CN112647299A - Preparation method of antioxidant hydrophobic polyphenylene sulfide fiber - Google Patents
Preparation method of antioxidant hydrophobic polyphenylene sulfide fiber Download PDFInfo
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- CN112647299A CN112647299A CN202011276719.XA CN202011276719A CN112647299A CN 112647299 A CN112647299 A CN 112647299A CN 202011276719 A CN202011276719 A CN 202011276719A CN 112647299 A CN112647299 A CN 112647299A
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- 239000000835 fiber Substances 0.000 title claims abstract description 72
- 239000004734 Polyphenylene sulfide Substances 0.000 title claims abstract description 66
- 229920000069 polyphenylene sulfide Polymers 0.000 title claims abstract description 66
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000003963 antioxidant agent Substances 0.000 title description 13
- 230000003078 antioxidant effect Effects 0.000 title description 13
- 238000002156 mixing Methods 0.000 claims abstract description 101
- 230000003647 oxidation Effects 0.000 claims abstract description 20
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims description 103
- 239000003795 chemical substances by application Substances 0.000 claims description 76
- 239000000853 adhesive Substances 0.000 claims description 37
- 230000001070 adhesive effect Effects 0.000 claims description 37
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 36
- 239000000203 mixture Substances 0.000 claims description 31
- -1 polytetrafluoroethylene Polymers 0.000 claims description 21
- 239000005995 Aluminium silicate Substances 0.000 claims description 20
- SPSPIUSUWPLVKD-UHFFFAOYSA-N 2,3-dibutyl-6-methylphenol Chemical compound CCCCC1=CC=C(C)C(O)=C1CCCC SPSPIUSUWPLVKD-UHFFFAOYSA-N 0.000 claims description 18
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 18
- 235000010354 butylated hydroxytoluene Nutrition 0.000 claims description 18
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 18
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 18
- 229920002545 silicone oil Polymers 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims description 17
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 claims description 17
- 235000002949 phytic acid Nutrition 0.000 claims description 17
- 229940068041 phytic acid Drugs 0.000 claims description 17
- 239000000467 phytic acid Substances 0.000 claims description 17
- IBLKWZIFZMJLFL-UHFFFAOYSA-N 1-phenoxypropan-2-ol Chemical compound CC(O)COC1=CC=CC=C1 IBLKWZIFZMJLFL-UHFFFAOYSA-N 0.000 claims description 16
- QCDWFXQBSFUVSP-UHFFFAOYSA-N 2-phenoxyethanol Chemical compound OCCOC1=CC=CC=C1 QCDWFXQBSFUVSP-UHFFFAOYSA-N 0.000 claims description 16
- 235000012211 aluminium silicate Nutrition 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 16
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 16
- CZBZUDVBLSSABA-UHFFFAOYSA-N butylated hydroxyanisole Chemical compound COC1=CC=C(O)C(C(C)(C)C)=C1.COC1=CC=C(O)C=C1C(C)(C)C CZBZUDVBLSSABA-UHFFFAOYSA-N 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 8
- 239000000347 magnesium hydroxide Substances 0.000 claims description 6
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 4
- MRBKEAMVRSLQPH-UHFFFAOYSA-N 3-tert-butyl-4-hydroxyanisole Chemical compound COC1=CC=C(O)C(C(C)(C)C)=C1 MRBKEAMVRSLQPH-UHFFFAOYSA-N 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 230000007547 defect Effects 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 description 53
- 230000000052 comparative effect Effects 0.000 description 23
- 239000000047 product Substances 0.000 description 18
- IJVRPNIWWODHHA-UHFFFAOYSA-N 2-cyanoprop-2-enoic acid Chemical group OC(=O)C(=C)C#N IJVRPNIWWODHHA-UHFFFAOYSA-N 0.000 description 14
- TVJPBVNWVPUZBM-UHFFFAOYSA-N [diacetyloxy(methyl)silyl] acetate Chemical group CC(=O)O[Si](C)(OC(C)=O)OC(C)=O TVJPBVNWVPUZBM-UHFFFAOYSA-N 0.000 description 14
- 235000004279 alanine Nutrition 0.000 description 13
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 12
- KFYRJJBUHYILSO-YFKPBYRVSA-N (2s)-2-amino-3-dimethylarsanylsulfanyl-3-methylbutanoic acid Chemical compound C[As](C)SC(C)(C)[C@@H](N)C(O)=O KFYRJJBUHYILSO-YFKPBYRVSA-N 0.000 description 11
- QNAYBMKLOCPYGJ-REOHCLBHSA-N L-alanine Chemical compound C[C@H](N)C(O)=O QNAYBMKLOCPYGJ-REOHCLBHSA-N 0.000 description 10
- 125000002147 dimethylamino group Chemical group [H]C([H])([H])N(*)C([H])([H])[H] 0.000 description 10
- 239000000463 material Substances 0.000 description 10
- 239000002131 composite material Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 239000002657 fibrous material Substances 0.000 description 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- DJBWYWDKHVKANE-BYPYZUCNSA-N (2s)-2-(2,2-dimethylhydrazinyl)propanoic acid Chemical group OC(=O)[C@H](C)NN(C)C DJBWYWDKHVKANE-BYPYZUCNSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229920006389 polyphenyl polymer Polymers 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
