CN113061250A - 一种聚萘二酰亚胺甲酮线形缩聚物光催化剂及其制备、酸化处理方法和应用 - Google Patents
一种聚萘二酰亚胺甲酮线形缩聚物光催化剂及其制备、酸化处理方法和应用 Download PDFInfo
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Abstract
本发明公开了一种聚萘二酰亚胺甲酮线形缩聚物光催化剂及其制备、酸化处理方法和应用,所述光催化剂的单体中含有萘二酰亚胺和甲酮结构,其结构通式如式Ⅰ所示。本发明的聚萘二酰亚胺甲酮线形缩聚物可作为光催化剂,用以降解罗丹明B染料,与传统降解材料相比,本发明的材料具有光催化降解性能,提高降解率,不仅符合环境友好理念,而且具有良好的市场应用前景,为快速、廉价、降解染料废水提供可靠的技术支持。
Description
技术领域
本发明属于光催化污水处理领域,具体涉及一种聚萘二酰亚胺甲酮线形缩聚物光催化剂及其制备、酸化处理方法和应用。
背景技术
水是生命之源,但是水污染对生态环境和人们的健康带来巨大的威胁,特别是水中的有机污染物,如多氯联苯、抗生素、染料及其中间体等。目前主要治理方法为物理吸附、化学转化和生物降解,但是效果并不十分理想。近年来,光催化氧化降解作为一种高级氧化技术,可将毒性大、难生物降解的有机污染物彻底矿化,然而,目前具有高活性和强矿化能力的光催化剂主要为TiO2等紫外光活性的催化剂,紫外光只占太阳光的4%~6%,太阳光利用率低。
发明内容
为了解决现有技术中存在的缺陷,本发明的目的在于针对印染行业污水处理过程中存在的技术不足,提供一种聚萘二酰亚胺甲酮线形缩聚物光催化剂及其制备、酸化处理方法和应用,大大提高了光催化效率同时降低经济成本。
本发明是通过以下技术方案实现的:
一种聚萘二酰亚胺甲酮线形缩聚物光催化剂,所述光催化剂的单体中含有萘二酰亚胺和甲酮结构,其结构通式如下式Ⅰ所示:
一种聚萘二酰亚胺甲酮线形缩聚物光催化剂的制备方法,包括以下步骤:
步骤1)向容器中加入尿素、1,4,5,8-萘四甲酸二酐、醋酸锌、咪唑,在140℃、氩气保护下,反应5~10h;
步骤2)待反应冷却至室温后加入盐酸,对反应体系进行真空过滤并用蒸馏水洗涤沉淀直至无氯离子,然后在真空箱中干燥;
步骤3)最后用二甲基亚砜洗涤干燥后的产物,洗涤至溶液无色,收集到的黄褐色固体即为所述聚萘二酰亚胺甲酮线形缩聚物光催化剂。
优选地,步骤1)所述尿素、1,4,5,8-萘四甲酸二酐、醋酸锌的摩尔比为1:1:1,步骤2)所述盐酸浓度为1mol/L。
一种聚萘二酰亚胺甲酮线形缩聚物光催化剂的酸化处理方法,包括以下步骤:称量所述聚萘二酰亚胺甲酮线形缩聚物光催化剂0.10~1.00g至容器中,向其中加入98%浓硫酸,超声,再加入50~200mL去离子水,待不溶性沉淀生成后静置30min,然后过滤烘干,即得到酸化处理过的聚萘二酰亚胺甲酮线形缩聚物。
一种聚萘二酰亚胺甲酮线形缩聚物光催化剂在催化降解染料废水中的应用。
一种聚萘二酰亚胺甲酮线形缩聚物的酸化产物在催化降解染料废水中的应用。
本发明的有益效果如下:
1、有机光催化剂具有结构可设计、自组装、能带可调控、光谱响应范围宽等特点,是光催化研究的新热点,其光催化机理的研究对有机光催化的发展具有重要意义。同时考虑到,纯有机光催化剂面向产业化后,其全生命周期的综合成本低。因此,本发明设计了一种聚萘二酰亚胺甲酮线形缩聚物光催化剂用以降解罗丹明B染料溶液,大大提高了光催化效率同时降低经济成本。
2、本发明的聚萘二酰亚胺甲酮线形缩聚物可作为光催化剂,用以降解罗丹明B染料,与传统降解材料相比,本发明的材料具有光催化降解性能,提高降解率,不仅符合环境友好理念,而且具有良好的市场应用前景,为快速、廉价、降解染料废水提供可靠的技术支持。
附图说明
图1为聚萘二酰亚胺甲酮线形缩聚物光催化剂的X-射线粉末衍射图;
图2为聚萘二酰亚胺甲酮线形缩聚物光催化剂的扫描电镜图:a)为酸化处理前;b)为酸化处理后;
图3为聚萘二酰亚胺甲酮线形缩聚物光催化剂酸化处理前后对于罗丹明B的降解曲线图。
具体实施方式
下面结合附图与具体实施例对本发明做进一步详细说明。
实施例1
