CN116556046A - Method for simply and conveniently preparing high-temperature-resistant antioxidant polyphenylene sulfide fibers and product thereof - Google Patents
Method for simply and conveniently preparing high-temperature-resistant antioxidant polyphenylene sulfide fibers and product thereof Download PDFInfo
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- CN116556046A CN116556046A CN202310620996.5A CN202310620996A CN116556046A CN 116556046 A CN116556046 A CN 116556046A CN 202310620996 A CN202310620996 A CN 202310620996A CN 116556046 A CN116556046 A CN 116556046A
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- 239000000835 fiber Substances 0.000 title claims abstract description 80
- 239000004734 Polyphenylene sulfide Substances 0.000 title claims abstract description 63
- 229920000069 polyphenylene sulfide Polymers 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000003963 antioxidant agent Substances 0.000 title claims abstract description 21
- 230000003078 antioxidant effect Effects 0.000 title claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 16
- 230000003647 oxidation Effects 0.000 claims abstract description 15
- 238000011282 treatment Methods 0.000 claims abstract description 13
- 239000007800 oxidant agent Substances 0.000 claims abstract description 10
- 230000001590 oxidative effect Effects 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 239000007791 liquid phase Substances 0.000 claims abstract description 9
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 239000003054 catalyst Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-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 6
- KFSLWBXXFJQRDL-UHFFFAOYSA-N Peracetic acid Chemical compound CC(=O)OO KFSLWBXXFJQRDL-UHFFFAOYSA-N 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- 239000004115 Sodium Silicate Substances 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 4
- 239000004327 boric acid Substances 0.000 claims description 4
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 4
- JQWHASGSAFIOCM-UHFFFAOYSA-M sodium periodate Chemical compound [Na+].[O-]I(=O)(=O)=O JQWHASGSAFIOCM-UHFFFAOYSA-M 0.000 claims description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 4
- 239000012286 potassium permanganate Substances 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- 239000005708 Sodium hypochlorite Substances 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- QGAVSDVURUSLQK-UHFFFAOYSA-N ammonium heptamolybdate Chemical compound N.N.N.N.N.N.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.[Mo].[Mo].[Mo].[Mo].[Mo].[Mo].[Mo] QGAVSDVURUSLQK-UHFFFAOYSA-N 0.000 claims description 2
- VTIIJXUACCWYHX-UHFFFAOYSA-L disodium;carboxylatooxy carbonate Chemical compound [Na+].[Na+].[O-]C(=O)OOC([O-])=O VTIIJXUACCWYHX-UHFFFAOYSA-L 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- 159000000003 magnesium salts Chemical class 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- -1 phthalic acid peroxide Chemical class 0.000 claims description 2
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 2
- 229940045872 sodium percarbonate Drugs 0.000 claims description 2
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 2
- QBVXKDJEZKEASM-UHFFFAOYSA-M tetraoctylammonium bromide Chemical compound [Br-].CCCCCCCC[N+](CCCCCCCC)(CCCCCCCC)CCCCCCCC QBVXKDJEZKEASM-UHFFFAOYSA-M 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N o-dicarboxybenzene Natural products OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims 1
- 239000003002 pH adjusting agent Substances 0.000 claims 1
- 230000014759 maintenance of location Effects 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 6
- 238000005260 corrosion Methods 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 5
- 230000007797 corrosion Effects 0.000 abstract description 4
- 238000012360 testing method Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 239000012295 chemical reaction liquid Substances 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000005543 nano-size silicon particle Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000000643 oven drying Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-N benzene-dicarboxylic acid Natural products OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 150000003457 sulfones Chemical class 0.000 description 1
- 150000003462 sulfoxides Chemical class 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 238000012795 verification 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
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with hydrogen peroxide or peroxides of metals; with persulfuric, permanganic, pernitric, percarbonic 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
- D06M11/77—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 silicon or compounds thereof
- D06M11/79—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 silicon or compounds thereof with silicon dioxide, silicic 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
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/188—Monocarboxylic acids; Anhydrides, halides or salts thereof
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a simple and convenient method for preparing high-temperature-resistant antioxidant polyphenylene sulfide fibers and products thereof, and belongs to the technical field of modified polyphenylene sulfide fibers. The invention evenly mixes the solvent, the oxidant, the auxiliary agent, the catalyst and the pH regulator to obtain the liquid phase reaction treating agent, the pH is kept between 2 and 6, and the temperature is kept between 20 and 50 ℃; and then immersing the polyphenylene sulfide fiber into the liquid phase reaction treating agent for oxidation treatment, and washing and drying to obtain the high-temperature-resistant antioxidant polyphenylene sulfide fiber. The high-temperature-resistant antioxidant polyphenylene sulfide fiber prepared by the method has the advantages of simple preparation process, good oxidation resistance, chemical corrosion resistance and high-temperature strength retention rate, and has important application value, and the product has the phenomena of no molten drop and molten shrinkage.
