CN108486861B - Preparation process of anti-ultraviolet aging PBO fiber - Google Patents
Preparation process of anti-ultraviolet aging PBO fiber Download PDFInfo
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- CN108486861B CN108486861B CN201810378821.7A CN201810378821A CN108486861B CN 108486861 B CN108486861 B CN 108486861B CN 201810378821 A CN201810378821 A CN 201810378821A CN 108486861 B CN108486861 B CN 108486861B
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- pbo fiber
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- pbo
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- 239000000835 fiber Substances 0.000 title claims abstract description 175
- 230000032683 aging Effects 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 94
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 69
- 239000010439 graphite Substances 0.000 claims abstract description 69
- 239000002253 acid Substances 0.000 claims abstract description 41
- 238000005530 etching Methods 0.000 claims abstract description 41
- 239000012298 atmosphere Substances 0.000 claims abstract description 35
- 230000001681 protective effect Effects 0.000 claims abstract description 35
- 230000004048 modification Effects 0.000 claims abstract description 33
- 238000012986 modification Methods 0.000 claims abstract description 33
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 238000011049 filling Methods 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- 238000002791 soaking Methods 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 24
- 229910052799 carbon Inorganic materials 0.000 claims description 22
- 239000002699 waste material Substances 0.000 claims description 22
- 230000010355 oscillation Effects 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 17
- 239000000725 suspension Substances 0.000 claims description 17
- 125000002723 alicyclic group Chemical group 0.000 claims description 15
- 239000003822 epoxy resin Substances 0.000 claims description 15
- 229920000647 polyepoxide Polymers 0.000 claims description 15
- 239000011259 mixed solution Substances 0.000 claims description 14
- 229920000137 polyphosphoric acid Polymers 0.000 claims description 14
- 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 12
- 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
- 230000001590 oxidative effect Effects 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- 239000012670 alkaline solution Substances 0.000 claims description 9
- 239000012535 impurity Substances 0.000 claims description 9
- CRZQGDNQQAALAY-UHFFFAOYSA-N Methyl benzeneacetate Chemical compound COC(=O)CC1=CC=CC=C1 CRZQGDNQQAALAY-UHFFFAOYSA-N 0.000 claims description 8
- FKRCODPIKNYEAC-UHFFFAOYSA-N ethyl propionate Chemical compound CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 230000006750 UV protection Effects 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000003607 modifier Substances 0.000 claims description 7
- 230000007935 neutral effect Effects 0.000 claims description 7
- 239000003960 organic solvent Substances 0.000 claims description 7
- 238000005728 strengthening Methods 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
- 239000011261 inert gas Substances 0.000 claims description 6
- 229940095102 methyl benzoate Drugs 0.000 claims description 6
- ZQBAKBUEJOMQEX-UHFFFAOYSA-N salicylic acid phenyl ester Natural products OC1=CC=CC=C1C(=O)OC1=CC=CC=C1 ZQBAKBUEJOMQEX-UHFFFAOYSA-N 0.000 claims description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 5
- 239000012286 potassium permanganate Substances 0.000 claims description 5
- 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 4
- NDRPHZPVTSFYLH-UHFFFAOYSA-N 2,4,6-tris(2-butoxyphenyl)-1,3,5-triazine Chemical compound C(CCC)OC1=C(C=CC=C1)C1=NC(=NC(=N1)C1=C(C=CC=C1)OCCCC)C1=C(C=CC=C1)OCCCC NDRPHZPVTSFYLH-UHFFFAOYSA-N 0.000 claims description 4
- VIXNWASTFGXPTN-UHFFFAOYSA-N 2-(5-chloro-2H-benzotriazol-4-yl)-4,6-bis(2-methylbutan-2-yl)phenol Chemical compound CCC(C)(C)C1=CC(C(C)(C)CC)=CC(C=2C=3N=NNC=3C=CC=2Cl)=C1O VIXNWASTFGXPTN-UHFFFAOYSA-N 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 claims description 4
- 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
- 238000007598 dipping method Methods 0.000 claims description 4
- DUWWHGPELOTTOE-UHFFFAOYSA-N n-(5-chloro-2,4-dimethoxyphenyl)-3-oxobutanamide Chemical compound COC1=CC(OC)=C(NC(=O)CC(C)=O)C=C1Cl DUWWHGPELOTTOE-UHFFFAOYSA-N 0.000 claims description 4
- QUAMTGJKVDWJEQ-UHFFFAOYSA-N octabenzone Chemical compound OC1=CC(OCCCCCCCC)=CC=C1C(=O)C1=CC=CC=C1 QUAMTGJKVDWJEQ-UHFFFAOYSA-N 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
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 4
- 235000019260 propionic acid Nutrition 0.000 claims description 4
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 239000011736 potassium bicarbonate Substances 0.000 claims description 3
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 3
- 235000015497 potassium bicarbonate Nutrition 0.000 claims description 3
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 3
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- UYSQHMXRROFKRN-UHFFFAOYSA-N (2,4-dimethylphenyl)-phenylmethanone Chemical compound CC1=CC(C)=CC=C1C(=O)C1=CC=CC=C1 UYSQHMXRROFKRN-UHFFFAOYSA-N 0.000 claims description 2
- KDYYFNARCRZVDG-UHFFFAOYSA-N (4-methoxy-2-methylphenyl)-phenylmethanone Chemical compound 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
- 230000002378 acidificating effect Effects 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 235000010233 benzoic acid Nutrition 0.000 claims description 2
- MCPKSFINULVDNX-UHFFFAOYSA-N drometrizole Chemical compound CC1=CC=C(O)C(N2N=C3C=CC=CC3=N2)=C1 MCPKSFINULVDNX-UHFFFAOYSA-N 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
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- 235000011181 potassium carbonates Nutrition 0.000 claims description 2
- GDESWOTWNNGOMW-UHFFFAOYSA-N resorcinol monobenzoate Chemical compound OC1=CC=CC(OC(=O)C=2C=CC=CC=2)=C1 GDESWOTWNNGOMW-UHFFFAOYSA-N 0.000 claims description 2
