CN108486861A - A kind of preparation process of anti-ultraviolet ageing pbo fiber - Google Patents
A kind of preparation process of anti-ultraviolet ageing pbo fiber Download PDFInfo
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- CN108486861A CN108486861A CN201810378821.7A CN201810378821A CN108486861A CN 108486861 A CN108486861 A CN 108486861A CN 201810378821 A CN201810378821 A CN 201810378821A CN 108486861 A CN108486861 A CN 108486861A
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- Prior art keywords
- pbo fiber
- preparation process
- acid
- ultraviolet ageing
- pbo
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- 239000000835 fiber Substances 0.000 title claims abstract description 122
- 230000032683 aging Effects 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 46
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 84
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 59
- 239000010439 graphite Substances 0.000 claims abstract description 59
- 238000005530 etching Methods 0.000 claims abstract description 49
- 239000002253 acid Substances 0.000 claims abstract description 39
- 239000012298 atmosphere Substances 0.000 claims abstract description 34
- 239000004411 aluminium Substances 0.000 claims abstract description 33
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 33
- 239000007788 liquid Substances 0.000 claims abstract description 32
- 230000004048 modification Effects 0.000 claims abstract description 29
- 238000012986 modification Methods 0.000 claims abstract description 29
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 239000000725 suspension Substances 0.000 claims abstract description 20
- 208000037656 Respiratory Sounds Diseases 0.000 claims abstract description 19
- 230000001681 protective effect Effects 0.000 claims abstract description 16
- 239000012670 alkaline solution Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- 238000005470 impregnation Methods 0.000 claims description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 16
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 229920000137 polyphosphoric acid Polymers 0.000 claims description 14
- 239000011353 cycloaliphatic epoxy resin Substances 0.000 claims description 13
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 12
- QPJVMBTYPHYUOC-UHFFFAOYSA-N methyl benzoate Chemical compound COC(=O)C1=CC=CC=C1 QPJVMBTYPHYUOC-UHFFFAOYSA-N 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- 238000002604 ultrasonography Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 239000002699 waste material Substances 0.000 claims description 11
- -1 glycolic Chemical compound 0.000 claims description 10
- 238000007654 immersion Methods 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical group OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 9
- 229960001484 edetic acid Drugs 0.000 claims description 9
- 239000012535 impurity Substances 0.000 claims description 9
- FKRCODPIKNYEAC-UHFFFAOYSA-N ethyl propionate Chemical compound CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 claims description 8
- CRZQGDNQQAALAY-UHFFFAOYSA-N Methyl benzeneacetate Chemical compound COC(=O)CC1=CC=CC=C1 CRZQGDNQQAALAY-UHFFFAOYSA-N 0.000 claims description 7
- 230000007935 neutral effect Effects 0.000 claims description 7
- 239000003960 organic solvent Substances 0.000 claims description 7
- 230000001590 oxidative effect Effects 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 6
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 6
- 239000012964 benzotriazole Substances 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 6
- 229940095102 methyl benzoate Drugs 0.000 claims description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 4
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 4
- 238000005660 chlorination reaction Methods 0.000 claims description 4
- 239000007800 oxidant agent Substances 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- KBIWNQVZKHSHTI-UHFFFAOYSA-N 4-n,4-n-dimethylbenzene-1,4-diamine;oxalic acid Chemical compound OC(=O)C(O)=O.CN(C)C1=CC=C(N)C=C1 KBIWNQVZKHSHTI-UHFFFAOYSA-N 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Natural products OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 3
- 239000000908 ammonium hydroxide Substances 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 3
- 239000012286 potassium permanganate Substances 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- YEYCMBWKTZNPDH-UHFFFAOYSA-N (2,2,6,6-tetramethylpiperidin-4-yl) benzoate Chemical compound C1C(C)(C)NC(C)(C)CC1OC(=O)C1=CC=CC=C1 YEYCMBWKTZNPDH-UHFFFAOYSA-N 0.000 claims description 2
- KDYYFNARCRZVDG-UHFFFAOYSA-N (4-methoxy-2-methylphenyl)-phenylmethanone Chemical class CC1=CC(OC)=CC=C1C(=O)C1=CC=CC=C1 KDYYFNARCRZVDG-UHFFFAOYSA-N 0.000 claims description 2
- WLJVXDMOQOGPHL-PPJXEINESA-N 2-phenylacetic acid Chemical compound O[14C](=O)CC1=CC=CC=C1 WLJVXDMOQOGPHL-PPJXEINESA-N 0.000 claims description 2
- 239000005711 Benzoic acid Substances 0.000 claims description 2
- HGRNRWNRNVPVMM-UHFFFAOYSA-N benzene-1,3-diol;benzoic acid Chemical compound OC1=CC=CC(O)=C1.OC(=O)C1=CC=CC=C1 HGRNRWNRNVPVMM-UHFFFAOYSA-N 0.000 claims description 2
- 235000010233 benzoic acid Nutrition 0.000 claims description 2
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 claims description 2
- 239000012965 benzophenone Substances 0.000 claims description 2
- GNOIPBMMFNIUFM-UHFFFAOYSA-N hexamethylphosphoric triamide Chemical compound CN(C)P(=O)(N(C)C)N(C)C GNOIPBMMFNIUFM-UHFFFAOYSA-N 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 150000008301 phosphite esters Chemical class 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- 235000019260 propionic acid Nutrition 0.000 claims description 2
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims 2
