CN105568693A - 一种煅烧陶瓷粉体改性碳纤维环氧上浆剂的制备方法 - Google Patents
一种煅烧陶瓷粉体改性碳纤维环氧上浆剂的制备方法 Download PDFInfo
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Abstract
本发明公开了一种煅烧陶瓷粉体改性碳纤维环氧上浆剂的制备方法，属于碳纤维上浆剂制备技术领域。本发明将氧化锆和氧化铝粉末混合，与去离子水搅拌，球磨处理，干燥得复合陶瓷粉末，经两次炭化，与环氧树脂、无水乙醇混合保温后，滴加二乙醇胺、盐酸溶液保温反应，旋转蒸发后，与二乙醇胺、去离子水混合，旋转蒸发制得环氧上浆剂。本发明的有益效果是：本发明制备步骤简单，所得产品与基体树脂的粘结性和润湿性好；有效促进纤维与基体树脂之间的化学结合，提高其界面结合强度。
Description
技术领域
本发明涉及一种煅烧陶瓷粉体改性碳纤维环氧上浆剂的制备方法，属于碳纤维上浆剂制备技术领域。
背景技术
碳纤维作为国防军工用的高科技材料，近年来，在民用领域得到广泛应用。碳纤维的性能直接决定着复合材料制品的性能。碳纤维伸长率低且脆，加工过程中受到反复弯曲、摩擦容易造成单丝断裂和毛丝。上浆剂的作用是保护碳纤维表面处理（特别是臭氧处理或等离子体处理）后产生的表面活性，避免纤维表面吸附空气中的水分和灰尘；有利于改善纤维与基体树脂的粘合力及后加工性能；提高纤维丝束的抱合力，在单丝表面成膜防止毛丝的产生。
目前碳纤维常用的上浆剂有环氧树脂型乳液上浆剂，将环氧树脂与乙二醇单乙醚按一定比例搅拌混合稀释，稀释后的环氧树脂与乳化剂按比例加热融化混合均匀，高速搅拌，转速为8000r/min，在高速搅拌下，缓慢加入45℃的温水，体系粘度逐渐增加，在相转变期停止加水，继续高速搅拌，完成转相后，可快速将剩余水加入，乳液总固含量质量分数为45%。搅拌时间为1h，得到混合均匀的白色乳状液。环氧树脂乳液型上浆剂，不含或者极少含有有机溶剂，不在导辊残余树脂，工艺性较好。但是大部分乳化剂与基体树脂的结合性较差，随主浆料涂覆与碳纤维表面后，不利于纤维与基体树脂之间的化学结合，导致其界面结合强度降低。
发明内容
本发明所要解决的技术问题：针对环氧树脂乳液型上浆剂中乳化剂与基体树脂的粘结性和润湿性较差，随主浆料涂覆于碳纤维表面后，不利于纤维与基体树脂之间的化学结合，导致其界面结合强度降低的弊端，提供了一种将氧化锆和氧化铝粉末混合，与去离子水搅拌，球磨处理，干燥得复合陶瓷粉末，经两次炭化，与环氧树脂、无水乙醇混合保温后，滴加二乙醇胺、盐酸溶液保温反应，旋转蒸发后，与二乙醇胺、去离子水混合，旋转蒸发制得环氧上浆剂的方法。本发明制备步骤简单，所得产品与基体树脂的粘结性和润湿性好。
为解决上述技术问题，本发明采用如下所述的技术方案是：
（1）按质量比1:1，将氧化锆与氧化铝粉末搅拌混合，在球磨机中搅拌混合，制备得混合粉体，按质量比1:5，将上述制备的混合粉体与去离子水搅拌混合，再在球磨机上球磨处理3～4h，随后将其至于65～80℃下干燥6～8h，制备得复合陶瓷粉末；
（2）将上述制备的复合陶瓷粉末置于150～270℃马弗炉中进行初步炭化，控制炭化时间为2～3h，待初步炭化完成后，按8℃/min的速率程序升温至650～800℃，保温炭化8～10h，随后静置冷却至20～30℃，制备得混合煅烧陶瓷粉末；
（3）按重量份数计，分别称量35～55份无水乙醇、15～25份上述制备的混合煅烧陶瓷粉末和30～40份环氧树脂于三口烧瓶中，在55～60℃下保温加热1～2h，随后对其滴加无水乙醇质量1/8的二乙醇胺，控制滴加速度为2mL/min；
（4）待滴加完成后，继续保温反应2～3h后，继续滴加与二乙醇胺质量相同的0.8mol/L的盐酸溶液，控制滴加时间为10～15min，随后继续保温加热反应30～45min，再旋转蒸发至原体积的1/9，制备得改性环氧树脂；
（5）按重量份数计，分别量取45～65份去离子水、15～25份二乙醇胺和20～30份上述制备的改性环氧树脂，将其搅拌混合并旋转蒸发至固含量为2～5%，即可制得一种煅烧陶瓷粉体改性碳纤维环氧上浆剂。
