CN108691206A - 一种超轻高强壳聚糖纤维织物的制备方法 - Google Patents
一种超轻高强壳聚糖纤维织物的制备方法 Download PDFInfo
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Abstract
本发明涉及一种超轻高强壳聚糖纤维织物的制备方法,首先将羧甲基壳聚糖溶于水后,经真空脱泡处理制得交联羧甲基壳聚糖上浆剂,再将壳聚糖纤维浸入交联羧甲基壳聚糖上浆剂中均匀上浆后烘干,然后将上浆后的壳聚糖纤维浸入交联剂溶液中交联,后烘干制得羧甲基壳聚糖上浆壳聚糖纤维,再以羧甲基壳聚糖上浆壳聚糖纤维为原料通过水刺交叉工艺制得制成超轻高强壳聚糖纤维织物。本发明的方法,操作简单、生产成本低、经济环保以及能耗低,采用的上浆方法提升了壳聚糖纤维的力学强度,最终制得产品克重仅为60~280g/m2,其干态下的纵向断裂强度可达55~66.5N/5cm,横向断裂强度可达19~22.5N/5cm,极具应用前景。
Description
技术领域
本发明属于纤维增强领域,涉及一种超轻高强壳聚糖纤维织物的制备方法。
背景技术
纤维是天然或人工合成的细丝状物质.在现代生活中,纤维的应用无处不在,应用最广的为合成纤维,合成纤维的化学组成和天然纤维完全不同,是从一些本身并不含有纤维素或蛋白质的物质如石油、煤、天然气、石灰石或农副产品,先合成单体,再用化学合成与机械加工的方法制成纤维,如聚酯纤维(涤纶)、聚酰胺纤维(锦纶或尼龙)、聚乙烯醇纤维(维纶)、聚丙烯腈纤维(腈纶)、聚丙烯纤维(丙纶)、聚氯乙烯纤维(氯纶)等。
尼龙纤维具有优良的力学性能和电性能,还具有耐磨、耐油、自润滑、耐腐蚀以及良好的加工性能等优点,但PA的吸水性大、低温及干态冲击韧性差、尺寸稳定性差,使其应用范围受到一定的限制。为适应不同领域的特殊要求,需要对PA进行改性,尤其是如何得到集高刚性、高强度和高韧性于一体的增强增韧改性材料,更是研究的热点。申请号为CN201310419384.6,名称为一种超临界CO2中张力作用下改性尼龙纤维的方法的专利申请,其主要技术方案是在一定外加张力作用下使尼龙纤维表面及内部在超临界CO2中与溶剂发生接枝反应,使其强度提高。
聚丙烯腈纤维(PAN)是性能优良的合成纤维,是纺织和工业用的重要纤维原料,在高品质特殊用途的聚丙烯腈原丝的制备过程中往往需要对干燥后的纤维再进行高温蒸汽拉伸,以提高纤维结构的规整度的和力学性能。公开号为CN102851756B,名称为一种聚丙烯腈纤维的拉伸方法的专利申请,其主要技术方案是聚丙烯腈纺丝溶液经过挤出,经过或不经过空气层,进入凝固浴成型,经导辊进入拉伸浴,然后将聚丙烯腈纤维在饱和水蒸汽中进行多级拉伸,提高了纤维的性能。
壳聚糖纤维属于天然材料,其作为组织支架、药物载体等具有促进伤口愈合、防止组织粘连、抗凝血、降脂、降胆固醇、抗溃疡、抗肿瘤等作用,可与其它纤维混纺做服装面料。但受原材料影响,制约壳聚糖纤维发展的主要原因是壳聚糖纤维力学强度不高,常规纺丝得到的壳聚糖纤维的断裂强度仅为1.07cN/dtex,远远达不到实际应用的要求。因此,对壳聚糖纤维进行改性以提高其力学性能具有重要意义。常见增强壳聚糖纤维的方法有:交联增强、复合增强和纺丝成形过程中增强,但至今还未见到交联上浆处理的报道。