- QUAMTGJKVDWJEQ-UHFFFAOYSA-N octabenzone Chemical compound OC1=CC(OCCCCCCCC)=CC=C1C(=O)C1=CC=CC=C1 QUAMTGJKVDWJEQ-UHFFFAOYSA-N 0.000 claims 2
- 239000004310 lactic acid Substances 0.000 claims 1
- 235000014655 lactic acid Nutrition 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 239000011248 coating agent Substances 0.000 abstract description 7
- 238000000576 coating method Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 3
- 239000011159 matrix material Substances 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 description 7
- 239000000843 powder Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000011049 filling Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000004753 textile Substances 0.000 description 4
- 238000001994 activation Methods 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000003014 reinforcing effect Effects 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 125000002723 alicyclic group Chemical group 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- WLJVXDMOQOGPHL-UHFFFAOYSA-N phenylacetic acid Chemical compound OC(=O)CC1=CC=CC=C1 WLJVXDMOQOGPHL-UHFFFAOYSA-N 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- UYSQHMXRROFKRN-UHFFFAOYSA-N (2,4-dimethylphenyl)-phenylmethanone Chemical class CC1=CC(C)=CC=C1C(=O)C1=CC=CC=C1 UYSQHMXRROFKRN-UHFFFAOYSA-N 0.000 description 1
- RJHSCCZVRVXSEF-UHFFFAOYSA-N (2-hydroxyphenyl) benzoate Chemical group OC1=CC=CC=C1OC(=O)C1=CC=CC=C1 RJHSCCZVRVXSEF-UHFFFAOYSA-N 0.000 description 1
- PAMIQIKDUOTOBW-UHFFFAOYSA-N 1-methylpiperidine Chemical compound CN1CCCCC1 PAMIQIKDUOTOBW-UHFFFAOYSA-N 0.000 description 1
- PEPBFCOIJRULGJ-UHFFFAOYSA-N 3h-1,2,3-benzodioxazole Chemical compound C1=CC=C2NOOC2=C1 PEPBFCOIJRULGJ-UHFFFAOYSA-N 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229920000265 Polyparaphenylene Polymers 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- NJSVDVPGINTNGX-UHFFFAOYSA-N [dimethoxy(propyl)silyl]oxymethanamine Chemical compound CCC[Si](OC)(OC)OCN NJSVDVPGINTNGX-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 238000013475 authorization Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- KMGARVOVYXNAOF-UHFFFAOYSA-N benzpiperylone Chemical compound C1CN(C)CCC1N1C(=O)C(CC=2C=CC=CC=2)=C(C=2C=CC=CC=2)N1 KMGARVOVYXNAOF-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- QNEFNFIKZWUAEQ-UHFFFAOYSA-N carbonic acid;potassium Chemical compound [K].OC(O)=O QNEFNFIKZWUAEQ-UHFFFAOYSA-N 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 239000003279 phenylacetic acid Substances 0.000 description 1
- 229960003424 phenylacetic acid Drugs 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 230000002633 protecting effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 125000000446 sulfanediyl group Chemical group *S* 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Classifications
-
- 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
- D06M11/68—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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
- D06M11/72—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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with metaphosphoric acids or their salts; with polyphosphoric acids or their salts; with perphosphoric acids or their salts
-
- 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
- D06M11/73—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 carbon or compounds thereof
- D06M11/74—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 carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
-
- 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
- D06M13/10—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
- D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
-
- 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
- D06M13/342—Amino-carboxylic acids; Betaines; Aminosulfonic acids; Sulfo-betaines
-
- 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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/55—Epoxy resins
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/25—Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments
-
- 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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/50—Modified hand or grip properties; Softening compositions
Abstract
The present invention relates to fiber preparation fields,More particularly to it is a kind of with super-elastic and high-modulus than etc. outstanding mechanical property anti-ultraviolet ageing pbo fiber preparation process,It is activated on pbo fiber surface first with acid etching modification liquid,And its surface is performed etching,Form shallower groove and microgroove,It is added dropwise during weakly alkaline solution neutralizes and shallower groove and microgroove is deepened,It is formed in the reacting of pbo fiber and the carbon-based suspension of crackle,Graphite oxide and atomized aluminium can be gradually filled in the crackle of pbo fiber,And aluminium restores graphite oxide to form expanded graphite in the heat treatment of vacuum or protective atmosphere,It originally formed the pbo fiber weakness of crackle in conjunction with the collective effect of heat treatment and can be broken,Breaking part is connected and is filled by expanded graphite,It is modified again by uvioresistant,One layer of uniform anti-ultraviolet ageing coating is covered on the surface of fiber,Ultraviolet light can be generated and reduce ultraviolet light to the generation aging of pbo fiber matrix.
Description
Technical field
The present invention relates to fiber preparation fields, more particularly to one kind having the outstanding mechanical property such as super-elastic and high-modulus ratio
The preparation process of the anti-ultraviolet ageing pbo fiber of energy.