Description
Technical Field
The invention belongs to the technical field of modified polyphenylene sulfide fibers, and particularly relates to a method for simply and conveniently preparing high-temperature-resistant antioxidant polyphenylene sulfide fibers and a product thereof.
Background
Polyphenylene Sulfide (PPS) fibers are widely used in industrial dust removal filter materials and thermosetting liquid separation materials, such as flue gas dust removal filters in power plants, steel plants, cement plants, due to their good chemical resistance, thermal stability, and excellent mechanical properties. However, because the bond energy between benzene ring and sulfur in PPS macromolecule is lower, it is easy to oxidize and break under high temperature and high oxygen condition, and the material is brittle and easy to break; in addition, under the strong corrosion working condition, the fiber cannot resist the corrosion of strong oxidants such as concentrated sulfuric acid, nitric acid and the like, so that the structure of the fiber is damaged, the strength is reduced, the service life of a product is seriously influenced, and the problems limit the application of the fiber in the high-oxygen and high-corrosion environment. With the development of high-technology research and application, higher requirements are put on the performance of high-temperature resistant materials.
In recent years, aiming at the problems that PPS fibers have low service life and are not oxidation-resistant at high temperature, scientific researchers carry out modification related treatment on the PPS fibers, and the prepared modified PPS fibers have better high-temperature resistance, corrosion resistance, oxidation resistance and other excellent performances, have good fiber stability, are materials which are urgently needed under extreme working conditions, can be widely applied to the fields of high-temperature filtration, protective materials, organic waste liquid separation and the like, and have huge market demands in the future.
In the prior art, as disclosed in the publication No. CN105113209A, the patent name is a preparation method of PPS fiber with self-extinguishing property and no molten drop, the preparation method takes polyphenylene sulfide fiber as a raw material, and prepares the PPS fiber with oxidation resistance and no molten drop through chemical modification, but a large amount of organic solvent is used in the preparation process reaction liquid, and the literature shows that the mechanical property of the fiber prepared by oxidation is easily destroyed at high temperature. The method adopts a silane coupling agent to load an antioxidant on the surface of nano silicon dioxide through a chemical grafting reaction, and then introduces polyphenylene sulfide and modified nano silicon dioxide into a screw extruder for melt extrusion to obtain PPS fibers, the method improves the high-temperature strength retention rate of the PPS fibers, improves the oxidation resistance of the PPS fibers to a certain extent, but fails to solve the problem of PPS fiber molten drop, and improves the oxidation effect. Therefore, a new modification means is needed to be developed, so that PPS fibers are endowed with higher oxidation resistance, the problems of shrinkage and molten drop are solved, and the high-temperature strength retention rate is improved.
Disclosure of Invention
In order to solve the problems of the prior art, the invention provides a simple and convenient method for preparing high-temperature-resistant antioxidant polyphenylene sulfide fibers and products thereof, which effectively solve the problems of low service life, no oxidization resistance and melt shrinkage and melt dripping of the polyphenylene sulfide fibers at high temperature, improve the high-temperature strength retention rate of the fibers, and the preparation method has the advantages of simple process, mild reaction condition, low energy consumption, cheap and easily available commercial raw materials, low cost, environment friendliness, reduced environmental pollution and suitability for further industrialized production and application.
