CN116459809A - 一种高吸附性和优异可再生性生物质基气凝胶及其制备 - Google Patents
一种高吸附性和优异可再生性生物质基气凝胶及其制备 Download PDFInfo
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Abstract
本发明公开一种应用于染料废水处理具备高效吸附性能和优异再生性能的生物质基气凝胶及其制备,其要点是对光催化纳米颗粒进行化学修饰,赋予其参与聚合反应的基本单元,使其参与到聚合反应,构成以光催化纳米颗粒为“交联点”的三维结构气凝胶。本发明以天然、环保、可降解的衣康酸、壳聚糖等生物质材料作为原料,并将光催化纳米颗粒引入作为气凝胶的“交联点”,实现光催化纳米颗粒的稳定引入,通过上述技术,解决现有技术中气凝胶吸附材料因吸附性能有限和再生性能差而实际应用受限的瓶颈问题,提高材料的实用价值和应用前景。
Description
技术领域
本发明属于环境污染治理和能源领域,具体涉及一种具备高效吸附性能和优异可再生性能的生物质基气凝胶及其制备方法。
背景技术
从环境污染治理的角度出发,开发高效且具有优异再生性能的吸附剂以移除污水中不易降解、毒性大的染料分子对实现水资源的再生利用意义重大。
现有报道中,基于功能材料的吸附分离技术,因成本低、操作便捷、适用范围广而被视为当前处理染料废水最有效的手段之一。
但大多数吸附材料吸附能力有限,且力学性能差和抗污染性能差导致其再生性能差,限制其广泛应用。
将光催化技术与染料吸附材料结合有望通过光催化作用降解染料打破原有的吸附平衡,是提高染料移除性能和抗污染性能的有效路径。
但大部分光催化材料是纳米颗粒的形式,直接使用易团聚,从而增大电子-空穴复合率而降低光催化性能,且不易回收,将其引入吸附材料中可避免团聚且赋予其优异的回收性能。
东华大学相恒学等将TiO2和g-C3N4负载在木质素衍生的碳纳米纤维(LCNFs)中,建立了TiO2/g-C3N4@LCNFs光催化材料,在太阳光下实现了优异的RhB降解性能(Zhai GX,Zhou JL,Xie M.et al.International Journal of Biological Macromolecules,2023,233,123588.)。
浙江工业大学盛嘉伟等采用浸渍法将N-TiO2和g-C3N4沉积到硅藻土(diatomite),制备了N-TiO2/g-C3N4@diatomite复合材料,证明N-TiO2和g-C3N4掺杂的催化剂可以协同增强对可见光区域的响应实现废水中Cr(Ⅵ)的优异还原效果(Sun Q,Hu XL,Zheng SL,et al.Environmental Pollution,2019,245,53-62.)。
气凝胶的力学性能直接影响循环使用过程的耐用性和再生性能。研究表明,引入纳米颗粒是实现气凝胶力学性能增强的一种有效手段。
瑞士联邦材料科学与技术研究所Matthias M.Koebel等将壳聚糖溶在硅酸中,制备了二氧化硅增韧的壳聚糖气凝胶,使抗压强度达到了7Mpa(Zhao SY,Malfait WJ,JeongE,et al.ACS Sustainable Chemistry Engineering,2016,10,5674-5683.)。
近期,四川大学李忠明等通过冷冻干燥和碳化制备了TiO2/纤维素纳米复合碳气凝胶,原位合成的TiO2(B)有效地增强了碳骨架,并通过光催化降解性能提高了气凝胶对染料的去除效率(Zhu JL,Chen SP,Ma GQ,et al.Journal of Colloid and InterfaceScience,2023,630,772-782.)。
当前研究表明,引入具备光催化活性的增韧纳米颗粒是提高气凝胶的染料移除性能和力学性能的一种潜在途径,但现有的物理掺杂、嵌入、负载及浸渍等方式缺乏稳定的连接,纳米颗粒存在脱落和二次污染风险,力学性能或光催化性能皆缺乏持久的保障,材料的耐用性能不佳,仍难以从根本上有效地解决气凝胶因染料移除性能有限和再生性能差而限制实际应用的技术瓶颈。
硅烷偶联剂作为一种表面修饰剂,能较好地赋予无机颗粒功能性基团,是将无机纳米颗粒引入气凝胶体系中的可靠途径。
