CN111501329A - 一种氢氧化镍/聚醚胺改性碳纤维的制备方法 - Google Patents
一种氢氧化镍/聚醚胺改性碳纤维的制备方法 Download PDFInfo
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- 238000007654 immersion Methods 0.000 claims abstract description 8
- RRIWRJBSCGCBID-UHFFFAOYSA-L nickel sulfate hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-]S([O-])(=O)=O RRIWRJBSCGCBID-UHFFFAOYSA-L 0.000 claims abstract description 8
- 229940116202 nickel sulfate hexahydrate Drugs 0.000 claims abstract description 8
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 3
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
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Abstract
一种氢氧化镍/聚醚胺改性碳纤维的制备方法。对碳纤维表面进行清洗和氧化处理;配置六水硫酸镍、过硫酸钾和去离子水沉积液;采用化学浴沉积法和浸渍法将碳纤维通过装有沉积液和聚醚胺有机溶剂溶液,后清洗干燥,即完成氢氧化镍/聚醚胺对碳纤维的改性。该方法充分利用氢氧化镍优异的电化学氧化还原反应性及聚醚胺的氨基基团提高纤维的电化学性能,同时利用氢氧化镍的三维蜂窝状结构和聚醚胺的反应性能提高复合材料界面结合强度,为碳纤维的改性和应用提供了一种绿色环保、简单高效的方法。
Description
技术领域
本发明属于材料的表面与界面改性领域,具体涉及一种氢氧化镍/聚醚胺改性碳纤维的制备方法。
背景技术
随着碳纤维复合材料生产技术的提高及应用领域的不断扩大,碳纤维复合材料的需求量逐年增加,与此同时,对于碳纤维复合材料的综合性能要求也一直在提高。碳纤维具有高比模量、高比强度等优异的力学性能,然而其表面缺少活性基团,表面能低,使其与树脂基体复合形成的界面粘结强度非常差,极大限制了碳纤维高性能的发挥,因此要想制得具有优异力学性能的复合材料需要对碳纤维表面进行改性处理。纳米材料,诸如石墨烯、碳纳米管、二氧化硅等,由于具有大的比表面积,优异的机械和功能特性而被广泛用于碳纤维表面改性以优化复合材料界面性能,然而纳米材料不易分散,含量较低且纳米材料改性过程中普遍存在耗时、高温、环境污染等问题进一步困扰着科研及生产工作者,亟待解决。因此寻求一种改进现有纳米材料存在的问题且基于纳米材料改性碳纤维以提高复合材料界面性能的简单、绿色、环保方法显得尤为重要。
氢氧化镍纳米片相互连接形成三维蜂窝状结构将有效解决复合材料界面改性中纳米材料不易分散和含量较低的问题,且氢氧化镍成本低、环境友好。此外,氢氧化镍纳米片由于其极大的比表面积、电化学氧化还原反应和短的离子扩散路径,在电池材料、超级电容器、电化学传感器以及电化学催化方面有着良好的发展前景。因此,氢氧化镍在改性碳纤维表面以提高复合材料界面粘结强度,同时提高材料的电化学性能方面具有新的潜力。
发明内容