纤维应用前一般都需进行上浆处理,上浆的作用主要是对纤维/纱线进行表面浆料的涂覆和纱束间的填充。经纱表面浆料的厚度、均匀性,以及浆料的渗透性对经纱的性能有很大的影响。
传统上浆方式主要是浸浆方式,近年来,高压上浆、预湿上浆、冷上浆及拖浆式上浆等新型上浆方法取得了巨大的进步。其中高压上浆可以紧密纱线结构,增强纤维耐磨性能,降低纤维毛羽,同时可以提高织机效率。预湿上浆可以改善吸浆条件,但它会使浆槽中浆液浓度出现较大波动。普通浸浆方法的浆料分子间主要通过分子间作用力连接,对纤维的力学性能增强有限。
采用交联上浆剂上浆可明显增加纤维/纱线的力学性能。目前交联改性的交联过程都是在上浆之前,交联过程中浆料浓度增大,不利于后续的上浆。
专利CN201510182592.8公开了一种中温纺织上浆方法,其步骤如下:首先制备上浆剂,将所需清水加入到调浆桶中,开动搅拌,将得到的上浆剂干品加入到调浆桶中,将普通未变性的淀粉加入到调浆桶中,搅拌,再次加入上浆剂干品,继续搅拌,然后开始通蒸汽加温,升温后,停止通蒸汽,保温搅拌30分钟,用泵输送到浆槽中,开动浆纱机,开始浆纱。此种方法虽然在浆料中加入了交联剂,但交联反应发生在上浆之前,浆料粘度增大,不利于上浆,此种方法制得的产品浆料分布不匀,产品力学强度提高有限。如能在上浆后再进行交联则可避免这一问题,但目前并未有上浆后交联处理的相关研究成果报道。
因此,亟待需要提供一种操作简单、生产成本低且使壳聚糖纤维力学性能强度显著提高的增强壳聚糖纤维的方法。
发明内容
本发明的目的是针对现有技术中壳聚糖纤维生产成本高和力学性能差等缺点,提供一种上浆交联增强壳聚糖纤维的方法进而将其制成织物,该织物机械性能优良且重量较轻,本发明将羧甲基壳聚糖配制成一定浓度的溶液,对壳聚糖纤维上浆,烘干后浸入交联剂溶液中交联,一方面显著提高壳聚糖纤维的断裂强度和打结强度,另一方面,上浆后再交联避免了交联浆料浓度增大,不利于上浆的问题,此外,较薄的厚度即可满足日常使用的机械强度。
为了达到上述目的,本发明采用的技术方案为:
一种超轻高强壳聚糖纤维织物的制备方法,首先将羧甲基壳聚糖溶于水后,经真空脱泡处理制得交联羧甲基壳聚糖上浆剂,再将壳聚糖纤维浸入交联羧甲基壳聚糖上浆剂中均匀上浆后烘干,然后将上浆后的壳聚糖纤维浸入交联剂溶液中交联,后烘干制得羧甲基壳聚糖上浆壳聚糖纤维,再以羧甲基壳聚糖上浆壳聚糖纤维为原料通过水刺交叉工艺制得制成超轻高强壳聚糖纤维织物;本发明的壳聚糖纤维是复丝纤维,但本发明的保护范围并不仅限于复丝纤维,单丝纤维也可适用于本发明;
所述羧甲基壳聚糖上浆壳聚糖纤维的断裂强度相比于壳聚糖纤维提高了71.7~90.2%,打结强度提高了67.5~88.4%;
所述超轻高强壳聚糖纤维织物的克重为60~280g/m2,其干态下的纵向断裂强度为55~66.5N/5cm,横向断裂强度为19~22.5N/5cm。本发明制得产品性能相较于现有技术提升巨大。
作为优选的技术方案:
如上所述的制备方法,所述羧甲基壳聚糖与水的质量比为2~7:100~150。比例过小,浆料粘度低,上浆率低;比例过大,浆料粘度高,浆料的渗透性差,不利用上浆。
如上所述的制备方法,所述羧甲基壳聚糖溶于水是在200~250rpm的速度下搅拌溶解的。搅拌速率小,溶解时间长;搅拌速率过大,可能会切断壳聚糖大分子链,造成分子量降低。
