CN109137503A - 螯合聚丙烯腈纤维材料的制备方法 - Google Patents
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Abstract
本发明涉及螯合聚丙烯腈纤维材料的制备方法,该技术是为了满足不同工业和市场应用需要达到更高纯的化学成分的需求而产生的。该功能化螯合聚丙烯腈纤维材料可用来从产品、工艺过程和废液中去除有机和无机化合物,气体净化与分离,阳离子和阴离子交换剂,金属层析材料,固相净化或提取材料,生物分子固定材料,固相合成材料和色谱材料等。本发明具有工艺流程简单、操作方便、效果稳定,投资少,材料可再生循环使用等优点。
Description
技术领域
本发明属于高分子材料技术领域,尤其涉及螯合聚丙烯腈纤维材料的制备方法。
背景技术
对常见的合成纤维或天然纤维进行功能化改性,使之既能保持纤维原有的特点与优点,又具备各种特殊的性能与用途,这一领域的研究近年来日益受到人们的关注。化学改性是对纤维进行功能化的重要手段,利用纤维表面所带有的化学基团,通过与特定的分子或离子发生化学反应,使纤维表面引入特定的官能基团,从而使纤维具备特定的化学属性,如去除有机和无机化合物,气体净化与分离,阳离子和阴离子交换剂,金属层析材料,固相净化或提取材料,生物分子固定材料,固相合成材料和色谱材料等新功能。
中国专利CN200910228776.8“一种含羧基和季氨基的离子交换纤维的制备方法”,将聚丙烯纤维在丙烯酸水溶液中用60Co γ-射线辐射,获得接枝丙烯酸的聚丙烯接枝纤维,然后再在甲基丙烯酰氧乙基三甲基氯化铵的溶液中进行紫外辐照,获得同时含有羧基和季氨基团的纤维材料。中国专利CN01142191“一种制备功能性离子交换纤维的新方法”,提出了用聚乙烯醇纤维先在脱水剂中预处理,再在高温下进行半碳化,后经酯化、浓硫酸磺化制备出一种功能性阳离子交换纤维。中国专利CN02129051.2“一种螯合功能纤维及合成方法”,将聚丙烯腈纤维依次经过水解、引入金属离子“桥”、涂敷聚乙烯亚胺、化学交联和转型,得到具有良好吸附功能的螯合纤维材料。
本专利发明提出了以商品化的聚丙烯腈纤维为原材料,通过第一步引入胺源:将一定体积的氨基化合物(或加入一定量的去离子水),投入反应釜中,搅拌均匀后加入一定量的聚丙烯腈纤维,原材料聚丙烯腈纤维的质量:氨基化合物的质量=1:3~1:50,反应温度为50~140℃,反应时间为1~20 h,反应结束后取出纤维,用去离子水洗涤,在50~80℃温度下烘干至恒重;第二步胺化反应:将一定量的氨基纤维放入0.1-1 mol/L的氢氧化钠溶液中溶胀12 h后加入二硫化碳,然后在50℃条件下反应36 h,所得产物经甲苯、乙醇等反复洗涤至无二硫化碳气味后,再用去离子水洗涤,在50~80℃温度下烘干至恒重,得到新型螯合聚丙烯腈纤维材料。本发明工艺简单,易于控制,操作可靠性高,效果稳定,投资少,材料可再生循环使用等优点。
综合现有技术,通过化学试剂直接改性纤维的合成方法报道较少。本发明采用特定的化学工艺改性聚丙烯腈纤维为基体材料,通过简单的反应使大分子在纤维上达到可观的接枝量和达到特定的功能化效果,目前尚未见有相同的报道。
发明内容
本发明的目的在于提供一类新型螯合聚丙烯腈纤维材料,又在于提供一种原料易得、操作简单、环境友好的功能化合成方法。本发明大大的提高了大分子官能团的接枝量,不仅保持纤维原有的特点与优点,又具备各种特殊的性能与用途,极大的提高了纤维的功能特性和应用范围,使其具备去除有机和无机化合物,气体净化与分离,阳离子和阴离子交换剂,金属层析材料,固相净化或提取材料,生物分子固定材料,固相合成材料和色谱材料等新属性。
本发明的技术方案是:一种螯合聚丙烯腈纤维材料的制备方法,主要包括以下步骤:
(1)制备胺源:将一定体积的氨基化合物(或加入一定量的去离子水),投入反应釜中,搅拌均匀后加入一定量的聚丙烯腈纤维,原材料聚丙烯腈纤维的质量:氨基化合物的质量=1:3~1:50,反应温度为50~140℃,反应时间为1~20 h,反应结束后取出纤维,用去离子水洗涤,在50~80℃温度下烘干至恒重,得到含氨基纤维材料;
(2)胺化反应:将一定量的氨基纤维放入0.1-1 mol/L的氢氧化钠溶液中溶胀12 h后加入二硫化碳,然后在50℃条件下反应36 h,所得产物经甲苯、乙醇等反复洗涤至无二硫化碳气味后,再用去离子水洗涤,在50~80℃温度下烘干至恒重。
