CN112647299A - 一种抗氧化性疏水性聚苯硫醚纤维制备方法 - Google Patents
一种抗氧化性疏水性聚苯硫醚纤维制备方法 Download PDFInfo
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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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Abstract
本发明公开了一种抗氧化性疏水性聚苯硫醚纤维制备方法,其包括如下步骤:共混1、共混2、共混3、共混4、纤维制备。本发明提供了一种兼具抗氧化性和疏水性的聚苯硫醚纤维的制备方法,改善了现今局苯硫醚纤维只具备阻燃性和耐热性同时使用寿命较短的缺点。
Description
技术领域
本发明涉及复合材料制造技术领域,特别是涉及一种抗氧化性疏水性聚苯 硫醚纤维制备方法。
背景技术
聚苯硫醚纤维,又称PPS纤维。由聚苯硫醚经熔融纺丝制得。聚苯硫醚纤 维具有良好的耐热性,主要用作高温过滤织物,耐受温度可达190℃。该纤维 还具有优良的耐化学试剂和水解性,以及阻燃性能。可用作阻燃织物、家庭装 饰织物、烟道气过滤材料等。聚苯硫醚纤维虽具耐热性、阻燃性等优点,但聚 苯硫醚大分子上的双硫键性能影响极大,会导致纤维热稳定性和力学性能变 差。并且纤维大分子上的硫容易发生深度变化,其结果会导致热氧化降解或氧 化交联,影响材料的使用寿命。有目前使用的材料大多为单一材料,不具抗氧 化性和疏水性的效果。
发明内容
本部分的目的在于概述本发明的实施例的一些方面以及简要介绍一些较 佳实施例。在本部分以及本申请的说明书摘要和发明名称中可能会做些简化或 省略以避免使本部分、说明书摘要和发明名称的目的模糊,而这种简化或省略 不能用于限制本发明的范围。
鉴于上述和/或现有聚苯硫醚产品中存在的问题,提出了本发明。
因此,本发明其中一个目的是,克服现有聚苯硫醚产品的不足,提供一种 抗氧化性疏水性聚苯硫醚纤维制备方法。
为解决上述技术问题,根据本发明的一个方面,本发明提供了如下技术方 案:一种抗氧化性疏水性聚苯硫醚纤维制备方法,其包括如下步骤,
共混1:混合聚四氟乙烯、硅油、溶剂,搅拌使其混合充分;
共混2:向混合完全的溶液中加入纳米级氢氧化镁、纳米级高岭土,共混, 混合均匀;
共混3:再向混合完全的溶液中加入丁基羟基茴香醚、二丁基羟基甲苯、 植酸,搅拌使其混合充分;
共混4:最后向混合充分的溶液中加入硅烷偶联剂、粘合剂、固化剂、成 膜剂,搅拌使其混合完全,得到混合物;
纤维制备:向得到的混合中放入聚苯硫醚纤维,搅拌混合完全,,取出后 烘干得到成品。
作为本发明所述抗氧化性疏水性聚苯硫醚纤维制备方法的一种优选方案, 其中,共混1中溶剂为水、无水乙醇中的一种。
作为本发明所述抗氧化性疏水性聚苯硫醚纤维制备方法的一种优选方案, 其中,共混1、共混2、共混3、共混4、纤维制备中采用的原料按照如下质量 比:聚苯硫醚纤维:聚四氟乙烯:硅油:纳米级氢氧化镁:纳米级高岭土:丁 基羟基茴香醚:二丁基羟基甲苯:植酸:硅烷偶联剂:粘合剂:固化剂:成膜 剂:溶剂=40~55:10~15:3~8:6~9:6~7:3~8:5~6:3~4:4~8:1~2:5~6: 3~5:80~110。
