CN111495323A - 一种吸附苯酚的磁性生物质碳气凝胶的制备及其应用 - Google Patents
一种吸附苯酚的磁性生物质碳气凝胶的制备及其应用 Download PDFInfo
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Abstract
本发明提供了一种吸附苯酚的磁性生物质碳气凝胶材料的制备方法，并将其应用于苯酚废水的吸附。由于苯酚废水污染日益严重，现有的苯酚废水处理吸附材料存在效果不理想、成本高、难以回收等缺点，有必要开发一种成本低廉、效果理想、技术简单的吸附材料与技术。现今碳气凝胶已成为国内外研究的热点之一，而生物质碳气凝胶作为第三代气凝胶，具有原料廉价易得、制备过程简单易行、质量轻、孔径丰富等优点，故在吸附方面有良好的应用前景；具有磁性的生物质碳气凝胶更易于回收利用，且磁化后的碳气凝胶孔径更为丰富。本发明将不同水热温度下得到的生物质碳气凝胶与不同比例的四氧化三铁进行配比合成磁性生物质碳气凝胶，并将其显示出良好的吸附性能，用于苯酚废水的吸附。
Description
技术领域
本发明涉及一种吸附苯酚的磁性生物质碳气凝胶的制备方法及其应用。
背景技术
伴随着社会经济的迅猛发展，能源已经成为了新科学技术革命的三大支柱产业之一，更成为了人类日常生活和社会经济发展的重要物质基础和支撑。近年来，由于人类的频繁活动和一些不可逆转的客观原因，使地球失去了原有的活力，并且面临着前所未有的挑战，能源短缺和环境污染问题便是其中最大的挑战。生物质作为地球上储备最丰富的可再生能源之一，不仅可以实现资源的高效转化，还可以防止环境污染。因此，废物资源的合理利用成为了热点研究领域。
碳气凝胶是继无机气凝胶和合成物气凝胶之后的第三代气凝胶，具有来源广泛、前驱体价格低廉、密度小、可悬浮于手中、孔径丰富、比表面积大、可回收利用等优点；因此，近年来成为新一代高分子材料中的佼佼者。之前的研究侧重于利用纤维素、木质素、壳聚糖和淀粉等生物质单一组分合成气凝胶，需要从生物质原料中提取这些组分，流程复杂且造成原料浪费，所以，全组分生物质碳气凝胶成了研究热点。
随着现代工业的快速发展，水体污染已经成为了不可忽视且亟待解决的环境问题之一。水中酚类污染物主要来源于焦化、煤气、炼油和以苯酚或酚醛为原料的化工、制药等生产过程产生的含酚废水的排放。由于其来源广、数量多、高毒性强、易扩散性以及难环境降解性，被美国环保局列入129种优先控制的污染物名单，也是我国重点控制的污染物之一。目前，含酚废水的处理方法很多，一般分为物理法、化学法和生物法三大类，吸附法属于物理、化学或物理化学方法的交叉方法，苯酚处理效率高、效果稳定。
本专利采用生物质原料西瓜皮为前驱体，省去复杂的提取过程，利用简单的水热法、冷冻干燥法和水浴法制备出生物质碳气凝胶复合物，即以生物质原料直接制备出可用于吸附废水中苯酚的、回收的碳气凝胶，为碳气凝胶更广泛的应用奠定理论基础。
发明内容
鉴于以上，本发明旨在开发一种清洁、无污染、易得、可回收利用、具有优异吸附性能的生物质碳气凝胶。将在此提供一种全组分生物质碳气凝胶的制备方法并将其应用于苯酚废水的吸附。该方法通过将不同水热温度下得到的碳气凝胶磁化，合成磁性生物质碳气凝胶，将多种组分协同利用可以使其具有良好的吸附性能。
本发明一方面提供了一种磁性生物质碳气凝胶的制备方法，另一方面提供此材料的用途，可用于苯酚废水的吸附。