如上所述的制备方法,所述烘干的温度为45~60℃。烘干温度过高会导致壳聚糖纤维分解。
如上所述的制备方法,所述交联剂溶液为Ca2+的水溶液,其浓度为3~9wt%。浓度低,交联程度不够,而浓度达到9wt%,交联度达到饱和。Ca2+的水溶液不仅可为氯化钙水溶液、磷酸二氢钙水溶液、硝酸钙水溶液、碳酸氢钙水溶液、硫酸氢钙水溶液、亚硫酸氢钙水溶液、次氯酸钙水溶液、溴化钙水溶液、碘化钙水溶液、氯酸钙水溶液、高氯酸钙水溶液、高锰酸钙水溶液,其他含有Ca2+的水溶液也可适用于本发明。
如上所述的制备方法,所述交联的时间为5~10min,交联温度为15~40℃。交联时间短,交联不完全;交联10min,交联度达到饱和,交联度不再随交联时间的增加而增加。
如上所述的制备方法,所述水刺交叉工艺是指以羧甲基壳聚糖上浆壳聚糖纤维为原料,依次经开松、梳理成网、交叉铺网、正反水刺、烘燥处理,其中正面水刺的水针能量为1~1.5MPa、1.5~2MPa、1.5~2MPa,反向水刺的水针能量为2~2.5MPa、2~2.5MPa、1.5~2MPa。
发明机理:
对上浆剂进行交联可明显增加浆料与纤维/纱线的结合的强度,目前现有技术中交联反应一般需要在液态环境下才能发生,即上浆前交联剂与浆料发生交联反应,而交联后的浆料浓度增大,不利于后续的上浆。
本发明采用壳聚糖纤维上浆从未使用过的原位交联技术,先对壳聚糖纤维进行上浆烘干,再将上浆后的壳聚糖纤维浸入交联剂中交联,保证了交联反应在上浆后发生,避免了浆料粘度增加的问题。上浆后交联的处理技术与现有的交联后上浆方式相比,一方面避免了浆料粘度增加的问题,另一方面,上浆后交联其交联剂、浆料与纤维的结合更加紧密,得到产品的交联度及上浆率更佳,产品性能更好,上浆后纤维的断裂强度相比原始纤维提高71.7~90.2%,打结强度提高了67.5~88.4%。进一步以上浆后制成的纤维制造织物,该织物继承了纤维高强的特性,由于织物强度较大,较薄的厚度即可满足日常使用的要求,降低了织物的重量,极具应用前景。
有益效果:
(1)本发明的一种超轻高强壳聚糖纤维织物的制备方法,在上浆后交联,避免了交联浆料浓度增大,不利于上浆的问题,极具应用前景;
(2)本发明的一种超轻高强壳聚糖纤维织物的制备方法,工艺简单,操作方便,成本低廉,易于实现工业化;
(3)本发明的一种超轻高强壳聚糖纤维织物的制备方法,在上浆交联增强后的纤维的基础上制得织物,该织物继承了纤维高强的特性,由于织物强度较大,较薄的厚度即可满足日常使用的要求,降低了织物的重量,极具应用前景。
具体实施方式
下面结合具体实施方式,进一步阐述本发明。应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解,在阅读了本发明讲授的内容之后,本领域技术人员可以对本发明作各种改动或修改,这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例1