作为本发明所述抗氧化性疏水性聚苯硫醚纤维制备方法的一种优选方案, 其中,共混1、共混2、共混3、共混4、纤维制备中采用的原料按照如下质量 比:聚苯硫醚纤维:聚四氟乙烯:硅油:纳米级氢氧化镁:纳米级高岭土:丁 基羟基茴香醚:二丁基羟基甲苯:植酸:硅烷偶联剂:粘合剂:固化剂:成膜 剂:溶剂=50:13:12:8:7:6:6:4:7:2:6:4:100。
作为本发明所述抗氧化性疏水性聚苯硫醚纤维制备方法的一种优选方案, 其中,成膜剂为N-甲基吡咯烷酮、乙二醇苯醚、丙二醇苯醚中的一种或者一 种以上。
作为本发明所述抗氧化性疏水性聚苯硫醚纤维制备方法的一种优选方案, 其中,共混1、共混2、共混3、共混4中搅拌的转速为30~60r/min,搅拌时间 为10~20min。
作为本发明所述抗氧化性疏水性聚苯硫醚纤维制备方法的一种优选方案, 其中,共混1中搅拌的转速为45r/min,搅拌时间为20min。
作为本发明所述抗氧化性疏水性聚苯硫醚纤维制备方法的一种优选方案, 其中,共混2中搅拌的转速为45r/min,搅拌时间为20min。
作为本发明所述抗氧化性疏水性聚苯硫醚纤维制备方法的一种优选方案, 其中,共混3中搅拌的转速为45r/min,搅拌时间为20min。
作为本发明所述抗氧化性疏水性聚苯硫醚纤维制备方法的一种优选方案, 其中,共混4中搅拌的转速为45r/min,搅拌时间为20min。
发明提供了一种以聚苯硫醚纤维作为基材的新型聚苯硫醚纤维材料,将几 种原料复合制备的新型聚苯硫醚纤维,改善了当今聚苯硫醚纤维只具备耐热和 阻燃性能的弊端,制得的新型聚苯硫醚纤维还具有良好的抗氧化性和疏水性, 延长了材料的使用寿命,制得的抗氧化性疏水性聚苯硫醚纤维无毒无害,效果 好,是一种有着较好的使用前景和经济价值的新型材料。
具体实施方式
为使本发明的上述目的、特征和优点能够更加明显易懂,下面结合说明书 实施例对本发明的具体实施方式做详细的说明。
在下面的描述中阐述了很多具体细节以便于充分理解本发明,但是本发明 还可以采用其他不同于在此描述的其它方式来实施,本领域技术人员可以在不 违背本发明内涵的情况下做类似推广,因此本发明不受下面公开的具体实施例 的限制。
其次,此处所称的“一个实施例”或“实施例”是指可包含于本发明至少 一个实现方式中的特定特征、结构或特性。在本说明书中不同地方出现的“在 一个实施例中”并非均指同一个实施例,也不是单独的或选择性的与其他实施 例互相排斥的实施例。
实施例1
在反应釜中加入聚四氟乙烯10份、硅油9份、水80份,在25℃的条件下共混, 45r/min搅拌20min混合完全,再向反应釜中加入纳米级氢氧化铝5份、纳米级高 岭土6份,在25℃的条件下进行共混,45r/min搅拌20min混合完全,然后向反应 釜中加入丁基羟基茴香醚3份、二丁基羟基甲苯5份、植酸3份在25℃的条件下, 45r/min搅拌20min,然后向反应釜中加入硅烷偶联剂4份、粘合剂1份、固化剂5 份、成膜剂2份在25℃的条件下,45r/min的转速搅拌20min,硅烷偶联剂为甲基 三乙酰氧基硅烷,粘合剂为α-氰基丙烯酸酯,固化剂为二甲氨基丙氨DMAPA, 成膜剂为N-甲基吡咯烷酮、乙二醇苯醚、丙二醇苯醚按照体积比1:1:1混合制得, 搅拌制得的混合物与40份聚苯硫醚纤维按照45r/min搅拌3~4h后,取出成品烘干。