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- 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
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/244—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons
- D06M15/256—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons containing fluorine
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- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
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- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/45—Oxides or hydroxides of elements of Groups 3 or 13 of the Periodic Table; Aluminates
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- 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
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- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/152—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen having a hydroxy group bound to a carbon atom of a six-membered aromatic ring
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Abstract
The invention discloses a preparation method of an oxidation-resistant hydrophobic polyphenylene sulfide fiber, which comprises the following steps: blending 1, blending 2, blending 3, blending 4 and preparing fibers. The invention provides a preparation method of polyphenylene sulfide fiber with oxidation resistance and hydrophobicity, which overcomes the defects that the conventional local polyphenylene sulfide fiber only has flame retardance and heat resistance and has short service life.
Description
Technical Field
The invention relates to the technical field of composite material manufacturing, in particular to a preparation method of antioxidant hydrophobic polyphenylene sulfide fibers.
Background
Polyphenylene sulfide fibers, also known as PPS fibers. Is prepared from polyphenyl thioether through fusing and spinning. The polyphenylene sulfide fiber has good heat resistance, is mainly used as a high-temperature filter fabric, and has the tolerance temperature of 190 ℃. The fiber also has excellent chemical and hydrolytic resistance, as well as flame retardant properties. Can be used as flame-retardant fabric, household decorative fabric, flue gas filter material, etc. Although polyphenylene sulfide fibers have the advantages of heat resistance, flame retardance and the like, disulfide bond properties on polyphenylene sulfide macromolecules are greatly influenced, and the thermal stability and mechanical properties of the fibers are deteriorated. Furthermore, sulfur on fiber macromolecules is easy to change deeply, and thermal oxidation degradation or oxidative crosslinking can be caused as a result, so that the service life of the material is influenced. Most of the materials used at present are single materials, and have no oxidation resistance and hydrophobicity effects.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made in view of the above and/or other problems occurring in the prior art polyphenylene sulfide products.
Therefore, one of the purposes of the present invention is to overcome the defects of the existing polyphenylene sulfide products and provide a preparation method of an oxidation-resistant hydrophobic polyphenylene sulfide fiber.
To solve the above technical problem, according to one aspect of the present invention, the present invention provides the following technical solutions: a preparation method of an oxidation-resistant hydrophobic polyphenylene sulfide fiber comprises the following steps,
blending 1: mixing polytetrafluoroethylene, silicone oil and solvent, and stirring to mix them fully;
blending 2: adding nano-magnesium hydroxide and nano-kaolin into the completely mixed solution, blending and uniformly mixing;
blending 3: adding butyl hydroxy anisol, dibutyl hydroxy toluene and phytic acid into the completely mixed solution, and stirring to fully mix the components;
blending 4: finally, adding the silane coupling agent, the adhesive, the curing agent and the film forming agent into the fully mixed solution, and stirring to completely mix the silane coupling agent, the adhesive, the curing agent and the film forming agent to obtain a mixture;
preparing fibers: adding polyphenylene sulfide fiber into the obtained mixture, stirring and mixing completely, taking out and drying to obtain the finished product.
As a preferable scheme of the preparation method of the antioxidant hydrophobic polyphenylene sulfide fiber, the solvent in the blending 1 is one of water and absolute ethyl alcohol.
As a preferable scheme of the preparation method of the antioxidant hydrophobic polyphenylene sulfide fiber, the raw materials adopted in the preparation of the fiber are as follows by mass ratio: polyphenylene sulfide fiber: polytetrafluoroethylene: silicone oil: nano-scale magnesium hydroxide: nano-grade kaolin: butyl hydroxyanisole: dibutylhydroxytoluene: phytic acid: silane coupling agent: adhesive: curing agent: film forming agent: 40-55% of solvent: 10-15: 3-8: 6-9: 6-7: 3-8: 5-6: 3-4: 4-8: 1-2: 5-6: 3-5: 80-110.