Background technology
The ultimate tensile strength of polyparaphenylene's benzo dioxazole fiber (pbo fiber) is up to 5.8GPa, and stretch modulus is up to
280~380GPa, be a kind of high intensity, high-modulus, low-density novel synthetic fibers, be known as " the super fibre of 21 century
Dimension ".It is also equipped with very excellent heat-resisting, chemical resistance and tensile property, is largely used to the high skills such as weaving and space flight and aviation
In art field, but pbo fiber is there is also apparent disadvantage, such as easily aging under light illumination, after short time ultraviolet light,
The tensile strength rapid decrease of fiber, and in use, often receiving ultraviolet light, such as in textile and field of aerospace
Strong ultraviolet light in sterilization process and space environment, therefore cause its service life extreme, using seriously being limited
System.
Patent Office of the People's Republic of China disclosed a kind of hair of the preparation method of binary graft modification pbo fiber on 2 17th, 2016
Bright license, Authorization Notice No. CN103820996B are realized fine to the functionalization and PBO of graphene oxide first
The activation process of dimension, and hydroxy functionalized processing is carried out to activation pbo fiber, then to through hydroxy functionalized treated PBO
Fiber carries out APTMS grafting and the grafting of surface oxidation graphene binary, and it is disconnected that realization is easily caused fiber molecule chain to it by elemental oxygen
The problem of in turn resulting in mechanical properties decrease is split to be solved, but its problem weak to its anti-ultraviolet ageing ability does not solve yet
Certainly.
High-performance pbo fiber surface is modified and its UV Aging Resistance studies .Journal of Functional
Materials.2018/01(49):It possesses some special knowledge to the resistance to UV aging of pbo fiber in 01112-01116, but it is in reality
The performance that pbo fiber itself is now largely affected after the ability of enhancing pbo fiber ageing resistance by ultraviolet light, weakens significantly
The high-performance benefits that pbo fiber itself has, practicability are poor.
Invention content
To solve pbo fiber easily aging under light illumination in the prior art, after short time ultraviolet light, the drawing of fiber
Stretch intensity rapid decrease, and in use, often receive ultraviolet light in textile and field of aerospace, such as sterilizing
Strong ultraviolet light in process and space environment, therefore cause its service life extreme, the problem of using being severely limited,
The first object of the present invention is to provide a kind of preparation process for the pbo fiber having outstanding anti-ultraviolet aging.
The second object of the present invention is to keep PBO fine while so that pbo fiber is had outstanding anti-ultraviolet aging
Tie up itself outstanding mechanical property.
Third object of the present invention be on the basis of keeping PBO existing original mechanical properties to its elastic property and
Flexibility is made further reinforcing and is improved.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation process of anti-ultraviolet ageing pbo fiber, the preparation process include following preparation process：
1) surface etch of pbo fiber is modified：Polyphosphoric acids is dissolved in organic monoacid solvent, stirs evenly and is configured to acid etching
The pbo fiber of clean drying is placed in acid etching immersion treatment in acid etching modification liquid by modification liquid, and it is molten that alkalescent is added dropwise in after treatment
Liquid tends to be neutral to it and continues impregnation, ultrasound rinsing is placed in water after impregnation and in vacuum or protective atmosphere
Under be dried to obtain etching pbo fiber；
2) preparation of carbon-based suspension：Sorting removal impurity is carried out to graphite waste, then it is crushed to fine-powdered, is utilized
Oxidant is oxidized to graphite oxide, and graphite oxide is mixed with water, forms mixed liquor, and atomized aluminium is added simultaneously into mixed liquor
Ultrasonic vibration is carried out, carbon-based suspension is obtained after ultrasonic vibration to graphite oxide and atomized aluminium are uniformly dispersed；
3) crackle fills intensive treatment：Etching pbo fiber obtained by step 1) is placed in the carbon-based suspension obtained by step 2) slowly
Speed stirs, and rinsing is taken out after ultrasonic vibration, is placed in vacuum or protective atmosphere and is heat-treated, and is obtained after heat treatment strong
Change pbo fiber；
4) uvioresistant is modified：Light modifying agent, cycloaliphatic epoxy resin and curing agent are dissolved in organic solvent and are configured to uvioresistant
Aging modification liquid will strengthen pbo fiber obtained by step 3) after stirring evenly and be placed in one, taken out after impregnation be placed in water it is super
Sound rinses and is dried to obtain anti-ultraviolet ageing pbo fiber under vacuum or protective atmosphere.
The structure of pbo fiber itself is partial to a kind of core-skin formula structure, which exists first with acid etching modification liquid
Pbo fiber surface is modified activation using polyphosphoric acids, to promote the preparation of follow-up anti-ultraviolet ageing coating, and by having
Machine faintly acid solvent carries out etching limited and appropriate to its surface, forms shallower groove and microgroove, then alkalescent is being added dropwise
Solution performs etching shallower groove and microgroove during neutralizing, deepens, and forms the crackle for having certain depth, flaw shape
Be in the more weak place of fibre structure at place itself, the pbo fiber that crackle is formed after over etching with it is carbon-based suspended
In the reaction process of liquid, graphite oxide and atomized aluminium can be gradually filled in the crackle of pbo fiber, and in vacuum or protective atmosphere
Heat treatment in atomized aluminium graphite oxide can be restored to form expanded graphite, and combine heat treatment collective effect originally formed
The pbo fiber weakness of crackle can be broken, and breaking part can be connected and be filled by expanded graphite, formed doping and strengthened, to it
Mechanical property, flexibility and elasticity generate the promotion effect of highly significant, while atomized aluminium aoxidizes the very fine and closely woven oxidation to be formed
Aluminium can be formed with expanded graphite and be acted synergistically, and raising is certain while generating connection, protecting effect to breaking part resists atom
The ability of oxygen attack has obtained reinforcing pbo fiber, then has been modified by the uvioresistant of resistance to UV aging, is strengthening pbo fiber
Surface cover one layer of uniform anti-ultraviolet ageing coating, can to ultraviolet light generate absorb, avoid ultraviolet light to pbo fiber
Matrix generates aging, while certain diffusion can occur in the coating for expanded graphite in the drying process so that coating it is uniform
Degree and two aspect of mechanical property are generated and are obviously improved.