本发明的目在于提供一种能够解决现有纳米材料改性碳纤维存在的纳米材料不易分散,含量较低且改性过程中普遍存在耗时、高温、环境污染等问题的氢氧化镍/聚醚胺改性碳纤维的制备方法,使改性后的碳纤维具有优异的电化学性能,提高了碳纤维/环氧复合材料界面粘结强度,拓宽碳纤维复合材料的应用领域。
为实现上述发明目的,本发明采用如下技术方案:
1)碳纤维表面氧化处理
以强酸为溶剂,采用索氏萃取法将表面清洗后的碳纤维在60℃~80℃冷凝回流2~6h,用去离子水清洗直至洗涤的去离子水pH=7,后在50℃~70℃下干燥2~4h得到氧化碳纤维;
2)沉积液的配置
按六水硫酸镍:过硫酸钾:去离子水=1:(0.15~0.2):(25~30)的摩尔比配置均匀沉积液;
3)碳纤维表面氢氧化镍涂层的制备
采用化学浴沉积法将步骤1)制备的氧化碳纤维浸入装有100ml沉积液的浆料槽,后向其中滴加5~20ml氨水溶液搅拌,后用去离子水冲洗干净后于50℃~70℃下干燥得到氢氧化镍改性的碳纤维;
4)碳纤维表面聚醚胺涂层的制备
采用浸渍法将氢氧化镍改性的碳纤维浸入装有聚醚胺/有机溶剂的混合浆料槽中5~15min,聚醚胺/有机溶剂的混合浆料按质量百分比含0.05%~0.6%的聚醚胺、99.4%~99.95%的有机溶剂,在50℃~70℃下干燥得到氢氧化镍/聚醚胺改性碳纤维。
所述步骤1)的强酸为硝酸、硫酸、硝酸和硫酸的混合液。
所述步骤1)的碳纤维为长聚丙烯腈基碳纤维丝束或碳纤维布。
所述步骤1)的碳纤维表面清洗以丙酮或石油醚为溶剂,采用索氏萃取法将碳纤维在70℃~80℃冷凝回流12~48h,后在60℃~80℃下干燥2~4h。
所述步骤3)滴加氨水溶液搅拌5~60min。
所述步骤3)采用去离子水冲洗3~5次。
所述步骤3)干燥时间为2~4h。
所述步骤4)的聚醚胺分子量为230~2000。
所述步骤4)的有机溶剂为二甲基甲酰胺、甲苯、四氢呋喃或二氯甲烷。
所述步骤4)干燥时间为2~4h。
本发明的优点:
1)本发明所制备的氢氧化镍涂层具有三维连接的蜂窝状结构,可以有效的促进应力从树脂向纤维的传递,同时聚醚胺起到改善纤维与树脂浸润性、增加纤维与树脂反应性的作用。氢氧化镍和聚醚胺的共同作用是复合材料的界面剪切强度提高。
2)本发明所制备的氢氧化镍/聚醚胺改性的碳纤维不仅复合材料界面性能提高,同时改性后纤维的电化学性能提高,赋予这种材料在力学和功能一体化复合材料方面的应用。
3)本发明中碳纤维的表面处理方法为化学浴沉积法和浸渍法,该方法绿色环保、简单高效、可重复性好,易于工业化生产。
附图说明
图1为本发明实施例1制备的氢氧化镍改性的碳纤维的扫描电镜图。
图2为本发明实施例1制备的氢氧化镍/聚醚胺改性的碳纤维的扫描电镜图。
具体实施方式
下面结合附图及实施例对本发明作进一步详细说明。
实施例1:
1)碳纤维表面清洗
以丙酮为溶剂,采用索氏萃取法将长聚丙烯腈基碳纤维丝束在80℃冷凝回流48h,后在60℃下干燥4h;
2)碳纤维表面氧化处理
以硝酸为溶剂,采用索氏萃取法将表面清洗后的碳纤维在80℃冷凝回流4h,用去离子水清洗直至洗涤的去离子水pH=7,后在60℃下干燥2h得到氧化碳纤维;
3)沉积液的配置
按六水硫酸镍:过硫酸钾:去离子水=1:0.18:28的摩尔比配置均匀得沉积液;
4)碳纤维表面氢氧化镍涂层的制备
采用化学浴沉积法将步骤2)制备的氧化碳纤维浸入装有100ml沉积液的浆料槽,后向其中滴加10ml氨水溶液搅拌15min,后用去离子水冲洗冲洗5次后于60℃下干燥2h得到氢氧化镍改性的碳纤维;
5)碳纤维表面聚醚胺涂层的制备
采用浸渍法将氢氧化镍改性的碳纤维浸入装有分子量为400的聚醚胺/二甲基甲酰胺的混合浆料槽中15min,聚醚胺/二甲基甲酰胺的混合浆料按质量百分比含0.1%的聚醚胺、99.9%的二甲基甲酰胺,在60℃下干燥2h得到氢氧化镍/聚醚胺改性碳纤维。