As a preferable scheme of the preparation method of the antioxidant hydrophobic polyphenylene sulfide fiber, the raw materials adopted in the preparation of the fiber are as follows by mass ratio: polyphenylene sulfide fiber: polytetrafluoroethylene: silicone oil: nano-scale magnesium hydroxide: nano-grade kaolin: butyl hydroxyanisole: dibutylhydroxytoluene: phytic acid: silane coupling agent: adhesive: curing agent: film forming agent: solvent 50: 13: 12: 8: 7: 6: 6: 4: 7: 2: 6: 4: 100.
as a preferable scheme of the preparation method of the antioxidant hydrophobic polyphenylene sulfide fiber, the film-forming agent is one or more of N-methyl pyrrolidone, ethylene glycol phenyl ether and propylene glycol phenyl ether.
As a preferable scheme of the preparation method of the antioxidant hydrophobic polyphenylene sulfide fiber, the rotation speed of stirring in the blending 1, the blending 2, the blending 3 and the blending 4 is 30-60 r/min, and the stirring time is 10-20 min.
As a preferable scheme of the preparation method of the antioxidant hydrophobic polyphenylene sulfide fiber, the stirring speed in the blending 1 is 45r/min, and the stirring time is 20 min.
As a preferable scheme of the preparation method of the antioxidant hydrophobic polyphenylene sulfide fiber, the stirring speed in the blending 2 is 45r/min, and the stirring time is 20 min.
As a preferable scheme of the preparation method of the antioxidant hydrophobic polyphenylene sulfide fiber, the stirring speed in the blending 3 is 45r/min, and the stirring time is 20 min.
As a preferable scheme of the preparation method of the antioxidant hydrophobic polyphenylene sulfide fiber, the rotation speed of stirring in the blending 4 is 45r/min, and the stirring time is 20 min.
The invention provides a novel polyphenylene sulfide fiber material with polyphenylene sulfide fiber as a base material, the novel polyphenylene sulfide fiber prepared by compounding a plurality of raw materials improves the defect that the conventional polyphenylene sulfide fiber only has heat resistance and flame retardance, the prepared novel polyphenylene sulfide fiber also has good oxidation resistance and hydrophobicity, the service life of the material is prolonged, and the prepared oxidation resistance and hydrophobicity polyphenylene sulfide fiber is nontoxic and harmless, has good effect and is a novel material with better use prospect and economic value.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, specific embodiments thereof are described in detail below with reference to examples of the specification.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1
Adding 10 parts of polytetrafluoroethylene, 9 parts of silicone oil and 80 parts of water into a reaction kettle, blending at 25 ℃, stirring at 45r/min for 20min to be completely mixed, adding 5 parts of nano-scale aluminum hydroxide and 6 parts of nano-scale kaolin into the reaction kettle, blending at 25 ℃, stirring at 45r/min for 20min to be completely mixed, then adding 3 parts of butyl hydroxy anisole, 5 parts of dibutyl hydroxy toluene and 3 parts of phytic acid into the reaction kettle, stirring at 45r/min for 20min at 25 ℃, then adding 4 parts of silane coupling agent, 1 part of adhesive, 5 parts of curing agent and 2 parts of film forming agent into the reaction kettle, stirring at 25 ℃ and 45r/min for 20min, wherein the silane coupling agent is methyl triacetoxy silane, the adhesive is alpha-cyanoacrylate, the curing agent is dimethylamino alanine DMAPA, the film forming agent is prepared by mixing N-methyl pyrrolidone, ethylene glycol phenyl ether and propylene glycol phenyl ether according to the volume ratio of 1:1:1, stirring the obtained mixture and 40 parts of polyphenylene sulfide fiber according to the volume ratio of 45r/min for 3-4 h, taking out and drying the finished product.
Example 2
Adding 11 parts of polytetrafluoroethylene, 10 parts of silicone oil and 90 parts of water into a reaction kettle, blending at 25 ℃, stirring at 45r/min for 20min to be completely mixed, adding 6 parts of nano-scale aluminum hydroxide and 6 parts of nano-scale kaolin into the reaction kettle, blending at 25 ℃, stirring at 45r/min for 20min to be completely mixed, adding 4 parts of butyl hydroxy anisole, 5 parts of dibutyl hydroxy toluene and 3 parts of phytic acid into the reaction kettle, stirring at 45r/min for 20min at 25 ℃, adding 6 parts of silane coupling agent, 1 part of adhesive, 5 parts of curing agent and 2 parts of film forming agent into the reaction kettle, stirring at 25 ℃ and 45r/min for 20min, wherein the silane coupling agent is methyl triacetoxy silane, the adhesive is alpha-cyanoacrylate, the curing agent is dimethylamino alanine DMAPA, the film forming agent is prepared by mixing N-methyl pyrrolidone, ethylene glycol phenyl ether and propylene glycol phenyl ether according to the volume ratio of 1:1:1, stirring the obtained mixture and 45 parts of polyphenylene sulfide fiber according to the volume ratio of 45r/min for 3-4 h, taking out and drying the finished product.