Preferably, step 1) the organic monoacid solvent includes acetic acid, phenylacetic acid, ethanedioic acid, glycolic, propyl alcohol
Acid, benzoic acid, propionic acid, butyric acid and phenol, the weakly alkaline solution include ammonium hydroxide, sodium carbonate liquor, sodium bicarbonate solution, carbonic acid
Potassium and saleratus.
Above-mentioned organic monoacid solvent acidity is weaker, is playing the role of dissolving polyphosphoric acids solvent meanwhile, it is capable to right
Pbo fiber surface carries out mildly selective etch, and weakly alkaline solution, which equally corrodes pbo fiber there are certain selectivity, to be made
With, thus it is in and weak acid while can corrode weak acid the groove and microgroove is deepened, and is formed and is easy to filling
Crackle.
Preferably, step 1) the acid etching immersion treatment time is 15~25min, the dipping after weakly alkaline solution is added dropwise
Processing time is 20~30min, and the protective atmosphere includes nitrogen protection atmosphere and inert gas shielding atmosphere.
The suitable duration of acid etching immersion treatment can form enough grooves and microgroove and ensure groove and microgroove
Quantity was unlikely to multipair pbo fiber structure and forms serious destruction, so that the characteristics such as the high-strength and high-modulus of itself is lost, while weak base
The property suitable duration of solution impregnation can form enough intensifications to groove and microgroove and keep groove and microgroove excessive
Expand, the excellent characteristic for seriously destroying and losing script is generated to pbo fiber basal body structure.
Preferably, the step 2) oxidant includes oxidizing acid and potassium permanganate.
Oxidizing acid and potassium permanganate can generate the efficient oxidation to graphite, form graphite oxide.
Preferably, the step 2) graphite waste by after sorted removal of impurities is crushed to 60~300 mesh, the atomized aluminium
Mesh number is 60~300 mesh.
The graphite waste of high mesh number forms the graphite oxide of high mesh number, after the graphite oxide and atomized aluminium of high mesh number are conducive to
The progress of continuous dispersion, diffusion and filling.
Preferably, the weight ratio used in the step 2) graphite oxide, atomized aluminium and water is (5~10)：(15~20)：
200。
Graphite oxide, water and the atomized aluminium of ratio mixing can keep preferable mobility and form more uniform dispersion
Suspension is conducive to the progress of dispersion, diffusion and filling.
Preferably, the step 3) rotating speed that mixes slowly is 60~100r/min, the time is 15~90min, the heat
Treatment conditions be 600~700 DEG C of heat treatment temperature, 3~6h of heat treatment time, the protective atmosphere include nitrogen protection atmosphere and
Inert gas shielding atmosphere.
Mixing slowly can promote graphite oxide and atomized aluminium to fill into crackle, and the heat treatment under the temperature condition can
Cause atomized aluminium reduction-oxidation graphite and form the reaction of expanded graphite, and it is disconnected to enable to the pbo fiber place of cracking to occur
It splits, and then the expanded graphite by restoring generation in crackle carries out good filling to crackle and generates connection, expansion in breaking part
Graphite has very excellent elastic property and flexibility, and the good characteristic with low-density, is not only able to avoid crackle drop
The mechanical property of low pbo fiber can more improve the Some Mechanical Properties of pbo fiber, improve its flexibility and elasticity, and it is even more to use to make it
In field of textiles.
Preferably, step 4) the smooth modifying agent includes septichen phenyl ester, 2- (2'- hydroxyl -5'- methylbenzenes
Base) benzotriazole, 2,4- dimethyl benzophenones, 2- methyl -4- methoxy benzophenones, 2- hydroxyl -4- n-octyloxies two
Benzophenone, 2- (two tertiary phenyl of 2'- hydroxyls -3,5'-) -5- chlorinations benzotriazole, single benzoic acid resorcinol, 2,2'- are thio
Bis- (4- t-octyl phenol oxygroup) nickel, three (1,2,2,6,6- pempidines base) phosphite esters, 4- benzoyloxys -2,2,6,6- four
Methyl piperidine, 2,4,6- tri- (2' n-butoxyphenyls) -1,3,5- triazines, hexamethylphosphoramide and (2'- hydroxyls -3', 5'-
Two tertiary amyl phenyl) -5- chlorinated benzotriazoles, curing agent is ethylenediamine tetra-acetic acid, and organic solvent includes ethyl acetate, phenylacetic acid
Methyl esters, methyl benzoate and ethyl propionate.
Above-mentioned organic solvent has good dissolubility and the characteristic of removal, cycloaliphatic epoxy resin is facilitated to have flexibility,
As the flexible substrate of coating, the pbo fiber properties after reinforcing are ensured, then curing agent promotes light modifying agent to form painting
Layer so that pbo fiber has excellent resistance to UV aging.