In order to achieve the above object, the present invention provides the following solutions:
the invention aims at providing a simple and convenient method for preparing high-temperature-resistant antioxidant polyphenylene sulfide fibers, which comprises the following steps:
(1) Preparing a liquid phase reaction treating agent: uniformly stirring and mixing a solvent, an oxidant, an auxiliary agent, a catalyst and a pH regulator, keeping the pH at 2-6 and keeping the temperature at 20-50 ℃;
(2) And immersing the polyphenylene sulfide fibers into the liquid phase reaction treating agent, continuously stirring, carrying out oxidation treatment, washing and drying to obtain the high-temperature-resistant antioxidant polyphenylene sulfide fibers.
Further, the solvent in the step (1) is water, no organic solvent is needed, and the mass ratio of the solvent to the whole reaction solution system is 10-50%.
Further, the oxidant in the step (1) is obtained by mixing one or more of hydrogen peroxide, sodium hypochlorite, sodium percarbonate, sodium periodate, potassium permanganate, peracetic acid and magnesium salt of terephthalic acid peroxide, and the oxidant accounts for 20-70% of the mass ratio of the whole reaction solution system.
Further, the auxiliary agent in the step (1) is obtained by mixing one or more of tetraoctyl ammonium bromide, ethanol, acetic acid, sodium silicate, ammonium titanate and aluminum oxide, and the auxiliary agent accounts for 2-30% of the mass ratio of the whole reaction solution system.
Further, the catalyst in the step (1) is any one of ferric chloride, boric acid, sodium tungstate, ammonium heptamolybdate, titanium dioxide, vanadium pentoxide and macroporous resin-15, and accounts for 0.1-2% of the mass ratio of the whole reaction solution system.
Further, the pH regulator in the step (1) is any one of oxalic acid, citric acid and sulfuric acid, and the pH value of the liquid phase reaction treating agent is regulated to be 2-6.
Further, the titer of the polyphenylene sulfide fiber in the step (2) is 1.11-6.66 dtex or the fiber diameter is 100 nm-30 mu m, and the length is 38-76 mm; the temperature of the oxidation treatment is 20-50 ℃ and the time is 30-90 min.
The second purpose of the invention is to provide the high-temperature-resistant antioxidant polyphenylene sulfide fiber prepared by the method for simply preparing the high-temperature-resistant antioxidant polyphenylene sulfide fiber.
The invention has the beneficial effects that:
according to the invention, the polyphenylene sulfide fiber is used as a production raw material, the process is simple to operate, the flow is short, the energy consumption is low, the modified polyphenylene sulfide fiber can be obtained through simple treatment of the liquid phase reaction treatment agent, and the method is environment-friendly and is beneficial to industrial production; the performance is excellent, the problem of molten drops of polyphenylene sulfide fibers is solved by selectively oxidizing unsaturated thioether bonds into sulfone or sulfoxide, the oxidation resistance is improved, the mechanical properties of the fibers are greatly improved by the action of silicon, and the high-temperature strength retention rate is good. The prepared modified polyphenylene sulfide fiber not only has great application in the field of high-temperature filtration, but also has good application prospect in the field of heat-resistant and acid-resistant clothing.
Drawings
FIG. 1 shows the results of differential thermal analyzer (DSC) test of polyphenylene sulfide fibers with the modified polyphenylene sulfide fibers obtained in examples 1-2.
Detailed Description
The present invention will be described in further detail with reference to examples for better understanding of the technical scheme of the present invention to those skilled in the art.
Example 1
(1) 100 parts of water, 150 parts of potassium permanganate, 50 parts of acetic acid and 10 parts of sodium silicate are placed in a reaction kettle, 2 parts of boric acid is added, the pH of the mixed solution is adjusted to 3 by dilute sulfuric acid, and the mixed solution is stirred for 30min at 30 ℃;
(2) Reflux treatment is carried out on the reaction process, a reflux device switch of the reaction vessel is opened, cooling water is introduced, and the temperature of the reaction liquid in the reaction vessel is controlled to be 30 ℃;
(3) Adding a certain amount of polyphenylene sulfide fibers with the thickness of 2.22dtex and 51mm into a reaction container, keeping the temperature unchanged, and continuously reacting for 40 minutes, wherein the molar ratio of the polyphenylene sulfide fibers to the oxidant is 1:2; after the reaction is finished, recovering the treatment liquid, adding water, stirring and flushing, spin-drying the fiber in a centrifuge, and then drying the water in a dryer to obtain the PPS-1 fiber.
