CN115245795A - 一种超疏水壳聚糖基气凝胶的制备方法 - Google Patents
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Abstract
本发明涉及一种超疏水壳聚糖基气凝胶的制备方法，所述方法步骤如下：（1）壳聚糖改性碳纳米管的制备，得到表面包覆壳聚糖的改性碳纳米管；（2）壳聚糖基气凝胶的制备：冰模板法控制气凝胶微观形貌，冷冻干燥得到改性碳纳米管填充的壳聚糖基气凝胶；（3）气凝胶烷基化疏水改性。本发明制备的气凝胶，原材料来源丰富，绿色环保，具有高效选择性吸附、循环可利用率高，可简便有效、绿色经济的应用于油水分离等领域。
Description
技术领域
本发明涉及一种超疏水壳聚糖基气凝胶的制备方法。
背景技术
近年来，人口数量快速增长，人民生活水平持续提高，发达国家和发展中国家的工业化和现代化程度不断加强，随之产生的废渣、废气、污水、雾霾、白色污染等问题日益严重，不断威胁生态环境和人类健康，受到了人们和社会的广泛关注。随着海洋油气资源开发力度的不断加大，海洋石油开采中的井喷事故、路上石油管道爆炸或破裂引起的石油泄漏事故频繁发生，石油中有毒有害化合物的存在，严重威胁到海洋生物链中的各个物种，从低等级的藻类植物到高等级的哺乳动物，海洋生态安全正在遭受着巨大的考验。因此，石油泄漏和海水污染问题亟待解决。
传统的油水分离方法包括重力法、过滤法、离心法、浮选法、电化学法、燃烧法等，但是，这些分离方法大多数耗时长、操作繁琐、分离效率低、价格昂贵，且并不适用于油水乳液的分离。具有特殊润湿性表面的油水分离材料，尤其是具有超疏水超亲油表面或超亲水超疏油表面的油水分离材料可实现快速高效的、自动的、可循环的油水分离。气凝胶由于具有轻的密度和大的比表面积等优点近几年被广泛的关注，疏水吸油气凝胶或许能为油水分离问题提供新的方向。
在绿色化学的思路指导下，保证产物功能高效的同时，原材料生态友好是不可缺少的重要条件。壳聚糖是虾、蟹和昆虫壳骨架中提取物甲壳素的脱乙酰产物，是自然界中唯一的碱性多糖。它来源丰富，是一种可再生的天然高分子材料。同时碳纳米管具有高度多孔和中空的结构、大比表面积、低质量密度等优点，近年来已经在解决环境污染问题受到了广泛关注。大量理论和实验证明，碳纳米管可以成功用于重金属离子，有机污染物吸附。
发明内容
本发明的目的是提供一种具有高效选择性吸附、循环可利用率高，可简便有效、绿色经济的应用于油水分离等领域的超疏水壳聚糖基气凝胶的制备方法。
本发明的技术方案如下：
（1）壳聚糖改性碳纳米管的制备：将碳纳米管和壳聚糖超声分散溶解在乙酸溶液中，得到碳纳米管乙酸溶液；在搅拌的同时，用稀氨水调整碳纳米管乙酸溶液至弱碱性，得到表面吸附壳聚糖的碳纳米管悬浮液；向悬浮液中滴入一定量的戊二醛溶液，室温下搅拌反应，随后产物用蒸馏水洗至中性，烘干后得到壳聚糖改性的碳纳米管，备用；
进一步的，步骤（1）中所述的乙酸溶液pH为2~4，碳纳米管、壳聚糖和乙酸溶液的质量比为2~4:1:100。
进一步的，步骤（1）中所述的稀氨水pH为9~12，溶液弱碱性为8~9。
进一步的，步骤（1）中所述的戊二醛溶液的质量分数为10~50%，用量为前述壳聚糖质量的2~5%，反应时间为5~10h。
（2）壳聚糖基气凝胶的制备：将壳聚糖和上述制备的壳聚糖表面包覆的碳纳米管溶解在乙酸溶液中，室温下搅拌分散，得到均匀壳聚糖溶液；向壳聚糖溶液中一定速度缓慢滴加戊二醛溶液，室温下静置反应成胶，随后放置在低温下冷冻成形，采用冰模板法控制气凝胶微观形貌；将冷冻后的壳聚糖用冷冻干燥机冷冻干燥，得到改性碳纳米管填充的壳聚糖基气凝胶，备用；
进一步的，步骤（2）中所述的乙酸溶液pH为9~12，壳聚糖、壳聚糖表面包覆的碳纳米管和乙酸的质量比为2~7:0.6:100。
进一步的，步骤（2）中所述的一定速度为20~30min/mL，戊二醛溶液的质量分数为5~30%，用量为前述壳聚糖质量的3~7%，冷冻温度为-20~-80℃，冷冻时间为4~10h。
进一步的，步骤（2）中所述的冷冻干燥冷阱温度为-60℃，压力为8Pa，冷冻干燥时间为24~48h。
（3）气凝胶的超疏水改性：将上述制备的气凝胶、甲基三甲基硅氧烷和去离子水放置在密闭环境中，一定温度下进行化学气相沉积，得到超疏水壳聚糖基气凝胶；