Example 3
Adding 13 parts of polytetrafluoroethylene, 13 parts of silicone oil and 100 parts of water into a reaction kettle, mixing under the condition of 25 ℃, stirring for 20min at 45r/min, completely mixing, adding 8 parts of nanoscale aluminum hydroxide and 7 parts of nanoscale kaolin into the reaction kettle, mixing under the condition of 25 ℃, stirring for 20min at 45r/min, completely mixing, then adding 6 parts of butyl hydroxy anisole, 6 parts of dibutyl hydroxy toluene and 4 parts of phytic acid into the reaction kettle, stirring for 20min at 45r/min under the condition of 25 ℃, then adding 7 parts of silane coupling agent, 2 parts of adhesive, 6 parts of curing agent and 4 parts of film forming agent into the reaction kettle, stirring for 20min at the rotating speed of 45r/min under the condition of 25 ℃, wherein the silane coupling agent is methyl triacetoxy silane, the adhesive is alpha-cyanoacrylate, the curing agent is dimethylamino alanine PA DMA, the film forming agent is prepared by mixing N-methyl pyrrolidone, ethylene glycol phenyl ether and propylene glycol phenyl ether according to the volume ratio of 1:1:1, stirring the obtained mixture and 50 parts of polyphenylene sulfide fiber according to the volume ratio of 45r/min for 3-4 h, taking out and drying the finished product.
Example 4
Adding 15 parts of polytetrafluoroethylene, 13 parts of silicone oil and 110 parts of water into a reaction kettle, mixing under the condition of 25 ℃, stirring for 20min at 45r/min, completely mixing, adding 9 parts of nanoscale aluminum hydroxide and 7 parts of nanoscale kaolin into the reaction kettle, mixing under the condition of 25 ℃, stirring for 20min at 45r/min, completely mixing, then adding 8 parts of butyl hydroxy anisole, 6 parts of dibutyl hydroxy toluene and 4 parts of phytic acid into the reaction kettle, stirring for 20min at 45r/min under the condition of 25 ℃, then adding 8 parts of silane coupling agent, 2 parts of adhesive, 6 parts of curing agent and 5 parts of film forming agent into the reaction kettle, stirring for 20min at the rotating speed of 45r/min under the condition of 25 ℃, wherein the silane coupling agent is methyl triacetoxy silane, the adhesive is alpha-cyanoacrylate, the curing agent is dimethylamino alanine PA DMA, the film forming agent is prepared by mixing N-methyl pyrrolidone, ethylene glycol phenyl ether and propylene glycol phenyl ether according to the volume ratio of 1:1:1, stirring the obtained mixture and 55 parts of polyphenylene sulfide fiber according to the volume ratio of 45r/min for 3-4 h, taking out and drying the finished product.
Comparative example 1
Adding 13 parts of silicone oil and 100 parts of water into a reaction kettle, blending at 25 ℃, stirring for 20min at 45r/min, completely mixing, adding 8 parts of nano-aluminum hydroxide and 7 parts of nano-kaolin into the reaction kettle, blending at 25 ℃, stirring for 20min at 45r/min, completely mixing, adding 6 parts of butyl hydroxy anisole, 6 parts of dibutyl hydroxy toluene and 4 parts of phytic acid into the reaction kettle, stirring for 20min at 25 ℃, adding 7 parts of silane coupling agent, 2 parts of adhesive, 6 parts of curing agent and 4 parts of film forming agent into the reaction kettle, stirring for 20min at 25 ℃ at a rotating speed of 45r/min, wherein the silane coupling agent is methyl triacetoxy silane, the adhesive is alpha-cyanoacrylate, the curing agent is dimethylamino alanine DMAPA, the film forming agent is N-methyl pyrrolidone, and the film forming agent is N-methyl pyrrolidone, The composite material is prepared by mixing ethylene glycol phenyl ether and propylene glycol phenyl ether according to the volume ratio of 1:1:1, stirring the mixture prepared by stirring with 50 parts of polyphenylene sulfide fiber according to the speed of 45r/min for 3-4 h, taking out and drying the finished product.
