CN107321333A - 一种吸附染料离子的水凝胶微球的制备方法 - Google Patents

一种吸附染料离子的水凝胶微球的制备方法 Download PDF

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CN107321333A
CN107321333A CN201710729047.5A CN201710729047A CN107321333A CN 107321333 A CN107321333 A CN 107321333A CN 201710729047 A CN201710729047 A CN 201710729047A CN 107321333 A CN107321333 A CN 107321333A
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刘钦泽
胡涛
董开杰
魏刚
高嵩
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Boglong (Zhejiang) Biotechnology Co.,Ltd.
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Abstract

本发明公开了一种吸附染料离子的水凝胶微球的制备方法。所述微球包含聚乙烯醇（PVA）、单宁酸（TA）、海藻酸钠（SA）。该微球制备步骤如下：先将聚乙烯醇和海藻酸钠完全混合溶解在水中，再加入一定量的单宁酸使其反应并混合均匀，最后用注射器将混合液滴入氯化钙‑硼酸饱和溶液中制成水凝胶微球。本发明制备的水凝胶微球稳定性好，不会发生团聚现象，制备工艺简单、操作性强、重复性好、成本低廉、性能稳定，可循环利用并无二次污染，在染料污水处理领域中得到广泛应用。

Description

一种吸附染料离子的水凝胶微球的制备方法
技术领域
本发明涉及吸附剂的制备，具体涉及一种吸附染料离子的水凝胶微球的制备方法。
背景技术
环境污染是当今世界面临的严峻的问题之一，也是急需解决的棘手问题之一。近年来，由于环境中的污染物含有大量的有毒物质，受到人们的广泛关注，尤其是排放废水的有机染料。这些毒性染料很容易随自然循环扩散到环境中，其产生于许多地方，主要为使用染料颜色产品的工厂，如纺织、造纸、染料、塑料等行业。大多数染料具有非生物降解性和致癌的作用，能通过饮用水进入生物体内，直接破坏人体的正常器官组织，危害生物体的健康安全。因此，一旦大量的染料分子积累在环境中，长期的毒性危害不容忽视。例如，染料的存在阻碍了水的审美质量，并可以减少在水生生态系统中阳光和氧气的渗透，影响水体系的正常流动。
到目前为止，已经开发了几种传统的方法，用来去除这些污染物的染料废水，包括生物处理、混凝/絮凝、化学氧化、膜过滤、光催化和吸附法等。上述方法大多有明显的去除效果，但需要大量的资金投入或高能量的设备，经济效益较差。然而，基于经济、环保、可持续的功能等优点，吸附法受到科研人员的较大关注，被认为是非常有前景的水处理方式。公开号为CN104525152A的专利公开了一种将酸化凹凸棒（PGS）与丙烯酰胺（AM）和2-丙烯酰胺-2-甲基丙磺酸（AMPS）共聚而得新型水凝胶吸附水溶液中的染料离子。公开号为CN104645947A的专利公开了一种选择性吸附污水中染料的氧化石墨烯基超分子水凝胶的制备方法，方法如下：（1）氧化石墨烯水溶液的配制,（2）掺有氧化石墨烯的a-环糊精水溶液的配制,（3）氧化石墨烯基超分子水凝胶的配制。通过改变掺入氧化石墨烯的量可以调节染料吸附的速率。公开号CN104829788A的专利公开了一种制备壳聚糖/2-丙烯酰胺基-2-甲基丙磺酸（CS/AMPS）水凝胶的新方法,是以壳聚糖、2-丙烯酰胺基-2-甲基丙磺酸为原料，N,N’-亚甲基双丙烯酰胺（MBA）为交联剂，在水溶液体系中直接进行交联反应而得，在染料和重金属离子废水净化方面具有广阔的应用前景。
水凝胶是一种经适度交联而具有三维网络结构的高分子材料,因其独特的吸水、保水及仿生特性,水凝胶被广泛应用于工业、农业、医药和生物工程材料等领域。近年来,水凝胶作为一种新型吸附材料,在环境水处理领域受到愈来愈多的重视,因其特殊的三维结构使之具有更大的空隙,易将客体（微生物、功能纳米粒子）固定在三维网络中,一方面提供吸附污染物的场所,另一方面防止客体泄露而造成二次污染。
聚乙烯醇（PVA）是一种无毒、生物可降解水溶性高分子材料,具有优异的力学性能、pH值稳定性和生物相容性,在染料污水处理中具有可循环利用,生物可降解,无二次污染等优点。因此,聚乙烯醇复合水凝胶在染料废水治理方面具有广阔的应用前景。
