps: placing the ceramic composite powder and polyethylene glycol terephthalate in a double-screw extruder with a vacuumizing device, and extruding, cooling, drawing strips, and granulating after melting; wherein the melting temperature is 250 ℃, and the master batch size is as follows: 3mm in length and 2.5mm in diameter.
Example 2
The embodiment provides a light-color heat-generating and heat-storing fiber master batch, which comprises the following raw materials, by weight, 10 parts of ceramic composite powder and 90 parts of polyethylene terephthalate;
the preparation method of the ceramic composite powder comprises the following steps: (1) Grinding and uniformly mixing cesium carbonate, tungstic acid and tungsten trioxide, and calcining at 400 ℃ for 8h to obtain tungsten bronze powder (the mass ratio of cesium to tungsten is 1; (2) Ethyl orthosilicate, aluminum nitrate and dodecyl amino propionic acid were mixed according to a ratio of 1:5:1 in deionized water (wherein, the ratio of the mesoporous oxide to the dodecylaminopropionic acid is 6; according to the mesoporous oxide source: the tungsten bronze powder is 0.5:1, adding the tungsten bronze powder into the solution in a mass ratio of 1, stirring and reacting for 8 hours, performing suction filtration, washing, drying and crushing to obtain a precursor, heating the precursor to 300 ℃ at a heating rate of 10 ℃/min, and calcining for 1 hour to obtain mesoporous oxide coated tungsten bronze powder; (3) Adding tungsten bronze powder coated with N-decanoic acid and mesoporous oxide into redistilled tetrahydrofuran, stirring for 40 minutes, adding N, N' -dicyclohexylcarbodiimide (the mass is 1.2 times of the mass of myristic acid) and 4-dimethylaminopyridine (the mass is 0.5 percent of the mass of myristic acid) under the protection of nitrogen, condensing, refluxing and stirring for 72 hours at 65 ℃, and filtering and drying after the completion; wherein the mass of the n-decanoic acid is 50% of that of the mesoporous oxide coated cesium tungsten bronze powder.
The preparation method of the master batch comprises the following steps: placing the ceramic composite powder and polyethylene glycol terephthalate in a double-screw extruder with a vacuumizing device, melting, extruding, cooling, drawing strips, and granulating; wherein the melting temperature is 240 ℃, and the master batch size is as follows: 4mm in length and 4mm in diameter.
Example 3
The embodiment provides a light-color heat-generating and heat-storing fiber master batch, which comprises the following raw materials, by weight, 40 parts of ceramic composite powder and 60 parts of polyethylene terephthalate;
the preparation method of the ceramic composite powder comprises the following steps: (1) Grinding and uniformly mixing cesium carbonate, tungstic acid and tungsten trioxide, and calcining at 850 ℃ for 2h to obtain tungsten bronze powder (the mass ratio of cesium to tungsten is 1; (2) Ethyl orthosilicate, aluminum nitrate and dodecyl amino propionic acid were mixed according to a ratio of 1:9:1 in deionized water (wherein, the ratio of the mesoporous oxide to the dodecylaminopropionic acid is 10; according to mesoporous oxide sources: the tungsten bronze powder is 3:1, adding the tungsten bronze powder into the solution, stirring and reacting for 3 hours, carrying out suction filtration, washing, drying and crushing to obtain a precursor, heating the precursor to 700 ℃ at the heating rate of 5 ℃/min, and calcining for 0.5 hour to obtain the mesoporous oxide coated tungsten bronze powder. (3) Adding tungsten bronze powder coated with N-decanoic acid and mesoporous oxide into redistilled tetrahydrofuran, stirring for 30 minutes, adding N, N' -dicyclohexylcarbodiimide (the mass is 1.5 times of the mass of myristic acid) and 4-dimethylaminopyridine (the mass is 2 percent of the mass of myristic acid) under the protection of nitrogen, condensing, refluxing and stirring for 48 hours at 75 ℃, filtering and drying after the reaction is finished; wherein the mass of the n-decanoic acid is 70% of that of the mesoporous oxide coated cesium tungsten bronze powder.
The preparation method of the master batch comprises the following steps: placing the ceramic composite powder and polyethylene glycol terephthalate in a double-screw extruder with a vacuumizing device, and extruding, cooling, drawing strips, and granulating after melting; wherein the melting temperature is 270 ℃, and the master batch size is as follows: 2mm in length and 1mm in diameter.
Example 4
Essentially in accordance with example 1, with the difference that: the mass ratio of cesium to tungsten is 1.