- WRVWOBJLGCVCSC-UHFFFAOYSA-N tris(1,2,2,6,6-pentamethylpiperidin-3-yl) phosphite Chemical compound CC1(C)N(C)C(C)(C)CCC1OP(OC1C(N(C)C(C)(C)CC1)(C)C)OC1C(C)(C)N(C)C(C)(C)CC1 WRVWOBJLGCVCSC-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 4
- 239000011248 coating agent Substances 0.000 abstract description 9
- 238000000576 coating method Methods 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 5
- 239000011159 matrix material Substances 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 230000009471 action Effects 0.000 abstract description 2
- 238000006386 neutralization reaction Methods 0.000 abstract description 2
- 230000003213 activating effect Effects 0.000 abstract 1
- 229960001484 edetic acid Drugs 0.000 description 11
- 239000007788 liquid Substances 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 238000007654 immersion Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000004753 textile Substances 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 238000007306 functionalization reaction Methods 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000000694 effects Effects 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
- 229910017604 nitric acid 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
- 229920000927 poly(p-phenylene benzobisoxazole) Polymers 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-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
- 230000004913 activation Effects 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229960003424 phenylacetic acid Drugs 0.000 description 1
- 239000003279 phenylacetic acid Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000004224 protection Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920006303 teflon fiber Polymers 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 invention relates to the field of fiber preparation, in particular to a preparation process of an anti-ultraviolet aging PBO fiber with excellent mechanical properties such as ultrahigh elasticity, high modulus ratio and the like, which comprises the steps of firstly activating the surface of the PBO fiber by using an acid etching modification solution, etching the surface of the PBO fiber to form shallow grooves and fine lines, deepening the shallow grooves and the fine lines in the process of dropwise adding an alkalescent solution for neutralization, gradually filling graphite oxide and fine aluminum powder in the cracks of the PBO fiber in the reaction of the PBO fiber with the cracks formed, reducing the graphite oxide to form expanded graphite in the heat treatment of vacuum or protective atmosphere, breaking the weak parts of the PBO fiber which originally form the cracks under the combined action of the heat treatment, connecting and filling the broken parts by the expanded graphite, covering a uniform anti-ultraviolet aging coating on the surface of the fiber through anti-ultraviolet modification, the ultraviolet light generation can be realized, and the aging of the PBO fiber matrix caused by the ultraviolet light can be reduced.
Description
Technical Field
The invention relates to the field of fiber preparation, in particular to a preparation process of an ultraviolet aging resistant PBO fiber with excellent mechanical properties such as ultrahigh elasticity, high modulus ratio and the like.
Background
The maximum tensile strength of the poly (p-phenylene benzobisoxazole) (PBO fiber) is up to 5.8GPa, the tensile modulus is up to 280-380 GPa, and the poly (p-phenylene benzobisoxazole) (PBO fiber) is a novel synthetic fiber with high strength, high modulus and low density and is known as a super fiber in the 21 st century. The PBO fiber has the obvious disadvantages that the PBO fiber is easy to age under illumination, the tensile strength of the fiber is rapidly reduced after short-time ultraviolet irradiation, and when the PBO fiber is used in the fields of textiles and aerospace, the PBO fiber can often receive ultraviolet irradiation, such as strong ultraviolet irradiation in a sterilization process and a space environment, so that the service life of the PBO fiber is extremely long, and the application of the PBO fiber is severely limited.
The patent office of china disclosed a preparation method of binary graft modified PBO fiber in 2016, 2, 17, the patent publication number of which is CN103820996B, the method comprises the steps of firstly performing functionalization treatment on graphene oxide and activation treatment on PBO fiber, performing hydroxyl functionalization treatment on the activated PBO fiber, and then performing APTMS grafting and surface graphene oxide binary grafting on the PBO fiber subjected to the hydroxyl functionalization treatment, so as to solve the problem that the mechanical property is reduced due to the fact that the molecular chain of the fiber is easily broken by atomic oxygen, but the problem that the ultraviolet aging resistance of the fiber is weak is not solved.
Journal of functional materials.2018/01(49):01112-01116, the anti-ultraviolet aging performance of the PBO fiber is studied, but the performance of the PBO fiber is greatly influenced after the anti-ultraviolet aging capability of the PBO fiber is enhanced, the high-performance advantage of the PBO fiber is greatly weakened, and the practicability is poor.
Disclosure of Invention
In order to solve the problems that in the prior art, PBO fibers are extremely easy to age under illumination, the tensile strength of the fibers is rapidly reduced after short-time ultraviolet irradiation, and when the PBO fibers are used in the fields of textiles and aerospace, the PBO fibers often receive ultraviolet irradiation, such as strong ultraviolet irradiation in a sterilization process and a space environment, so that the service life of the PBO fibers is extremely long and the application of the PBO fibers is severely limited, the invention provides a preparation process of the PBO fibers with excellent ultraviolet aging resistance.
The second object of the present invention is to provide PBO fibers with excellent ultraviolet light aging resistance while maintaining excellent mechanical properties of the PBO fibers themselves.