一种超轻高强壳聚糖纤维织物的制备方法,步骤如下:首先将羧甲基壳聚糖在230rpm的速度下搅拌溶解于水后,经真空脱泡处理制得交联羧甲基壳聚糖上浆剂,其中羧甲基壳聚糖和水的质量比为6:100,然后将壳聚糖纤维浸入交联羧甲基壳聚糖上浆剂中均匀上浆后在50℃的温度下烘干,最后将上浆后的壳聚糖纤维浸入温度为38℃、浓度为3wt%的高锰酸钙水溶液中交联8min,在45℃的温度下烘干制得羧甲基壳聚糖上浆壳聚糖纤维,再以羧甲基壳聚糖上浆壳聚糖纤维为原料依次经开松、梳理成网、交叉铺网、正反水刺、烘燥处理制得制成超轻高强壳聚糖纤维织物,其中正面水刺的水针能量为1MPa、1.5MPa、1.5MPa,反向水刺的水针能量为2.5MPa、2.5MPa、2MPa。
制得的羧甲基壳聚糖上浆壳聚糖纤维的断裂强度相比于壳聚糖纤维提高了89.0%,打结强度提高了85.1%,最终制得超轻高强壳聚糖纤维织物的克重为60g/m2,其干态下的纵向断裂强度为58N/5cm,横向断裂强度为19N/5cm。
实施例2
一种超轻高强壳聚糖纤维织物的制备方法,步骤如下:首先将羧甲基壳聚糖在250rpm的速度下搅拌溶解于水后,经真空脱泡处理制得交联羧甲基壳聚糖上浆剂,其中羧甲基壳聚糖和水的质量比为5:130,然后将壳聚糖纤维浸入交联羧甲基壳聚糖上浆剂中均匀上浆后在45℃的温度下烘干,最后将上浆后的壳聚糖纤维浸入温度为20℃、浓度为4wt%的溴化钙水溶液中交联6min,在50℃的温度下烘干制得羧甲基壳聚糖上浆壳聚糖纤维,再以羧甲基壳聚糖上浆壳聚糖纤维为原料依次经开松、梳理成网、交叉铺网、正反水刺、烘燥处理制得制成超轻高强壳聚糖纤维织物,其中正面水刺的水针能量为1.5MPa、2MPa、2MPa,反向水刺的水针能量为2MPa、2MPa、1.5MPa。
制得的羧甲基壳聚糖上浆壳聚糖纤维的断裂强度相比于壳聚糖纤维提高了74.3%,打结强度提高了71.5%,最终制得超轻高强壳聚糖纤维织物的克重为180g/m2,其干态下的纵向断裂强度为66.5N/5cm,横向断裂强度为20.5N/5cm。
实施例3
一种超轻高强壳聚糖纤维织物的制备方法,步骤如下:首先将羧甲基壳聚糖在240rpm的速度下搅拌溶解于水后,经真空脱泡处理制得交联羧甲基壳聚糖上浆剂,其中羧甲基壳聚糖和水的质量比为3:140,然后将壳聚糖纤维浸入交联羧甲基壳聚糖上浆剂中均匀上浆后在55℃的温度下烘干,最后将上浆后的壳聚糖纤维浸入温度为33℃、浓度为9wt%的氯酸钙水溶液中交联5min,在55℃的温度下烘干制得羧甲基壳聚糖上浆壳聚糖纤维,再以羧甲基壳聚糖上浆壳聚糖纤维为原料依次经开松、梳理成网、交叉铺网、正反水刺、烘燥处理制得制成超轻高强壳聚糖纤维织物,其中正面水刺的水针能量为1.5MPa、1.8MPa、1.8MPa,反向水刺的水针能量为2.5MPa、2.5MPa、2MPa。
制得的羧甲基壳聚糖上浆壳聚糖纤维的断裂强度相比于壳聚糖纤维提高了83.7%,打结强度提高了81.2%,最终制得超轻高强壳聚糖纤维织物的克重为280g/m2,其干态下的纵向断裂强度为66.5N/5cm,横向断裂强度为22.5N/5cm。
实施例4
一种超轻高强壳聚糖纤维织物的制备方法,步骤如下:首先将羧甲基壳聚糖在200rpm的速度下搅拌溶解于水后,经真空脱泡处理制得交联羧甲基壳聚糖上浆剂,其中羧甲基壳聚糖和水的质量比为7:100,然后将壳聚糖纤维浸入交联羧甲基壳聚糖上浆剂中均匀上浆后在60℃的温度下烘干,最后将上浆后的壳聚糖纤维浸入温度为25℃、浓度为5wt%的硫酸氢钙水溶液中交联9min,在60℃的温度下烘干制得羧甲基壳聚糖上浆壳聚糖纤维,再以羧甲基壳聚糖上浆壳聚糖纤维为原料依次经开松、梳理成网、交叉铺网、正反水刺、烘燥处理制得制成超轻高强壳聚糖纤维织物,其中正面水刺的水针能量为1.2MPa、1.6MPa、1.7MPa,反向水刺的水针能量为2.4MPa、2.4MPa、1.8MPa。