实施例2
在反应釜中加入聚四氟乙烯11份、硅油10份、水90份,在25℃的条件下共混, 45r/min搅拌20min混合完全,再向反应釜中加入纳米级氢氧化铝6份、纳米级高 岭土6份,在25℃的条件下进行共混,45r/min搅拌20min混合完全,然后向反应 釜中加入丁基羟基茴香醚4份、二丁基羟基甲苯5份、植酸3份在25℃的条件下,45r/min搅拌20min,然后向反应釜中加入硅烷偶联剂6份、粘合剂1份、固化剂5 份、成膜剂2份在25℃的条件下,45r/min的转速搅拌20min,硅烷偶联剂为甲基 三乙酰氧基硅烷,粘合剂为α-氰基丙烯酸酯,固化剂为二甲氨基丙氨DMAPA, 成膜剂为N-甲基吡咯烷酮、乙二醇苯醚、丙二醇苯醚按照体积比1:1:1混合制得, 搅拌制得的混合物与45份聚苯硫醚纤维按照45r/min搅拌3~4h后,取出成品烘干。
实施例3
在反应釜中加入聚四氟乙烯13份、硅油13份、水100份,在25℃的条件下共 混,45r/min搅拌20min混合完全,再向反应釜中加入纳米级氢氧化铝8份、纳米 级高岭土7份,在25℃的条件下进行共混,45r/min搅拌20min混合完全,然后向 反应釜中加入丁基羟基茴香醚6份、二丁基羟基甲苯6份、植酸4份在25℃的条件 下,45r/min搅拌20min,然后向反应釜中加入硅烷偶联剂7份、粘合剂2份、固化 剂6份、成膜剂4份在25℃的条件下,45r/min的转速搅拌20min,硅烷偶联剂为甲 基三乙酰氧基硅烷,粘合剂为α-氰基丙烯酸酯,固化剂为二甲氨基丙氨DMAPA, 成膜剂为N-甲基吡咯烷酮、乙二醇苯醚、丙二醇苯醚按照体积比1:1:1混合制得, 搅拌制得的混合物与50份聚苯硫醚纤维按照45r/min搅拌3~4h后,取出成品烘干。
实施例4
在反应釜中加入聚四氟乙烯15份、硅油13份、水110份,在25℃的条件下共 混,45r/min搅拌20min混合完全,再向反应釜中加入纳米级氢氧化铝9份、纳米 级高岭土7份,在25℃的条件下进行共混,45r/min搅拌20min混合完全,然后向 反应釜中加入丁基羟基茴香醚8份、二丁基羟基甲苯6份、植酸4份在25℃的条件 下,45r/min搅拌20min,然后向反应釜中加入硅烷偶联剂8份、粘合剂2份、固化 剂6份、成膜剂5份在25℃的条件下,45r/min的转速搅拌20min,硅烷偶联剂为甲 基三乙酰氧基硅烷,粘合剂为α-氰基丙烯酸酯,固化剂为二甲氨基丙氨DMAPA, 成膜剂为N-甲基吡咯烷酮、乙二醇苯醚、丙二醇苯醚按照体积比1:1:1混合制得, 搅拌制得的混合物与55份聚苯硫醚纤维按照45r/min搅拌3~4h后,取出成品烘干。
对照例1
在反应釜中加入硅油13份、水100份,在25℃的条件下共混,45r/min搅拌 20min混合完全,再向反应釜中加入纳米级氢氧化铝8份、纳米级高岭土7份,在 25℃的条件下进行共混,45r/min搅拌20min混合完全,然后向反应釜中加入丁基 羟基茴香醚6份、二丁基羟基甲苯6份、植酸4份在25℃的条件下,45r/min搅拌20min,然后向反应釜中加入硅烷偶联剂7份、粘合剂2份、固化剂6份、成膜剂4 份在25℃的条件下,45r/min的转速搅拌20min,硅烷偶联剂为甲基三乙酰氧基硅 烷,粘合剂为α-氰基丙烯酸酯,固化剂为二甲氨基丙氨DMAPA,成膜剂为N-甲 基吡咯烷酮、乙二醇苯醚、丙二醇苯醚按照体积比1:1:1混合制得,搅拌制得的混 合物与50份聚苯硫醚纤维按照45r/min搅拌3~4h后,取出成品烘干。
