CN113828290A - 一种光催化多孔水凝胶的制备方法 - Google Patents
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Abstract
本发明公开了一种光催化多孔水凝胶的制备方法,该方法利用水包油高内相乳液聚合方法聚合物质A和可聚合并负载有纳米二氧化钛的氧化石墨烯,获得光催化多孔水凝胶。本发明的制备工艺简单,制备的负载有纳米二氧化钛多孔水凝胶具有高吸水膨胀性性能,水凝胶中负载的纳米TiO2具有光催化能力,能够用于水中污染物的降解。
Description
技术领域
本发明涉及光催化材料技术领域,具体涉及一种光催化多孔水凝胶的制备方法。
背景技术
随着工业生产的快速发展,在工业用水量日益趋增的同时,排放的污水量也不断增加,全世界污水排放量已达到4000亿立方米,使5.5万亿立方米水体受到污染,占全世界径流总量的14%以上,因此工业用水造成的废水的排放及净化是当前减少淡水缺失的主要途径。我国是全球高度工业化国家之一,工业用水量名列前茅,尤其在印染、化工、生物医药等方面对水资源用量极大,而印染、化工、生物医药废水的排放导致环境中染料,重金属及抗生素含量增加,导致水体受到严重污染,生态环境遭到破坏,对水污染的彻底处理是我们的愿望。
光催化技术是近十来年发展起来能有效处理水污染、空气污染的手段,光催化的原理是借助光催化剂可以在太阳辐射下在水中产生高氧化活性物种,使有机污染物降解的技术,因此,光催化技术是一种简单、环保的解决水污染、问题的方法。在众多光催化剂中,纳米二氧化钛(TiO2)因其具有高效、无毒、化学性质稳定等优点,使其成为一种具有大规模应用潜力的光催化剂,然而,纳米TiO2通常以粉末形式存在,在其使用上出现不易回收利用等缺点。
因此,有必要研究一种改进负载有纳米二氧化钛多孔水凝胶的制备方法。
发明内容
为解决现有技术的不足,本发明的目的在于提供一种可在紫外、可见光下实现光催化降解污染物,且可实现纳米二氧化钛循环利用的光催化多孔水凝胶的制备方法。
为了实现上述目标,本发明采用如下的技术方案:
一种光催化多孔水凝胶的制备方法,包括以下制备步骤:
S1、将纳米二氧化钛、氧化石墨烯和2-氨基乙基甲基丙烯酸酯溶于水中,超声分散30min,在40oC反应6h,静置过滤,得到可聚合氧化石墨烯复合物;
S2、在反应器中,按照一定比例将物质A、N,N-亚甲基双丙烯酰胺、聚氧乙烯聚丙乙烯三嵌段聚合物F127、引发剂、氧化石墨烯复合物和去离子水,在超声作用下混合均匀,在500转/min的搅拌速度下,将一定比例的甲苯滴加到反应器中,得到乳液体系;
S3、将乳液体系转移到固定容器中,在密封、60℃的条件下反应12h,反应结束后使用乙醇浸泡洗涤,再用水洗,得到光催化多孔水凝胶。
优选地,前述步骤S1中,纳米二氧化钛和氧化石墨烯的质量比为(4:1)~(1:4),2-氨基乙基甲基丙烯酸酯的质量为氧化石墨烯质量的0.5~2倍。
再优选地,前述步骤S2中,物质A选用丙烯酰胺、2-丙烯酰胺基-2-甲基-1-丙烷磺酸钠或阳离子型单体中的一种,阳离子型单体为(3-丙烯酰胺丙基)三甲基氯化铵、(乙烯基苄基)三甲基氯化铵或甲基丙烯酰氧乙基三甲基氯化铵中的一种。
更优选地,前述步骤S2中,N,N-亚甲基双丙烯酰胺的质量为物质A质量的2~20%,聚氧乙烯聚丙乙烯三嵌段聚合物F127的质量为物质A质量的5~10%,去离子水的质量为物质A质量的0.5~2倍。
进一步优选地,前述步骤S2中,氧化石墨烯复合物的质量为物质A质量的1~10%,甲苯的质量为物质A质量的6~9倍。
具体地,前述步骤S2中,引发剂为水溶性引发剂,采用过硫酸钾、过硫酸铵、偶氮二异丁咪唑啉盐酸盐(V044)和偶氮二异丁基脒盐酸盐(V50)中的一种,其质量为物质A质量的0.1~5%。
本发明的有益之处在于:
(1)本发明的工艺过程操作简单、成本低廉,能够适应大规模实际生产;
(2)本发明制备的光催化多孔水凝胶可在紫外、可见光下实现光催化降解污染物;