发明内容
本发明提供一种吸附染料离子的水凝胶微球的制备方法，该制备方法操作方便、过程简单、工艺可控、重复性好、成本低廉、便于推广使用，制得的水凝胶微球吸附材料具有良好的染料污染物的性能，同时还可以减少污染、清洁环境，具有广泛的应用前景。
为实现本发明的目的，提供以下技术方案：
一种吸附染料离子的水凝胶微球的制备方法，其特征在于以下步骤：
（1）将一定质量的聚乙烯醇、海藻酸钠、去离子水加入三口瓶中并置于85～100℃的水中，机械搅拌1～4h使其完全溶解并混合均匀;
（2）将上述溶液降至50～80℃的水浴中加热，同时加入一定量的单宁酸，并搅拌0.5～1.5h，使混合液混合均匀;
（3）将以上制备好的混合液采用注射器滴入氯化钙-硼酸饱和溶液中进行化学交联制备成粒径大小为1.0～1.5mm的均一的球形颗粒水凝胶并浸泡6～18h，最后用去离子水冲洗2～4次，冷冻干燥，即可制得水凝胶微球。
进一步的，所述的聚乙烯醇和海藻酸钠的质量比为1:0.1～0.16。
进一步的，所述的聚乙烯醇的浓度为10～60g/L,优选为33g/L。
进一步的，所述的加入聚乙烯醇和单宁酸的质量比为1: 0.011～0.11。
进一步的，所述的步骤（2）中，将上述溶液降至50～80℃的水浴中加热，优选为65℃。
进一步的，所述的步骤（2）中单宁酸的浓度为0.37～7.4 g/L，优选为3.7 g/L。
进一步的，所述的水凝胶微球的用途,其特征在于,所述复合水凝胶用于吸附染料离子。
本发明具有以下有益效果：
（a）本发明的水凝胶微球制备工艺简单,操作性强且制备的水凝胶性能稳定,可循环利用并无二次污染,利于环境可持续发展;
（b）本发明的水凝胶微球具有快速高效、高吸附容量的特点,对染料离子的吸附具有显著的效果;
（c）本发明的水凝胶微球性能稳定、再生重复利用性好,易于分离的特点,即可用于工业染料污水处理,也可用于生活饮用水中染料离子的吸附。
具体实施方式
下面通过具体实施方式对本发明作进一步说明。以下实施例旨在说明本发明而不是对本发明的进一步限定。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：
称取2g聚乙烯醇、0.26g海藻酸钠和60ml去离子水加入三口烧瓶中，在95℃的水浴中加热，机械搅拌2h使其完全混合均匀，然后在65℃的水浴中加热2h，再加入0.22g单宁酸，并用机械搅拌1h。将上述制备好的混合液用注射器缓慢滴入到3%氯化钙-硼酸饱和溶液中制备粒径为1.0～1.5mm水凝胶小球，并固化24h，最后用去离子水洗涤3次，冷冻干燥。
通过以上方法制得的水凝胶微球吸附材料对亚甲基蓝的吸附量为150mg/g。
实施例2：
称取2g聚乙烯醇、0.26g海藻酸钠和60ml去离子水加入三口烧瓶中，在95℃的水浴中加热，机械搅拌2h使其完全混合均匀，然后在65℃的水浴中加热2h，再加入0.088g单宁酸，并用机械搅拌1h。将上述制备好的混合液用注射器缓慢滴入到3%氯化钙-硼酸饱和溶液中制备粒径为1.0～1.5mm水凝胶小球，并固化24h，最后用去离子水洗涤3次，冷冻干燥。
通过以上方法制得的水凝胶微球吸附材料对亚甲基蓝的吸附量为119mg/g。
实施例3：
称取2g聚乙烯醇、0.26g海藻酸钠和60ml去离子水加入三口烧瓶中，在95℃的水浴中加热，机械搅拌2h使其完全混合均匀，然后在65℃的水浴中加热2h，再加入0.044g单宁酸，并用机械搅拌1h。将上述制备好的混合液用注射器缓慢滴入到3%氯化钙-硼酸饱和溶液中制备粒径为1.0～1.5mm水凝胶小球，并固化24h，最后用去离子水洗涤3次，冷冻干燥。
通过以上方法制得的水凝胶微球吸附材料对刚果红的吸附量为191mg/g。
实施例4：
称取2g聚乙烯醇、0.26g海藻酸钠和60ml去离子水加入三口烧瓶中，在95℃的水浴中加热，机械搅拌2h使其完全混合均匀，然后在65℃的水浴中加热2h，再加入0.0225g单宁酸，并用机械搅拌1h。将上述制备好的混合液用注射器缓慢滴入到3%氯化钙-硼酸饱和溶液中制备粒径为1.0～1.5mm水凝胶小球，并固化24h，最后用去离子水洗涤3次，冷冻干燥。
通过以上方法制得的水凝胶微球吸附材料对亚甲基蓝的吸附量为83mg/g。
实施例5：
对比示例
称取2g聚乙烯醇、0.26g海藻酸钠和60ml去离子水加入三口烧瓶中，在95℃的水浴中加热，机械搅拌2h使其完全混合均匀，然后在65℃的水浴中加热2h。将上述制备好的混合液用注射器缓慢滴入到3%氯化钙-硼酸饱和溶液中制备粒径为1.0～1.5mm水凝胶小球，并固化24h，最后用去离子水洗涤3次，冷冻干燥。
通过以上方法制得的水凝胶微球吸附材料对亚甲基蓝的吸附量为75mg/g。