本发明的优点和积极效果是:
1、本发明采用聚丙烯腈纤维材料作为基体材料,改良传统的聚丙烯纤维、聚乙烯醇纤维等只能采用辐射发接枝的工艺,创新采用直接化学改性法;
2、本发明采用一步法引入胺源工艺,通过纯溶剂法或加入少量去离子水工艺,使剩余的胺源可以循环使用,既节约了反应原料,又避免溶剂浪费,破坏环境;
3、本发明中胺化反应结束后的洗涤有机溶剂,可以反复循环利用,未反应的原料可以分离提取,避免了环境污染,无三废产生;
4、本发明选用的原料丰富,价格低廉,本发明工艺简单,易于控制,操作可靠性强,使用范围较广。
附图说明
图1为本发明功能化改性聚丙烯腈纤维的化学反应(片段)示意路线图。
具体实施方式
实施例1
将600 mL二乙烯溶剂直接放入反应瓶里,搅拌均匀后,加入15 g聚丙烯腈纤维,在105℃下搅拌均匀反应4 h。反应结束后,冷却取出纤维,用70℃去离子水洗涤至中性,得到淡黄色含氨基纤维材料。将10 g含氨基纤维材料放入600 mL 0.25 mol/L的氢氧化钠溶液中溶胀12 h,加入400 mL二硫化碳,然后在50℃条件下反应36 h,所得产物经乙醇等反复洗涤至无二硫化碳气味后,再用去离子水洗涤,在50~80℃温度下烘干至恒重。
实施例2
将750 mL二乙烯三胺溶剂直接放入反应瓶里,搅拌均匀后,加入15 g聚丙烯腈纤维,在115℃下搅拌均匀反应3.5 h。反应结束后,冷却取出纤维,用70℃去离子水洗涤至中性,得到淡黄色含氨基纤维材料。将5 g含氨基纤维材料放入300 mL 0.25 mol/L的氢氧化钠溶液中溶胀12 h,加入250 mL二硫化碳,然后在50℃条件下反应36 h,所得产物经乙醇等反复洗涤至无二硫化碳气味后,再用去离子水洗涤,在50~80℃温度下烘干至恒重。
实施例3
将750 mL多乙烯多胺溶剂直接放入反应瓶里,搅拌均匀后,加入15 g聚丙烯腈纤维,在110℃下搅拌均匀反应3 h。反应结束后,冷却取出纤维,用70℃去离子水洗涤至中性,得到淡黄色含氨基纤维材料。将5 g含氨基纤维材料放入150 mL 0.25 mol/L的氢氧化钠溶液中溶胀12 h,然后加入150 mL丙醇,再加入400 mL二硫化碳,然后在50℃条件下反应36 h,所得产物经乙醇等反复洗涤至无二硫化碳气味后,再用去离子水洗涤,在50~80℃温度下烘干至恒重。
以上三种技术配方显示和描述了本发明的基本原理、主要特征和本发明的优点。本行业技术人员应该了解,本发明不受上述实施例的限制,以上实施例和说明书中描述的只说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书以及等效物界定。
Claims (5)
1.螯合聚丙烯腈纤维材料的制备方法,主要包括以下步骤:
(1)制备胺源:以聚丙烯腈纤维为原材料纤维,通过纤维与氨基化合物的化学反应引入胺源,得到含氨基纤维材料;
(2)胺化反应:在强碱性条件下,加入二硫化碳与步骤(1)中得到的含氨基纤维材料进行反应,反应后用清水洗涤干净得到目标产物。
2.根据权利要求1所述的方法,其特征在于所述的氨基化合物为:乙二胺、二乙烯三胺、三乙烯四胺、四乙烯五胺、多乙烯多胺等中的任意一种或多种。
3.根据权利要求1所述的方法,其特征在于所述的制备胺源的反应条件为:将一定体积的氨基化合物(或加入一定量的去离子水),投入反应釜中,搅拌均匀后加入一定量的聚丙烯腈纤维,原材料聚丙烯腈纤维的质量:氨基化合物的质量=1:3~1:50,反应温度为50~140℃,反应时间为1~20 h,反应结束后取出纤维,用去离子水洗涤,在50~80℃温度下烘干至恒重。
4.根据权利要求1所述的方法,其特征在于所述的胺化反应条件为:将一定量的氨基纤维放入0.1-1 mol/L的氢氧化钠溶液中溶胀12 h后加入二硫化碳,然后在50℃条件下反应36 h,所得产物经甲苯、乙醇等反复洗涤至无二硫化碳气味后,再用去离子水洗涤,在50~80℃温度下烘干至恒重。
5.根据权利要求1所述的方法,其特征在于所述的原材料聚丙烯腈纤维为长度为1~10cm,纤度为1~5 dtex,纤维分子结构中含有90%以上的丙烯腈单元的商品纤维或腈纶织物。
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