CN112831085A - 一种油水分离纤维素气凝胶的制备 - Google Patents
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Abstract
本发明利用仿生粘合技术将聚多巴胺嫁接到蕉芋纤维素上,并与甲基三甲氧基硅烷(MTMS)疏水剂结合形成稳定结构,加强疏水剂牢固性,制备得到高效超疏水超亲油油水分离材料;本发明纤维素/聚多巴胺气凝胶具有比表面积大,吸附容量大等特点,因而吸油能力强;本发明制备方法具有操作简单、条件温和、无毒害、能耗低等优点,便于工业化推广应用,同时本发明的蕉芋培育简单,聚多巴胺制备简单,均可简单获取,降低制备成本。
Description
技术领域
本发明涉及一种油水分离材料,具体涉及一种油水分离纤维素气凝胶的制备及其应用。
背景技术
油水分离技术在许多如化工、家庭、环保等领域都有着广泛的应用。尤其是与环保领域有关的海上溢油处理方向。通常,油在水中有漂浮、分散、溶解、乳化四种状态。目前市场上的分离技术有重力分离、电解分离、气浮分离等。在这些技术中,综合考虑到环保、经济、难易程度等因素,采用吸油材料收集和去除油污是较经济和有效的手段,对环境无不良影响。目前,吸油材料主要可分为四大类:天然有机类、合成有机、多孔无机矿物质类和纳米碳基类。然而,在天然有机类材料中,由于天然有机材料的孔隙结构较差,其吸附能力通常很低且缺乏选择性;多孔无机矿物质类材料具有吸附效率低、成本高、浮力低、吸附饱和后再生困难等特点;纳米碳基类材料其生物制备成本高,降解能力差,会对自然产生二次污染。因此,与之前材料相比,合成有机类材料具有良好的疏水性,吸油倍率高、吸附速率高,往往这类吸油材料一直是研究的热点。
发明内容
本发明提供了一种油水分离纤维素气凝胶的制备,一种油水分离纤维素气凝胶的制备,其包括以下步骤:
1)蕉芋纤维素提取实验:将蕉芋茎晾晒一周,去除里面的水分;人工去皮后,将其切成小块,用乙醇清洗后,将清洗过后的蕉芋茎块用万能粉碎机粉碎成粉末,得到蕉芋茎粉末;取蕉芋茎粉末浸入氢氧化钠水溶液中,磁力搅拌水浴80℃,3小时;抽滤再浸入双氧水溶液中,在磁力搅拌水浴90℃,1小时,用蒸馏水清洗至中性,抽滤,60℃烘干得蕉芋纤维素;
2)聚多巴胺溶液的制备
取PH=8.5的磷酸盐缓冲溶液,加入盐酸多巴胺,在黑暗的环境下搅拌24h,让该溶液中的盐酸多巴胺充分聚合反应后,即得到聚多巴胺溶液;
3)甲基三甲氧基硅烷改性聚多巴胺/纤维素气凝胶的制备
取步骤1)中制备得到的蕉芋纤维素放入步骤2)中制备好的聚多巴胺溶液中,在黑暗的环境下磁力搅拌搅拌24小时,得到聚多巴胺/纤维素悬浮液;在聚多巴胺/纤维素悬浮液,加入疏水剂甲基三甲氧基硅烷(MTMS),磁力搅拌2小时使MTMS充分与聚多巴胺/纤维素反应;将上述混合液倒入膜具,冷冻干燥48h,得到超疏水超亲油油水分离材料甲基三甲氧基硅烷改性聚多巴胺/纤维素气凝胶。
作为优选,所述步骤1)中蕉芋茎粉末与氢氧化钠水溶液的重量体积比g/ml为1:10。
作为优选,所述步骤1)中氢氧化钠水溶液为2wt%的氢氧化钠水溶液。
作为优选,所述步骤1)中双氧水溶液中蒸馏水:双氧水体积比为3:2。
作为优选,所述步骤1)中蕉芋茎粉末与双氧水溶液的重量体积比g/ml为1:10。
