CN105949688A - 一种碳纳米管/聚四氟乙烯复合材料及其制备方法 - Google Patents
一种碳纳米管/聚四氟乙烯复合材料及其制备方法 Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 21
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- 238000000034 method Methods 0.000 claims abstract description 11
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 8
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 8
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 8
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 8
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- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 36
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- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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Abstract
本发明公开了一种碳纳米管/聚四氟乙烯复合材料及其制备方法,其特征在于,不仅使用钢纤维、碳纤维来提高聚四氟乙烯的抗拉伸强度、摩擦性能,同时利用改进过的熔融法将细的填料如 SiO2、Al粉等在高温下烧结到聚四氟乙烯表面,改善了聚四氟乙烯的表面烧结状态,使胶接强度得到明显提高。此外,还配合添加了碳纳米管,有效提高了复合材料的强度、耐高温、抗氧化、耐腐蚀性能,降低了复合材料的摩擦系数。
Description
技术领域
本发明涉及碳纤维、钢纤维表面改性和聚四氟乙烯改性材料领域,尤其涉及一种碳纳米管/聚四氟乙烯复合材料及其制备方法。
背景技术
聚四氟乙烯(PTFE)耐高温和低温 、耐化学腐蚀、不吸水、摩擦系数低、介电性能优异 ,有“塑料王“之称.但是因为表面能低(表面张力为(31 ~ 34)×10 -3 N/m)、结晶度高和分子链结构对称呈现非极性, 致使其难于被粘结,制约其在阀门密封材料领域的应用。为此,科学工作者采取多种手段尝试解决 PTFE 的表面粘结问题,其中关于改变PTFE 的表面结构或性质的研究较多.主要有:1)化学处理法 ,如用钠-萘络合物或硅酸处理, 使 PTFE表面润湿角减小,表面张力提高,使其由难粘转变为可粘.2)低温等离子体技术处理, 将空气、惰性气体及可反应气体离解,与 PTFE 表面发生作用,形成极性基团。3)辐射接枝法, 采用Co 60的能源将苯乙烯、甲基丙烯酸酯等可反应单体与 PTFE 表面发生化学接枝聚合,在 PTFE 表面形成一层易于粘合的接枝聚合物。4)高温熔融法,在高温下使 PTFE 中嵌入表面能高、易粘合物质。这种方法由于易粘物质介入 PTFE 分子中, 可以达到比其他几种方法更高的粘结强度。
但PTFE作为阀门密封材料使用,还存在抗蠕变性差 、易冷流 、 回弹性差、承载能力低、线膨胀系数大、在高温 (260 ℃)下易软化等明显缺点。为了克服这些缺点,国内外研究者一般采用碳纤维、玻璃纤维、锡青铜粉、石墨、二氧化硫等作为密封材料来填充聚四氟乙烯,其中碳纤维是应用比较广泛且效果良好的填充材料,可以改善PTFE复合材料的物理系能、力学性能、耐磨性能等,可广泛应用于液压油缸、气缸密封元件、阀门密封元件、流体传动机械等行业。同样的,钢纤维由于其密度大,力学性能优异而被广泛应用于各个领域。
但是钢纤维和碳纤维表面惰性大,直接影响了复合材料的力学性能,限制了钢纤维和碳纤维高性能的发挥。因此需要对碳纤维和钢纤维表面进行改性处理,以提高其对基体的粘结性,改善界面性能,进而提高复合材料的密封性能。