Example 5
Essentially in accordance with example 1, with the difference that: the ratio of ethyl orthosilicate to aluminum nitrate in the step (2) is 1.
Example 6
Essentially in accordance with example 1, except that the ratio of ethyl orthosilicate to aluminum nitrate in step (2) was 1.
Example 7
Essentially in accordance with example 1, with the difference that: the ratio of mesoporous oxide source to dodecylaminopropionic acid in step (2) is 4.
Example 8
Essentially in accordance with example 1, with the difference that: the ratio of mesoporous oxide source to dodecylaminopropionic acid in step (2) is 14.
Example 9
Essentially in accordance with example 1, with the difference that: and the stirring reaction time in the step (2) is 10h.
Example 10
Essentially in accordance with example 1, with the difference that: the concentration of the mesoporous oxide source in the step (2) is 0.25mol/L.
Example 11
Essentially in accordance with example 1, with the difference that: the calcination temperature in the step (2) is 900 ℃.
Example 12
Essentially in accordance with example 1, with the difference that: essentially in accordance with example 1, with the difference that: the calcination temperature in the step (1) is 950 ℃.
Example 13
Essentially in accordance with example 1, with the difference that: in the step (3), the mass of the n-decanoic acid is 80% of that of the mesoporous oxide coated cesium tungsten bronze powder.
Example 14
Essentially in accordance with example 1, with the difference that: only ethyl orthosilicate is added in the process of coating the tungsten bronze powder by the mesoporous oxide in the step (2), and aluminum nitrate is not added.
Example 15
Essentially in accordance with example 1, with the difference that: only aluminum nitrate is added in the process of coating the tungsten bronze powder with the mesoporous oxide obtained in the step (2), and tetraethoxysilane is not added.
Example 16
Essentially in accordance with example 1, with the difference that: adjusting the mass ratio of the mesoporous oxide source to the tungsten bronze powder in the step (2) to be 0.2:1.
example 17
Essentially in accordance with example 1, with the difference that: adjusting the mass ratio of the mesoporous oxide source to the tungsten bronze powder in the step (2) to be 4:1.
comparative example 1
Essentially in accordance with example 1, with the difference that: in the preparation method of the master batch, the melting temperature is 300 ℃.
Comparative example 2
Essentially in accordance with example 1, with the difference that: the ceramic composite powder used in the master batch of the comparative example is the mesoporous oxide coated tungsten bronze powder prepared in the step (2).
Comparative example 3
Essentially in accordance with example 1, with the difference that: the step (3) is as follows: mixing and stirring the n-decanoic acid and the mesoporous oxide coated tungsten bronze powder uniformly, and drying; wherein the mass of the n-decanoic acid is 60% of that of the mesoporous oxide coated cesium tungsten bronze powder.
The performance test method comprises the following steps:
according to the following steps of 1:9, respectively mixing the master batches and PET in the examples and the comparative examples, then carrying out melt blending and spinning, carrying out traction winding to prepare heating fibers, wherein the melting temperature is 220 ℃, the spinning speed is 2700m/min, processing to prepare 83dtex/72F fibers and corresponding fabrics, and carrying out the following tests;
(1) Fiber color: the Lab value of the fiber was measured using a Sanyne TS8210 spectrocolorimeter, and the larger the L value, the lighter the color of the fiber, 5 samples were taken from each example, and the average value was shown in Table 1.
(2) And (3) testing the heating effect: adopting an indoor far infrared lamp for testing, wherein the testing conditions are as follows: a 150W infrared light source with the receiving distance of about 45cm, an infrared thermosensitive thermometer is used for detecting the surface temperature of the sample after illumination for 10 minutes, and the surface temperature difference before and after the illumination is recorded, namely the temperature difference before washing;
(3) Wash durability test: the fabrics of examples and comparative examples were washed according to the method specified in AATCC 135, dried at 60 ℃ after 100 times of washing, and the heating effect of the fabrics after washing was measured according to the method of (2) heating effect test to obtain the temperature difference after washing.
And (3) performance test results:
TABLE 1
Analyzing the data, the following data are obtained:
the heat-generating and heat-storing tungsten bronze composite powder prepared in the embodiments 1 to 3 has a high L value, good stability and good heat-generating and heat-storing effects, wherein the temperature difference before washing of the fabric prepared in the embodiment 2 is relatively small due to a little powder content and a small grafting amount of the organic heat storage body on the surface layer in the embodiment 2; in example 3, the whiteness is reduced due to the large amount of the added powder, and the temperature difference is slightly lower than that in example 1, which is probably because the heat generation and storage capacity reaches the peak value after the content of the powder reaches a certain content, and the heat generation effect of the tungsten bronze is slightly influenced by the large amount of the fatty acid coated on the outer layer in example 3.