(3)本发明制备的光催化多孔水凝胶,可实现纳米二氧化钛的循环利用,并在氧化石墨烯的隔离下,避免光催化对水凝胶的腐蚀;
(4)物质A选用2-丙烯酰胺基-2-甲基-1-丙烷磺酸钠,制备得到的多孔水凝胶可选择性吸附阳离子化合物;物质A选用阳离子型单体,制备得到的多孔水凝胶可选择性吸附阴离子化合物;
(5)本发明制备的水凝胶通过在步骤S2中引入内相使凝胶呈多孔结构,可以提高污染物在凝胶中的扩散速率,可以缩短污染物去除的时间,并且在凝胶中引入离子型结构单元,从而实现对污染物的选择性去除。
附图说明
图1是本发明的实施例1中制备的光催化多孔水凝胶的扫描电镜图;
图2是本发明的实施例2中制备的光催化多孔水凝胶的扫描电镜图;
图3是本发明的实施例2中的局部放大示意图;
图4是本发明的实施例3中制备的光催化多孔水凝胶的扫描电镜图;
图5 是本发明的实施例3中制备的光催化多孔水凝胶和对照样品对诱惑红染料去除率曲线图;
图6是本发明的实施例3中制备的光催化多孔水凝胶和纳米二氧化钛对诱惑红染料去除循环使用情况图;
图7是本发明的实施例3中制备的光催化多孔水凝胶对诱惑红染料和亚甲基蓝去除紫外光谱图;
图8是本发明的实施例2制备的光催化多孔水凝胶对四环素去除紫外光谱图。
具体实施方式
以下结合附图和具体实施例对本发明作具体的介绍。
实施例1
一种光催化多孔水凝胶的制备方法,包括以下制备步骤:
S1、将4g的纳米二氧化钛、1g的氧化石墨烯和0.5g的2-氨基乙基甲基丙烯酸酯溶于200mL水中,超声分散30min,在40oC反应6小时,静置过滤,得到可聚合氧化石墨烯复合物;
S2、在反应器中,加入10 g的丙烯酰胺、0.2g的N,N-亚甲基双丙烯酰胺、0.5g的聚氧乙烯聚丙乙烯三嵌段聚合物F127、0.01g的过硫酸钾、0.1g的氧化石墨烯复合物和5g的去离子水,在超声作用下混合均匀,在500转/分钟的搅拌速度下,将60g的甲苯滴加到反应器中,得到乳液体系;
S3、将乳液体系转移到固定容器中,在密封、60℃的条件下反应12小时,反应结束后使用乙醇浸泡洗涤,再用水洗得到光催化多孔水凝胶。
该实施例制备的光催化多孔水凝胶的微观形貌如图1所示,通过图1可以看出,材料呈多孔结构。
实施例2
本实施例的制备方法与实施例相同,区别在于物质A选用2-丙烯酰胺基-2-甲基-1-丙烷磺酸钠。
该实施例制备的光催化多孔水凝胶的微观形貌如图2所示,通过图2可以看出,材料呈多孔结构,从多孔结构放大照片中可看出TiO2纳米粒子,如图3所示。该实施例制备的光催化多孔水凝胶对阳离子化合物四环素去除的紫外光谱图见图8,通过图8可看出,随着处理时间增加四环素的吸收峰值持续下降,在200分钟后四环素的吸收峰几乎变为零,说明本发明制备的光催化多孔水凝胶对阳离子化合物四环素具有去除能力。
实施例3
本实施例的制备方法与实施例相同,区别在于物质A选用(3-丙烯酰胺丙基)三甲基氯化铵。
该实施例制备的光催化多孔水凝胶的微观形貌如图4所示,通过图4可以看出,材料呈多孔结构。该实施例制备的光催化多孔水凝胶对诱惑红染料和亚甲基蓝去除的紫外光谱图见图7,通过图7可看出,随着处理时间增加诱惑红的吸收峰值持续下降,在 12 小时后峰值不在降低,说明诱惑红已被降解完全,而整个过程中亚甲基蓝吸收峰几乎不变,说明其不受凝胶吸附并降解,验证了本发明制备的光催化多孔水凝胶的选择性去除阴离子化合物。
实施例4
一种光催化多孔水凝胶的制备方法,包括以下制备步骤:
S1、将1g的纳米二氧化钛、4g的氧化石墨烯和8g的2-氨基乙基甲基丙烯酸酯溶于750mL水中,超声分散30min,在40oC反应6小时,静置过滤,得到可聚合氧化石墨烯复合物;
S2、在反应器中,加入10 g的丙烯酰胺、2g的N,N-亚甲基双丙烯酰胺、1g的聚氧乙烯聚丙乙烯三嵌段聚合物F127、0.01g的过硫酸胺、1g的氧化石墨烯复合物和20g的去离子水,在超声作用下混合均匀,在500转/分钟的搅拌速度下,将90g的甲苯滴加到反应器中,得到乳液体系;
S3、将乳液体系转移到固定容器中,在密封、60℃的条件下反应12小时,反应结束后使用乙醇浸泡洗涤,再用水洗得到光催化多孔水凝胶。
实施例5