Claims (7)

1.一种吸附染料离子的水凝胶微球的制备方法，其特征在于以下步骤：
（1）将一定质量的聚乙烯醇、海藻酸钠、去离子水加入三口瓶中并置于85～100℃的水中，机械搅拌1～4h使其完全溶解并混合均匀。
（2）将上述溶液降至50～80℃的水浴中加热，同时加入一定量的单宁酸，并搅拌0.5～1.5h，使混合液混合均匀。
（3）将以上制备好的混合液采用注射器滴入氯化钙-硼酸饱和溶液中进行化学交联制备成粒径大小为1.0～1.5mm的均一的球形颗粒水凝胶并浸泡6～18h，最后用去离子水冲洗2～4次，冷冻干燥，即可制得水凝胶微球。
2.根据权利要求1所述的聚乙烯醇和海藻酸钠的质量比为1:0.1～0.16。
3.根据权利要求1所述的聚乙烯醇的浓度为10～60g/L,优选为33g/L。
4.根据权利要求1所述的加入聚乙烯醇和单宁酸的质量比为1:0.011～0.11。
5.根据权利要求1所述的步骤（2）中，将上述溶液降至50～80℃的水浴中加热，优选为65℃。
6. 根据权利要求1所述的步骤（2）中单宁酸的浓度为0.37～7.4 g/L，优选为3.7 g/L。
7.权利要求1-6任一项所述的水凝胶微球的用途,其特征在于,所述复合水凝胶用于吸附染料离子。
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