CN114505059A - 一种多孔纤维素纳米晶-海藻酸钠凝胶微球的制备方法 - Google Patents
一种多孔纤维素纳米晶-海藻酸钠凝胶微球的制备方法 Download PDFInfo
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Abstract
本发明涉及一种多孔纤维素纳米晶‑海藻酸钠凝胶微球的制备方法，属于高分子材料领域。包括如下步骤：常温条件下，分别在超纯水中加入CNC，然后加入NaHCO3和海藻酸钠，恒温搅拌至海藻酸钠完全溶解后加入CaCO3，继续搅拌至CaCO3均匀分布，配制成含CNC的海藻酸钠溶液，超声脱泡后静置，借助推进设备，将海藻酸钠溶液匀速滴入盛有交联液的低速搅拌的烧杯中，滴制完毕后高速搅拌30min，过滤多孔微球，反复冲洗至清洗液pH值为7，得到多孔CNC‑ALG凝胶微球。其吸附表面积大、电负性强、机械性能好、吸附去除率高、环境友好，对于充分利用生物质资源、解决染料废水污染问题具有重要的实际意义。
Description
技术领域
本发明属于高分子材料技术领域，具体涉及一种多孔纤维素纳米晶-海藻酸钠凝胶微球的制备方法。
背景技术
水是国家保持繁荣昌盛必不可少的资源。由于人类的工业活动和人口迅速增长，人们对净水的需求也在不断增加。地表水和地下水大都受到了工业、农业和市政等污废水的污染。近年来，随着全球经济的发展，人类消费水平的提高，人们对于纺织品的需求量以惊人的速度增长，纺织、皮革、橡胶、塑料和纸张等行业逐渐增多，与此同时，伴生了大量废水的排放。在这些污染水体的污染物中，来自纺织工业的染料废水成为一个主要问题，排放到水体的染料废水的量十分可观。由于染料及助剂种类繁多、应用广泛，含染料的印染废水已经成为工业废水中重要的组成部分。
海藻酸钠(ALG)是一种阴离子天然多糖，主要来源于藻类等生物体。海藻酸钠分子链上大量的羟基、羧基可以吸附金属离子和有机污染物，因其生物相容性高、低毒性和在钙离子存在下的温和凝胶化，在食品、水处理、制药行业等领域中得到了广泛的应用。
纤维素纳米晶(CNC)是去除无定形态纤维素后获得的棒状晶体，由于天然胶质及非晶态纤维素被大量去除，CNC具有相对完善的结晶结构，表现出高结晶度、高强度和高模量的特征，且具有良好的热稳定性。CNC具有纳米尺寸，经适当改性后具有良好的分散性，可用于印染废水处理。
乳化交联法因其过程简便且成球形貌较好成为一种海藻酸钠凝胶球的比较传统的制备方法，该方法得到的微球粒径范围介于1～100μm。该方法涉及的实验步骤是将含有表面活性剂的有机溶剂和海藻酸钠溶液形成稳定的油包水乳液，最后掺入钙离子或其他的交联剂进行交联和固化，借助表面活性剂去除油相，最终得到海藻酸钠微球。因此，开发一种环境友好的多孔海藻酸钠微球吸附剂，对于充分利用生物质资源、解决染料废水污染问题具有重要的实际意义。
发明内容
本发明以海藻酸钠作为原材料，通过加入复合材料CNC，制备了环境友好的多孔海藻酸钠微球吸附剂。藻酸盐水凝胶球因固有的离子电荷和多孔结构使其具备较强的吸附能力，从而具有高吸附容量和可再循环性。将CNC结合到海藻酸钠水凝胶系统中，使其吸附表面积更大、电负性更强、机械性能更好。
为实现上述目的，本发明采用的技术方案为：一种多孔纤维素纳米晶-海藻酸钠凝胶微球的制备方法，包括如下步骤：
1)常温条件下，在50mL超纯水中加入CNC，然后加入0.2g NaHCO3和1g海藻酸钠，70℃恒温搅拌至海藻酸钠完全溶解后加入1g CaCO3，继续搅拌至CaCO3均匀分布，配制成含CNC的海藻酸钠溶液；
2)将步骤1)配制成的海藻酸钠溶液超声脱泡后静置，借助推进设备，将海藻酸钠溶液匀速滴入盛有交联液的低速搅拌的烧杯中，滴制完毕后高速搅拌30min，得到多孔微球与交联液的混合液；
3)将步骤2)得到的多孔微球过滤，反复冲洗至清洗液pH值为7，得到多孔CNC-ALG凝胶微球。
进一步的，上述的制备方法，步骤1)中，CNC加入量为0.05g或0.1g。
进一步的，上述的制备方法，步骤2)中，交联液是按体积比含3％乙酸和6％乙醇的水溶液。
进一步的，上述的制备方法，步骤2)中，低速搅拌速度为200rpm。
进一步的，上述的制备方法，步骤2)中，高速搅拌速度为600rpm。
进一步的，上述的制备方法，制备得到的多孔CNC-ALG凝胶微球25℃下保存。
按照上述的方法制备的多孔纤维素纳米晶-海藻酸钠凝胶微球在吸附偶氮染料中的应用。
本发明的有益效果为：
1、本发明以海藻酸钠作为原材料，通过加入复合材料CNC，制备得到的多孔CNC-ALG凝胶微球吸附剂环境友好。