一种光催化多孔水凝胶的制备方法,包括以下制备步骤:
S1、将2g的纳米二氧化钛、2g的氧化石墨烯和2g的2-氨基乙基甲基丙烯酸酯溶于500mL水中,超声分散30min,在40oC反应6小时,静置过滤,得到可聚合氧化石墨烯复合物;
S2、在反应器中,加入10 g的丙烯酰胺、0.5g的N,N-亚甲基双丙烯酰胺、0.75g的聚氧乙烯聚丙乙烯三嵌段聚合物F127、0.02g的V50、0.5g的氧化石墨烯复合物和15g的去离子水,在超声作用下混合均匀,在500转/分钟的搅拌速度下,将70g的甲苯滴加到反应器中,得到乳液体系;
S3、将乳液体系转移到固定容器中,在密封、60℃的条件下反应12小时,反应结束后使用乙醇浸泡洗涤,再用水洗得到光催化多孔水凝胶。
性能检测试验:
(1)将实施例3中制备的2g多孔水凝胶加入到100mL浓度为10 mg/L的诱惑红染料溶液中,测试了对污染物的去除效果,并设置空白实验(不含纳米二氧化钛多孔水凝胶),对诱惑红染料的去除率曲线图见图5。
如图5所示,不含纳米二氧化钛多孔水凝胶的空白实验的去除率只有70%,实施例3中制备的多孔水凝胶对染料的去除率可达98.5%,说明多孔水凝胶中加入纳米二氧化钛能显著提高污染物的去除率。
(2)对实施例3中制备的多孔水凝胶和相同量的纳米二氧化钛对诱惑红染料的去除进行循环测试,对诱惑红染料的去除率见图6。
如图6所示,实施例3中制备的多孔水凝胶表现出良好的循环利用性,而单纯的纳米二氧化钛由于在使用过程中的丢失,导致随着循环利用次数的增加而呈现逐步降低的催化效果,这说明将纳米二氧化钛负载在多孔水凝胶中能够显著提高其重复利用性能。
以上显示和描述了本发明的基本原理、主要特征和优点。本行业的技术人员应该了解,上述实施例不以任何形式限制本发明,凡采用等同替换或等效变换的方式所获得的技术方案,均落在本发明的保护范围内。
Claims (6)
1.一种光催化多孔水凝胶的制备方法,其特征在于,包括以下制备步骤:
S1、将纳米二氧化钛、氧化石墨烯和2-氨基乙基甲基丙烯酸酯溶于水中,超声分散30min,在40oC反应6h,静置过滤,得到可聚合氧化石墨烯复合物;
S2、在反应器中,按照一定比例将物质A、N,N-亚甲基双丙烯酰胺、聚氧乙烯聚丙乙烯三嵌段聚合物F127、引发剂、氧化石墨烯复合物和去离子水,在超声作用下混合均匀,在500转/min的搅拌速度下,将一定比例的甲苯滴加到反应器中,得到乳液体系;
S3、将乳液体系转移到固定容器中,在密封、60℃的条件下反应12h,反应结束后使用乙醇浸泡洗涤,再用水洗,得到光催化多孔水凝胶。
2.根据权利要求1所述的一种光催化多孔水凝胶的制备方法,其特征在于,所述步骤S1中,纳米二氧化钛和氧化石墨烯的质量比为(4:1)~(1:4),2-氨基乙基甲基丙烯酸酯的质量为氧化石墨烯质量的0.5~2倍。
3.根据权利要求1所述的一种光催化多孔水凝胶的制备方法,其特征在于,所述步骤S2中,物质A选用丙烯酰胺、2-丙烯酰胺基-2-甲基-1-丙烷磺酸钠或阳离子型单体中的一种,所述阳离子型单体为(3-丙烯酰胺丙基)三甲基氯化铵、(乙烯基苄基)三甲基氯化铵或甲基丙烯酰氧乙基三甲基氯化铵中的一种。
4.根据权利要求1所述的一种光催化多孔水凝胶的制备方法,其特征在于,所述步骤S2中,N,N-亚甲基双丙烯酰胺的质量为物质A质量的2~20%,聚氧乙烯聚丙乙烯三嵌段聚合物F127的质量为物质A质量的5~10%,去离子水的质量为物质A质量的0.5~2倍。
5.根据权利要求1所述的一种光催化多孔水凝胶的制备方法,其特征在于,所述步骤S2中,氧化石墨烯复合物的质量为物质A质量的1~10%,甲苯的质量为物质A质量的6~9倍。
6.根据权利要求1所述的一种光催化多孔水凝胶的制备方法,其特征在于,所述步骤S2中,引发剂为水溶性引发剂,采用过硫酸钾、过硫酸铵、偶氮二异丁咪唑啉盐酸盐(V044)和偶氮二异丁基脒盐酸盐(V50)中的一种,其质量为丙烯酰胺质量的0.1~5%。
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