CN109107608A - 一种对硝基苯甲酸铀酰配合物光催化剂及其制备方法 - Google Patents
一种对硝基苯甲酸铀酰配合物光催化剂及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种对硝基苯甲酸铀酰配合物光催化剂，该光催化剂的分子式为(H2‑bipy)[(UO2)4(μ3‑O)2(p‑nba)6]，分子式中bipy为4，4’‑联吡啶，Hp‑nba为对硝基苯甲酸，该催化剂在氙灯光源的照射下，300分钟内将浓度为40mg/L的盐酸四环素溶液降解到9.1％，是一种在可见光下对盐酸四环素有催化降解性能的铀酰配合物光催化剂。
Description
技术领域
本发明涉及光催化剂，具体涉及一种对硝基苯甲酸铀酰配合物光催化剂及其制备方法。
背景技术
自1928年Alexander Fleming发现了青霉素，1948年威廉·贝娜德从放线菌类的链霉菌中提取出金霉素，到目前为止，抗生素的种类已达几千种，被广泛应用于治疗人体疾病、预防畜禽、水产品的细菌性病害中。然而，生活和医疗上抗生素的过度使用和滥用、制药企业、动物饲料及水产养殖业等废水的排放，使得目前水环境中含有大量的抗生素污染物，造成了日益严重的环境问题，若不加以有效去除，则对饮用水体、生态环境和人类健康产生长期潜在的威胁。目前处理废水中抗生素的常见技术有物理法、化学法、生物法、光催化法等。其中，物理法以吸附污染物的方式进行抗生素废水的处理，其存在选择性差和不能连续操作等缺点；生物法则利用微生物的酶氧化和还原有机分子从而达到去除抗生素的作用，其存在操作条件苛刻、微生物中毒以及降解不彻底等问题；化学法则通过物质间的化学反应来去除废水中的抗生素，但在处理后会造成二次污染，且成本较高，在工业生产中受到一定的限制；而光催化技术是一种在能源和环境领域有着重要应用前景的绿色技术，其优点是：适用范围广、反应速率快；理论上可以完全矿化污染物且不会产生二次污染；运行成本低。因此，光催化技术在清除有机污染物方面有着广阔的应用前景。同时，光催化剂的制备也引起了人们的广泛关注。
半导体光催化剂在室温下可将废水中有机污染物氧化成H2O、CO2或无机离子等，且无二次污染。目前，光催化技术中最常用到的催化剂为TiO2半导体材料，该材料以其对生物无毒、化学性质稳定、耐光腐蚀、紫外光下催化效率高、价廉易得等优点，被公认为是目前最佳的光催化剂。如公开号为CN102698727A的发明专利申请，就公开了一种制备高热稳定性的负载型TiO2光催化剂的方法；但是，TiO2光催化材料在实际应用中仍存在致命的缺点：光响应范围窄，因为只能利用太阳光能量4％的紫外光，且量子效率低下。为了提升其在可见光区域的光催化性能，人们对TiO2展开了大量的改性研究，如染料光敏化、半导体复合、金属掺杂、非金属掺杂等，如公开号为CN103007938A的发明专利公开了一种Cu掺杂改性的TiO2光催化剂及其制备方法，但这些手段仍然存在许多不足。因此，开发新型光催化材料是解决废水中四环素类抗生素污染问题的关键。铀酰离子具有独特的可见光波段的强吸收和响应，具有更高的光催化效率，有望解决TiO2光催化剂中存在的光响应范围窄、量子效率低等缺点，成为颇具应用潜力的光催化剂，如公开号为CN103447090A的发明专利公开了一种对甲基苯甲酸铀酰配合物光催化剂，该催化剂在氙灯下对罗丹明B有优异的降解性能。而且，铀酰基配合物用于废水中抗生素污染物的降解，为环境中抗生素污染物的治理提供了一条切实可行的途径，也为铀酰基光催化剂的开发奠定了很好的基础，因此，本发明采用水热法，合成了一种在可见光下对盐酸四环素有催化降解性能的铀酰配合物光催化剂。
发明内容
本发明所要解决的技术问题是提供一种可降解盐酸四环素的对硝基苯甲酸铀酰配合物光催化剂。
本发明解决上述技术问题所采用的技术方案为：一种对硝基苯甲酸铀酰配合物光催化剂，其分子式为(H2-bipy)[(UO2)4(μ3-O)2(p-nba)6]，分子式中bipy＝4，4’-联吡啶，Hp-nba＝对硝基苯甲酸。该对硝基苯甲酸铀酰配合物光催化剂晶体的晶胞参数为：α＝85.07(3)°，β＝74.65(3)°，γ(°)＝73.38(3)°，为三斜晶系，属于P-1空间群。