It is understood from the comparison between examples 1 and 4 that the amount of doped cesium affects the infrared absorption of the composite powder by affecting the crystal structure and surface roughness of the tungsten bronze powder, and when the amount of cesium is too large, part of cesium exists in the form of cesium oxide, resulting in a decrease in the infrared absorption capability.
Comparing example 1 with examples 5 to 6, it is known that when the amount of tetraethoxysilane in the mesoporous oxide source is too large, the heat generation and heat storage effects are correspondingly reduced, wherein the amount of hydroxyl groups of the mesoporous silica is greater than that of the mesoporous alumina, so it is presumed that the heat generation effect is reduced because the content of the mesoporous silica is increased to increase the number of hydroxyl chains, and further, the fatty acid graft layer is too thick, but the thicker fatty acid graft layer is beneficial to the uniform dispersion of the ceramic composite powder in the polymer system, and the heat generation and heat storage effects of the fabric are reduced less after multiple washing; when the consumption of the tetraethoxysilane is too low, the content of the coated mesoporous silica is low, so that the grafting of the fatty acid is reduced, the heating and heat storage effects of the ceramic composite powder are influenced, and the dispersibility of the ceramic composite powder in a polymer system is relatively poor due to the thin fatty acid grafting layer, so that the heating and heat storage effects are reduced more after the ceramic composite powder is washed for many times.
Comparing example 1 with examples 7-8, it is clear that the surfactant also has a significant effect on the exothermic effect of the product, for the following reasons: the existence of the surfactant can improve the dispersion of the mesoporous oxide source in water, and further influence the grafting of surface fatty acid by influencing the structure of the mesoporous oxide. When the surfactant amount is too large, the particle size of colloidal particles in water is too small, so that partial tungsten bronze is possibly incompletely coated or the coating degree is not enough, the surface grafting effect and the material stability are influenced, and the heat storage effect of the material is further influenced; when the content of the surfactant is not sufficient, the mesoporous oxide inside may agglomerate, and the particle size and distribution of the calcined crystal are not uniform, which may affect not only the heating effect of the tungsten bronze powder, but also the grafting and stability of the organic heat accumulator on the surface layer.
It is known from the comparison between example 1 and examples 9 to 10 that when the reaction time is too long or the total concentration of the mesoporous silica and the mesoporous alumina is too high, the thickness of the mesoporous oxide layer is too thick, and although the whiteness is increased, the heat conduction effect is affected, and the light absorption effect of the tungsten bronze powder is also affected, so that the heating effect of the prepared fiber is reduced.
It is understood from comparison between example 1 and example 11 that when the calcination temperature of the mesoporous oxide is too high, the heat generation effect of the base particles and the fibers thereof is reduced, and it is presumed that the too high temperature causes collapse or deformation of the mesoporous structure of the mesoporous oxide, which affects not only the whiteness, but also the absorption of the light by the tungsten bronze powder of the core layer, and also the grafting of the surface fatty acid, thereby comprehensively affecting the heat generation effect of the base particles and the fibers thereof.
It is understood from comparative example 1 and example 12 that the increase in the calcination temperature of the tungsten bronze powder not only reduces the heat generation effect of the master batch and the fiber thereof, but also significantly deepens the color of the fiber, presumably because when the temperature is too high, both the doping of cesium and the crystal growth are disordered, and the crystal grain size becomes large, resulting in the occurrence of agglomeration.
It is understood from the comparison between example 1 and example 13 that when the grafting amount of the fatty acid is too high, the absorption capability of the core layer to light is affected, the heat generation and storage effect of the master batch is weakened, and the surface hydroxyl groups of the mesoporous oxide are limited, and part of the fatty acid does not form a grafted ester bond, which results in loss after thermal cycling and reduced thermal stability.
Comparing example 1 with examples 14 to 15, it is known that when the mesoporous oxide source is only ethyl orthosilicate, the amount of hydroxyl groups of mesoporous silica is greater than that of mesoporous alumina, and thus the heat generation and storage effects may be reduced accordingly, and it is presumed that the increased content of mesoporous silica increases the number of hydroxyl chains, which in turn causes the fatty acid graft layer to be too thick, and finally the heat generation effect is reduced; when the mesoporous oxide source is only aluminum nitrate, the total amount of hydroxyl chains is reduced, so that the grafting of fatty acid is reduced, and the heating and heat storage effects of the mesoporous oxide source are influenced.