作为优选,所述步骤2)中盐酸多巴胺与磷酸盐缓冲溶液的重量体积比g/ml为1:1000ml。
作为优选,所述步骤3)中蕉芋纤维素与聚多巴胺溶液的重量体积比g/ml为1:200。
作为优选,所述步骤3)中蕉芋纤维素与疏水剂甲基三甲氧基硅烷的重量体积比为1:4。
本发明以天然生物质材料(蕉芋)为基体,利用仿生粘合技术对其进行超疏水改性,从而使其拥有油水分离特性;;该新型油水分离材料具有一系列优点,如较快的吸附速率、可生物降解、较高的吸油率等,可有效克服有机吸油材料的缺点;本发明利用仿生粘合技术将聚多巴胺嫁接到用蕉芋纤维素上,并与甲基三甲氧基硅烷(MTMS)疏水剂结合形成稳定结构,加强疏水剂牢固性,制备得到高效超疏水超亲油油水分离材料;本发明纤维素/聚多巴胺气凝胶具有比表面积大,吸附容量大等特点,因而吸油能力强;本发明制备方法具有操作简单、条件温和、无毒害、能耗低等优点,便于工业化推广应用,同时本发明的蕉芋培育简单,聚多巴胺制备简单,均可简单获取,降低制备成本。
具体实施方式
下列实施例用于进一步解释说明本发明,但是,它们并不构成对本发明范围的限制或限定。
本实验采用的蕉芋产自浙江舟山;乙醇(国药分析纯);盐酸多巴胺(阿拉丁分析纯);甲基三甲氧基硅烷(阿拉丁分析纯)。
PH=8.5的磷酸盐缓冲溶液的配置:0.144g磷酸二氢钠,3.38g磷酸氢二钠,500ml蒸馏水配制出ph值8.5的磷酸盐缓冲溶液。
实施例1蕉芋纤维素提取实验
首先将蕉芋茎晾晒一周,去除里面的水分。人工去皮后,将其切成小块,用乙醇清洗后,将清洗过后的蕉芋茎块用万能粉碎机粉碎成粉末,得到蕉芋茎粉末;取10g蕉芋茎粉末浸入2wt%的氢氧化钠水溶液(500ml蒸馏水:10g氢氧化钠),在磁力搅拌水浴80℃,3小时。抽滤再浸入体积比为3:2的双氧水溶液中(60ml蒸馏水:40ml双氧水),在磁力搅拌水浴90℃,1小时,得到了较为纯净的蕉芋纤维素溶液;用蒸馏水清洗至中性,抽滤,60℃烘干取得纤维素2.8g。
实施例2聚多巴胺溶液的制备
取100ml的PH=8.5的磷酸盐缓冲溶液,0.1g盐酸多巴胺;在有氧黑暗的环境下搅拌24h,待到该溶液中的盐酸多巴胺充分聚合反应后,即得聚多巴胺溶液100ml。
实施例3甲基三甲氧基硅烷改性纤维素/聚多巴胺气凝胶的制备实验
取0.5g纤维素放入制备好的聚多巴胺溶液(100ml的PH=8.5的磷酸盐缓冲溶液:0.1g盐酸多巴胺)中,磁力搅拌搅拌24小时,得到聚多巴胺/纤维素悬浮液;在聚多巴胺/纤维素悬浮液,加入2ml疏水剂甲基三甲氧基硅烷(MTMS),磁力搅拌2小时使MTMS充分与聚多巴胺/纤维素反应;将上述混合液倒入膜具。冷冻干燥48h得到27块(长:宽:高=2cm:2cm:1cm)超疏水超亲油油水分离材料甲基三甲氧基硅烷改性聚多巴胺/纤维素气凝胶,每块质量为0.02g。
吸附速率测试实验及结果