本发明拟通过TMSPA修饰光催化纳米颗粒,并将其作为气凝胶三维结构的“交联点”,实现增韧光催化纳米颗粒的稳定引入,保障材料的耐用性能,从根本上解决气凝胶染料移除性能有限和再生性能差的问题。
发明内容
本发明的目的是从根本上有效地解决气凝胶因染料移除性能有限和再生性能差而限制实际应用的技术瓶颈,提供一种高效吸附性能和优异可再生性能的生物质基气凝胶及其制备方法。
上述材料的特征为:所述材料是以光催化纳米颗粒为气凝胶三维结构的“交联点”。
为达到上述目的,本发明采用的技术方案为:通过对光催化纳米颗粒进行修饰,使其参与聚合反应,替代传统的交联剂,构成以光催化纳米颗粒为“交联点”的三维网络结构气凝胶。
上述生物质基气凝胶的制备方法,具体包括以下步骤:
A.乙烯功能化光催化纳米颗粒的制备
将硅烷偶联剂TMSPA加入到乙醇和水的混合溶液中水解,然后加入光催化纳米颗粒,待反应完成后,洗去多余未反应的TMSPA,得到乙烯功能化光催化纳米颗粒。
B.生物质基气凝胶的制备
将上述步骤制备得到的乙烯功能化光催化纳米颗粒分散在水中,加入提前配制好的生物质原料溶液(质量比10-40%),加入引发剂过硫酸铵(APS)(质量比0.05-0.1%),在一定温度条件下匀速搅拌反应4h,获得以乙烯功能化光催化纳米颗粒为三维结构“交联点”的生物质基水凝胶,冷冻干燥48h后得到气凝胶。
光催化纳米颗粒包括银/氯化银(Ag/AgCl)、迈克烯(MXene)、硫化铬/二氧化铯(CdS/CeO2)、、二氧化钛(TiO2),三氧化二铁(Fe2O3),三氧化钨(WO3),氧化锌(ZnO),氧化铋(Bi2O3),氧化铟(In2O3),氧化锡(SnO2),氧化铜(Cu2O),钒酸铋(BiVO4)、钨酸铋(Bi2WO6)、钼酸铋(Bi2MoO6)、磷酸银(Ag3PO4)、铬酸银(Ag2CrO4)、溴化银(AgBr)、石墨相氮化碳(g-C3N4)、TiO2/g-C3N4,金属有机框架材料(MOFs)、共轭微孔聚合物(CMPs)、共价有机框架材料(COFs)。
生物质原料包括壳聚糖、衣康酸、海藻酸盐、植酸、纤维素、木质素、几丁质、琼脂糖、明胶。
根据[0016]所述的高效吸附性能和优异再生性能的生物质基气凝胶的制备方法,其特征在于:反应温度为30-80℃。
根据[0016]所述的高效吸附性能和优异再生性能的生物质基气凝胶,以同等条件下采用普通交联剂制备的气凝胶为参照样,分别对材料的染料移除性能和再生性能(力学性能和抗污染性能)进行测试,获得的光催化纳米颗粒为“交联点”的气凝胶具备更优异的染料移除能力和再生性能。
具体实施方式
一种高效吸附性能和优异再生性能的生物质基气凝胶的制备方法,包括乙烯功能化光催化纳米颗粒的制备和生物质基气凝胶的制备两个步骤。为了更好的理解本发明,下面用具体的实例来详细说明本发明的技术方案,但是本发明并不局限于此。
实施例1
在30%的壳聚糖和衣康酸溶液(质量比为1:1)中,加入乙烯功能化Ag/AgCl,加入引发剂APS(0.05%),在40℃条件下匀速搅拌反应4h,获得以乙烯功能化光催化纳米颗粒为三维结构“交联点”的生物质基水凝胶,冷冻干燥48h后得到气凝胶。
对比例1
以同等交联基团摩尔比的普通交联剂代替实施例1中所用的乙烯功能化Ag/AgCl,并加入与实施例1中同等摩尔比的Ag/AgCl,在30%的壳聚糖和衣康酸溶液(质量比为1:1)中,加入引发剂APS(0.05%),在40℃条件下匀速搅拌反应4h,获得Ag/AgCl共混生物质基水凝胶,冷冻干燥48h后得到气凝胶。
实施例2
在40%的海藻酸钠和衣康酸溶液(质量比为1:1)中,加入乙烯功能化TiO2/g-C3N4,加入引发剂APS(0.1%),在50℃条件下匀速搅拌反应4h,获得以乙烯功能化光催化纳米颗粒为三维结构“交联点”的生物质基水凝胶,冷冻干燥48h后得到气凝胶。
对比例2
以同等交联基团摩尔比的普通交联剂代替实施例2中所用的乙烯功能化TiO2/g-C3N4,并加入与实施例2中同等摩尔比的TiO2/g-C3N4,在40%的壳聚糖和衣康酸溶液(质量比为1:1)中,加入引发剂APS(0.1%),在50℃条件下匀速搅拌反应4h,获得TiO2/g-C3N4共混生物质基水凝胶,冷冻干燥48h后得到气凝胶。
实施例3