Comparative example 2
Adding 13 parts of polytetrafluoroethylene and 100 parts of water into a reaction kettle, blending at 25 ℃, stirring for 20min at 45r/min, completely mixing, adding 8 parts of nano-aluminum hydroxide and 7 parts of nano-kaolin into the reaction kettle, blending at 25 ℃, stirring for 20min at 45r/min, completely mixing, adding 6 parts of butyl hydroxy anisole, 6 parts of dibutyl hydroxy toluene and 4 parts of phytic acid into the reaction kettle, stirring for 20min at 25 ℃, adding 7 parts of silane coupling agent, 2 parts of adhesive, 6 parts of curing agent and 4 parts of film forming agent into the reaction kettle, stirring for 20min at 25 ℃ at a rotating speed of 45r/min, wherein the silane coupling agent is methyl triacetoxy silane, the adhesive is alpha-cyanoacrylate, the curing agent is dimethylamino alanine DMAPA, the film forming agent is N-methyl pyrrolidone, and the film forming agent is N-methyl pyrrolidone, The composite material is prepared by mixing ethylene glycol phenyl ether and propylene glycol phenyl ether according to the volume ratio of 1:1:1, stirring the mixture prepared by stirring with 50 parts of polyphenylene sulfide fiber according to the speed of 45r/min for 3-4 h, taking out and drying the finished product.
Comparative example 3
Adding 8 parts of nano aluminum hydroxide, 7 parts of nano kaolin and 100 parts of water into a reaction kettle, blending at 25 ℃, stirring at 45r/min for 20min, completely mixing, adding 6 parts of butyl hydroxy anisole, 6 parts of dibutyl hydroxy toluene and 4 parts of phytic acid into the reaction kettle, stirring at 45r/min for 20min at 25 ℃, adding 7 parts of silane coupling agent, 2 parts of adhesive, 6 parts of curing agent and 4 parts of film forming agent into the reaction kettle, stirring at 45r/min for 20min at 25 ℃, mixing the silane coupling agent with methyl triacetoxy silane, the adhesive with alpha-cyanoacrylate, the curing agent with dimethylamino alanine DMAPA, the film forming agent with N-methyl pyrrolidone, ethylene glycol phenyl ether and propylene glycol phenyl ether at a volume ratio of 1:1:1, mixing the mixture obtained by stirring with 50 parts of polyphenylene sulfide fibers for 3-4 h at 45r/min, taking out the finished product and drying.
Comparative example 4
Adding 13 parts of polytetrafluoroethylene, 13 parts of silicone oil and 100 parts of water into a reaction kettle, mixing at 25 ℃, stirring at 45r/min for 20min, completely mixing, adding 8 parts of nanoscale aluminum hydroxide and 7 parts of nanoscale kaolin into the reaction kettle, mixing at 25 ℃, stirring at 45r/min for 20min, completely mixing, adding 6 parts of dibutyl hydroxy toluene and 4 parts of phytic acid into the reaction kettle, stirring at 25 ℃ for 20min at 45r/min, adding 7 parts of silane coupling agent, 2 parts of adhesive, 6 parts of curing agent and 4 parts of film-forming agent into the reaction kettle, stirring at 25 ℃ and 45r/min for 20min, wherein the silane coupling agent is methyl triacetoxy silane, the adhesive is alpha-cyanoacrylate, the curing agent is dimethylamino alanine DMAPA, the film-forming agent is N-methylpyrrolidone, The composite material is prepared by mixing ethylene glycol phenyl ether and propylene glycol phenyl ether according to the volume ratio of 1:1:1, stirring the mixture prepared by stirring and 50 parts of polyphenylene sulfide fiber according to the speed of 45r/min for 3-4 h, taking out and drying the finished product.