本发明的应用方法：将本发明制得的煅烧陶瓷粉体改性碳纤维环氧上浆剂稀释到2.5～3.0%，稀释后放入上浆槽中，将碳纤维在上浆槽中经过压辊挤压进行上浆，随后在115～125℃下烘干，再经收丝架卷绕制得成品，即可。该环氧上浆剂与基体树脂的粘结性和润湿性好，碳纤维界面结合强度提高了78～82%，断裂伸长率提高了1.0～1.2%，拉伸强度为3.28～3.42GPa，毛丝量减少了90%以上，值得推广与使用。
本发明与其他方法相比，有益技术效果是：
（1）本发明制备步骤简单，所得产品与基体树脂的粘结性和润湿性好；
（2）有效促进纤维与基体树脂之间的化学结合，提高其界面结合强度。
具体实施方式
首先按质量比1:1，将氧化锆与氧化铝粉末搅拌混合，在球磨机中搅拌混合，制备得混合粉体，按质量比1:5，将上述制备的混合粉体与去离子水搅拌混合，再在球磨机上球磨处理3～4h，随后将其至于65～80℃下干燥6～8h，制备得复合陶瓷粉末；然后将上述制备的复合陶瓷粉末置于150～270℃马弗炉中进行初步炭化，控制炭化时间为2～3h，待初步炭化完成后，按8℃/min的速率程序升温至650～800℃，保温炭化8～10h，随后静置冷却至20～30℃，制备得混合煅烧陶瓷粉末；再按重量份数计，分别称量35～55份无水乙醇、15～25份上述制备的混合煅烧陶瓷粉末和30～40份环氧树脂于三口烧瓶中，在55～60℃下保温加热1～2h，随后对其滴加无水乙醇质量1/8的二乙醇胺，控制滴加速度为2mL/min；待滴加完成后，继续保温反应2～3h后，继续滴加与二乙醇胺质量相同的0.8mol/L的盐酸溶液，控制滴加时间为10～15min，随后继续保温加热反应30～45min，再旋转蒸发至原体积的1/9，制备得改性环氧树脂；最后按重量份数计，分别量取45～65份去离子水、15～25份二乙醇胺和20～30份上述制备的改性环氧树脂，将其搅拌混合并旋转蒸发至固含量为2～5%，即可制得一种煅烧陶瓷粉体改性碳纤维环氧上浆剂。
实例1
首先按质量比1:1，将氧化锆与氧化铝粉末搅拌混合，在球磨机中搅拌混合，制备得混合粉体，按质量比1:5，将上述制备的混合粉体与去离子水搅拌混合，再在球磨机上球磨处理3h，随后将其至于65℃下干燥6h，制备得复合陶瓷粉末；然后将上述制备的复合陶瓷粉末置于150℃马弗炉中进行初步炭化，控制炭化时间为2h，待初步炭化完成后，按8℃/min的速率程序升温至650℃，保温炭化8h，随后静置冷却至20℃，制备得混合煅烧陶瓷粉末；再按重量份数计，分别称量35份无水乙醇、25份上述制备的混合煅烧陶瓷粉末和40份环氧树脂于三口烧瓶中，在55℃下保温加热1h，随后对其滴加无水乙醇质量1/8的二乙醇胺，控制滴加速度为2mL/min；待滴加完成后，继续保温反应2h后，继续滴加与二乙醇胺质量相同的0.8mol/L的盐酸溶液，控制滴加时间为10min，随后继续保温加热反应30min，再旋转蒸发至原体积的1/9，制备得改性环氧树脂；最后按重量份数计，分别量取45份去离子水、25份二乙醇胺和30份上述制备的改性环氧树脂，将其搅拌混合并旋转蒸发至固含量为2%，即可制得一种煅烧陶瓷粉体改性碳纤维环氧上浆剂。
将本发明制得的煅烧陶瓷粉体改性碳纤维环氧上浆剂稀释到2.5%，稀释后放入上浆槽中，将碳纤维在上浆槽中经过压辊挤压进行上浆，随后在115℃的干燥炉烘干，再经收丝架卷绕制得成品，即可。该环氧上浆剂与基体树脂的粘结性和润湿性好，碳纤维界面结合强度提高了78%，断裂伸长率提高了1.0%，拉伸强度为3.28GPa，毛丝量减少了90.3%，值得推广与使用。
实例2