It is understood from comparison between example 1 and examples 16 to 17 that the heat generation and storage effect is affected when the amount of the mesoporous oxide used for coating tungsten bronze is too large or too small. When the mesoporous oxide used for coating the tungsten bronze is too much, the number of hydroxyl chains is increased after the mesoporous oxide layer is too much, so that the fatty acid grafting layer is too thick, the light absorption heating effect of the tungsten bronze inside is influenced, and the heating effect is reduced finally; when the amount of the mesoporous oxide is too small, the whiteness is reduced, and the total amount of hydroxyl chains is reduced, so that the grafting of fatty acid is reduced, the compatibility of the ceramic composite powder and a resin matrix is affected, the ceramic composite powder is easy to run off in the washing process, and the heating and heat storage effects after washing are affected.
Comparative example 1 and comparative example 1 demonstrate that an appropriate melting temperature can improve the dispersibility of the heat-generating powder in the polymer carrier and improve the heat-generating effect, but an excessively high temperature can destroy the structure of the organic heat storage layer, resulting in a reduction in the heat-generating effect.
It can be seen from comparison of example 1 and comparative examples 2 to 3 that the organic thermal storage layer can effectively improve the heating capacity of the fiber, and the grafting of the organic thermal storage layer can greatly affect the stability and durability of the heating performance of the fiber masterbatch.
Claims (10)
1. The light-color heat-generating and heat-accumulating fiber master batch is characterized by comprising the following raw materials in parts by weight: 1-50 parts of ceramic composite powder and 50-100 parts of polymer carrier; the ceramic composite powder is prepared by compounding tungsten bronze, mesoporous oxide and fatty acid.
2. The light-colored heat-generating and heat-storing fiber master batch as claimed in claim 1, wherein the ceramic composite powder has a three-layer structure, and the core layer has a general formula M x WO 3 The middle layer of the tungsten bronze is mesoporous oxide, and the outer layer of the tungsten bronze is fatty acid.
3. The light-colored heat-emitting and heat-storing fiber master batch as claimed in claim 2, wherein the general formula is M x WO 3 In the tungsten bronze, M is selected from any one of lanthanum, neodymium, erbium, lithium, sodium, potassium, rubidium and cesium, and x is 0.01-0.5.
4. The light-colored heat-generating and heat-accumulating fiber master batch of claim 2, wherein the general formula is M x WO 3 The preparation method of the tungsten bronze comprises any one of the following methods:
the method comprises the following steps: the ratio of the amount of the substances is 1: mixing 2-100 of M and tungsten uniformly, and then keeping the temperature for 1-10h at the calcining temperature of 400-1000 ℃ to obtain tungsten bronze powder;
the second method comprises the following steps: dispersing a tungsten source and tungsten trioxide in a hydrogen peroxide solution to obtain sol, adding an M source accounting for 0.01-0.5 time of the tungsten substance, stirring, and drying to obtain a precursor;
grinding the powder, and calcining the powder for 1 to 10 hours at the temperature of between 400 and 1000 ℃ to obtain the tungsten bronze powder.
5. The light-colored heat-emitting and heat-storing fiber master batch according to claim 1, wherein the thickness of the intermediate layer is less than or equal to 25nm.
6. The light-colored heat-emitting and heat-storing fiber master batch according to claim 1, wherein the mesoporous oxide is silicon oxide and aluminum oxide.
7. The light-colored heat-emitting and heat-storing fiber master batch according to claim 1, wherein the fatty acid is a linear saturated fatty acid.
8. The light-colored heat-emitting and heat-storing fiber master batch according to claim 7, wherein the fatty acid has 8 to 18 carbon atoms.
9. The light-colored heat-emitting and heat-storing fiber master batch according to claim 8, wherein the mass of the fatty acid is 30-80% of that of the tungsten bronze powder coated with the mesoporous oxide.
10. The preparation method of the light-colored heat-emitting and heat-storing fiber master batch according to any one of claims 1 to 9, wherein the preparation method comprises the following steps: mixing the ceramic composite powder and a polymer carrier, putting the mixture into a double-screw extruder with a vacuumizing device, and performing melting, extrusion, cooling, bracing, traction and grain cutting; wherein the melting temperature is 240-270 ℃.
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| CN117364286A (en) * | 2023-12-07 | 2024-01-09 | 天津包钢稀土研究院有限责任公司 | Rare earth-based light-absorbing heat-insulating hollow fiber and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117364286A (en) * | 2023-12-07 | 2024-01-09 | 天津包钢稀土研究院有限责任公司 | Rare earth-based light-absorbing heat-insulating hollow fiber and preparation method and application thereof |
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