The third purpose of the invention is to further strengthen and improve the elasticity and flexibility of the PBO on the basis of keeping the prior original mechanical property of the PBO.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation process of anti-ultraviolet aging PBO fiber comprises the following preparation steps:
1) surface etching modification of PBO fiber: dissolving polyphosphoric acid in an organic weak acid solvent, uniformly stirring to prepare an acid etching modified solution, placing the cleaned and dried PBO fiber in the acid etching modified solution for acid etching and soaking treatment, dropwise adding a weak alkaline solution until the PBO fiber is neutral after the treatment is finished, continuing soaking treatment, placing the PBO fiber in water for ultrasonic rinsing after the soaking treatment is finished, and drying the PBO fiber in vacuum or protective atmosphere to obtain the etched PBO fiber;
2) preparing carbon-based suspension: sorting the graphite waste to remove impurities, crushing the graphite waste into fine powder, oxidizing the fine powder into graphite oxide by using an oxidant, mixing the graphite oxide with water to form a mixed solution, adding fine aluminum powder into the mixed solution, performing ultrasonic oscillation, and obtaining a carbon-based suspension after the graphite oxide and the fine aluminum powder are uniformly dispersed by the ultrasonic oscillation;
3) and (3) crack filling and strengthening treatment: placing the etched PBO fiber obtained in the step 1) into the carbon-based suspension obtained in the step 2) for slow stirring, taking out and rinsing after the ultrasonic oscillation is finished, placing in vacuum or protective atmosphere for heat treatment, and obtaining the reinforced PBO fiber after the heat treatment is finished;
4) ultraviolet resistance modification: dissolving a light modifier, alicyclic epoxy resin and a curing agent in an organic solvent to prepare an anti-ultraviolet aging modified solution, uniformly stirring, placing the reinforced PBO fiber obtained in the step 3) in the modified solution, taking out the fiber after dipping treatment, placing the fiber in water for ultrasonic rinsing, and drying the fiber in vacuum or protective atmosphere to obtain the anti-ultraviolet aging PBO fiber.
The PBO fiber structure is biased to a sheath-core structure, the preparation process comprises the steps of firstly utilizing acid etching modification liquid to modify and activate the surface of the PBO fiber by polyphosphoric acid to promote the preparation of a subsequent ultraviolet aging resistant coating, carrying out limited and proper etching on the surface of the PBO fiber by using an organic weak acid solvent to form shallow grooves and fine lines, then carrying out etching and deepening on the shallow grooves and the fine lines in the process of dropwise adding weak alkaline solution for neutralization to form cracks with a certain depth, wherein the crack forming part is positioned at a weak part of the fiber structure, graphite oxide and fine aluminum powder are gradually filled in the cracks of the PBO fiber in the reaction process of the etched PBO fiber with carbon-based suspension, the fine aluminum powder can reduce the graphite oxide to form expanded graphite in the heat treatment of vacuum or protective atmosphere, and the weak part of the PBO fiber which originally forms the cracks can be broken under the combined action of the heat treatment, the fracture part is connected and filled by the expanded graphite to form doping reinforcement, so that the mechanical property, flexibility and elasticity of the fiber are remarkably improved, meanwhile, the fine aluminum oxide formed by oxidizing the fine aluminum powder and the expanded graphite form a synergistic effect, the connection and protection effects on the fracture part are realized, the capability of resisting atomic oxygen corrosion is improved to a certain extent, the reinforced PBO fiber is obtained, then, the ultraviolet ageing resistance performance is subjected to ultraviolet ageing resistance modification, a uniform ultraviolet ageing resistance coating is covered on the surface of the reinforced PBO fiber, the ultraviolet light can be absorbed, the PBO fiber matrix is prevented from being aged by the ultraviolet light, meanwhile, the expanded graphite can be diffused to a certain extent in the coating in the drying process, and the uniformity and the mechanical property of the coating are remarkably improved.
Preferably, the organic weak acidic solvent of step 1) comprises acetic acid, phenylacetic acid, oxalic acid, glycolic acid, propanoic acid, benzoic acid, propanoic acid, butanoic acid and phenol, and the weak alkaline solution comprises ammonia, sodium carbonate solution, sodium bicarbonate solution, potassium carbonate and potassium bicarbonate.
The weak organic weak acid solvent has weak acidity, can slightly and selectively etch the surface of the PBO fiber while playing a role in dissolving the polyphosphoric acid solvent, and the weak alkaline solution also has a certain selective erosion effect on the PBO fiber, so that the weak acid solvent can deepen the groove and the fine line eroded by the weak acid while neutralizing the weak acid, and a crack easy to fill is formed.
Preferably, the acid etching and soaking treatment time in the step 1) is 15-25 min, and the soaking treatment time after the dropwise addition of the weak alkaline solution is 20-30 min, wherein the protective atmosphere comprises a nitrogen protective atmosphere and an inert gas protective atmosphere.
The proper duration of the acid etching soaking treatment can form enough grooves and fine lines and can ensure that the quantity of the grooves and the fine lines is not too much to cause serious damage to the PBO fiber structure, so that the characteristics of high strength, high modulus and the like of the PBO fiber structure are lost, and the proper duration of the weak alkaline solution soaking treatment can form enough deepening to the grooves and the fine lines and excessively enlarge the grooves and the fine lines to cause serious damage to the PBO fiber matrix structure and lose the original excellent characteristics.
Preferably, the oxidizing agent of step 2) includes an oxidizing acid and potassium permanganate.