对照例2
在反应釜中加入聚四氟乙烯13份、水100份,在25℃的条件下共混,45r/min 搅拌20min混合完全,再向反应釜中加入纳米级氢氧化铝8份、纳米级高岭土7份, 在25℃的条件下进行共混,45r/min搅拌20min混合完全,然后向反应釜中加入丁 基羟基茴香醚6份、二丁基羟基甲苯6份、植酸4份在25℃的条件下,45r/min搅拌 20min,然后向反应釜中加入硅烷偶联剂7份、粘合剂2份、固化剂6份、成膜剂4 份在25℃的条件下,45r/min的转速搅拌20min,硅烷偶联剂为甲基三乙酰氧基硅 烷,粘合剂为α-氰基丙烯酸酯,固化剂为二甲氨基丙氨DMAPA,成膜剂为N-甲 基吡咯烷酮、乙二醇苯醚、丙二醇苯醚按照体积比1:1:1混合制得,搅拌制得的混 合物与50份聚苯硫醚纤维按照45r/min搅拌3~4h后,取出成品烘干。
对比例3
在反应釜中加入纳米级氢氧化铝8份、纳米级高岭土7份、水100份,在25℃ 的条件下进行共混,45r/min搅拌20min混合完全,然后向反应釜中加入丁基羟基 茴香醚6份、二丁基羟基甲苯6份、植酸4份在25℃的条件下,45r/min搅拌20min, 然后向反应釜中加入硅烷偶联剂7份、粘合剂2份、固化剂6份、成膜剂4份在25℃ 的条件下,45r/min的转速搅拌20min,硅烷偶联剂为甲基三乙酰氧基硅烷,粘合 剂为α-氰基丙烯酸酯,固化剂为二甲氨基丙氨DMAPA,成膜剂为N-甲基吡咯烷 酮、乙二醇苯醚、丙二醇苯醚按照体积比1:1:1混合制得,搅拌制得的混合物与50 份聚苯硫醚纤维按照45r/min搅拌3~4h后,取出成品烘干。
对照例4
在反应釜中加入聚四氟乙烯13份、硅油13份、水100份,在25℃的条件下共 混,45r/min搅拌20min混合完全,再向反应釜中加入纳米级氢氧化铝8份、纳米 级高岭土7份,在25℃的条件下进行共混,45r/min搅拌20min混合完全,然后向 反应釜中加入二丁基羟基甲苯6份、植酸4份在25℃的条件下,45r/min搅拌20min, 然后向反应釜中加入硅烷偶联剂7份、粘合剂2份、固化剂6份、成膜剂4份在25℃ 的条件下,45r/min的转速搅拌20min,硅烷偶联剂为甲基三乙酰氧基硅烷,粘合 剂为α-氰基丙烯酸酯,固化剂为二甲氨基丙氨DMAPA,成膜剂为N-甲基吡咯烷 酮、乙二醇苯醚、丙二醇苯醚按照体积比1:1:1混合制得,搅拌制得的混合物与50 份聚苯硫醚纤维按照45r/min搅拌3~4h后,取出成品烘干。
对照例5