进一步的，步骤（3）中所述的气凝胶、甲基三甲基硅氧烷和去离子水的质量比为3:1:1，一定温度为70~90℃，化学气相沉积时间为5~10h。
本发明以壳聚糖为基体，表面包覆壳聚糖的改性碳纳米管为增强填料，通过冷冻干燥法、硅烷化疏水改性，制得具有超疏水亲油的壳聚糖基气凝胶材料，其具有以下特点和益处：
1、碳纳米管具有多孔中空、大比表面积和高效的吸附特性，但与基体相容性差，通过简单易行的实验设计实现壳聚糖表面包覆改性，解决了碳纳米管在基体中的分散性问题，发挥其选择吸附特性的同时增强了材料的力学强度。
2、复合气凝胶材料内部具有高孔隙率和碳纳米管中空结构特性，通过表面烷基化疏水改性，实现对于油性液体的高效选择性吸收，吸收量大，循环利用性强。
3、所用原材料为绿色材料，来源丰富，无毒无害，环境友好，可生物降解，属于绿色环保型吸附剂材料。
具体实施方式
下文将对本发明的实施例进行进一步的描述，其中，各实施例仅为本发明示例性的实施方式，并不意图构成对本发明范围的限定。本领域技术人员可以根据上文的说明以及下文对实施例的描述作出多种不同的改进和变形，其均不会背离本发明的精神和实质。据此，本发明的范围仅意图通过各项权利要求所要求保护的范围来进行限定。
实施1：
按照如下步骤制造超疏水壳聚糖基气凝胶：
（1）壳聚糖改性碳纳米管的制备：称取2质量份碳纳米管和1质量份壳聚糖超声分散溶解在100质量份pH=2的乙酸溶液中，在搅拌的同时，滴加pH=11的稀氨水调整碳纳米管乙酸溶液至弱碱性pH=8，随后向悬浮液中加入0.03质量份的5%戊二醛溶液，室温下搅拌反应7h，随后产物用蒸馏水洗至中性，烘干后得到壳聚糖改性的碳纳米管，备用；
（2）壳聚糖基气凝胶的制备：称取3质量份的壳聚糖和0.6质量份上述制备的壳聚糖表面包覆的碳纳米管溶解在pH=2的100质量份的乙酸溶液中，室温下搅拌分散至均匀，随后向溶液中以20min/mL的速度缓慢滴加0.09质量份的10%戊二醛溶液，室温下静置反应成胶，随后放置在-20℃低温下冷冻10h成形。然后将冷冻后的壳聚糖溶胶在-60℃，8Pa的条件下冷冻干燥48h，得到改性碳纳米管填充的壳聚糖基气凝胶，备用；
（3）气凝胶的超疏水改性：将上述制备的3质量份气凝胶、1质量份甲基三甲基硅氧烷和1质量份去离子水放置在密闭环境中，70℃下进行化学气相沉积5h，得到超疏水壳聚糖基气凝胶。
由此获得的超疏水壳聚糖基气凝胶的三维孔径为5~100μm，对各类液体的吸附效率如表1。
| 有机试剂 | 硅油 | 正己烷 | 甲苯 | 石油醚 | 正己烷 |
| 吸附含量 | 30 | 18 | 23 | 21 | 19 |
注：吸附含量=（吸附平衡后气凝胶质量-吸附前气凝胶质量）/吸附前气凝胶质量x100%。
Claims (2)
1.一种超疏水壳聚糖基气凝胶的制备方法，其特征在于，包括如下步骤：
（1）壳聚糖改性碳纳米管的制备：将碳纳米管和壳聚糖超声分散溶解在乙酸溶液中，得到碳纳米管乙酸溶液；在搅拌的同时，用稀氨水调整碳纳米管乙酸溶液至弱碱性，得到表面吸附壳聚糖的碳纳米管悬浮液；向悬浮液中滴入一定量的戊二醛溶液，室温下搅拌反应，随后产物用蒸馏水洗至中性，烘干后得到壳聚糖改性的碳纳米管，备用；
（2）壳聚糖基气凝胶的制备：将壳聚糖和上述制备的壳聚糖表面包覆的碳纳米管溶解在乙酸溶液中，室温下搅拌分散，得到均匀壳聚糖溶液；向壳聚糖溶液中一定速度缓慢滴加戊二醛溶液，室温下静置反应成胶，随后放置在低温下冷冻成形，采用冰模板法控制气凝胶微观形貌；将冷冻后的壳聚糖用冷冻干燥机冷冻干燥，得到改性碳纳米管填充的壳聚糖基气凝胶，备用；
（3）气凝胶的超疏水改性：将上述制备的气凝胶、甲基三甲基硅氧烷和去离子水放置在密闭环境中，一定温度下进行化学气相沉积，得到超疏水壳聚糖基气凝胶。
2.根据权利要求1所述的一种超疏水壳聚糖基气凝胶的制备方法，其特征在于，步骤（1）中所述的乙酸溶液pH为2~4，碳纳米管、壳聚糖和乙酸溶液的质量比为2~4:1:100；稀氨水pH为9~12，溶液弱碱性为8~9；戊二醛溶液的质量分数为10~50%，用量为前述壳聚糖质量的2~5%，反应时间为5~10h；步骤（2）中所述的乙酸溶液pH为9~12，壳聚糖、壳聚糖表面包覆的碳纳米管和乙酸的质量比为2~7:0.6:100。
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