The oxidizing acid and the potassium permanganate can effectively oxidize the graphite to form the graphite oxide.
Preferably, the graphite waste after sorting and impurity removal in the step 2) is crushed to 60-300 meshes, and the mesh number of the fine aluminum powder is 60-300 meshes.
The high-mesh graphite waste forms high-mesh graphite oxide, and the high-mesh graphite oxide and the fine aluminum powder are beneficial to subsequent dispersion, diffusion and filling.
Preferably, the weight ratio of the graphite oxide, the fine aluminum powder and the water in the step 2) is (5-10): (15-20): 200.
the graphite oxide, the water and the fine aluminum powder which are mixed according to the proportion can keep better fluidity and form more uniform dispersion turbid liquid, and the dispersion, the diffusion and the filling are favorably carried out.
Preferably, in the step 3), the slow stirring speed is 60-100 r/min, the time is 15-90 min, the heat treatment condition is that the heat treatment temperature is 600-700 ℃, the heat treatment time is 3-6 h, and the protective atmosphere comprises a nitrogen protective atmosphere and an inert gas protective atmosphere.
The slow stirring can promote the graphite oxide and the fine aluminum powder to be filled into the cracks, the heat treatment under the temperature condition can initiate the reaction of the fine aluminum powder reducing the graphite oxide to form the expanded graphite, the PBO fibers can be fractured at the cracks, the expanded graphite generated by reduction in the cracks can well fill the cracks and can be connected at the fractures, the expanded graphite has excellent elastic property and flexibility and has the excellent characteristic of low density, the mechanical property of the PBO fibers can be prevented from being reduced by the cracks, the partial mechanical property of the PBO fibers can be improved, the flexibility and the elasticity of the PBO fibers can be improved, and the PBO fibers are more applicable to the textile field.
Preferably, the light modifier in the step 4) includes phenyl o-hydroxybenzoate, 2- (2 '-hydroxy-5' -methylphenyl) benzotriazole, 2, 4-dimethylbenzophenone, 2-methyl-4-methoxybenzophenone, 2-hydroxy-4-n-octyloxybenzophenone, 2- (2 '-hydroxy-3, 5' -di-tert-phenyl) -5-chlorobenzotriazole, resorcinol monobenzoate, 2,2 '-thiobis (4-tert-octylphenoloxy) nickel, tris (1,2,2,6, 6-pentamethylpiperidinyl) phosphite, 4-benzoyloxy-2, 2,6, 6-tetramethylpiperidine, 2,4, 6-tris (2' n-butoxyphenyl) -1,3, 5-triazine, hexamethylphosphoric triamide and (2' -hydroxy-3 ',5' -ditert-amyl-phenyl) -5-chlorobenzotriazole, the curing agent is ethylenediamine tetraacetic acid, and the organic solvent comprises ethyl acetate, methyl phenylacetate, methyl benzoate and ethyl propionate.
The organic solvent has the characteristics of good solubility and convenient removal, the alicyclic epoxy resin has flexibility and is used as a flexible matrix of the coating to ensure various properties of the reinforced PBO fiber, and the curing agent promotes the light modifier to form the coating, so that the PBO fiber has excellent ultraviolet aging resistance.
Preferably, the use weight ratio of the light modifier, the alicyclic epoxy resin, the curing agent and the organic solvent in the step 4) is (15-20): (5-15): (8-13): 200, the dipping treatment time is 5-20 min, and the drying temperature is 80-120 ℃.
The components have better uniformity and quality of the coating texture than the formed coating.
Preferably, the protective atmosphere in step 4) includes a nitrogen protective atmosphere and an inert gas protective atmosphere.
The invention has the beneficial effects that:
1) the anti-ultraviolet ageing capability is provided for the PBO fiber, the use limit of the PBO fiber is greatly reduced, and the service life of the PBO fiber is prolonged;
2) the anti-ultraviolet aging capability of the PBO fiber is provided, meanwhile, the original excellent performance of the PBO fiber is ensured not to be reduced, and the original excellent mechanical property is maintained;
3) the flexibility and elasticity of the PBO fiber are improved, so that the PBO fiber can be better applied in the textile field;
4) realizes the recycling of graphite waste materials and accords with the green process.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, belong to the scope of the present invention.
Example 1
A preparation process of anti-ultraviolet aging PBO fiber comprises the following preparation steps:
1) surface etching modification of PBO fiber: dissolving polyphosphoric acid in an acetic acid solution, uniformly stirring to prepare an acid etching modification solution, placing the cleaned and dried PBO fiber in the acid etching modification solution for acid etching and soaking for 15min, dripping ammonia water until the PBO fiber tends to be neutral after the treatment is finished, continuing to soak for 20min, placing the PBO fiber in water for ultrasonic rinsing after the soaking treatment is finished, and drying the PBO fiber in vacuum to obtain the etched PBO fiber, wherein the concentration of polyphosphoric acid in the acid etching modification solution is 15 wt%;
2) preparing carbon-based suspension: sorting the graphite waste to remove impurities, then smashing the graphite waste into 60-mesh fine powder, oxidizing the graphite waste into graphite oxide by using dilute nitric acid, mixing the graphite oxide with water to form a mixed solution, adding 60-mesh fine aluminum powder into the mixed solution, performing ultrasonic oscillation, and obtaining carbon-based turbid liquid after the graphite oxide and the fine aluminum powder are uniformly dispersed after the ultrasonic oscillation, wherein the weight ratio of the graphite oxide to the fine aluminum powder to the water is 5: 15: 200 of a carrier;
3) and (3) crack filling and strengthening treatment: placing the etched PBO fiber obtained in the step 1) into the carbon-based suspension obtained in the step 2), slowly stirring at a rotating speed of 60r/min for 90min, taking out and rinsing after ultrasonic oscillation is finished, placing in vacuum for heat treatment at 600 ℃ for 6h, and obtaining the reinforced PBO fiber after the heat treatment is finished;
4) ultraviolet resistance modification: dissolving phenyl ortho-hydroxybenzoate, alicyclic epoxy resin and ethylene diamine tetraacetic acid in ethyl propionate to prepare an anti-ultraviolet aging modified solution, uniformly stirring, placing the reinforced PBO fiber obtained in the step 3) in the modified solution, performing immersion treatment for 5min, taking out, placing in water, performing ultrasonic rinsing, and drying at 80 ℃ under vacuum to obtain the anti-ultraviolet aging PBO fiber, wherein the using weight ratio of the phenyl ortho-hydroxybenzoate, the alicyclic epoxy resin, the ethylene diamine tetraacetic acid and the ethyl propionate is 15: 5: 8: 200.