2、将CNC结合到海藻酸钠水凝胶系统中，使其吸附表面积更大、电负性更强、机械性能更好。
3、本发明制备得到的多孔CNC-ALG凝胶微球吸附偶氮染料吸附去除率高，对于充分利用生物质资源、解决染料废水污染问题具有重要的实际意义。
附图说明
图1是多孔5％CNC-ALG凝胶微球吸附一级动力学拟合曲线
图2是多孔10％CNC-ALG凝胶微球吸附一级动力学拟合曲线
具体实施方式
实施例1多孔10％CNC-ALG凝胶微球的制备
包括如下步骤：
1)常温条件下，在50mL超纯水中加入0.1g CNC，然后加入0.2g NaHCO3和1g海藻酸钠，70℃恒温搅拌至海藻酸钠完全溶解后加入1g CaCO3，继续搅拌至CaCO3均匀分布，配制成含10％CNC的海藻酸钠溶液；
2)将步骤1)配制成的海藻酸钠溶液超声脱泡后静置，借助推进设备，将海藻酸钠溶液匀速滴入盛有含3％乙酸和6％乙醇的交联液的低速搅拌的烧杯中，滴制完毕后高速搅拌30min，搅拌速度为600rpm，得到多孔微球与交联液的混合液；
3)将步骤2)得到的多孔微球过滤，用超纯水反复冲洗至清洗液pH值为7，得到多孔10％CNC-ALG凝胶微球，25℃下保存。
实施例2多孔5％CNC-ALG凝胶微球的制备
包括如下步骤：
1)常温条件下，在50mL超纯水中加入0.05g CNC，然后加入0.2g NaHCO3和1g海藻酸钠，70℃恒温搅拌至海藻酸钠完全溶解后加入1g CaCO3，继续搅拌至CaCO3均匀分布，配制成含5％CNC的海藻酸钠溶液；
2)将步骤1)配制成的海藻酸钠溶液超声脱泡后静置，借助推进设备，将海藻酸钠溶液匀速滴入盛有含3％乙酸和6％乙醇的交联液的低速搅拌的烧杯中，滴入的速度、高度、搅拌速度、搅拌时间与实施例1步骤2)一致，滴制完毕后高速搅拌30min，搅拌速度为600rpm，得到多孔微球与交联液的混合液；
3)将步骤2)得到的多孔微球过滤，用超纯水反复冲洗至清洗液pH值为7，得到多孔5％CNC-ALG凝胶微球，25℃下保存。
实施例3多孔纤维素纳米晶-海藻酸钠凝胶微球吸附染料废水试验
1)按照实施例1和实施例2的制备方法，制备多孔10％和5％CNC-ALG凝胶微球；
2)使用50mg/L的亚甲基蓝(MB)溶液来模拟染料废水，分别称取1.2g多孔5％CNC-ALG凝胶微球和1.2g多孔10％CNC-ALG凝胶微球，分别加入到40ml MB溶液中，在摇床中25℃、200rpm条件下持续振荡240min，每隔30min分别取样，在波长664nm处测定其吸光度并记录，考察染料浓度的变化，即考察5％和10％多孔CNC-ALG凝胶微球的吸附效果。
结果如图1和图2所示，随着吸附时间的延长，多孔CNC-ALG凝胶微球的吸附容量逐渐增加，去除率也随之增加，60min后达到一个平台状态，吸附量基本维持稳定，此时多孔5％CNC-ALG凝胶微球吸附容量达到1.23mg/L，吸附去除率达76.24％；多孔10％CNC-ALG凝胶微球吸附容量达到1.27mg/L，吸附去除率达79.01％。
Claims (6)
1.一种多孔纤维素纳米晶-海藻酸钠凝胶微球的制备方法，其特征在于，包括如下步骤：
1）常温条件下，在50 mL超纯水中加入纤维素纳米晶，然后加入0.2g 碳酸氢钠和1g海藻酸钠，70℃恒温搅拌至海藻酸钠完全溶解后加入1g 碳酸钙，继续搅拌至碳酸钙均匀分布，配制成含纤维素纳米晶的海藻酸钠溶液；
2）将步骤1）配制成的海藻酸钠溶液超声脱泡后静置，借助推进设备，将海藻酸钠溶液匀速滴入盛有交联液的低速搅拌的烧杯中，滴制完毕后高速搅拌30min，得到多孔微球与交联液的混合液；
3）将步骤2）得到的多孔微球过滤，反复冲洗至清洗液pH值为7，得到多孔纤维素纳米晶-海藻酸钠凝胶微球。
2.根据权利要求1所述的一种多孔纤维素纳米晶-海藻酸钠凝胶微球的制备方法，其特征在于，步骤1）中，所述纤维素纳米晶加入量为0.05g或0.1g。
3.根据权利要求1所述的一种多孔纤维素纳米晶-海藻酸钠凝胶微球的制备方法，其特征在于，步骤2）中，所述交联液含3 %乙酸和6 %乙醇的水溶液。
4.根据权利要求1所述的一种多孔纤维素纳米晶-海藻酸钠凝胶微球的制备方法，其特征在于，步骤2）中，所述低速搅拌速度为200rpm。
5.根据权利要求1所述的一种多孔纤维素纳米晶-海藻酸钠凝胶微球的制备方法，其特征在于，步骤2）中，所述高速搅拌速度为600rpm。
6.根据权利要求1-5任意一项所述的方法制备的多孔纤维素纳米晶-海藻酸钠凝胶微球在吸附偶氮染料中的应用。
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