针对现有技术的不足，其特征在于磁性生物质碳气凝胶复合物的制备是按照以下步骤完成的：
一、前驱体的处理：将前驱体上残留的软组织洗掉，并切成相同大小，再用去离子水洗涤三次以去除其可溶性组织；
二、水热：将洗涤过的前驱体转移至装有100 mL去离子水的聚四氟乙烯内衬的反应釜中，将其密闭放置于恒温鼓风干燥箱内，160～200 ℃水热24 h；
三、洗涤：待反应完成后，取出黑色块状水凝胶产物，并用去离子水与乙醇的混合溶液洗涤数次，以去除可溶性杂质；
四、冷冻干燥：将洗涤干净的黑色块状水凝胶产物置于冰箱内冷冻，然后将冻实后的产物置于冷冻干燥机内冷冻干燥，干燥温度为-71 ℃，干燥时间为36 h，得到黑色块状产物，即碳气凝胶；
五、铁源的合成及复合：由0.49 g FeCl3·6H2O和0.25 g FeSO4·7H2O（此时Fe3O4含量为100 %）（调节FeCl3·6H2O和FeSO4·7H2O含量得到85 %、90 %、95 % 的Fe3O4）加入到20 mL去离子水中，取一块步骤四所制备出的碳气凝胶水热3 h，再加入1 mL氨水加热3 h，即可得到碳气凝胶复合物。步骤一中所述的前驱体为西瓜皮，步骤五中的铁源为四氧化三铁。
本发明的优点：
一、本发明制备的生物质碳气凝胶复合物的前驱体属于废弃生物质再利用、环保无污染、廉价易得。
二、本发明方法制备的生物质碳气凝胶属全组分生物质碳气凝胶，不需要复杂的提取过程，也不会造成原料的浪费。
三、本发明的制备方法与其他制备方法相比耗时短，所用仪器常见且操作简便。
四、制备的磁性生物质碳气凝胶（CA）具有磁性，可回收再利用。
附图说明
图1为具体实施办法一制备所得的可悬浮于水面的西瓜皮生物质碳气凝胶样品图。
图2为具体实施办法一、具体实施方法二、具体实施方法三的SEM图。
图3为具体实施方法一、具体实施方法二、具体实施方法三的FTIR图。
图4为具体实施方法一的苯酚吸附图。
具体实施方法
以下将叙述本发明的具体实施办法，该领域内研究人员可通过此说明书内容了解本发明的优点及用途。以下具体实施办法仅是部分实施案例，并不是全部实施案例。
具体实施方法一：
本实施方法西瓜皮生物质碳气凝胶的制备方法：一、将西瓜皮的软组织去除干净，并切成相同的大小，并用去离子水洗涤3次得到干净的前驱体；二、将步骤一得到的干净的前驱体转移至200 mL的聚四氟乙烯内衬的反应釜中，将其密封放置于恒温鼓风干燥箱内水热12h后取出，得到黑色块状水凝胶；三、将步骤二得到的黑色块状水凝胶用水与乙醇的混合溶液(体积比1:1)洗涤若干次，以去除可溶性杂质；四、接着将步骤三得到的洗涤干净的黑色块状水凝胶放置于冰箱内进行冷冻，然后将冷冻的水凝胶用冷冻干燥机冷冻干燥，干燥温度为-71 ℃，干燥时间36 h，得到黑色块状生物质碳气凝胶；五、准确称取0.49 g的FeC13·6H2O (1.8×10-3mol)和0.25 g的FeSO4·7H2O (0.9×10-3mol)置于烧杯中，然后加入20 mL去离子水搅拌20 min形成均一的混合溶液；六、称取一块步骤五制备的生物质碳气凝胶，将其浸没在上述溶液中并加热到90 ℃保持3 h，接着量取1 mL氨水溶液慢慢滴加到烧杯中，90 ℃保温3 h得到黑色块状磁性生物质碳气凝胶；七、将步骤七得到的产物用去离子水和乙醇各洗涤若干次以去除未参与反应的反应物；八、将步骤七得到的干净的生物质磁性碳气凝胶放入冰箱进行冷冻，然后转移至冷冻干燥机内，冷冻干燥温度为-71 ℃，时间为36h，得到最终的磁性生物质碳气凝胶。其中，步骤步骤二中的水热温度T=160 ℃，步骤五中配制的四氧化三铁比例为100 %。