Preferably, the use weight of step 4) the smooth modifying agent, cycloaliphatic epoxy resin, curing agent and organic solvent
Than for (15~20)：(5~15)：(8~13)：200, the impregnation time is 5~20min, and the drying temperature is 80
~120 DEG C.
Ingredient degree more homogeneous than the coating of formation and quality are preferable.
Preferably, the step 4) protective atmosphere includes nitrogen protection atmosphere and inert gas shielding atmosphere.
The beneficial effects of the invention are as follows：
1) ability that anti-ultraviolet ageing is provided for pbo fiber greatly reduces the use limitation of pbo fiber, and extending it makes
Use the service life；
2) while providing pbo fiber anti-ultraviolet ageing ability, it ensure that the excellent in performance that pbo fiber originally had is not sent out
Drop is given birth to, its original outstanding mechanical property is kept；
3) flexibility and elasticity for improving pbo fiber, make it that can preferably be used in field of textiles；
4) recycling is realized to graphite waste, meets friendly process.
Specific implementation mode
With reference to the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described, shows
Right described embodiment is only a part of the embodiment of the present invention, rather than whole embodiments.Based on the embodiments of the present invention, originally
The every other embodiment that field those of ordinary skill is obtained without making creative work, belongs to the present invention
Protection domain.
Embodiment 1
A kind of preparation process of anti-ultraviolet ageing pbo fiber, the preparation process include following preparation process：
1) surface etch of pbo fiber is modified：Polyphosphoric acids is dissolved in acetic acid solution, stirs evenly and is configured to acid etching modification
The pbo fiber of clean drying is placed in acid etching immersion treatment 15min in acid etching modification liquid by liquid, and ammonium hydroxide is added dropwise extremely in after treatment
It tends to be neutral and continues impregnation 20min, and ultrasound is placed in water after impregnation and rinses and is dried under vacuum
To etching pbo fiber, a concentration of 15wt% of polyphosphoric acids wherein in acid etching modification liquid；
2) preparation of carbon-based suspension：Sorting removal impurity is carried out to graphite waste, then it is crushed to 60 targeted fine powders
Shape is oxidized to graphite oxide using dust technology, and graphite oxide is mixed with water, forms mixed liquor, is added into mixed liquor
The atomized aluminium of 60 mesh simultaneously carries out ultrasonic vibration, is obtained after ultrasonic vibration to graphite oxide and atomized aluminium are uniformly dispersed carbon-based suspended
Weight ratio used in liquid, wherein graphite oxide, atomized aluminium and water is 5：15：200；
3) crackle fills intensive treatment：Will etching pbo fiber obtained by step 1) be placed in the carbon-based suspension obtained by step 2) into
Row rotating speed is 60r/min, and the time is mixing slowly for 90min, and rinsing is taken out after ultrasonic vibration, is placed in vacuum and carries out
600 DEG C of heat treatment 6h, strengthened pbo fiber after heat treatment；
4) uvioresistant is modified：Septichen phenyl ester, cycloaliphatic epoxy resin and ethylenediamine tetra-acetic acid are dissolved in ethyl propionate
In be configured to anti-ultraviolet ageing modification liquid, will strengthen pbo fiber obtained by step 3) after stirring evenly is placed in one, impregnation
Taken out after 5min be placed in water ultrasound rinsing and under vacuum 80 DEG C be dried to obtain anti-ultraviolet ageing pbo fiber, wherein adjacent hydroxyl
Phenol benzoate, cycloaliphatic epoxy resin, ethylenediamine tetra-acetic acid and ethyl propionate use weight ratio be 15：5：8：200.
Embodiment 2
A kind of preparation process of anti-ultraviolet ageing pbo fiber, the preparation process include following preparation process：
1) surface etch of pbo fiber is modified：Polyphosphoric acids is dissolved in phenylacetic acid solution, stirs evenly and is configured to acid etching modification
The pbo fiber of clean drying is placed in acid etching immersion treatment 25min in acid etching modification liquid by liquid, and sodium carbonate is added dropwise in after treatment
Solution tends to be neutral to it and continues impregnation 30min, and ultrasound rinsing is placed in water after impregnation and is protected in nitrogen
It is dried to obtain etching pbo fiber under shield atmosphere, a concentration of 18wt% of polyphosphoric acids wherein in acid etching modification liquid；
2) preparation of carbon-based suspension：Sorting removal impurity is carried out to graphite waste, then it is crushed to 300 targeted fine powders
Shape is oxidized to graphite oxide using liquor potassic permanganate, and graphite oxide is mixed with water, mixed liquor is formed, to mixed liquor
The middle atomized aluminium that 300 mesh are added simultaneously carries out ultrasonic vibration, is obtained after ultrasonic vibration to graphite oxide and atomized aluminium are uniformly dispersed
Weight ratio used in carbon-based suspension, wherein graphite oxide, atomized aluminium and water is 10：20：200；
3) crackle fills intensive treatment：Will etching pbo fiber obtained by step 1) be placed in the carbon-based suspension obtained by step 2) into
Row rotating speed is 100r/min, and the time is mixing slowly for 15min, and rinsing is taken out after ultrasonic vibration, is placed in nitrogen protection
700 DEG C of heat treatment 3h is carried out in atmosphere, strengthened pbo fiber after heat treatment；
4) uvioresistant is modified：By 4 benzoyloxy 2,2,6,6 tetramethyl piperidine, cycloaliphatic epoxy resin and ethylenediamine tetrem
Acid, which is dissolved in methyl phenylacetate, is configured to anti-ultraviolet ageing modification liquid, and will strengthen pbo fiber obtained by step 3) after stirring evenly sets
Taken out in wherein, after impregnation 20min be placed in water ultrasound rinsing and under nitrogen protection atmosphere 120 DEG C be dried to obtain anti-purple
Outer aging pbo fiber, wherein 4- benzoyloxys -2,2,6,6- tetramethyl piperidines, cycloaliphatic epoxy resin, ethylenediamine tetra-acetic acid
Use weight ratio with methyl phenylacetate is 20：15：13：200.
