CN112760889B - 一种由熔喷布为基础碳化制备碳纤维布的方法 - Google Patents
一种由熔喷布为基础碳化制备碳纤维布的方法 Download PDFInfo
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Abstract
本发明提供一种由熔喷布为基础碳化制备碳纤维布的方法,涉及碳纤维布制备领域。该由熔喷布为基础碳化制备碳纤维布的方法,包括以下步骤:S1.准备原料;S2.对熔喷布改性;S3.熔喷布上包覆氧化铁膜;S4.干燥处理;S5.对熔喷布进行预氧化和碳化;S6.制成碳纤维布。通过表面改性剂先对熔喷布进行改性,然后加入氧化铁前驱物和氨水,通过化学液相沉淀在熔喷布表面沉淀氧化铁膜,然后再放入气氛炉中进行预氧化和碳化制得碳纤维布,这样可以使聚丙烯纤维在预氧化过程中提供以氧化铁为催化基础的预氧化,使聚丙烯纤维逐渐转变为碳链为主的结构,提高了纤维的抗温变性能,进而能在高温状态下发生高温碳化的时候保持形态,值得大力推广。
Description
技术领域
本发明涉及碳纤维布制备领域,具体为一种由熔喷布为基础碳化制备碳纤维布的方法。
背景技术
熔喷布是口罩最核心的材料,熔喷布主要以聚丙烯为主要原料,纤维直径可以达到1~5微米,空隙多、结构蓬松、抗褶皱能力好,具有独特的毛细结构的超细纤维增加单位面积纤维的数量和表面积,从而使熔喷布具有很好的过滤性、屏蔽性、绝热性和吸油性,可用于空气、液体过滤材料、隔离材料、吸纳材料、口罩材料、保暖材料、吸油材料及擦拭布等领域。
熔喷布是由聚丙烯在高速气流喷射下形成的一种无纺布,因此对于极性分子吸附性能极差,并且聚丙烯纤维不能够直接进行碳化成碳纤维布。
发明内容
(一)解决的技术问题
针对现有技术的不足,本发明提供了一种由熔喷布为基础碳化制备碳纤维布的方法,解决了熔喷布不能直接碳化制成碳纤维布的问题。
(二)技术方案
为实现以上目的,本发明通过以下技术方案予以实现:一种由熔喷布为基础碳化制备碳纤维布的方法,包括以下步骤:
S1.准备
首先准备以下重量份的原材料:熔喷布100份、氧化铁前驱物3~30份、表面改性剂0.1~1份;
S2.改性
先将耐蚀槽中注满水,然后将温度升高至90℃,再将熔喷布浸泡在耐蚀槽中,然后将表面改性剂加入到耐蚀槽中,搅拌均匀;
S3.覆膜
将氧化铁前驱物加入到耐蚀槽中,并向耐蚀槽中鼓入空气,使耐蚀槽内的溶液变成红棕色后,再缓慢滴加氨水,通过化学液相沉淀在熔喷布纤维表面沉淀氧化铁膜,观察熔喷布的上色情况,若熔喷布上红棕色均匀,则补加等量的氧化铁前驱物,同时继续鼓入空气,并缓慢滴加氨水至溶液pH值小于5后停止加入氨水,若熔喷布上红棕色不均匀,则补加等量的表面改性剂,同时继续鼓入空气,然后再缓慢滴加氨水至溶液pH值小于5后停止加入氨水;
S4.干燥
将上色均匀的熔喷布从耐蚀槽中捞出,用清水漂洗至水洗液为中性即可,然后放入干燥箱内,在100~110℃条件下进行干燥处理;
S5.碳化
将干燥的改性熔喷布放入气氛炉中,并向气氛炉内通入氮气保护,然后升温至130℃后,通过湿度检测设备对气氛炉尾气中的水份含量进行检测,当没有水份存在时,升温5℃并保温30mi n,依次反复升温至150℃后,向气氛炉中通入还原气体,并将氮气通入量调至最低,保温30mi n,然后每隔5mi n升温5℃直至400℃,之后每隔3mi n升温10℃直至1000℃为止,即可将改性熔喷布碳化成碳纤维布;
S6.成品
关闭气氛炉的加热,继续保持氮气的最低通入量,使气氛炉内温度缓慢降低至室温后将碳纤维布取出,用稀盐酸溶解碳纤维布表面的铁层后,再水洗至水溶液为中性,然后进行干燥处理即可得到碳纤维布成品。
优选的,所述表面改性剂为硅烷偶联剂、钛酸酯偶联剂、铝酸酯偶联剂中的一种。
优选的,所述氧化铁前驱物为氯化亚铁、氯化铁、硫酸铁或硫酸亚铁中的一种。
优选的,所述气氛炉内温度范围在130~150℃时为预氧化。
优选的,所述还原气体为氢气-一氧化碳。
(三)有益效果
本发明提供了一种由熔喷布为基础碳化制备碳纤维布的方法。具备以下有益效果:
本发明通过表面改性剂先对熔喷布进行改性,然后加入氧化铁前驱物和氨水,通过化学液相沉淀在熔喷布表面沉淀氧化铁膜,然后再放入气氛炉中进行预氧化和碳化制得碳纤维布,这样可以使聚丙烯纤维在预氧化过程中提供以氧化铁为催化基础的预氧化,使聚丙烯纤维逐渐转变为碳链为主的结构,提高了纤维的抗温变性能,进而能在高温状态下发生高温碳化的时候保持形态,从而可以直接对熔喷布进行碳化制成碳纤维布,工艺更简单,值得大力推广。
具体实施方式
下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例一:
本发明实施例提供一种由熔喷布为基础碳化制备碳纤维布的方法,包括以下步骤:
S1.准备
首先准备以下重量份的原材料:熔喷布100份、氧化铁前驱物3份、表面改性剂0.1份;
S2.改性
先将耐蚀槽中注满水,然后将温度升高至90℃,再将熔喷布浸泡在耐蚀槽中,然后将表面改性剂加入到耐蚀槽中,搅拌均匀,熔喷布的基材是聚丙烯材料,对于极性分子吸附性能极差,因此通过加入表面改性剂对聚丙烯纤维进行表面改性,使其对极性分子的亲和性增强,而且熔喷布的生产过程是高速气流带动拉丝,纤维粗细有别,生产批次的比表面也完全不同,所以添加的表面改性剂的量需保持在熔喷布量的0.1~1%;
S3.覆膜
将氧化铁前驱物加入到耐蚀槽中,并向耐蚀槽中鼓入空气,使耐蚀槽内的溶液变成红棕色后,再缓慢滴加氨水,通过化学液相沉淀在熔喷布纤维表面沉淀氧化铁膜,观察熔喷布的上色情况,若熔喷布上红棕色均匀,则补加等量的氧化铁前驱物,同时继续鼓入空气,并缓慢滴加氨水至溶液pH值小于5后停止加入氨水,若熔喷布上红棕色不均匀,则补加等量的表面改性剂,同时继续鼓入空气,然后再缓慢滴加氨水至溶液pH值小于5后停止加入氨水,经过改性和覆膜后,可以使聚丙烯纤维在预氧化过程中提供以氧化铁为催化基础的预氧化,使聚丙烯纤维逐渐转变为碳链为主的结构,提高了纤维的抗温变性能,进而能在高温状态下发生高温碳化的时候保持形态,从而可以直接对熔喷布进行碳化制成碳纤维布;
S4.干燥
将上色均匀的熔喷布从耐蚀槽中捞出,用清水漂洗至水洗液为中性即可,然后放入干燥箱内,在100℃条件下进行干燥处理;
S5.碳化
将干燥的改性熔喷布放入气氛炉中,并向气氛炉内通入氮气保护,然后升温至130℃后,通过湿度检测设备对气氛炉尾气中的水份含量进行检测,当没有水份存在时,升温5℃并保温30mi n,依次反复升温至150℃后,向气氛炉中通入还原气体,并将氮气通入量调至最低,保温30mi n,然后每隔5mi n升温5℃直至400℃,之后每隔3mi n升温10℃直至1000℃为止,即可将改性熔喷布碳化成碳纤维布;
S6.成品
关闭气氛炉的加热,继续保持氮气的最低通入量,使气氛炉内温度缓慢降低至室温后将碳纤维布取出,用稀盐酸溶解碳纤维布表面的铁层后,再水洗至水溶液为中性,然后进行干燥处理即可得到碳纤维布成品。
表面改性剂为硅烷偶联剂、钛酸酯偶联剂、铝酸酯偶联剂中的一种。
氧化铁前驱物为氯化亚铁、氯化铁、硫酸铁或硫酸亚铁中的一种,其中氯化亚铁中含酸根先对三价来说少,物料消耗也相对少,所以主要还是使用氯化亚铁。
气氛炉内温度范围在130~150℃时为预氧化。
还原气体为氢气-一氧化碳。
实施例二:
本发明实施例提供一种由熔喷布为基础碳化制备碳纤维布的方法,包括以下步骤:
S1.准备
首先准备以下重量份的原材料:熔喷布100份、氧化铁前驱物30份、表面改性剂1份;
S2.改性
先将耐蚀槽中注满水,然后将温度升高至90℃,再将熔喷布浸泡在耐蚀槽中,然后将表面改性剂加入到耐蚀槽中,搅拌均匀,熔喷布的基材是聚丙烯材料,对于极性分子吸附性能极差,因此通过加入表面改性剂对聚丙烯纤维进行表面改性,使其对极性分子的亲和性增强,而且熔喷布的生产过程是高速气流带动拉丝,纤维粗细有别,生产批次的比表面也完全不同,所以添加的表面改性剂的量需保持在熔喷布量的0.1~1%;
S3.覆膜