如图1所示碳纤维表面的氢氧化镍涂层具有三维连接的蜂窝状结构,且氢氧化镍纳米片在纤维表面均匀分布。如图2所示,涂覆氢氧化镍/聚醚胺涂层后,三维蜂窝状结构仍然保持完整,聚醚胺涂层在氢氧化镍表面均匀分布。相比未改性碳纤维,氢氧化镍/聚醚胺改性后的碳纤维在电流密度为0.5A/g下提高了625%,其环氧复合材料的界面性能提高了7.9%。
实施例2:
1)碳纤维表面清洗
以石油醚为溶剂,采用索氏萃取法将碳纤维布在70℃冷凝回流12h,后在80℃下干燥2h;
2)碳纤维表面氧化处理
以硫酸为溶剂,采用索氏萃取法将表面清洗后的碳纤维在60℃冷凝回流6h,用去离子水清洗直至洗涤的去离子水pH=7,后在70℃下干燥3h得到氧化碳纤维;
3)沉积液的配置
按六水硫酸镍:过硫酸钾:去离子水=1:0.15:25的摩尔比配置均匀得沉积液;
4)碳纤维表面氢氧化镍涂层的制备
采用化学浴沉积法将步骤2)制备的氧化碳纤维浸入装有100ml沉积液的浆料槽,后向其中滴加5ml氨水溶液搅拌5min,后用去离子水冲洗冲洗3次后于70℃下干燥3h得到氢氧化镍改性的碳纤维;
5)碳纤维表面聚醚胺涂层的制备
采用浸渍法将氢氧化镍改性的碳纤维浸入装有分子量为2000的聚醚胺/甲苯的混合浆料槽中5min,聚醚胺/甲苯的混合浆料按质量百分比含0.05%的聚醚胺、99.95%的甲苯,在70℃下干燥3h得到氢氧化镍/聚醚胺改性碳纤维。
实施例3:
1)碳纤维表面清洗
以丙酮为溶剂,采用索氏萃取法将长聚丙烯腈基碳纤维丝束在80℃冷凝回流24h,后在70℃下干燥3h;
2)碳纤维表面氧化处理
以硝酸和硫酸的混合液为溶剂,采用索氏萃取法将表面清洗后的碳纤维在80℃冷凝回流2h,用去离子水清洗直至洗涤的去离子水pH=7,后在50℃下干燥4h得到氧化碳纤维;
3)沉积液的配置
按六水硫酸镍:过硫酸钾:去离子水=1:0.2:30的摩尔比配置均匀沉积液;
4)碳纤维表面氢氧化镍涂层的制备
采用化学浴沉积法将步骤2)制备的氧化碳纤维浸入装有100ml沉积液的浆料槽,后向其中滴加20ml氨水溶液搅拌60min,后用去离子水冲洗冲洗4次后于50℃下干燥4h得到氢氧化镍改性的碳纤维;
5)碳纤维表面聚醚胺涂层的制备
采用浸渍法将氢氧化镍改性的碳纤维浸入装有分子量为230的聚醚胺/二氯甲烷的混合浆料槽中10min,聚醚胺/二氯甲烷的混合浆料按质量百分比含0.3%的聚醚胺、99.7%的二氯甲烷,在50℃下干燥4h得到氢氧化镍/聚醚胺改性碳纤维。
实施例4:
1)碳纤维表面清洗
以石油醚为溶剂,采用索氏萃取法将碳纤维布在73℃冷凝回流40h,后在65℃下干燥3h;
2)碳纤维表面氧化处理
以硝酸为溶剂,采用索氏萃取法将表面清洗后的碳纤维在70℃冷凝回流5h,用去离子水清洗直至洗涤的去离子水pH=7,后在55℃下干燥4h得到氧化碳纤维;
3)沉积液的配置
按六水硫酸镍:过硫酸钾:去离子水=1:0.16:29的摩尔比配置均匀沉积液;
4)碳纤维表面氢氧化镍涂层的制备
采用化学浴沉积法将步骤2)制备的氧化碳纤维浸入装有100ml沉积液的浆料槽,后向其中滴加15ml氨水溶液搅拌40min,后用去离子水冲洗冲洗5次后于55℃下干燥4h得到氢氧化镍改性的碳纤维;
5)碳纤维表面聚醚胺涂层的制备
采用浸渍法将氢氧化镍改性的碳纤维浸入装有分子量为1000的聚醚胺/四氢呋喃的混合浆料槽中12min,聚醚胺/四氢呋喃的混合浆料按质量百分比含0.5%的聚醚胺、99.5%的四氢呋喃,在65℃下干燥3h得到氢氧化镍/聚醚胺改性碳纤维。
实施例5:
1)碳纤维表面清洗
以丙酮为溶剂,采用索氏萃取法将碳纤维布在78℃冷凝回流20h,后在75℃下干燥2h;
2)碳纤维表面氧化处理
以硝酸和硫酸的混合液为溶剂,采用索氏萃取法将表面清洗后的碳纤维在75℃冷凝回流3h,用去离子水清洗直至洗涤的去离子水pH=7,后在65℃下干燥3h得到氧化碳纤维;
3)沉积液的配置
按六水硫酸镍:过硫酸钾:去离子水=1:0.19:26的摩尔比配置均匀得沉积液;
4)碳纤维表面氢氧化镍涂层的制备
采用化学浴沉积法将步骤1)制备的氧化碳纤维浸入装有100ml沉积液的浆料槽,后向其中滴加10ml氨水溶液搅拌、30min,后用去离子水冲洗冲洗4次后于65℃下干燥3h得到氢氧化镍改性的碳纤维;
5)碳纤维表面聚醚胺涂层的制备
采用浸渍法将氢氧化镍改性的碳纤维浸入装有分子量为1600的聚醚胺/二甲基甲酰胺的混合浆料槽中8min,聚醚胺/二甲基甲酰胺的混合浆料按质量百分比含0.6%的聚醚胺、99.4%的二甲基甲酰胺,在55℃下干燥4h得到氢氧化镍/聚醚胺改性碳纤维。
Claims (10)
1.一种氢氧化镍/聚醚胺改性碳纤维的制备方法,其特征在于包括以下步骤:
1)碳纤维表面氧化处理
以强酸为溶剂,采用索氏萃取法将表面清洗后的碳纤维在60℃~80℃冷凝回流2~6h,用去离子水清洗直至洗涤的去离子水pH=7,后在50℃~70℃下干燥2~4h得到氧化碳纤维;
2)沉积液的配置
按六水硫酸镍:过硫酸钾:去离子水=1:(0.15~0.2):(25~30)的摩尔比配置均匀沉积液;
3)碳纤维表面氢氧化镍涂层的制备
采用化学浴沉积法将步骤1)制备的氧化碳纤维浸入装有100ml沉积液的浆料槽,后向其中滴加5~20ml氨水溶液搅拌,后用去离子水冲洗干净后于50℃~70℃下干燥得到氢氧化镍改性的碳纤维;
4)碳纤维表面聚醚胺涂层的制备
采用浸渍法将氢氧化镍改性的碳纤维浸入装有聚醚胺/有机溶剂的混合浆料槽中5~15min,聚醚胺/有机溶剂的混合浆料按质量百分比含0.05%~0.6%的聚醚胺、99.4%~99.95%的有机溶剂,在50℃~70℃下干燥得到氢氧化镍/聚醚胺改性碳纤维。
2.根据权利要求1所述的氢氧化镍/聚醚胺改性碳纤维的制备方法,其特征在于:所述步骤1)的强酸为硝酸、硫酸、硝酸和硫酸的混合液。
3.根据权利要求1所述的氢氧化镍/聚醚胺改性碳纤维的制备方法,其特征在于:所述步骤1)的碳纤维为长聚丙烯腈基碳纤维丝束或碳纤维布。
4.根据权利要求1所述的氢氧化镍/聚醚胺改性碳纤维的制备方法,其特征在于:所述步骤1)的碳纤维表面清洗以丙酮或石油醚为溶剂,采用索氏萃取法将碳纤维在70℃~80℃冷凝回流12~48h,后在60℃~80℃下干燥2~4h。
5.根据权利要求1所述的氢氧化镍/聚醚胺改性碳纤维的制备方法,其特征在于:所述步骤3)滴加氨水溶液搅拌5~60min。
6.根据权利要求1所述的氢氧化镍/聚醚胺改性碳纤维的制备方法,其特征在于:所述步骤3)采用去离子水冲洗3~5次。
7.根据权利要求1所述的氢氧化镍/聚醚胺改性碳纤维的制备方法,其特征在于:所述步骤3)干燥时间为2~4h。
8.根据权利要求1所述的氢氧化镍/聚醚胺改性碳纤维的制备方法,其特征在于:所述步骤4)的聚醚胺分子量为230~2000。
9.根据权利要求1所述的氢氧化镍/聚醚胺改性碳纤维的制备方法,其特征在于:所述步骤4)的有机溶剂为二甲基甲酰胺、甲苯、四氢呋喃或二氯甲烷。
10.根据权利要求1所述的氢氧化镍/聚醚胺改性碳纤维的制备方法,其特征在于:所述步骤4)干燥时间为2~4h。
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