在25%的明胶和植酸溶液(质量比为1:1)中,加入乙烯功能化CdS/CeO2,加入引发剂APS(0.1%),在50℃条件下匀速搅拌反应4h,获得以乙烯功能化光催化纳米颗粒为三维结构“交联点”的生物质基水凝胶,冷冻干燥48h后得到气凝胶。
对比例3
以同等交联基团摩尔比的普通交联剂代替实施例3中所用的乙烯功能化CdS/CeO2,并加入与实施例3中同等摩尔比的CdS/CeO2,加入引发剂APS(0.1%),在50℃条件下匀速搅拌反应4h,获得CdS/CeO2共混生物质基水凝胶,冷冻干燥48h后得到气凝胶。
试验例1:对亚甲基蓝染料的移除性能测试(最大吸附量)
样品 | 最大吸附量 |
实施例1 | 688.3mg/g |
对比例1 | 426.1mg/g |
实施例2 | 669.5mg/g |
对比例2 | 389.5mg/g |
实施例3 | 800.3mg/g |
对比例3 | 462.3mg/g |
由上表结果可以看出,本发明的实施例1、2、3均具有优异的染料吸附性能,对比例1、2、3在制备过程中通过共混方式加入了相同摩尔比的光催化剂,但是物理引入的方式不能保证光催化剂稳定且均匀地存在于气凝胶中,从而影响光催化效率。
试验例2:再生性能测试(力学性能和抗污染性能测试)
由上表结果可以看出,本发明的实施例1、2、3具有较高的抗压强度和优异的抗污染性能,对比例1、2、3在制备过程中通过共混方式加入了相同摩尔比的光催化剂,但是共混方式加入光催化纳米颗粒的增韧作用较弱,且不光诱导自清洁性能(抗污染性能)不佳。
Claims (7)
1.一种具备高效吸附性能和优异再生性能的生物质基气凝胶,其特征在于:所述材料结构是以光催化纳米颗粒为气凝胶三维结构的“交联点”。
2.根据权利要求1所述的具备高效吸附性能和优异再生性能的生物质基气凝胶的制备方法,其特征在于:
首先通过硅烷偶联剂对光催化纳米颗粒进行修饰,获得乙烯功能化光催化纳米颗粒,然后使其参与气凝胶制备的聚合反应,获得以光催化纳米颗粒为三维结构的“交联点”的生物质基气凝胶。
3.根据权利要求2所述的具备高效吸附性能和优异再生性能的生物质基气凝胶的制备方法,其特征在于,具体包括以下步骤:
A.乙烯功能化光催化纳米颗粒的制备
将硅烷偶联剂丙烯酸3-(三甲氧硅基)丙酯(TMSPA)加入到乙醇和水的混合溶液中水解,然后加入光催化纳米颗粒,待反应完成后,洗去多余未反应的TMSPA,得到乙烯功能化光催化纳米颗粒;
B.生物质基气凝胶的制备
将步骤A制备得到的乙烯功能化光催化纳米颗粒分散在水中,加入提前配制好的生物质原料溶液(质量比10-40%),加入引发剂过硫酸铵(APS)(质量比0.05-0.1%),在一定温度条件下匀速搅拌反应4h,获得以乙烯功能化光催化纳米颗粒为三维结构“交联点”的生物质基水凝胶,冷冻干燥48h后得到气凝胶。
4.根据权利要求3所述的高效吸附性能和优异再生性能的生物质基气凝胶的制备方法,其特征在于:所述光催化纳米颗粒包括银/氯化银(Ag/AgCl)、迈克烯(MXene)、硫化铬/二氧化铯(CdS/CeO2)、、二氧化钛(TiO2),三氧化二铁(Fe2O3),三氧化钨(WO3),氧化锌(ZnO),氧化铋(Bi2O3),氧化铟(In2O3),氧化锡(SnO2),氧化铜(Cu2O),钒酸铋(BiVO4)、钨酸铋(Bi2WO6)、钼酸铋(Bi2MoO6)、磷酸银(Ag3PO4)、铬酸银(Ag2CrO4)、溴化银(AgBr)、石墨相氮化碳(g-C3N4)、TiO2/g-C3N4,金属有机框架材料(MOFs)、共轭微孔聚合物(CMPs)、共价有机框架材料(COFs)。
5.根据权利要求3所述的高效吸附性能和优异再生性能的生物质基气凝胶的制备方法,其特征在于:所述生物质原料包括壳聚糖、衣康酸、海藻酸盐、植酸、纤维素、木质素、几丁质、琼脂糖、明胶。
6.根据权利要求3所述的高效吸附性能和优异再生性能的生物质基气凝胶的制备方法,其特征在于:反应温度为30-80℃。
7.根据权利要求1所述的具备高效吸附性能和优异再生性能的生物质基气凝胶,以同等条件下采用普通交联剂制备的气凝胶为参照样,分别对材料的染料移除性能和再生性能(力学性能和抗污染性能)进行测试,获得的光催化纳米颗粒为“交联点”的气凝胶具备更优异的染料移除能力和再生性能。
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