本实施方法及以下十种实施方法对苯酚的吸附效果均通过下述方案实现：将20mg/L的苯酚废水称取30 mL，放入50 mL的烧杯中，称取一块相同质量的碳气凝胶放入烧杯中，吸附时间均为5 h，离心后测苯酚吸光度，得到苯酚吸附后的浓度。
具体实施方法二：本实施方法与具体实施方法一不同的是：步骤二中的水热温度T=180 ℃，其他与具体实施方法一相同。
具体实施方法三：本实施方法与具体实施方法一不同的是：步骤二中的水热温度T=200 ℃，其他与具体实施方法一相同。
具体实施方法四：本实施方法与具体实施方法一不同的是：步骤五配制的四氧化三铁的比例为95 %。
具体实施方法五：本实施方法与具体实施方法一不同的是：步骤五配制的四氧化三铁的比例为90 %。
具体实施方法六：本实施方法与具体实施方法一不同的是：步骤五配制的四氧化三铁的比例为85 %。
具体实施方法八：本实施方法与具体实施方法一不同的是：吸附的苯酚浓度c=40mg/L。
具体实施方法九：本实施方法与具体实施方法一不同的是：吸附的苯酚浓度c=60mg/L。
具体实施方法十：本实施方法与具体实施方法一不同的是：吸附的苯酚浓度c=80mg/L。
具体实施方法十一：本实施方法与具体实施方法一不同的是：吸附的苯酚浓度c=100 mg/L。
Claims (8)
1.一种磁性生物质基碳气凝胶，其特征在于磁性生物质碳气凝胶是由前驱体和铁源制备而成的复合材料。
2.根据权利要求1中所述的磁性生物质碳气凝胶，其特征在于所述的前驱体为西瓜皮。
3.根据权利要求1中所述的磁性生物质碳气凝胶，其特征在于所述的铁源为四氧化三铁。
4.一种磁性生物质碳气凝胶的制备方法，其特征在于磁性生物质碳气凝胶的制备是按照以下步骤完成的：首先将前驱体去皮取其软组织，并切成相同大小，再用去离子水洗涤三次以去除其可溶性组织；然后将洗涤过的前驱体软组织转移至装有100 mL去离子水的聚四氟乙烯内衬的反应釜中，将其密闭放置于恒温鼓风干燥箱内，160～200 ℃水热24 h；待反应完成后，取出黑色块状水凝胶产物，并用去离子水与乙醇的混合溶液洗涤数次，以去除可溶性杂质；将洗涤干净的黑色块状水凝胶产物置于冰箱内冷冻，然后将冻实后的产物置于冷冻干燥机内冷冻干燥，干燥温度为-71 ℃，干燥时间为36 h，得到黑色块状产物，即生物质碳气凝胶。
5.取0.49 g的FeCl3·6H2O和0.25 g的FeSO4·7H2O（此时Fe3O4含量为100 %）（调节调节FeCl3·6H2O和FeSO4·7H2O含量得到85 %、90 %、95 % 的Fe3O4）加入到20 mL去离子水中，取一块制备出的碳气凝胶放入上述溶液中水热3 h，再加入1 mL氨水继续加热3 h，得到黑色块状产物，即未干燥过的磁性生物质碳气凝胶；将制备出的未干燥的磁性生物质碳气凝胶放入冰箱冷冻，再放入冷冻干燥机内冷冻干燥，干燥温度为-71 ℃，时间为36 h，即可得到磁性生物质碳气凝胶。
6.步骤一中所述的前驱体为西瓜皮，步骤五中的铁源为四氧化三铁。
7.根据权利要求4中所述的一种磁性生物质碳气凝胶，其特征在于步骤一中的前驱体为西瓜皮。
8.根据权利要求4中所述的一种磁性生物质碳气凝胶，其特征在于步骤五中的铁源为四氧化三铁。
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