Example 2
(1) 100 parts of water and 100 parts of H 2 O 2 Placing 100 parts of peracetic acid and 10 parts of sodium silicate into a reaction kettle, adding 2 parts of boric acid, adjusting the pH of the mixed solution to 3 by using dilute sulfuric acid, and stirring for 30min at 30 ℃;
(2) Reflux treatment is carried out on the reaction process, a reflux device switch of the reaction vessel is opened, cooling water is introduced, and the temperature of the reaction liquid in the reaction vessel is controlled to be 30 ℃;
(3) Adding a certain amount of polyphenylene sulfide fibers with the thickness of 2.22dtex and 51mm into a reaction container, keeping the temperature unchanged, and continuously reacting for 40 minutes, wherein the molar ratio of the polyphenylene sulfide fibers to the oxidant is 1:3; after the reaction is finished, recovering the treatment liquid, adding water, stirring and flushing, spin-drying the fiber in a centrifuge, and then drying the water in a dryer to obtain the PPS-2 fiber.
Effect verification
1. The fiber products of examples 1 and 2 have excellent stability, aging for 168 hours at 230℃in air, substantially unchanged strength, and dimensional stability and can be used for a long period of time at 230 ℃.
2. The PPS fibers and the modified PPS fibers obtained in examples 1-2 were subjected to test analysis using a differential thermal analyzer (DSC), and the results are shown in FIG. 1. As can be seen from the DSC graph, the PPS fibers have a melting point of 279.2 ℃whereas the modified PPS fibers of the examples have no melting point.
3. The PPS fibers were subjected to performance testing with the modified PPS fibers prepared in examples 1 and 2 under the following test conditions:
(1) And (3) testing mechanical properties of the fiber: the test was carried out using GB/T14337-2008 method for testing tensile properties of chemical fibers and staple fibers.
(2) High temperature resistance test: the fibers were placed in an oven at 230℃and after a 7-day stand treatment, the strength change was measured.
(3) H resistance 2 SO 4 Performance test: soaking the fiber in 98% thick H 2 SO 4 Soaking in solution at 85deg.C for 24 hr, washing with distilled water, oven drying, and testing the change of its strength.
(4) HNO resistance 3 Performance test: soaking the fiber in HNO with mass fraction of 60% 3 Soaking in solution at 85deg.C for 24 hr, washing with distilled water, oven drying, and testing the change of its strength.
The performance comparison of the raw PPS fibers with the modified PPS fibers of examples 1 and 2 is shown in table 1:
TABLE 1
Experiments prove that the modified PPS fiber prepared by the invention has the phenomena of self-extinguishment, no molten drop and melt shrinkage, good chemical resistance and high-temperature strength retention rate. In addition, the preparation method has mild reaction conditions, simple operation, environmental friendliness and less pollution.
The above embodiments are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope defined by the claims of the present invention without departing from the design spirit of the present invention.
Claims (8)
1. The method for simply and conveniently preparing the high-temperature-resistant antioxidant polyphenylene sulfide fiber is characterized by comprising the following steps of:
(1) Preparing a liquid phase reaction treating agent: uniformly stirring and mixing a solvent, an oxidant, an auxiliary agent, a catalyst and a pH regulator, keeping the pH at 2-6 and keeping the temperature at 20-50 ℃;
(2) And immersing the polyphenylene sulfide fiber into the liquid phase reaction treating agent for oxidation treatment, and washing and drying to obtain the high-temperature-resistant and antioxidant polyphenylene sulfide fiber.
2. The method for simply and conveniently preparing the high-temperature-resistant antioxidant polyphenylene sulfide fiber according to claim 1, wherein the solvent in the step (1) is water, and the solvent accounts for 10-50% of the mass ratio of the whole reaction solution system.