Embodiment 3
A kind of preparation process of anti-ultraviolet ageing pbo fiber, the preparation process include following preparation process：
1) surface etch of pbo fiber is modified：Polyphosphoric acids is dissolved in ethanedioic acid solution, stirs evenly and is configured to acid etching modification
The pbo fiber of clean drying is placed in acid etching immersion treatment 20min in acid etching modification liquid by liquid, and bicarbonate is added dropwise in after treatment
Sodium solution tends to be neutral to it and continues impregnation 25min, ultrasound rinsing is placed in water after impregnation and in argon gas
Etching pbo fiber is dried to obtain under protective atmosphere, a concentration of 16wt% of polyphosphoric acids wherein in acid etching modification liquid；
2) preparation of carbon-based suspension：Sorting removal impurity is carried out to graphite waste, then it is crushed to 180 targeted fine powders
Shape is oxidized to graphite oxide using the concentrated sulfuric acid, and graphite oxide is mixed with water, forms mixed liquor, is added into mixed liquor
The atomized aluminium of 180 mesh simultaneously carries out ultrasonic vibration, is obtained after ultrasonic vibration to graphite oxide and atomized aluminium are uniformly dispersed carbon-based outstanding
Weight ratio used in turbid, wherein graphite oxide, atomized aluminium and water is 8：15：200；
3) crackle fills intensive treatment：Will etching pbo fiber obtained by step 1) be placed in the carbon-based suspension obtained by step 2) into
Row rotating speed is 80r/min, and the time is mixing slowly for 60min, and rinsing is taken out after ultrasonic vibration, is placed in argon gas protection gas
650 DEG C of heat treatment 4h is carried out in atmosphere, strengthened pbo fiber after heat treatment；
4) uvioresistant is modified：By 2,4,6- tri- (2' n-butoxyphenyls) -1,3,5- triazines, cycloaliphatic epoxy resin and ethylenediamine
Tetraacethyl, which is dissolved in methyl benzoate, is configured to anti-ultraviolet ageing modification liquid, and it is fine to strengthen PBO obtained by step 3) after stirring evenly
Dimension is placed in one, after impregnation 15min take out be placed in water ultrasound rinsing and under argon atmosphere 100 DEG C be dried to obtain
Anti-ultraviolet ageing pbo fiber, wherein 2,4,6- tri- (2' n-butoxyphenyls) -1,3,5-triazines, cycloaliphatic epoxy resin, second two
The use weight ratio of amine tetraacethyl and methyl benzoate is 18：10：11：200.
Embodiment 4
A kind of preparation process of anti-ultraviolet ageing pbo fiber, the preparation process include following preparation process：
1) surface etch of pbo fiber is modified：Polyphosphoric acids is dissolved in propionic acid solution, stirs evenly and is configured to acid etching modification
The pbo fiber of clean drying is placed in acid etching immersion treatment 25min in acid etching modification liquid by liquid, and potassium carbonate is added dropwise in after treatment
Solution tends to be neutral to it and continues impregnation 20min, and ultrasound rinsing and under vacuum is placed in water after impregnation
It is dried to obtain etching pbo fiber, a concentration of 20wt% of polyphosphoric acids wherein in acid etching modification liquid；
2) preparation of carbon-based suspension：Sorting removal impurity is carried out to graphite waste, then it is crushed to 200 targeted fine powders
Shape is oxidized to graphite oxide using concentrated nitric acid, and graphite oxide is mixed with water, forms mixed liquor, is added into mixed liquor
The atomized aluminium of 200 mesh simultaneously carries out ultrasonic vibration, is obtained after ultrasonic vibration to graphite oxide and atomized aluminium are uniformly dispersed carbon-based outstanding
Weight ratio used in turbid, wherein graphite oxide, atomized aluminium and water is 9：17：200；
3) crackle fills intensive treatment：Will etching pbo fiber obtained by step 1) be placed in the carbon-based suspension obtained by step 2) into
Row rotating speed is 90r/min, and the time is mixing slowly for 45min, and rinsing is taken out after ultrasonic vibration, is placed in vacuum and carries out
650 DEG C of heat treatment 4.5h, strengthened pbo fiber after heat treatment；
4) uvioresistant is modified：By (bis- tertiary amyl phenyl of 2'- hydroxyl -3', 5'-) -5- chlorinated benzotriazoles, cycloaliphatic epoxy resin
It is dissolved in methyl benzoate with ethylenediamine tetra-acetic acid and is configured to anti-ultraviolet ageing modification liquid, it will be strong obtained by step 3) after stirring evenly
Change pbo fiber be placed in one, after impregnation 15min take out be placed in water ultrasound rinsing and under vacuum 110 DEG C be dried to obtain
Anti-ultraviolet ageing pbo fiber, wherein (bis- tertiary amyl phenyl of 2'- hydroxyls -3', 5'-) -5- chlorinated benzotriazoles, alicyclic epoxy
The use weight ratio of resin, ethylenediamine tetra-acetic acid and methyl benzoate is 15：15：13：200.