将氧化铁前驱物加入到耐蚀槽中,并向耐蚀槽中鼓入空气,使耐蚀槽内的溶液变成红棕色后,再缓慢滴加氨水,通过化学液相沉淀在熔喷布纤维表面沉淀氧化铁膜,观察熔喷布的上色情况,若熔喷布上红棕色均匀,则补加等量的氧化铁前驱物,同时继续鼓入空气,并缓慢滴加氨水至溶液pH值小于5后停止加入氨水,若熔喷布上红棕色不均匀,则补加等量的表面改性剂,同时继续鼓入空气,然后再缓慢滴加氨水至溶液pH值小于5后停止加入氨水,经过改性和覆膜后,可以使聚丙烯纤维在预氧化过程中提供以氧化铁为催化基础的预氧化,使聚丙烯纤维逐渐转变为碳链为主的结构,提高了纤维的抗温变性能,进而能在高温状态下发生高温碳化的时候保持形态,从而可以直接对熔喷布进行碳化制成碳纤维布;
S4.干燥
将上色均匀的熔喷布从耐蚀槽中捞出,用清水漂洗至水洗液为中性即可,然后放入干燥箱内,在110℃条件下进行干燥处理;
S5.碳化
将干燥的改性熔喷布放入气氛炉中,并向气氛炉内通入氮气保护,然后升温至130℃后,通过湿度检测设备对气氛炉尾气中的水份含量进行检测,当没有水份存在时,升温5℃并保温30mi n,依次反复升温至150℃后,向气氛炉中通入还原气体,并将氮气通入量调至最低,保温30mi n,然后每隔5mi n升温5℃直至400℃,之后每隔3mi n升温10℃直至1000℃为止,即可将改性熔喷布碳化成碳纤维布;
S6.成品
关闭气氛炉的加热,继续保持氮气的最低通入量,使气氛炉内温度缓慢降低至室温后将碳纤维布取出,用稀盐酸溶解碳纤维布表面的铁层后,再水洗至水溶液为中性,然后进行干燥处理即可得到碳纤维布成品。
表面改性剂为硅烷偶联剂、钛酸酯偶联剂、铝酸酯偶联剂中的一种。
氧化铁前驱物为氯化亚铁、氯化铁、硫酸铁或硫酸亚铁中的一种,其中氯化亚铁中含酸根先对三价来说少,物料消耗也相对少,所以主要还是使用氯化亚铁。
气氛炉内温度范围在130~150℃时为预氧化。
还原气体为氢气-一氧化碳。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (4)
1.一种由熔喷布为基础碳化制备碳纤维布的方法,其特征在于:包括以下步骤:
S1.准备
首先准备以下重量份的原材料:熔喷布100份、氧化铁前驱物3~30份、表面改性剂0.1~1份,所述表面改性剂为硅烷偶联剂、钛酸酯偶联剂、铝酸酯偶联剂中的一种,所述熔喷布的基材是聚丙烯材料;
S2.改性
先将耐蚀槽中注满水,然后将温度升高至90℃,再将熔喷布浸泡在耐蚀槽中,然后将表面改性剂加入到耐蚀槽中,搅拌均匀;
S3.覆膜
将氧化铁前驱物加入到耐蚀槽中,并向耐蚀槽中鼓入空气,使耐蚀槽内的溶液变成红棕色后,再缓慢滴加氨水,通过化学液相沉淀在熔喷布纤维表面沉淀氧化铁膜,观察熔喷布的上色情况,若熔喷布上红棕色均匀,则补加等量的氧化铁前驱物,同时继续鼓入空气,并缓慢滴加氨水至溶液pH值小于5后停止加入氨水,若熔喷布上红棕色不均匀,则补加等量的表面改性剂,同时继续鼓入空气,然后再缓慢滴加氨水至溶液pH值小于5后停止加入氨水;
S4.干燥
将上色均匀的熔喷布从耐蚀槽中捞出,用清水漂洗至水洗液为中性即可,然后放入干燥箱内,在100~110℃条件下进行干燥处理;
S5.碳化
将干燥的改性熔喷布放入气氛炉中,并向气氛炉内通入氮气保护,然后升温至130℃后,通过湿度检测设备对气氛炉尾气中的水份含量进行检测,当没有水份存在时,升温5℃并保温30min,依次反复升温至150℃后,向气氛炉中通入还原气体,并将氮气通入量调至最低,保温30min,然后每隔5min升温5℃直至400℃,之后每隔3min升温10℃直至1000℃为止,即可将改性熔喷布碳化成碳纤维布;
S6.成品
关闭气氛炉的加热,继续保持氮气的最低通入量,使气氛炉内温度缓慢降低至室温后将碳纤维布取出,用稀盐酸溶解碳纤维布表面的铁层后,再水洗至水溶液为中性,然后进行干燥处理即可得到碳纤维布成品。
2.根据权利要求1所述的一种由熔喷布为基础碳化制备碳纤维布的方法,其特征在于:所述氧化铁前驱物为氯化亚铁、氯化铁、硫酸铁或硫酸亚铁中的一种。
3.根据权利要求1所述的一种由熔喷布为基础碳化制备碳纤维布的方法,其特征在于:所述气氛炉内温度范围在130~150℃时为预氧化。
4.根据权利要求1所述的一种由熔喷布为基础碳化制备碳纤维布的方法,其特征在于:所述还原气体为氢气-一氧化碳。
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