与现有技术相比，本发明的优点在于一种对硝基苯甲酸铀酰配合物光催化剂，该光催化剂的分子式为(H2-bipy)[(UO2)4(μ3-O)2(p-nba)6]，分子式中bipy为4，4’-联吡啶，Hp-nba为对硝基苯甲酸，该对硝基苯甲酸铀酰配合物光催化剂可降解盐酸四环素，且该对甲基苯甲酸铀酰配合物光催化剂可用离心分离方法回收再利用，避免该催化剂可能引起的二次污染。
附图说明
图1为本发明对硝基苯甲酸铀酰配合物光催化剂的分子结构图；
图2为本发明对硝基苯甲酸铀酰配合物光催化剂的PXRD图谱与单晶模拟PXRD图谱的对比图；
图3为本发明对硝基苯甲酸铀酰配合物光催化剂对盐酸四环素的光催化降解曲线图。
具体实施方式
以下结合附图实施例对本发明作进一步详细描述。
实施例1
称取0.25mmol醋酸双氧铀溶于5mL H2O中，溶解得黄色溶液，另称取0.5mmol对硝基苯甲酸和0.2mmol的4，4’-联吡啶加入上述混合溶液中搅拌，溶液变浑浊，继续搅拌30min，测得pH＝2.11，将混合溶液转移至23mL的聚四氟乙烯反应釜内衬中，密封，并在140℃下保持72h。冷却后得到黄色产物，该黄色产物为分子式(H2-bipy)[(UO2)4(μ3-O)2(Hp-nba)6]的一种对硝基苯甲酸铀酰配合物光催化剂。将黄色产物研磨成粉末，称取48mg置于60mL含有浓度为40mg/L盐酸四环素的水溶液中，并置于光催化剂反应器中，开启搅拌器，在氙灯300W可见光照射下，用光源为300W的氙灯，可见光下对其进行光催化降解，每隔30min取适量的溶液，离心后用紫外-可见分光光度计监测溶液中盐酸四环素的变化，300分钟可将水溶液中的盐酸四环素降解91.9％，得到如图3所示的光催化降解曲线图，对照实验在不加入对硝基苯甲酸铀酰配合物光催化剂的条件下进行，步骤同上。
由图3可见，在300W氙灯照射没有催化剂的情况下，未加上述催化剂盐酸四环素并没有发生降解，加入上述催化剂后，盐酸四环素发生明显降解，300min后，降解率为91.9％，是对盐酸四环素有降解作用的光催化剂。该配合物作为光催化剂可用离心分离的方法回收再利用。采用Bruker D8 Focus粉末衍射仪2θ角度范围为5-50°，以10°/min的扫描速度对该铀酰配合物光催化剂进行扫描，在室温下收集样品的粉末衍射图谱(PXRD)，并与单晶模拟PXRD图对比，可以完美拟合，说明产物为纯相，纯度不低于99％。
实施例2
与实施例1基本相同，所不同的只是醋酸双氧铀由硝酸双氧铀替代。
Claims (3)
1.一种对硝基苯甲酸铀酰配合物光催化剂，其特征在于该铀酰配合物光催化剂的分子式为(H2-bipy)[(UO2)4(μ3-O)2(p-nba)6]，其中bipy＝4，4’-联吡啶，Hp-nba＝对硝基苯甲酸，其特征在于该对硝基苯甲酸铀酰配合物光催化剂的晶体的晶胞参数为：α(°)＝85.07(3)°，β(°)＝74.65(3)°，γ(°)＝73.38(3)°，该光催化剂为能通过100目筛的黄色粉体，纯度不低于99％，在可见光下对盐酸四环素有催化降解性能的铀酰配合物光催化剂。
2.权利要求1所述的对硝基苯甲酸铀酰配合物光催化剂的制备方法，其特征在于步骤如下：
a)称取0.1～0.5mmol醋酸双氧铀溶于3～10mL H2O中，溶解得黄色溶液待用；
b)称取0.2～1mmol对硝基苯甲酸和0.1～0.5mmol的4，4’-联吡啶加入上述步骤a)混合溶液中搅拌，溶液变浑浊，继续搅拌10～60min；
c)将步骤b)的混合液转移至23mL的聚四氟乙烯反应釜内衬中，密封120～160℃反应48～72h，冷却至室温，过滤，将黄色块状品体研磨成过100目筛的粉体，得到纯度不低于99％的对硝基苯甲酸铀酰光催化剂。
3.如权利要求2所述的对硝基苯甲酸铀酰配合物光催化剂的制备方法，其特征在于硝酸双氧铀替代醋酸双氧铀。
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| CN111495430B (zh) * | 2020-04-21 | 2023-03-14 | 周口师范学院 | 一种基于目标铀酰多钨酸盐光催化剂及制备方法和应用 |
| CN114558621A (zh) * | 2022-03-08 | 2022-05-31 | 西安医学院 | 异氰脲酸双(2-羧乙基)酯铀酰配合物光催化剂及方法 |
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