example 2
A preparation process of anti-ultraviolet aging PBO fiber comprises the following preparation steps:
1) surface etching modification of PBO fiber: dissolving polyphosphoric acid in a phenylacetic acid solution, uniformly stirring to prepare an acid etching modification solution, placing the cleaned and dried PBO fiber in the acid etching modification solution for acid etching and soaking for 25min, dropwise adding a sodium carbonate solution until the PBO fiber tends to be neutral after the treatment is finished, continuing to perform soaking treatment for 30min, placing the PBO fiber in water for ultrasonic rinsing after the soaking treatment is finished, and drying the PBO fiber in a nitrogen protective atmosphere to obtain the etched PBO fiber, wherein the concentration of polyphosphoric acid in the acid etching modification solution is 18 wt%;
2) preparing carbon-based suspension: sorting the graphite waste to remove impurities, then smashing the graphite waste into fine powder of 300 meshes, utilizing potassium permanganate solution to oxidize the graphite waste into graphite oxide, mixing the graphite oxide with water to form a mixed solution, adding 300-mesh fine aluminum powder into the mixed solution and carrying out ultrasonic oscillation, obtaining carbon-based turbid liquid after the ultrasonic oscillation is carried out until the graphite oxide and the fine aluminum powder are uniformly dispersed, wherein the weight ratio of the graphite oxide to the fine aluminum powder to the water is 10: 20: 200 of a carrier;
3) and (3) crack filling and strengthening treatment: placing the etched PBO fiber obtained in the step 1) into the carbon-based suspension obtained in the step 2), slowly stirring at the rotating speed of 100r/min for 15min, taking out and rinsing after ultrasonic oscillation is finished, placing in a nitrogen protective atmosphere, and performing heat treatment at 700 ℃ for 3h to obtain a reinforced PBO fiber;
4) ultraviolet resistance modification: dissolving 4-benzoyloxy-2, 2,6, 6-tetramethylpiperidine, alicyclic epoxy resin and ethylene diamine tetraacetic acid in methyl phenylacetate to prepare an anti-ultraviolet aging modified solution, uniformly stirring, placing the reinforced PBO fiber obtained in the step 3) in the modified solution, taking out the fiber after immersion treatment for 20min, placing the fiber in water for ultrasonic rinsing, and drying the fiber at 120 ℃ under a nitrogen protective atmosphere to obtain the anti-ultraviolet aging PBO fiber, wherein the using weight ratio of the 4-benzoyloxy-2, 2,6, 6-tetramethylpiperidine, the alicyclic epoxy resin, the ethylene diamine tetraacetic acid and the methyl phenylacetate is 20: 15: 13: 200.
example 3
A preparation process of anti-ultraviolet aging PBO fiber comprises the following preparation steps:
1) surface etching modification of PBO fiber: dissolving polyphosphoric acid in oxalic acid solution, stirring uniformly to prepare acid etching modification solution, placing the cleaned and dried PBO fiber in the acid etching modification solution for acid etching and soaking for 20min, dropwise adding sodium bicarbonate solution until the PBO fiber tends to be neutral after the treatment is finished, continuing to perform immersion treatment for 25min, placing the PBO fiber in water for ultrasonic rinsing after the immersion treatment is finished, and drying the PBO fiber in an argon protective atmosphere to obtain etched PBO fiber, wherein the concentration of polyphosphoric acid in the acid etching modification solution is 16 wt%;
2) preparing carbon-based suspension: sorting the graphite waste to remove impurities, crushing the graphite waste into 180-mesh fine powder, oxidizing the fine powder into graphite oxide by using concentrated sulfuric acid, mixing the graphite oxide with water to form a mixed solution, adding 180-mesh fine aluminum powder into the mixed solution, performing ultrasonic oscillation, and obtaining carbon-based turbid liquid after the graphite oxide and the fine aluminum powder are uniformly dispersed by the ultrasonic oscillation, wherein the weight ratio of the graphite oxide to the fine aluminum powder to the water is 8: 15: 200 of a carrier;
3) and (3) crack filling and strengthening treatment: placing the etched PBO fiber obtained in the step 1) into the carbon-based suspension obtained in the step 2), slowly stirring at a rotating speed of 80r/min for 60min, taking out and rinsing after ultrasonic oscillation is finished, placing in an argon protective atmosphere for heat treatment at 650 ℃ for 4h, and obtaining the reinforced PBO fiber after the heat treatment is finished;
4) ultraviolet resistance modification: dissolving 2,4, 6-tris (2 'n-butoxyphenyl) -1,3, 5-triazine, alicyclic epoxy resin and ethylene diamine tetraacetic acid in methyl benzoate to prepare an ultraviolet aging resistant modified solution, uniformly stirring, placing the reinforced PBO fiber obtained in the step 3) in the modified solution, soaking for 15min, taking out, placing in water, ultrasonically rinsing, and drying at 100 ℃ under an argon protective atmosphere to obtain the ultraviolet aging resistant PBO fiber, wherein the use weight ratio of the 2,4, 6-tris (2' n-butoxyphenyl) -1,3, 5-triazine, alicyclic epoxy resin, ethylene diamine tetraacetic acid and methyl benzoate is 18: 10: 11: 200.