在反应釜中加入聚四氟乙烯13份、硅油12份、水100份,在25℃的条件下共 混,45r/min搅拌20min混合完全,再向反应釜中加入纳米级氢氧化铝8份、纳米 级高岭土7份,在25℃的条件下进行共混,45r/min搅拌20min混合完全,然后向 反应釜中加入二丁基羟基甲苯6份、植酸4份在25℃的条件下,45r/min搅拌20min, 然后向反应釜中加入硅烷偶联剂7份、粘合剂2份、固化剂6份、成膜剂4份在25℃ 的条件下,45r/min的转速搅拌20min,硅烷偶联剂为甲基三乙酰氧基硅烷,粘合 剂为α-氰基丙烯酸酯,固化剂为二甲氨基丙氨DMAPA,成膜剂为N-甲基吡咯烷 酮、乙二醇苯醚、丙二醇苯醚按照体积比1:1:1混合制得,搅拌制得的混合物与50 份聚苯硫醚纤维按照45r/min搅拌3~4h后,取出成品烘干。
对照例6
在反应釜中加入聚四氟乙烯13份、硅油12份、水100份,在25℃的条件下共 混,45r/min搅拌20min混合完全,再向反应釜中加入纳米级氢氧化铝8份、纳米 级高岭土7份,在25℃的条件下进行共混,45r/min搅拌20min混合完全,然后向 反应釜中加入丁基羟基茴香醚6份、二丁基羟基甲苯6份在25℃的条件下,45r/min 搅拌20min,然后向反应釜中加入硅烷偶联剂7份、粘合剂2份、固化剂6份、成膜 剂4份在25℃的条件下,45r/min的转速搅拌20min,硅烷偶联剂为甲基三乙酰氧 基硅烷,粘合剂为α-氰基丙烯酸酯,固化剂为二甲氨基丙氨DMAPA,成膜剂为 N-甲基吡咯烷酮、乙二醇苯醚、丙二醇苯醚按照体积比1:1:1混合制得,搅拌制 得的混合物与50份聚苯硫醚纤维按照45r/min搅拌3~4h后,取出成品烘干。
对照例7
在反应釜中加入聚四氟乙烯13份、硅油12份、水100份,在25℃的条件下共 混,45r/min搅拌20min混合完全,再向反应釜中加入纳米级氢氧化铝8份、纳米 级高岭土7份,在25℃的条件下进行共混,45r/min搅拌20min混合完全,然后向 反应釜中加入植酸4份在25℃的条件下,45r/min搅拌20min,然后向反应釜中加 入硅烷偶联剂7份、粘合剂2份、固化剂6份、成膜剂4份在25℃的条件下,45r/min 的转速搅拌20min,硅烷偶联剂为甲基三乙酰氧基硅烷,粘合剂为α-氰基丙烯酸 酯,固化剂为二甲氨基丙氨DMAPA,成膜剂为N-甲基吡咯烷酮、乙二醇苯醚、 丙二醇苯醚按照体积比1:1:1混合制得,搅拌制得的混合物与50份聚苯硫醚纤维按 照45r/min搅拌3~4h后,取出成品烘干。
对照例8
在反应釜中加入聚四氟乙烯13份、硅油12份、水100份,在25℃的条件下共 混,45r/min搅拌20min混合完全,再向反应釜中加入纳米级氢氧化铝8份、纳米 级高岭土7份,在25℃的条件下进行共混,45r/min搅拌20min混合完全,然后向 反应釜中加入二丁基羟基甲苯6份在25℃的条件下,45r/min搅拌20min,然后向 反应釜中加入硅烷偶联剂7份、粘合剂2份、固化剂6份、成膜剂4份在25℃的条件 下,45r/min的转速搅拌20min,硅烷偶联剂为甲基三乙酰氧基硅烷,粘合剂为α- 氰基丙烯酸酯,固化剂为二甲氨基丙氨DMAPA,成膜剂为N-甲基吡咯烷酮、乙 二醇苯醚、丙二醇苯醚按照体积比1:1:1混合制得,搅拌制得的混合物与50份聚苯 硫醚纤维按照45r/min搅拌3~4h后,取出成品烘干。
对照例9