Embodiment 5
A kind of preparation process of anti-ultraviolet ageing pbo fiber, the preparation process include following preparation process：
1) surface etch of pbo fiber is modified：Polyphosphoric acids is dissolved in butyric acid solution, stirs evenly and is configured to acid etching modification
The pbo fiber of clean drying is placed in acid etching immersion treatment 25min in acid etching modification liquid by liquid, and bicarbonate is added dropwise in after treatment
Potassium solution tends to be neutral to it and continues impregnation 25min, ultrasound rinsing is placed in water after impregnation and in nitrogen
Etching pbo fiber is dried to obtain under protective atmosphere, a concentration of 19wt% of polyphosphoric acids wherein in acid etching modification liquid；
2) preparation of carbon-based suspension：Sorting removal impurity is carried out to graphite waste, then it is crushed to 300 targeted fine powders
Shape is oxidized to graphite oxide using liquor potassic permanganate, and graphite oxide is mixed with water, mixed liquor is formed, to mixed liquor
The middle atomized aluminium that 300 mesh are added simultaneously carries out ultrasonic vibration, is obtained after ultrasonic vibration to graphite oxide and atomized aluminium are uniformly dispersed
Weight ratio used in carbon-based suspension, wherein graphite oxide, atomized aluminium and water is 10：18：200；
3) crackle fills intensive treatment：Will etching pbo fiber obtained by step 1) be placed in the carbon-based suspension obtained by step 2) into
Row rotating speed is 85r/min, and the time is mixing slowly for 35min, and rinsing is taken out after ultrasonic vibration, is placed in nitrogen protection gas
650 DEG C of heat treatment 4.5h is carried out in atmosphere, strengthened pbo fiber after heat treatment；
4) uvioresistant is modified：By 2- (two tertiary phenyl of 2'- hydroxyls -3,5'-) -5- chlorinations benzotriazole, cycloaliphatic epoxy resin and
Ethylenediamine tetra-acetic acid, which is dissolved in ethyl acetate, is configured to anti-ultraviolet ageing modification liquid, will strengthen obtained by step 3) after stirring evenly
Pbo fiber is placed in one, and is taken out after impregnation 10min and is placed in water ultrasound rinsing and 80 DEG C of dryings under nitrogen protection atmosphere
Obtain anti-ultraviolet ageing pbo fiber, wherein 2- (bis- tertiary phenyl of 2'- hydroxyls -3,5'-) -5- chlorinations benzotriazole, alicyclic epoxy
The use weight ratio of resin, ethylenediamine tetra-acetic acid and ethyl acetate is 18：11：11：200.
Comparative example
Pbo fiber long filament is produced by Fushan City, Guangdong Province Telon fiber Science and Technology Ltd..
Examples 1 to 5 and comparative example are detected, testing result and comparison are as shown in the table：
Wherein in the detection of tensile set rate, comparative example high-strength pbo fiber tensile elongation is the 3% of total length, right
The high model pbo fiber tensile elongation of ratio is the 1.5% of total length, and the tensile elongation of embodiment anti-ultraviolet ageing pbo fiber is equal
It is the 15% of total length, it can thus be seen that anti-ultraviolet ageing pbo fiber elasticity is obviously due to comparative example obtained by Examples 1 to 5.
Claims (10)
1. a kind of preparation process of anti-ultraviolet ageing pbo fiber, which is characterized in that the preparation process includes following preparation step
Suddenly：
1) surface etch of pbo fiber is modified：Polyphosphoric acids is dissolved in organic monoacid solvent, stirs evenly and is configured to acid etching
The pbo fiber of clean drying is placed in acid etching immersion treatment in acid etching modification liquid by modification liquid, and it is molten that alkalescent is added dropwise in after treatment
Liquid tends to be neutral to it and continues impregnation, ultrasound rinsing is placed in water after impregnation and in vacuum or protective atmosphere
Under be dried to obtain etching pbo fiber；
2) preparation of carbon-based suspension：Sorting removal impurity is carried out to graphite waste, then it is crushed to fine-powdered, is utilized
Oxidant is oxidized to graphite oxide, and graphite oxide is mixed with water, forms mixed liquor, and atomized aluminium is added simultaneously into mixed liquor
Ultrasonic vibration is carried out, carbon-based suspension is obtained after ultrasonic vibration to graphite oxide and atomized aluminium are uniformly dispersed；
3) crackle fills intensive treatment：Etching pbo fiber obtained by step 1) is placed in the carbon-based suspension obtained by step 2) slowly
Speed stirs, and rinsing is taken out after ultrasonic vibration, is placed in vacuum or protective atmosphere and is heat-treated, and is obtained after heat treatment strong
Change pbo fiber；
4) uvioresistant is modified：Light modifying agent, cycloaliphatic epoxy resin and curing agent are dissolved in organic solvent and are configured to uvioresistant
Aging modification liquid will strengthen pbo fiber obtained by step 3) after stirring evenly and be placed in one, taken out after impregnation be placed in water it is super
Sound rinses and is dried to obtain anti-ultraviolet ageing pbo fiber under vacuum or protective atmosphere.