example 4
A preparation process of anti-ultraviolet aging PBO fiber comprises the following preparation steps:
1) surface etching modification of PBO fiber: dissolving polyphosphoric acid in a propionic acid solution, uniformly stirring to prepare an acid etching modification solution, placing the cleaned and dried PBO fiber in the acid etching modification solution for acid etching and soaking for 25min, dropwise adding a potassium carbonate solution until the PBO fiber is neutral after the treatment is finished, continuing to perform soaking treatment for 20min, placing the PBO fiber in water for ultrasonic rinsing after the soaking treatment is finished, and drying the PBO fiber under vacuum to obtain etched PBO fiber, wherein the concentration of polyphosphoric acid in the acid etching modification solution is 20 wt%;
2) preparing carbon-based suspension: sorting the graphite waste to remove impurities, then crushing the graphite waste into 200-mesh fine powder, oxidizing the graphite waste into graphite oxide by using concentrated nitric acid, mixing the graphite oxide with water to form a mixed solution, adding 200-mesh fine aluminum powder into the mixed solution, performing ultrasonic oscillation, and obtaining carbon-based turbid liquid after the graphite oxide and the fine aluminum powder are uniformly dispersed after the ultrasonic oscillation is performed, wherein the weight ratio of the graphite oxide to the fine aluminum powder to the water is 9: 17: 200 of a carrier;
3) and (3) crack filling and strengthening treatment: placing the etched PBO fiber obtained in the step 1) into the carbon-based suspension obtained in the step 2), slowly stirring at a rotating speed of 90r/min for 45min, taking out and rinsing after ultrasonic oscillation is finished, placing in vacuum for heat treatment at 650 ℃ for 4.5h, and obtaining the reinforced PBO fiber after the heat treatment is finished;
4) ultraviolet resistance modification: dissolving (2 '-hydroxy-3', 5 '-ditert-pentylphenyl) -5-chlorobenzotriazole, alicyclic epoxy resin and ethylene diamine tetraacetic acid in methyl benzoate to prepare an ultraviolet aging resistant modified solution, uniformly stirring, placing the reinforced PBO fiber obtained in the step 3) in the modified solution, taking out the fiber after immersion treatment for 15min, placing the fiber in water for ultrasonic rinsing, and drying at 110 ℃ under vacuum to obtain the ultraviolet aging resistant PBO fiber, wherein the using weight ratio of the (2' -hydroxy-3 ',5' -ditert-pentylphenyl) -5-chlorobenzotriazole, the alicyclic epoxy resin, the ethylene diamine tetraacetic acid and the methyl benzoate is 15: 15: 13: 200.
example 5
A preparation process of anti-ultraviolet aging PBO fiber comprises the following preparation steps:
1) surface etching modification of PBO fiber: dissolving polyphosphoric acid in a butyric acid solution, uniformly stirring to prepare an acid etching modification solution, placing the cleaned and dried PBO fiber in the acid etching modification solution for acid etching and soaking for 25min, dropwise adding a potassium bicarbonate solution until the PBO fiber tends to be neutral after the treatment is finished, continuing to soak for 25min, placing the PBO fiber in water for ultrasonic rinsing after the soaking treatment is finished, and drying the PBO fiber in a nitrogen protective atmosphere to obtain the etched PBO fiber, wherein the concentration of polyphosphoric acid in the acid etching modification solution is 19 wt%;
2) preparing carbon-based suspension: sorting the graphite waste to remove impurities, then smashing the graphite waste into fine powder of 300 meshes, utilizing potassium permanganate solution to oxidize the graphite waste into graphite oxide, mixing the graphite oxide with water to form a mixed solution, adding 300-mesh fine aluminum powder into the mixed solution and carrying out ultrasonic oscillation, obtaining carbon-based turbid liquid after the ultrasonic oscillation is carried out until the graphite oxide and the fine aluminum powder are uniformly dispersed, wherein the weight ratio of the graphite oxide to the fine aluminum powder to the water is 10: 18: 200 of a carrier;
3) and (3) crack filling and strengthening treatment: placing the etched PBO fiber obtained in the step 1) into the carbon-based suspension obtained in the step 2) for slow stirring at the rotating speed of 85r/min for 35min, taking out and rinsing after ultrasonic oscillation is finished, placing in a nitrogen protective atmosphere for heat treatment at 650 ℃ for 4.5h, and obtaining the reinforced PBO fiber after the heat treatment is finished;
4) ultraviolet resistance modification: dissolving 2- (2 '-hydroxy-3, 5' -di-tert-phenyl) -5-chlorobenzotriazole, alicyclic epoxy resin and ethylene diamine tetraacetic acid in ethyl acetate to prepare an anti-ultraviolet aging modified solution, uniformly stirring, placing the reinforced PBO fiber obtained in the step 3) in the modified solution, taking out the fiber after immersion treatment for 10min, placing the fiber in water for ultrasonic rinsing, and drying the fiber at 80 ℃ under a nitrogen protective atmosphere to obtain the anti-ultraviolet aging PBO fiber, wherein the using weight ratio of the 2- (2 '-hydroxy-3, 5' -di-tert-phenyl) -5-chlorobenzotriazole, the alicyclic epoxy resin, the ethylene diamine tetraacetic acid and the ethyl acetate is 18: 11: 11: 200.
comparative example
PBO fiber filament is manufactured by Teflon fiber technologies, Inc. of Foshan, Guangdong.