在反应釜中加入聚四氟乙烯13份、硅油12份、水100份,在25℃的条件下共 混,45r/min搅拌20min混合完全,再向反应釜中加入纳米级氢氧化铝8份、纳米 级高岭土7份,在25℃的条件下进行共混,45r/min搅拌20min混合完全,然后向 反应釜中加入丁基羟基茴香醚6份、二丁基羟基甲苯6份、植酸4份在25℃的条件 下,45r/min搅拌20min,然后向反应釜中加入硅烷偶联剂7份、粘合剂2份、固化 剂6份、成膜剂4份在25℃的条件下,45r/min的转速搅拌20min,硅烷偶联剂为甲 基三乙酰氧基硅烷,粘合剂为α-氰基丙烯酸酯,固化剂为二甲氨基丙氨DMAPA, 成膜剂为N-甲基吡咯烷酮、乙二醇苯醚、丙二醇苯醚按照体积比1:1:1混合制得, 搅拌制得的混合物与50份聚苯硫醚纤维按照45r/min搅拌3~4h后,取出成品烘干。
对照例10
在反应釜中加入聚四氟乙烯13份、硅油12份、水100份,在25℃的条件下共 混,45r/min搅拌20min混合完全,再向反应釜中加入纳米级氢氧化铝8份、纳米 级高岭土7份,在25℃的条件下进行共混,45r/min搅拌20min混合完全,然后向 反应釜中加入硅烷偶联剂7份、粘合剂2份、固化剂6份、成膜剂4份在25℃的条件 下,45r/min的转速搅拌20min,硅烷偶联剂为甲基三乙酰氧基硅烷,粘合剂为α- 氰基丙烯酸酯,固化剂为二甲氨基丙氨DMAPA,成膜剂为N-甲基吡咯烷酮、乙 二醇苯醚、丙二醇苯醚按照体积比1:1:1混合制得,搅拌制得的混合物与50份聚苯 硫醚纤维按照45r/min搅拌3~4h后,取出成品烘干。
实施例5
将实施例1~4和对照例1~10中制得的成品选取大小完全一致共14个样品进 行性能测试,性能测试方法如下:
抗氧化能力测定:将14块纤维进行ORAC测试;
接触角测试:将14块纤维放入接触角测试,进行水滴滴在处理后的纤维材 料的接触角测试。
根据上述实验结果制得表1。
表1实施例1~4和对照例1~10的荧光强度数据和接触角数据
序号 | 荧光强度 | 接触角 |
实施例1 | 深粉色 | 141° |
实施例2 | 深粉色 | 146° |
实施例3 | 梅粉色 | 150° |
实施例4 | 深粉色 | 148° |
对照例1 | 梅粉色 | 124° |
对照例2 | 梅粉色 | 106° |
对照例3 | 梅粉色 | 87° |
对照例4 | 粉色 | 150° |
对照例5 | 粉色 | 150° |
对照例6 | 粉色 | 150° |
对照例7 | 浅粉色 | 150° |
对照例8 | 浅粉色 | 150° |
对照例9 | 浅粉色 | 150° |
对照例10 | 无色 | 150° |
根据表1中实施例1~4的荧光强度和接触角数据可得,实施例3的荧光强度和 接触角数据最好,当原料的比例从实施例3更换为实施例1、2、3中任一比例时, 会导致荧光强度性能和疏水性能的下降,实施例3中的原料为最佳的原料比例。
根据表1中实施例3和对照例1~10中荧光强度和接触角数据可得,相较实施 例3中的荧光强度和接触角性能,当出现成分的缺失时,会导致成品的荧光强度 性能和接触角性能的下降,当出现多种成分的缺失时,荧光强度和接触角性能 下降的幅度大于单种成分缺失的性能下降幅度之和。
本发明提供了一种以聚苯硫醚纤维作为基材的新型聚苯硫醚纤维材料,将 几种原料复合制备的新型聚苯硫醚纤维,改善了当今聚苯硫醚纤维只具备耐热 和阻燃性能的弊端,制得的新型聚苯硫醚纤维还具有良好的抗氧化性和疏水性, 延长了材料的使用寿命,制得的抗氧化性疏水性聚苯硫醚纤维无毒无害,效果 好,是一种有着较好的使用前景和经济价值的新型材料。