Comparative example 5
Adding 13 parts of polytetrafluoroethylene, 12 parts of silicone oil and 100 parts of water into a reaction kettle, mixing at 25 ℃, stirring at 45r/min for 20min, mixing completely, adding 8 parts of nanoscale aluminum hydroxide and 7 parts of nanoscale kaolin into the reaction kettle, mixing at 25 ℃, stirring at 45r/min for 20min, adding 6 parts of dibutyl hydroxy toluene and 4 parts of phytic acid into the reaction kettle, stirring at 25 ℃ for 20min, adding 7 parts of silane coupling agent, 2 parts of adhesive, 6 parts of curing agent and 4 parts of film-forming agent into the reaction kettle, stirring at 45r/min for 20min at 25 ℃, wherein the silane coupling agent is methyl triacetoxy silane, the adhesive is alpha-cyanoacrylate, the curing agent is dimethylamino alanine DMAPA, the film-forming agent is N-methylpyrrolidone, the adhesive is N-methyl triacetoxy silane, the mixture is sodium hydroxide, the composite material is prepared by mixing ethylene glycol phenyl ether and propylene glycol phenyl ether according to the volume ratio of 1:1:1, stirring the mixture prepared by stirring and 50 parts of polyphenylene sulfide fiber according to the speed of 45r/min for 3-4 h, taking out and drying the finished product.
Comparative example 6
Adding 13 parts of polytetrafluoroethylene, 12 parts of silicone oil and 100 parts of water into a reaction kettle, mixing at 25 ℃, stirring at 45r/min for 20min, completely mixing, adding 8 parts of nanoscale aluminum hydroxide and 7 parts of nanoscale kaolin into the reaction kettle, mixing at 25 ℃, stirring at 45r/min for 20min, completely mixing, adding 6 parts of butyl hydroxy anisole and 6 parts of dibutyl hydroxy toluene into the reaction kettle, stirring at 25 ℃ for 20min at 45r/min, adding 7 parts of silane coupling agent, 2 parts of adhesive, 6 parts of curing agent and 4 parts of film forming agent, stirring at 25 ℃ and 45r/min for 20min, wherein the silane coupling agent is methyl triacetoxy silane, the adhesive is alpha-cyanoacrylate, the curing agent is dimethylamino alanine DMAPA, the film forming agent is N-methyl pyrrolidone, the silicon dioxide and the like, The composite material is prepared by mixing ethylene glycol phenyl ether and propylene glycol phenyl ether according to the volume ratio of 1:1:1, stirring the mixture prepared by stirring and 50 parts of polyphenylene sulfide fiber according to the speed of 45r/min for 3-4 h, taking out and drying the finished product.
Comparative example 7
Adding 13 parts of polytetrafluoroethylene, 12 parts of silicone oil and 100 parts of water into a reaction kettle, mixing at 25 ℃, stirring at 45r/min for 20min, completely mixing, adding 8 parts of nanoscale aluminum hydroxide and 7 parts of nanoscale kaolin into the reaction kettle, mixing at 25 ℃, stirring at 45r/min for 20min, adding 4 parts of phytic acid into the reaction kettle, stirring at 25 ℃ for 20min, adding 7 parts of silane coupling agent, 2 parts of adhesive, 6 parts of curing agent and 4 parts of film forming agent into the reaction kettle, stirring at 25 ℃ for 20min at a rotating speed of 45r/min, wherein the silane coupling agent is methyltriacetoxysilane, the adhesive is alpha-cyanoacrylate, the curing agent is dimethylamino alanine DMAPA, the film forming agent is N-methyl pyrrolidone, ethylene glycol phenyl ether, And (3) mixing propylene glycol phenyl ether according to the volume ratio of 1:1:1, stirring the mixture obtained by stirring and 50 parts of polyphenylene sulfide fiber at the speed of 45r/min for 3-4 h, taking out and drying the finished product.
Comparative example 8
Adding 13 parts of polytetrafluoroethylene, 12 parts of silicone oil and 100 parts of water into a reaction kettle, mixing at 25 ℃, stirring at 45r/min for 20min, completely mixing, adding 8 parts of nanoscale aluminum hydroxide and 7 parts of nanoscale kaolin into the reaction kettle, mixing at 25 ℃, stirring at 45r/min for 20min, completely mixing, adding 6 parts of dibutyl hydroxy toluene into the reaction kettle, stirring at 25 ℃ for 20min at 45r/min, adding 7 parts of silane coupling agent, 2 parts of adhesive, 6 parts of curing agent and 4 parts of film forming agent into the reaction kettle, stirring at 25 ℃ for 20min at 45r/min, wherein the silane coupling agent is methyl triacetoxy silane, the adhesive is alpha-cyanoacrylate, the curing agent is dimethylamino alanine DMAPA, the film forming agent is N-methyl pyrrolidone, The composite material is prepared by mixing ethylene glycol phenyl ether and propylene glycol phenyl ether according to the volume ratio of 1:1:1, stirring the obtained mixture and 50 parts of polyphenylene sulfide fiber according to the volume ratio of 45r/min for 3-4 h, taking out and drying the finished product.