The examples 1-5 and the comparative example were tested, and the results and comparisons are shown in the following table:
in the tensile set rate test, the tensile length of the high-strength PBO fiber of the comparative example is 3% of the total length, the tensile length of the high-model PBO fiber of the comparative example is 1.5% of the total length, and the tensile lengths of the ultraviolet aging resistant PBO fibers of the examples are 15% of the total length, so that the elasticity of the ultraviolet aging resistant PBO fibers prepared in the examples 1 to 5 is obviously the same as that of the comparative example.
Claims (8)
1. The preparation process of the anti-ultraviolet aging PBO fiber is characterized by comprising the following preparation steps:
1) surface etching modification of PBO fiber: dissolving polyphosphoric acid in an organic weak acid solvent, uniformly stirring to prepare an acid etching modified solution, placing the cleaned and dried PBO fiber in the acid etching modified solution for acid etching and soaking treatment, dropwise adding a weak alkaline solution until the PBO fiber is neutral after the treatment is finished, continuing soaking treatment, placing the PBO fiber in water for ultrasonic rinsing after the soaking treatment is finished, and drying the PBO fiber in vacuum or protective atmosphere to obtain the etched PBO fiber;
wherein the acid etching soaking treatment time is 15-25 min, the soaking treatment time after the dropwise addition of the weak alkaline solution is 20-30 min, and the protective atmosphere comprises a nitrogen protective atmosphere and an inert gas protective atmosphere;
2) preparing carbon-based suspension: sorting the graphite waste to remove impurities, crushing the graphite waste into fine powder, oxidizing the fine powder into graphite oxide by using an oxidant, mixing the graphite oxide with water to form a mixed solution, adding fine aluminum powder into the mixed solution, performing ultrasonic oscillation, and obtaining a carbon-based suspension after the graphite oxide and the fine aluminum powder are uniformly dispersed by the ultrasonic oscillation;
3) and (3) crack filling and strengthening treatment: placing the etched PBO fiber obtained in the step 1) into the carbon-based suspension obtained in the step 2) for slow stirring, taking out and rinsing after the ultrasonic oscillation is finished, placing in vacuum or protective atmosphere for heat treatment, and obtaining the reinforced PBO fiber after the heat treatment is finished;
the slow stirring speed is 60-100 r/min, the time is 15-90 min, the heat treatment condition is that the heat treatment temperature is 600-700 ℃, the heat treatment time is 3-6 h, and the protective atmosphere comprises a nitrogen protective atmosphere and an inert gas protective atmosphere;
4) ultraviolet resistance modification: dissolving a light modifier, alicyclic epoxy resin and a curing agent in an organic solvent to prepare an anti-ultraviolet aging modified solution, uniformly stirring, placing the reinforced PBO fiber obtained in the step 3) in the modified solution, taking out the fiber after dipping treatment, placing the fiber in water for ultrasonic rinsing, and drying the fiber in vacuum or protective atmosphere to obtain the anti-ultraviolet aging PBO fiber.
2. The process for preparing anti-ultraviolet aging PBO fiber as claimed in claim 1, wherein the organic weak acidic solvent of step 1) comprises acetic acid, phenylacetic acid, oxalic acid, glycolic acid, propanoic acid, benzoic acid, propanoic acid, butanoic acid and phenol, and the weak alkaline solution comprises ammonia, sodium carbonate solution, sodium bicarbonate solution, potassium carbonate and potassium bicarbonate.
3. The process for preparing the anti-ultraviolet aging PBO fiber according to claim 1, wherein the oxidant in step 2) comprises oxidizing acid and potassium permanganate.
4. The preparation process of the anti-ultraviolet aging PBO fiber according to claim 1 or 3, characterized in that the graphite waste in the step 2) is sorted to remove impurities, and then is crushed into fine powder of 60-300 meshes, wherein the mesh number of the fine aluminum powder is 60-300 meshes.
5. The preparation process of the anti-ultraviolet-aging PBO fiber according to claim 3, characterized in that the weight ratio of the graphite oxide, the fine aluminum powder and the water in the step 2) is (5-10): (15-20): 200.
6. the process for preparing an anti-UV aging PBO fiber according to claim 1, wherein the light modifier of step 4) comprises phenyl o-hydroxybenzoate, 2- (2' -hydroxy-5 ' -methylphenyl) benzotriazole, 2, 4-dimethylbenzophenone, 2-methyl-4-methoxybenzophenone, 2-hydroxy-4-n-octyloxybenzophenone, 2- (2' -hydroxy-3, 5' -di-tert-phenyl) -5-chlorobenzotriazole, resorcinol monobenzoate, 2,2' -thiobis (4-tert-octylphenoloxy) nickel, tris (1,2,2,6, 6-pentamethylpiperidinyl) phosphite, 4-benzoyloxy-2, 2,6, 6-tetramethylpiperidine, 2,4, 6-tris (2 'n-butoxyphenyl) -1,3, 5-triazine, hexamethylphosphoric triamide and (2' -hydroxy-3 ',5' -ditert-pentylphenyl) -5-chlorobenzotriazole, the curing agent is ethylenediamine tetraacetic acid, and the organic solvent includes ethyl acetate, methyl phenylacetate, methyl benzoate and ethyl propionate.