制得的羧甲基壳聚糖上浆壳聚糖纤维的断裂强度相比于壳聚糖纤维提高了90.2%,打结强度提高了85.4%,最终制得超轻高强壳聚糖纤维织物的克重为80g/m2,其干态下的纵向断裂强度为55N/5cm,横向断裂强度为20N/5cm。
实施例5
一种超轻高强壳聚糖纤维织物的制备方法,步骤如下:首先将羧甲基壳聚糖在210rpm的速度下搅拌溶解于水后,经真空脱泡处理制得交联羧甲基壳聚糖上浆剂,其中羧甲基壳聚糖和水的质量比为2:150,然后将壳聚糖纤维浸入交联羧甲基壳聚糖上浆剂中均匀上浆后在45℃的温度下烘干,最后将上浆后的壳聚糖纤维浸入温度为30℃、浓度为7wt%的碳酸氢钙水溶液中交联10min,在45℃的温度下烘干制得羧甲基壳聚糖上浆壳聚糖纤维,再以羧甲基壳聚糖上浆壳聚糖纤维为原料依次经开松、梳理成网、交叉铺网、正反水刺、烘燥处理制得制成超轻高强壳聚糖纤维织物,其中正面水刺的水针能量为1.2MPa、1.6MPa、1.7MPa,反向水刺的水针能量为2.2MPa、2.4MPa、1.5MPa。
制得的羧甲基壳聚糖上浆壳聚糖纤维的断裂强度相比于壳聚糖纤维提高了77.9%,打结强度提高了69.8%,最终制得超轻高强壳聚糖纤维织物的克重为280g/m2,其干态下的纵向断裂强度为66.5N/5cm,横向断裂强度为21.6N/5cm。
实施例6
一种超轻高强壳聚糖纤维织物的制备方法,步骤如下:一种壳聚糖纤维交联羧甲基壳聚糖的上浆方法,首先将羧甲基壳聚糖在250rpm的速度下搅拌溶解于水后,经真空脱泡处理制得交联羧甲基壳聚糖上浆剂,其中羧甲基壳聚糖和水的质量比为4:130,然后将壳聚糖纤维浸入交联羧甲基壳聚糖上浆剂中均匀上浆后在50℃的温度下烘干,最后将上浆后的壳聚糖纤维浸入温度为20℃、浓度为6wt%的硝酸钙水溶液中交联7min,在50℃的温度下烘干制得羧甲基壳聚糖上浆壳聚糖纤维,再以羧甲基壳聚糖上浆壳聚糖纤维为原料依次经开松、梳理成网、交叉铺网、正反水刺、烘燥处理制得制成超轻高强壳聚糖纤维织物,其中正面水刺的水针能量为1.4MPa、1.6MPa、1.8MPa,反向水刺的水针能量为2MPa、2MPa、1.7MPa。
制得的羧甲基壳聚糖上浆壳聚糖纤维的断裂强度相比于壳聚糖纤维提高了71.7%,打结强度提高了77.5%,最终制得超轻高强壳聚糖纤维织物的克重为150g/m2,其干态下的纵向断裂强度为60.2N/5cm,横向断裂强度为22.2N/5cm。
实施例7
一种超轻高强壳聚糖纤维织物的制备方法,步骤如下:首先将羧甲基壳聚糖在220rpm的速度下搅拌溶解于水后,经真空脱泡处理制得交联羧甲基壳聚糖上浆剂,其中羧甲基壳聚糖和水的质量比为5:100,然后将壳聚糖纤维浸入交联羧甲基壳聚糖上浆剂中均匀上浆后在45℃的温度下烘干,最后将上浆后的壳聚糖纤维浸入温度为40℃、浓度为9wt%的磷酸二氢钙水溶液中交联6min,在40℃的温度下烘干制得羧甲基壳聚糖上浆壳聚糖纤维,再以羧甲基壳聚糖上浆壳聚糖纤维为原料依次经开松、梳理成网、交叉铺网、正反水刺、烘燥处理制得制成超轻高强壳聚糖纤维织物,其中正面水刺的水针能量为1.5MPa、2MPa、1.5MPa,反向水刺的水针能量为2MPa、2.5MPa、1.6MPa。