Comparative example 9
Adding 13 parts of polytetrafluoroethylene, 12 parts of silicone oil and 100 parts of water into a reaction kettle, mixing under the condition of 25 ℃, stirring for 20min at 45r/min, completely mixing, adding 8 parts of nanoscale aluminum hydroxide and 7 parts of nanoscale kaolin into the reaction kettle, mixing under the condition of 25 ℃, stirring for 20min at 45r/min, completely mixing, then adding 6 parts of butyl hydroxy anisole, 6 parts of dibutyl hydroxy toluene and 4 parts of phytic acid into the reaction kettle, stirring for 20min at 45r/min under the condition of 25 ℃, then adding 7 parts of silane coupling agent, 2 parts of adhesive, 6 parts of curing agent and 4 parts of film forming agent into the reaction kettle, stirring for 20min at the rotating speed of 45r/min under the condition of 25 ℃, wherein the silane coupling agent is methyl triacetoxy silane, the adhesive is alpha-cyanoacrylate, the curing agent is dimethylamino alanine PA DMA, the film forming agent is prepared by mixing N-methyl pyrrolidone, ethylene glycol phenyl ether and propylene glycol phenyl ether according to the volume ratio of 1:1:1, stirring the obtained mixture and 50 parts of polyphenylene sulfide fiber according to the volume ratio of 45r/min for 3-4 h, taking out and drying the finished product.
Comparative example 10
Adding 13 parts of polytetrafluoroethylene, 12 parts of silicone oil and 100 parts of water into a reaction kettle, mixing at 25 ℃, stirring at 45r/min for 20min, mixing completely, adding 8 parts of nanoscale aluminum hydroxide and 7 parts of nanoscale kaolin into the reaction kettle, mixing at 25 ℃, stirring at 45r/min for 20min, mixing completely, adding 7 parts of silane coupling agent, 2 parts of adhesive, 6 parts of curing agent and 4 parts of film forming agent into the reaction kettle, stirring at 25 ℃ and a rotating speed of 45r/min for 20min, wherein the silane coupling agent is methyl triacetoxy silane, the adhesive is alpha-cyanoacrylate, the curing agent is dimethylamino-alanine (DMAPA), the film forming agent is N-methyl pyrrolidone, ethylene glycol phenyl ether and propylene glycol phenyl ether in a volume ratio of 1:1:1, mixing the mixture obtained by stirring with 50 parts of polyphenylene sulfide fiber according to a volume ratio of 1:1:1, stirring for 3-4 h, taking out the finished product and drying.
Example 5
The performance test of 14 samples with completely consistent sizes was carried out on the finished products prepared in examples 1 to 4 and comparative examples 1 to 10, and the performance test method was as follows:
and (3) measuring the antioxidant capacity: subjecting 14 pieces of the fiber to an ORAC test;
contact angle test: the 14 pieces of fiber were placed in a contact angle test and a contact angle test was performed with a drop of water on the treated fiber material.
Table 1 was prepared based on the above experimental results.
TABLE 1 fluorescence intensity data and contact angle data for examples 1-4 and comparative examples 1-10
| Serial number | Intensity of fluorescence | Contact angle |
| Example 1 | Dark pink colour | 141° |
| Example 2 | Dark pink colour | 146° |
| Example 3 | Pink plum color | 150° |
| Example 4 | Dark pink colour | 148° |
| Comparative example 1 | Pink plum color | 124° |
| Comparative example 2 | Pink plum color | 106° |
| Comparative example 3 | Pink plum color | 87° |
| Comparative example 4 | Pink colour | 150° |
| Comparative example 5 | Pink colour | 150° |
| Comparative example 6 | Pink colour | 150° |
| Comparative example 7 | Light pink colour | 150° |
| Comparative example 8 | Light pink colour | 150° |
| Comparative example 9 | Light pink colour | 150° |
| Comparative example 10 | Colorless and colorless | 150° |
The fluorescence intensity and contact angle data of examples 1 to 4 in table 1 show that the fluorescence intensity and contact angle data of example 3 are the best, and when the ratio of the raw materials is changed from example 3 to any one of examples 1, 2 and 3, the fluorescence intensity performance and the water repellency performance are reduced, and the raw materials in example 3 are the best raw material ratio.
As can be seen from the fluorescence intensity and contact angle data in example 3 and comparative examples 1 to 10 in Table 1, when the absence of a component occurs, the fluorescence intensity performance and contact angle performance of the final product are reduced, and when the absence of a plurality of components occurs, the reduction range of the fluorescence intensity and contact angle performance is larger than the sum of the reduction ranges of the single component absence performance, compared with the fluorescence intensity and contact angle performance in example 3.