应说明的是,以上实施例仅用以说明本发明的技术方案而非限制,尽管参 照较佳实施例对本发明进行了详细说明,本领域的普通技术人员应当理解,可 以对本发明的技术方案进行修改或者等同替换,而不脱离本发明技术方案的精 神和范围,其均应涵盖在本发明的权利要求范围当中。
Claims (10)
1.一种抗氧化性疏水性聚苯硫醚纤维制备方法,其特征在于:包括如下步骤:
共混1:混合聚四氟乙烯、硅油、溶剂,搅拌使其混合充分;
共混2:向混合完全的溶液中加入纳米级氢氧化镁、纳米级高岭土,共混,混合均匀;
共混3:再向混合完全的溶液中加入丁基羟基茴香醚、二丁基羟基甲苯、植酸,搅拌使其混合充分;
共混4:最后向混合充分的溶液中加入硅烷偶联剂、粘合剂、固化剂、成膜剂,搅拌使其混合完全,得到混合物;
纤维制备:向得到的混合中放入聚苯硫醚纤维,搅拌混合完全,,取出后烘干得到成品。
2.根据权利要求1所述的抗氧化性疏水性聚苯硫醚纤维制备方法,其特征在于:所述共混1中溶剂为水、无水乙醇中的一种。
3.根据权比例要求1所述的抗氧化性疏水性聚苯硫醚制备方法,其特征在于:所述共混1、共混2、共混3、共混4、纤维制备中采用的原料按照如下质量比:聚苯硫醚纤维:聚四氟乙烯:硅油:纳米级氢氧化镁:纳米级高岭土:丁基羟基茴香醚:二丁基羟基甲苯:植酸:硅烷偶联剂:粘合剂:固化剂:成膜剂:溶剂=40~55:10~15:3~8:6~9:6~7:3~8:5~6:3~4:4~8:1~2:5~6:3~5:80~110。
4.根据权利要求3所述的抗氧化性疏水性聚苯硫醚纤维制备方法,其特征在于:所述共混1、共混2、共混3、共混4、纤维制备中采用的原料按照如下质量比:聚苯硫醚纤维:聚四氟乙烯:硅油:纳米级氢氧化镁:纳米级高岭土:丁基羟基茴香醚:二丁基羟基甲苯:植酸:硅烷偶联剂:粘合剂:固化剂:成膜剂:溶剂=50:13:12:8:7:6:6:4:7:2:6:4:100。
5.根据权利要求1、3、4中任一所述抗氧化性疏水性聚苯硫醚纤维制备方法,其特征在于:所述成膜剂为N-甲基吡咯烷酮、乙二醇苯醚、丙二醇苯醚中的一种或者一种以上。
6.根据权利要求1中所述的抗氧化性疏水性聚苯硫醚纤维制备方法,其特征在于:所述共混1、共混2、共混3、共混4中搅拌的转速为30~60r/min,搅拌时间为10~20min。
7.根据权利要求1或6中所述的抗氧化性疏水性聚苯硫醚纤维制备方法,其特征在于:所述共混1中搅拌的转速为45r/min,搅拌时间为20min。
8.根据权利要求1或6中所述的抗氧化性疏水性聚苯硫醚纤维制备方法,其特征在于:所述共混2中搅拌的转速为45r/min,搅拌时间为20min。
9.根据权利要求1或6中所述的抗氧化性疏水性聚苯硫醚纤维制备方法,其特征在于:所述共混3中搅拌的转速为45r/min,搅拌时间为20min。
10.根据权利要求1或6中所述的抗氧化性疏水性聚苯硫醚纤维制备方法,其特征在于:所述共混4中搅拌的转速为45r/min,搅拌时间为20min。
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