制得的羧甲基壳聚糖上浆壳聚糖纤维的断裂强度相比于壳聚糖纤维提高了83.1%,打结强度提高了88.4%。最终制得超轻高强壳聚糖纤维织物的克重为170g/m2,其干态下的纵向断裂强度为66.5N/5cm,横向断裂强度为19.5N/5cm。
实施例8
一种超轻高强壳聚糖纤维织物的制备方法,步骤如下:首先将羧甲基壳聚糖在200rpm的速度下搅拌溶解于水后,经真空脱泡处理制得交联羧甲基壳聚糖上浆剂,其中羧甲基壳聚糖和水的质量比为3:120,然后将壳聚糖纤维浸入交联羧甲基壳聚糖上浆剂中均匀上浆后在55℃的温度下烘干,最后将上浆后的壳聚糖纤维浸入温度为15℃、浓度为3wt%的氯化钙水溶液中交联8min,在55℃的温度下烘干制得羧甲基壳聚糖上浆壳聚糖纤维,再以羧甲基壳聚糖上浆壳聚糖纤维为原料依次经开松、梳理成网、交叉铺网、正反水刺、烘燥处理制得制成超轻高强壳聚糖纤维织物,其中正面水刺的水针能量为1.5MPa、1.5MPa、1.5MPa,反向水刺的水针能量为2MPa、2MPa、2MPa。
制得的羧甲基壳聚糖上浆壳聚糖纤维的断裂强度相比于壳聚糖纤维提高了78.2%,打结强度提高了67.5%,最终制得超轻高强壳聚糖纤维织物的克重为220g/m2,其干态下的纵向断裂强度为64.5N/5cm,横向断裂强度为19.8N/5cm。
Claims (7)
1.一种超轻高强壳聚糖纤维织物的制备方法,其特征是:首先将羧甲基壳聚糖溶于水后,经真空脱泡处理制得交联羧甲基壳聚糖上浆剂,再将壳聚糖纤维浸入交联羧甲基壳聚糖上浆剂中均匀上浆后烘干,然后将上浆后的壳聚糖纤维浸入交联剂溶液中交联,后烘干制得羧甲基壳聚糖上浆壳聚糖纤维,再以羧甲基壳聚糖上浆壳聚糖纤维为原料通过水刺交叉工艺制得制成超轻高强壳聚糖纤维织物;
所述羧甲基壳聚糖上浆壳聚糖纤维的断裂强度相比于壳聚糖纤维提高了71.7~90.2%,打结强度提高了67.5~88.4%;
所述超轻高强壳聚糖纤维织物的克重为60~280g/m2,其干态下的纵向断裂强度为55~66.5N/5cm,横向断裂强度为19~22.5N/5cm。
2.根据权利要求1所述的制备方法,其特征在于,所述羧甲基壳聚糖与水的质量比为2~7:100~150。
3.根据权利要求1所述的制备方法,其特征在于,所述羧甲基壳聚糖溶于水是在200~250rpm的速度下搅拌溶解的。
4.根据权利要求1所述的制备方法,其特征在于,所述烘干的温度为45~60℃。
5.根据权利要求1所述的制备方法,其特征在于,所述交联剂溶液为Ca2+的水溶液,其浓度为3~9wt%。
6.根据权利要求1所述的制备方法,其特征在于,所述交联的时间为5~10min,交联温度为15~40℃。
7.根据权利要求1所述的制备方法,其特征在于,所述水刺交叉工艺是指以羧甲基壳聚糖上浆壳聚糖纤维为原料,依次经开松、梳理成网、交叉铺网、正反水刺、烘燥处理,其中正面水刺的水针能量为1~1.5MPa、1.5~2MPa、1.5~2MPa,反向水刺的水针能量为2~2.5MPa、2~2.5MPa、1.5~2MPa。
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