The invention provides a novel polyphenylene sulfide fiber material with polyphenylene sulfide fiber as a base material, the novel polyphenylene sulfide fiber is prepared by compounding a plurality of raw materials, the defect that the conventional polyphenylene sulfide fiber only has heat resistance and flame retardance is overcome, the prepared novel polyphenylene sulfide fiber also has good oxidation resistance and hydrophobicity, the service life of the material is prolonged, and the prepared oxidation resistance and hydrophobicity polyphenylene sulfide fiber is non-toxic and harmless, has good effect and is a novel material with better use prospect and economic value.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (10)
1. The preparation method of the oxidation-resistant hydrophobic polyphenylene sulfide fiber is characterized by comprising the following steps: the method comprises the following steps:
blending 1: mixing polytetrafluoroethylene, silicone oil and solvent, and stirring to mix them fully;
blending 2: adding nano-magnesium hydroxide and nano-kaolin into the completely mixed solution, blending and uniformly mixing;
blending 3: adding butyl hydroxy anisol, dibutyl hydroxy toluene and phytic acid into the completely mixed solution, and stirring to fully mix the components;
blending 4: finally, adding the silane coupling agent, the adhesive, the curing agent and the film forming agent into the fully mixed solution, and stirring to fully mix the silane coupling agent, the adhesive, the curing agent and the film forming agent to obtain a mixture;
preparing fibers: adding polyphenylene sulfide fiber into the obtained mixture, stirring and mixing completely, taking out and drying to obtain the finished product.
2. The method for preparing the oxidation-resistant hydrophobic polyphenylene sulfide fiber according to claim 1, wherein the method comprises the following steps: the solvent in the blending 1 is one of water and absolute ethyl alcohol.
3. The preparation method of the oxidation-resistant hydrophobic polyphenylene sulfide according to claim 1, wherein: the raw materials adopted in the preparation of the blend 1, the blend 2, the blend 3, the blend 4 and the fiber are in the following mass ratio: polyphenylene sulfide fiber: polytetrafluoroethylene: silicone oil: nano-scale magnesium hydroxide: nano-grade kaolin: butyl hydroxyanisole: dibutylhydroxytoluene: phytic acid: silane coupling agent: adhesive: curing agent: film-forming agent: 40-55% of solvent: 10-15: 3-8: 6-9: 6-7: 3-8: 5-6: 3-4: 4-8: 1-2: 5-6: 3-5: 80-110.
4. The method for preparing the oxidation-resistant hydrophobic polyphenylene sulfide fiber according to claim 3, wherein the method comprises the following steps: the raw materials adopted in the preparation of the blend 1, the blend 2, the blend 3, the blend 4 and the fiber are in the following mass ratio: polyphenylene sulfide fiber: polytetrafluoroethylene: silicone oil: nano-scale magnesium hydroxide: nano-grade kaolin: butyl hydroxyanisole: dibutylhydroxytoluene: phytic acid: silane coupling agent: adhesive: curing agent: film-forming agent: solvent 50: 13: 12: 8: 7: 6: 6: 4: 7: 2: 6: 4: 100.
5. the method for preparing the oxidation-resistant hydrophobic polyphenylene sulfide fiber according to any one of claims 1, 3 and 4, wherein: the film forming agent is one or more than one of N-methyl pyrrolidone, ethylene glycol phenyl ether and propylene glycol phenyl ether.
6. The method for preparing the oxidation-resistant hydrophobic polyphenylene sulfide fiber according to claim 1, wherein: the stirring speed in the blending 1, the blending 2, the blending 3 and the blending 4 is 30-60 r/min, and the stirring time is 10-20 min.
7. The method for preparing oxidation-resistant hydrophobic polyphenylene sulfide fiber according to claim 1 or 6, wherein: the stirring speed in the blending 1 is 45r/min, and the stirring time is 20 min.
8. The method for preparing oxidation-resistant hydrophobic polyphenylene sulfide fiber according to claim 1 or 6, wherein: the stirring speed in the blending 2 is 45r/min, and the stirring time is 20 min.
9. The method for preparing oxidation-resistant hydrophobic polyphenylene sulfide fiber according to claim 1 or 6, wherein: the stirring speed in the blending 3 is 45r/min, and the stirring time is 20 min.
10. The method for preparing oxidation-resistant hydrophobic polyphenylene sulfide fiber according to claim 1 or 6, wherein: the stirring speed in the blending 4 is 45r/min, and the stirring time is 20 min.
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