2. a kind of preparation process of anti-ultraviolet ageing pbo fiber according to claim 1, which is characterized in that step 1) institute
It includes acetic acid, phenylacetic acid, ethanedioic acid, glycolic, lactic acid, benzoic acid, propionic acid, butyric acid and phenol to state organic monoacid solvent,
The weakly alkaline solution includes ammonium hydroxide, sodium carbonate liquor, sodium bicarbonate solution, potassium carbonate and saleratus.
3. a kind of preparation process of anti-ultraviolet ageing pbo fiber according to claim 1 or 2, which is characterized in that step 1)
The acid etching immersion treatment time is 15~25min, and it is 20~30min, institute that the impregnation time after weakly alkaline solution, which is added dropwise,
It includes nitrogen protection atmosphere and inert gas shielding atmosphere to state protective atmosphere.
4. a kind of preparation process of anti-ultraviolet ageing pbo fiber according to claim 1, which is characterized in that step 2) institute
It includes oxidizing acid and potassium permanganate to state oxidant.
5. a kind of preparation process of anti-ultraviolet ageing pbo fiber according to claim 1 or 4, which is characterized in that step 2)
The graphite waste by after sorted removal of impurities is crushed to 60~300 mesh, and the atomized aluminium mesh number is 60~300 mesh.
6. a kind of preparation process of anti-ultraviolet ageing pbo fiber according to claim 5, which is characterized in that step 2) institute
It is (5~10) to state the weight ratio used in graphite oxide, atomized aluminium and water：(15~20)：200.
7. a kind of preparation process of anti-ultraviolet ageing pbo fiber according to claim 1, which is characterized in that step 3) institute
State mix slowly rotating speed be 60~100r/min, the time be 15~90min, the heat treatment condition be heat treatment temperature 600~
700 DEG C, 3~6h of heat treatment time, the protective atmosphere includes nitrogen protection atmosphere and inert gas shielding atmosphere.
8. a kind of preparation process of anti-ultraviolet ageing pbo fiber according to claim 1, which is characterized in that step 4) institute
It includes septichen phenyl ester, 2- (2'- hydroxyl -5'- aminomethyl phenyls) benzotriazole, 2,4- dimethyl two to state light modifying agent
Benzophenone, 2- methyl -4- methoxy benzophenones, 2-hydroxy-4-n-octoxybenzophenone, 2- (two uncles of 2'- hydroxyls -3,5'-
Phenyl) -5- chlorinations benzotriazole, single benzoic acid resorcinol, 2,2'- thiobis (4- t-octyl phenol oxygroup) nickel, three (1,2,
2,6,6- pempidines base) phosphite ester, 4 benzoyloxy 2,2,6,6 tetramethyl piperidine, (the 2' n-butoxies of 2,4,6- tri-
Phenyl) -1,3,5-triazines, hexamethylphosphoramide and (bis- tertiary amyl phenyl of 2'- hydroxyls -3', 5'-) -5- chlorinated benzotriazoles,
Curing agent is ethylenediamine tetra-acetic acid, and organic solvent includes ethyl acetate, methyl phenylacetate, methyl benzoate and ethyl propionate.
9. a kind of preparation process of anti-ultraviolet ageing pbo fiber according to claim 1 or 8, which is characterized in that step 4)
The smooth modifying agent, cycloaliphatic epoxy resin, curing agent and organic solvent use weight ratio be (15~20)：(5~15)：(8
~13)：200, the impregnation time is 5~20min, and the drying temperature is 80~120 DEG C.
10. a kind of preparation process of anti-ultraviolet ageing pbo fiber according to claim 9, which is characterized in that step 4) institute
It includes nitrogen protection atmosphere and inert gas shielding atmosphere to state protective atmosphere.
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| CN111088539A (en) * | 2020-01-13 | 2020-05-01 | 中原工学院 | Micro-nano fiber material with linear groove characteristic and ordered forming method thereof |
| CN111926438A (en) * | 2020-08-18 | 2020-11-13 | 中国科学院宁波材料技术与工程研究所 | Ultraviolet-resistant high-strength high-modulus PBO fiber and preparation method thereof |
| CN113366165A (en) * | 2018-11-26 | 2021-09-07 | Sceye股份公司 | Graphene oxide grafted PBO (Toilong) fiber, production method thereof and application thereof in airship hull and lighter-than-air aircraft |
| CN114790652A (en) * | 2021-01-26 | 2022-07-26 | 中国科学院化学研究所 | Poly (p-phenylene benzobisoxazole) nano fiber and preparation method thereof |
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| CN111088539A (en) * | 2020-01-13 | 2020-05-01 | 中原工学院 | Micro-nano fiber material with linear groove characteristic and ordered forming method thereof |
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| CN114790652A (en) * | 2021-01-26 | 2022-07-26 | 中国科学院化学研究所 | Poly (p-phenylene benzobisoxazole) nano fiber and preparation method thereof |
| CN114790652B (en) * | 2021-01-26 | 2023-09-22 | 中国科学院化学研究所 | Poly (p-phenylene benzobisoxazole) nanofiber and preparation method thereof |
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