一种聚萘二酰亚胺甲酮线形缩聚物光催化剂,其单体中含有萘二酰亚胺和甲酮结构,其结构通式如下式Ⅰ所示:
其合成方案的具体步骤如下:
在500mL单颈烧瓶中加入尿素(0.12g,2.0mmol)、1,4,5,8-萘四甲酸二酐(0.54g,2.0mmol)、醋酸锌(0.37g,2.0mmol)、5.0g咪唑(溶剂),在140℃高温以及氩气保护下反应5h,待反应冷却到室温后加入250mL盐酸(1mol/L),搅拌混合至无进一步沉淀,然后对反应体系进行真空过滤并用蒸馏水洗涤沉淀直至无氯离子,之后再在真空箱中干燥,最后用二甲基亚砜洗涤直至溶液无色,收集到黄褐色固体0.47g,即为所述聚萘二酰亚胺甲酮线形缩聚物光催化剂,产率为71.2%。
其XRD衍射图以及扫描电镜图如图1所示,由图1可知,聚萘二酰亚胺甲酮线形缩聚物的衍射峰较尖锐,说明结晶度高,通过计算,其结晶度达到74.6%。
实施例2
一种聚萘二酰亚胺甲酮线形缩聚物光催化剂的酸化处理方案,具体步骤如下:
称量0.1g聚萘二酰亚胺甲酮线形缩聚物光催化剂(Urea-NDI)至200mL的烧杯中,向其中加入10mL 98%浓硫酸后进行超声5min,再向其中加入150mL的去离子水,待不溶性沉淀生成后静置30min,然后过滤烘干,得到的泥白色固体即为酸化处理过的聚萘二酰亚胺甲酮线形缩聚物(Urea-NDI-AT)。其酸化处理前后的扫描电镜图如图2所示,由图2(a)到图2(b)的变化可知,经酸化后的聚萘二酰亚胺甲酮线形缩聚物光催化剂体量级数更小,更加纳米化,比表面积增大。
实施例3
一种聚萘二酰亚胺甲酮线形缩聚物光催化剂对罗丹明B的降解方案,具体步骤如下:
(1)向盛有罗丹明B溶液的光反应瓶中加入10mg实施例1制得的聚萘二酰亚胺甲酮线形缩聚物光催化剂,将光反应瓶置于暗处,同时打开循环冷凝水,保持在室温的条件,在搅拌下保持60min后取样离心后打开光源,进行光催化降解,并开启光化学反应器计时,每隔1h取一次溶液进行离心抽样。
(2)另取一只光反应瓶向其中加入10mg实施例2制得的Urea-NDI-AT,重复(1)的操作。
(3)标曲溶液配制:取5只100mL的容量瓶编号1-5,向其中分别加入20mL、40mL、60mL、80mL、100mL的罗丹明B溶液(5mg/L)并定容至100mL。
(4)标曲与光催化降解曲线的绘制:对配制好的标曲溶液进行吸光度测定并绘制标准曲线,由标准曲线绘测定样品浓度,并绘制光催化降解曲线图如图3所示,其中前60min两组光反应瓶都处于黑暗条件下达到吸附平衡,之后打开氙灯进行光催化降解。
由图3可知,经酸化处理后的聚萘二酰亚胺甲酮线形缩聚物光催化剂,即Urea-NDI-AT,较酸化处理前的Urea-NDI,其光催化降解性能得到很大提高。
Claims (6)
2.权利要求1所述的一种聚萘二酰亚胺甲酮线形缩聚物光催化剂的制备方法,其特征在于,包括以下步骤:
步骤1)向容器中加入尿素、1,4,5,8-萘四甲酸二酐、醋酸锌、咪唑,在140℃、氩气保护下,反应5~10h;
步骤2)待反应冷却至室温后加入盐酸,对反应体系进行真空过滤并用蒸馏水洗涤沉淀直至无氯离子,然后在真空箱中干燥;
步骤3)最后用二甲基亚砜洗涤干燥后的产物,洗涤至溶液无色,收集到的黄褐色固体即为所述聚萘二酰亚胺甲酮线形缩聚物光催化剂。
3.根据权利要求2所述的一种聚萘二酰亚胺甲酮线形缩聚物光催化剂的制备方法,其特征在于,步骤1)所述尿素、1,4,5,8-萘四甲酸二酐、醋酸锌的摩尔比为1:1:1,步骤2)所述盐酸浓度为1mol/L。
4.权利要求1所述的一种聚萘二酰亚胺甲酮线形缩聚物光催化剂的酸化处理方法,其特征在于,包括以下步骤:称量所述聚萘二酰亚胺甲酮线形缩聚物光催化剂0.10~1.00g至容器中,向其中加入98%浓硫酸,超声,再加入50~200mL去离子水,待不溶性沉淀生成后静置30min,然后过滤烘干,即得到酸化处理过的聚萘二酰亚胺甲酮线形缩聚物。
5.权利要求1所述的一种聚萘二酰亚胺甲酮线形缩聚物光催化剂在催化降解染料废水中的应用。
6.权利要求4所得聚萘二酰亚胺甲酮线形缩聚物的酸化产物在催化降解染料废水中的应用。
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