使用动力粘度为0.563mPa·s,密度为1.4840cm3的氯仿,和动力粘度为242.4Pa·s,密度为0.8510cm3的润滑油对实施例3制备的甲基三甲氧基硅烷改性聚多巴胺/纤维素气凝胶进行吸油检测,其吸油量随时间的变化如表1所述。从表1中可以看出,甲基三甲氧基硅烷改性聚多巴胺/纤维素气凝胶对氯仿和润滑油的吸油倍率随吸油时间的增加而增加;开始时快速升高,在吸油1min时,对氯仿和润滑油的吸油倍率分别为38.5g/g和13.2g/g,分别达到饱和吸油量的83.3%和86.4%,然后缓慢升高,在5min左右达到平衡,甲基三甲氧基硅烷改性聚多巴胺/纤维素气凝胶对氯仿和润滑油的吸油倍率随时间的增加,开始迅速升高,再缓慢增高直至达到平衡状态。
表1
吸油率测试实验
为了验证甲基三甲氧基硅烷改性纤维素/聚多巴胺气凝胶对不同的油类或有机物的吸油效率,我们分别对环己烷、氯仿、润滑油、泵油、柴油、葵花籽油进行吸油检测,结果见表2。
表2
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明披露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (8)
1.一种油水分离纤维素气凝胶的制备,其包括以下步骤:
1)蕉芋纤维素提取实验:将蕉芋茎晾晒一周,去除里面的水分;人工去皮后,将其切成小块,用乙醇清洗后,将清洗过后的蕉芋茎块用万能粉碎机粉碎成粉末,得到蕉芋茎粉末;取蕉芋茎粉末浸入氢氧化钠水溶液中,磁力搅拌水浴80℃,3小时;抽滤再浸入双氧水溶液中,在磁力搅拌水浴90℃,1小时,用蒸馏水清洗至中性,抽滤,60℃烘干得蕉芋纤维素;
2)聚多巴胺溶液的制备
取PH=8.5的磷酸盐缓冲溶液,加入盐酸多巴胺,在黑暗的环境下搅拌24h,让该溶液中的盐酸多巴胺充分聚合反应后,即得到聚多巴胺溶液;
3)甲基三甲氧基硅烷改性聚多巴胺/纤维素气凝胶的制备
取步骤1)中制备得到的蕉芋纤维素放入步骤2)中制备好的聚多巴胺溶液中,在黑暗的环境下磁力搅拌搅拌24小时,得到聚多巴胺/纤维素悬浮液;在聚多巴胺/纤维素悬浮液,加入疏水剂甲基三甲氧基硅烷(MTMS),磁力搅拌2小时使MTMS充分与聚多巴胺/纤维素反应;将上述混合液倒入膜具,冷冻干燥48h,得到超疏水超亲油油水分离材料甲基三甲氧基硅烷改性聚多巴胺/纤维素气凝胶。
2.根据权利要求1所述一种油水分离纤维素气凝胶的制备,其特征在于所述步骤1)中蕉芋茎粉末与氢氧化钠水溶液的重量体积比g/ml为1:10。
3.根据权利要求1所述一种油水分离纤维素气凝胶的制备,其特征在于所述步骤1)中氢氧化钠水溶液为2wt%的氢氧化钠水溶液。
4.根据权利要求1所述一种油水分离纤维素气凝胶的制备,其特征在于所述步骤1)中双氧水溶液中蒸馏水:双氧水体积比为3:2。
5.根据权利要求1所述一种油水分离纤维素气凝胶的制备,其特征在于所述步骤1)中蕉芋茎粉末与双氧水溶液的重量体积比g/ml为1:10。
6.根据权利要求1所述一种油水分离纤维素气凝胶的制备,其特征在于所述步骤2)中盐酸多巴胺与磷酸盐缓冲溶液的重量体积比g/ml为1:1000ml。
7.根据权利要求1所述一种油水分离纤维素气凝胶的制备,其特征在于所述步骤3)中蕉芋纤维素与聚多巴胺溶液的重量体积比g/ml为1:200。
8.根据权利要求1所述一种油水分离纤维素气凝胶的制备,其特征在于所述步骤3)中蕉芋纤维素与疏水剂甲基三甲氧基硅烷的重量体积比为1:4。
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