3. The method for simply and conveniently preparing high-temperature-resistant antioxidant polyphenylene sulfide fibers according to claim 1, wherein the oxidant in the step (1) is obtained by mixing one or more of hydrogen peroxide, sodium hypochlorite, sodium percarbonate, sodium periodate, potassium permanganate, peracetic acid and magnesium salt of phthalic acid peroxide, and the oxidant accounts for 20-70% of the mass ratio of the whole reaction solution system.
4. The method for simply and conveniently preparing the high-temperature-resistant antioxidant polyphenylene sulfide fiber according to claim 1, wherein the auxiliary agent in the step (1) is obtained by mixing one or more of tetraoctyl ammonium bromide, ethanol, acetic acid, sodium silicate, ammonium titanate and aluminum oxide, and the auxiliary agent accounts for 2-30% of the mass ratio of the whole reaction solution system.
5. The method for simply and conveniently preparing the high-temperature-resistant antioxidant polyphenylene sulfide fiber according to claim 1, wherein the catalyst in the step (1) is any one of ferric chloride, boric acid, sodium tungstate, ammonium heptamolybdate, titanium dioxide, vanadium pentoxide and macroporous resin-15, and the mass ratio of the catalyst to the whole reaction solution system is 0.1-2%.
6. The method for preparing high temperature resistant and oxidation resistant polyphenylene sulfide fiber according to claim 1, wherein the pH adjuster in step (1) is any one of oxalic acid, citric acid and sulfuric acid, and the pH of the liquid phase reaction treating agent is adjusted to 2-6.
7. The method for simply and conveniently preparing high-temperature-resistant antioxidant polyphenylene sulfide fibers according to claim 1, wherein the titer of the polyphenylene sulfide fibers in the step (2) is 1.11-6.66 dtex or the fiber diameter is 100 nm-30 μm and the length is 38-76 mm; the temperature of the oxidation treatment is 20-50 ℃ and the time is 30-90 min.
8. A high temperature resistant and antioxidant polyphenylene sulfide fiber produced by the method for simply and conveniently producing a high temperature resistant and antioxidant polyphenylene sulfide fiber according to any one of claims 1 to 7.
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| CN101537280A (en) * | 2009-04-07 | 2009-09-23 | 厦门三维丝环保股份有限公司 | Preparation method of nano-particle modified polyphenyl thioether filter material |
| CN103225124A (en) * | 2013-04-24 | 2013-07-31 | 浙江东华纤维制造有限公司 | Preparation method of antioxidant modified polyphenylene sulfide fiber |
| CN105113209A (en) * | 2015-09-29 | 2015-12-02 | 苏州金泉新材料股份有限公司 | Preparation method of PPS fibers with self-extinguishment and free of molten drops |
| CN112080930A (en) * | 2020-09-24 | 2020-12-15 | 福州大学 | Method for rapidly preparing polyphenylene sulfone sulfoxide fiber through liquid-phase oxidation at normal temperature and normal pressure |
| CN116122043A (en) * | 2023-03-30 | 2023-05-16 | 福州大学 | Method for preparing PPSSO fibers by in-situ modification of PPS fibers |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101537280A (en) * | 2009-04-07 | 2009-09-23 | 厦门三维丝环保股份有限公司 | Preparation method of nano-particle modified polyphenyl thioether filter material |
| CN103225124A (en) * | 2013-04-24 | 2013-07-31 | 浙江东华纤维制造有限公司 | Preparation method of antioxidant modified polyphenylene sulfide fiber |
| CN105113209A (en) * | 2015-09-29 | 2015-12-02 | 苏州金泉新材料股份有限公司 | Preparation method of PPS fibers with self-extinguishment and free of molten drops |
| CN112080930A (en) * | 2020-09-24 | 2020-12-15 | 福州大学 | Method for rapidly preparing polyphenylene sulfone sulfoxide fiber through liquid-phase oxidation at normal temperature and normal pressure |
| CN116122043A (en) * | 2023-03-30 | 2023-05-16 | 福州大学 | Method for preparing PPSSO fibers by in-situ modification of PPS fibers |
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