7. The preparation process of the anti-ultraviolet aging PBO fiber according to claim 1 or 6, characterized in that the usage weight ratio of the light modifier, the alicyclic epoxy resin, the curing agent and the organic solvent in the step 4) is (15-20): (5-15): (8-13): 200, the dipping treatment time is 5-20 min, and the drying temperature is 80-120 ℃.
8. The process for preparing the anti-ultraviolet-aging PBO fiber according to claim 7, wherein the protective atmosphere in the step 4) comprises a nitrogen protective atmosphere and an inert gas protective atmosphere.
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| CN111088539B (en) * | 2020-01-13 | 2022-03-04 | 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 |
| 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 |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002266236A (en) * | 2001-02-27 | 2002-09-18 | Seiren Co Ltd | Processed fiber material for preventing photodeterioration |
| CN102277726A (en) * | 2011-09-02 | 2011-12-14 | 北京理工大学 | Anti-ultraviolet aging method for p-phenylene benzobisoxazole (PBO) fiber |
| CN102634976A (en) * | 2012-04-20 | 2012-08-15 | 哈尔滨工业大学 | Method for enhancing ultraviolet resistance stability of PBO (poly-p-phenylenebenzobisthiazole) fibers by depositing (POSS (polyhedral oligomeric silsesquioxane)/TiO2)n films on surfaces |
| CN102691207A (en) * | 2012-05-31 | 2012-09-26 | 华东理工大学 | Preparation method for ultraviolet resistant and damp-heat aging resistant PBO (polybenzoxazole) fiber |
| CN103014901A (en) * | 2012-12-12 | 2013-04-03 | 哈尔滨工业大学 | Preparation method of graphene/PBO (Poly-P-Phenylene Benzobisoxazazole) composite fiber |
| CN103160950A (en) * | 2011-12-12 | 2013-06-19 | 金发科技股份有限公司 | Preparation method for ultraviolet-resistant PBO fibers |
| CN103820996A (en) * | 2014-03-04 | 2014-05-28 | 哈尔滨工业大学 | Preparation method for binary grafted modified PBO fiber |
| CN105908489A (en) * | 2016-05-12 | 2016-08-31 | 哈尔滨工业大学 | Graphene nanoribbon interface-modified PBO (polyparaphenylene benzobisoxazole) fiber and preparation method thereof |
| CN107385919A (en) * | 2017-07-06 | 2017-11-24 | 国网湖南省电力公司带电作业中心 | The coating material being modified for pbo fiber surface；Surface is modified pbo fiber, preparation and its application |
| CN107620204A (en) * | 2017-11-09 | 2018-01-23 | 成都新晨新材科技有限公司 | A kind of pbo fiber of ultraviolet resistance and preparation method thereof |
-
2018
- 2018-04-25 CN CN201810378821.7A patent/CN108486861B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002266236A (en) * | 2001-02-27 | 2002-09-18 | Seiren Co Ltd | Processed fiber material for preventing photodeterioration |
| CN102277726A (en) * | 2011-09-02 | 2011-12-14 | 北京理工大学 | Anti-ultraviolet aging method for p-phenylene benzobisoxazole (PBO) fiber |
| CN103160950A (en) * | 2011-12-12 | 2013-06-19 | 金发科技股份有限公司 | Preparation method for ultraviolet-resistant PBO fibers |
| CN102634976A (en) * | 2012-04-20 | 2012-08-15 | 哈尔滨工业大学 | Method for enhancing ultraviolet resistance stability of PBO (poly-p-phenylenebenzobisthiazole) fibers by depositing (POSS (polyhedral oligomeric silsesquioxane)/TiO2)n films on surfaces |
| CN102691207A (en) * | 2012-05-31 | 2012-09-26 | 华东理工大学 | Preparation method for ultraviolet resistant and damp-heat aging resistant PBO (polybenzoxazole) fiber |
| CN103014901A (en) * | 2012-12-12 | 2013-04-03 | 哈尔滨工业大学 | Preparation method of graphene/PBO (Poly-P-Phenylene Benzobisoxazazole) composite fiber |
| CN103820996A (en) * | 2014-03-04 | 2014-05-28 | 哈尔滨工业大学 | Preparation method for binary grafted modified PBO fiber |
| CN105908489A (en) * | 2016-05-12 | 2016-08-31 | 哈尔滨工业大学 | Graphene nanoribbon interface-modified PBO (polyparaphenylene benzobisoxazole) fiber and preparation method thereof |
| CN107385919A (en) * | 2017-07-06 | 2017-11-24 | 国网湖南省电力公司带电作业中心 | The coating material being modified for pbo fiber surface；Surface is modified pbo fiber, preparation and its application |
| CN107620204A (en) * | 2017-11-09 | 2018-01-23 | 成都新晨新材科技有限公司 | A kind of pbo fiber of ultraviolet resistance and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 聚对苯撑苯并双噁唑纤维改性技术的研究进展;卢珊珊等;《合成纤维工业》;20180215;第41卷(第1期);47-52 * |
| 高性能PBO纤维表面改性及抗紫外光性能研究;李芝华等;《功能材料》;20180130;第49卷(第1期);01112-01116 * |
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