首先按质量比1:1，将氧化锆与氧化铝粉末搅拌混合，在球磨机中搅拌混合，制备得混合粉体，按质量比1:5，将上述制备的混合粉体与去离子水搅拌混合，再在球磨机上球磨处理4h，随后将其至于72℃下干燥7h，制备得复合陶瓷粉末；然后将上述制备的复合陶瓷粉末置于210℃马弗炉中进行初步炭化，控制炭化时间为3h，待初步炭化完成后，按8℃/min的速率程序升温至720℃，保温炭化9h，随后静置冷却至25℃，制备得混合煅烧陶瓷粉末；再按重量份数计，分别称量45份无水乙醇、20份上述制备的混合煅烧陶瓷粉末和35份环氧树脂于三口烧瓶中，在58℃下保温加热2h，随后对其滴加无水乙醇质量1/8的二乙醇胺，控制滴加速度为2mL/min；待滴加完成后，继续保温反应3h后，继续滴加与二乙醇胺质量相同的0.8mol/L的盐酸溶液，控制滴加时间为13min，随后继续保温加热反应37min，再旋转蒸发至原体积的1/9，制备得改性环氧树脂；最后按重量份数计，分别量取55份去离子水、20份二乙醇胺和25份上述制备的改性环氧树脂，将其搅拌混合并旋转蒸发至固含量为3%，即可制得一种煅烧陶瓷粉体改性碳纤维环氧上浆剂。
将本发明制得的煅烧陶瓷粉体改性碳纤维环氧上浆剂稀释到2.8%，稀释后放入上浆槽中，将碳纤维在上浆槽中经过压辊挤压进行上浆，随后在120℃的干燥炉烘干，再经收丝架卷绕制得成品，即可。该环氧上浆剂与基体树脂的粘结性和润湿性好，碳纤维界面结合强度提高了80%，断裂伸长率提高了1.1%，拉伸强度为3.35GPa，毛丝量减少了90.8%，值得推广与使用。
实例3
首先按质量比1:1，将氧化锆与氧化铝粉末搅拌混合，在球磨机中搅拌混合，制备得混合粉体，按质量比1:5，将上述制备的混合粉体与去离子水搅拌混合，再在球磨机上球磨处理4h，随后将其至于80℃下干燥8h，制备得复合陶瓷粉末；然后将上述制备的复合陶瓷粉末置于270℃马弗炉中进行初步炭化，控制炭化时间为3h，待初步炭化完成后，按8℃/min的速率程序升温至800℃，保温炭化10h，随后静置冷却至30℃，制备得混合煅烧陶瓷粉末；再按重量份数计，分别称量55份无水乙醇、15份上述制备的混合煅烧陶瓷粉末和30份环氧树脂于三口烧瓶中，在60℃下保温加热2h，随后对其滴加无水乙醇质量1/8的二乙醇胺，控制滴加速度为2mL/min；待滴加完成后，继续保温反应3h后，继续滴加与二乙醇胺质量相同的0.8mol/L的盐酸溶液，控制滴加时间为15min，随后继续保温加热反应45min，再旋转蒸发至原体积的1/9，制备得改性环氧树脂；最后按重量份数计，分别量取65份去离子水、15份二乙醇胺和20份上述制备的改性环氧树脂，将其搅拌混合并旋转蒸发至固含量为5%，即可制得一种煅烧陶瓷粉体改性碳纤维环氧上浆剂。
将本发明制得的煅烧陶瓷粉体改性碳纤维环氧上浆剂稀释到3.0%，稀释后放入上浆槽中，将碳纤维在上浆槽中经过压辊挤压进行上浆，随后在125℃的干燥炉烘干，再经收丝架卷绕制得成品，即可。该环氧上浆剂与基体树脂的粘结性和润湿性好，碳纤维界面结合强度提高了82%，断裂伸长率提高了1.2%，拉伸强度为3.42GPa，毛丝量减少了91.2%，值得推广与使用。
Claims (1)
1.一种煅烧陶瓷粉体改性碳纤维环氧上浆剂的制备方法，其特征在于具体制备步骤为：
（1）按质量比1:1，将氧化锆与氧化铝粉末搅拌混合，在球磨机中搅拌混合，制备得混合粉体，按质量比1:5，将上述制备的混合粉体与去离子水搅拌混合，再在球磨机上球磨处理3～4h，随后将其至于65～80℃下干燥6～8h，制备得复合陶瓷粉末；
（2）将上述制备的复合陶瓷粉末置于150～270℃马弗炉中进行初步炭化，控制炭化时间为2～3h，待初步炭化完成后，按8℃/min的速率程序升温至650～800℃，保温炭化8～10h，随后静置冷却至20～30℃，制备得混合煅烧陶瓷粉末；
（3）按重量份数计，分别称量35～55份无水乙醇、15～25份上述制备的混合煅烧陶瓷粉末和30～40份环氧树脂于三口烧瓶中，在55～60℃下保温加热1～2h，随后对其滴加无水乙醇质量1/8的二乙醇胺，控制滴加速度为2mL/min；
（4）待滴加完成后，继续保温反应2～3h后，继续滴加与二乙醇胺质量相同的0.8mol/L的盐酸溶液，控制滴加时间为10～15min，随后继续保温加热反应30～45min，再旋转蒸发至原体积的1/9，制备得改性环氧树脂；
（5）按重量份数计，分别量取45～65份去离子水、15～25份二乙醇胺和20～30份上述制备的改性环氧树脂，将其搅拌混合并旋转蒸发至固含量为2～5%，即可制得一种煅烧陶瓷粉体改性碳纤维环氧上浆剂。
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