发明内容
本发明主要解决的技术问题是提供一种改性聚四氟乙烯阀门密封材料的配方,依照该配方制作的聚四氟乙烯材料强度高、耐高温、抗氧化、耐腐蚀。
本发明所要解决的技术问题采用以下的技术方案来实现 :
1. 一种碳纳米管/聚四氟乙烯复合材料,其特征在于,由下述重量份的原料制得:
碳纳米管5-10,聚四氟乙烯80-90,碳纤维10-15, 丙酮15-20,钢纤维5-10,氟橡胶胶粉20-25,玻璃纤维1-2,氧化石墨烯1-3,SiO2 5-10,硅烷偶联剂KH550 15-20,95%乙醇30-40,乙酸适量,聚异氰酸酯JQ-1 5-10,二甲基甲酰胺(DMF)15-20,4-二甲氨基吡啶(DMAP) 10-15,二环己基碳二亚胺 (DCC) 15-20,水 90-100份;
所述的碳纤维中值长度为75-150μm,钢纤维中值长度为50-150μm,氟橡胶胶粉粒度为80-200目。
2. 所述的一种碳纳米管/聚四氟乙烯复合材料的制备方法,其特征在于,由以下具体步骤制成:
a. 将碳纳米管和玻璃纤维用玛瑙研钵、研棒进行研磨后,加入到丙酮溶液中,超声分散1-3小时,抽滤,烘干。
b. 将碳纤维加入20-25份95%的乙醇溶剂中,超声分散均匀,加入乙酸调节pH为4-5,加入8-12份硅烷偶联剂KH550,搅拌8-15h,之后用去离子水洗涤,真空干燥;
c. 在剩余的95%乙醇溶剂中,通过辉光放电等离子技术,将氧化石墨烯氧化成过氧化石墨烯;
d. 将步骤b得到的过氧化石墨烯加入到二甲基甲酰胺 (DMF) 中,超声 2 ~ 3h,搅拌,依次加入 4- 二甲氨基吡啶 (DMAP)、二环己基碳二亚胺 (DCC) 和步骤b所得的碳纤维,常温反应 18-36h,之后用去离子水洗涤,真空干燥,得到过氧化石墨烯接枝后的碳纤维;
e. 将胶粉加入到聚异氰酸酯JQ-1中,机械搅拌均匀后,加入干燥的钢纤维,持续机械搅拌1-3小时,水洗,干燥;
f. 将步骤a所得碳纳米管和玻璃纤维,步骤d所得过氧化石墨烯接枝后的碳纤维,步骤e所得混合物,与70-75份的聚四氟乙烯一起于高速混合机中混合均匀,冷压成型后,空气气氛中360-390℃烧结成型;得到直径150-250 mm、厚度 3~ 4mm 的板状试样;
g. 将步骤f所得的板状试样浸入浸涂液中,4-8分钟后取出,在80-100℃的烘箱中烘干后,放到马弗炉中在120-200℃的温度下烧结10-30分钟,取出即可;
所述浸涂液的配制方法为: SiO2经研磨机研磨后,与剩余的聚四氟乙烯和剩余的硅烷偶联剂KH550一起分散在水中,超声分散均匀即得。
本发明的有益效果是:接枝氧化石墨烯后的碳纤维表面粗糙度显著增加,进而提高其表面浸润性和粘结性,改善碳纤维复合材料的界面粘接质量。用聚异氰酸酯JQ-1 处理的钢纤维与胶粉和聚异氰酸酯JQ-1粘接在一起,增加了钢纤维于基体的粘结性,有利于复合材料力学性能的提高。进一步地,通过高温熔融法将SiO2填充到聚四氟乙烯复合材料表面,可明显复合材料的胶接强度,且操作步骤简单,易于施用。此外,此外,还配合添加了碳纳米管,有效提高了复合材料的强度、耐高温、抗氧化、耐腐蚀性能,降低了复合材料的摩擦系数。
具体实施方式
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解,下面结合具体实施例,进一步阐述本发明。
实施例1
本发明所要解决的技术问题采用以下的技术方案来实现 :
一种碳纳米管/聚四氟乙烯复合材料,其特征在于,由下述重量份的原料制得:
碳纳米管5,聚四氟乙烯80,碳纤维10, 丙酮15,钢纤维5,氟橡胶胶粉20,玻璃纤维1,氧化石墨烯1,SiO2 5,硅烷偶联剂KH550 15,95%乙醇30,乙酸适量,聚异氰酸酯JQ-1 5,二甲基甲酰胺(DMF)15,4-二甲氨基吡啶(DMAP) 10,二环己基碳二亚胺 (DCC) 15,水100份;
所述的碳纤维中值长度为75-150μm,钢纤维中值长度为50-150μm,氟橡胶胶粉粒度为80-200目。
所述的一种碳纳米管/聚四氟乙烯复合材料的制备方法,其特征在于,由以下具体步骤制成:
a. 将碳纳米管和玻璃纤维用玛瑙研钵、研棒进行研磨后,加入到丙酮溶液中,超声分散1-3小时,抽滤,烘干。
b. 将碳纤维加入25份95%的乙醇溶剂中,超声分散均匀,加入乙酸调节pH为4-5,加入10份硅烷偶联剂KH550,搅拌8-15h,之后用去离子水洗涤,真空干燥;
c. 在剩余的95%乙醇溶剂中,通过辉光放电等离子技术,将氧化石墨烯氧化成过氧化石墨烯;
d. 将步骤b得到的过氧化石墨烯加入到二甲基甲酰胺 (DMF) 中,超声 2 ~ 3h,搅拌,依次加入 4- 二甲氨基吡啶 (DMAP)、二环己基碳二亚胺 (DCC) 和步骤b所得的碳纤维,常温反应 18-36h,之后用去离子水洗涤,真空干燥,得到过氧化石墨烯接枝后的碳纤维;
e. 将胶粉加入到聚异氰酸酯JQ-1中,机械搅拌均匀后,加入干燥的钢纤维,持续机械搅拌1-3小时,水洗,干燥;
f. 将步骤a所得碳纳米管和玻璃纤维,步骤d所得过氧化石墨烯接枝后的碳纤维,步骤e所得混合物,与70份的聚四氟乙烯一起于高速混合机中混合均匀,冷压成型后,空气气氛中360-390℃烧结成型;得到直径150-250 mm、厚度 3~ 4mm 的板状试样;
g. 将步骤f所得的板状试样浸入浸涂液中,4-8分钟后取出,在80-100℃的烘箱中烘干后,放到马弗炉中在120-200℃的温度下烧结10-30分钟,取出即可;
所述浸涂液的配制方法为: SiO2经研磨机研磨后,与剩余的聚四氟乙烯和剩余的硅烷偶联剂KH550一起分散在水中,超声分散均匀即得。
经测试 :
拉伸强度 17MPa ;
断裂伸长率 205% ;
冲击强度 28KJ/m ;
弯曲强度 30MPa 。
Claims (2)
1.一种碳纳米管/聚四氟乙烯复合材料,其特征在于,由下述重量份的原料制得:
碳纳米管5-10,聚四氟乙烯80-90,碳纤维10-15, 丙酮15-20,钢纤维5-10,氟橡胶胶粉20-25,玻璃纤维1-2,氧化石墨烯1-3,SiO2 5-10,硅烷偶联剂KH550 15-20,95%乙醇30-40,乙酸适量,聚异氰酸酯JQ-1
5-10,二甲基甲酰胺(DMF)15-20,4-二甲氨基吡啶(DMAP)
10-15,二环己基碳二亚胺
(DCC) 15-20,水 90-100份;
所述的碳纤维中值长度为75-150μm,钢纤维中值长度为50-150μm,氟橡胶胶粉粒度为80-200目。
2.根据权利要求1所述的一种碳纳米管/聚四氟乙烯复合材料的制备方法,其特征在于,由以下具体步骤制成:
a. 将碳纳米管和玻璃纤维用玛瑙研钵、研棒进行研磨后,加入到丙酮溶液中,超声分散1-3小时,抽滤,烘干;
b. 将碳纤维加入20-25份95%的乙醇溶剂中,超声分散均匀,加入乙酸调节pH为4-5,加入8-12份硅烷偶联剂KH550,搅拌8-15h,之后用去离子水洗涤,真空干燥;
c. 在剩余的95%乙醇溶剂中,通过辉光放电等离子技术,将氧化石墨烯氧化成过氧化石墨烯;
d. 将步骤b得到的过氧化石墨烯加入到二甲基甲酰胺 (DMF) 中,超声 2 ~ 3h,搅拌,依次加入 4- 二甲氨基吡啶 (DMAP)、二环己基碳二亚胺 (DCC) 和步骤b所得的碳纤维,常温反应 18-36h,之后用去离子水洗涤,真空干燥,得到过氧化石墨烯接枝后的碳纤维;
e. 将胶粉加入到聚异氰酸酯JQ-1中,机械搅拌均匀后,加入干燥的钢纤维,持续机械搅拌1-3小时,水洗,干燥;
f. 将步骤a所得碳纳米管和玻璃纤维,步骤d所得过氧化石墨烯接枝后的碳纤维,步骤e所得混合物,与70-75份的聚四氟乙烯一起于高速混合机中混合均匀,冷压成型后,空气气氛中360-390℃烧结成型;得到直径150-250 mm、厚度 3~ 4mm 的板状试样;
g. 将步骤f所得的板状试样浸入浸涂液中,4-8分钟后取出,在80-100℃的烘箱中烘干后,放到马弗炉中在120-200℃的温度下烧结10-30分钟,取出即可;
所述浸涂液的配制方法为:
SiO2经研磨机研磨后,与剩余的聚四氟乙烯和剩余的硅烷偶联剂KH550一起分散在水中,超声分散均匀即得。
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