CN107200378B - 一种高效降解四环素的混合物粉末的简易制备方法 - Google Patents
一种高效降解四环素的混合物粉末的简易制备方法 Download PDFInfo
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Abstract
本发明是一种高效降解四环素的混合物粉末的简易制备方法。包括有如下步骤：1）将商业氧化铜与尿素、盐酸胍按照1：x:y(x=0.1‑5;y=0.01‑0.5)的比例混合置于设有盖体的陶瓷容器中；2）将上述陶瓷容器置于马弗炉中进行热处理0.5‑3小时，得到所需要的粉末样品,该粉末含有CuO、Cu2O、Cu的晶相，有C、N、Cl的掺入。本发明的制备方法将氧化铜处理成高速率、高效率降解四环素的掺碳、氮、氯的氧化铜混合物粉末；该粉末能在2分钟之内将四环素完全光催化降解。
Description
技术领域
本发明涉及一种降解四环素的混合物粉末制备方法，特别是一种高效降解四环素的混合物粉末的简易制备方法，属于高效降解四环素的混合物粉末的简易制备方法的创新技术。
背景技术
四环素是一种光谱抗菌药，对革兰氏阳性菌、阴性菌、立克次体、滤过性病毒、螺旋体属乃至原虫类都有很好的抑制作用。高浓度时还能杀灭多数立克次体属、支原体属、衣原体属、非典型分枝杆菌属、螺旋体等。该品临床主要用于：⑴立克次氏体病，包括流行性斑疹伤寒、地方性斑疹伤寒、落基山热、恙虫病和Q热。⑵支原体属感染。⑶衣原体属感染，包括鹦鹉热、性病、淋巴肉牙肿、非特异性尿道炎、输卵管炎、宫颈炎及沙眼。⑷细菌性感染包括回归热、布鲁菌病、霍乱、兔热病、鼠疫等。治疗布鲁菌病和鼠疫时需与链霉素等氨基糖苷类联合应用。⑸肺炎双球菌或流感杆菌所引起的急性呼吸道感染。⑹敏感的大肠杆菌与变形杆菌引起的尿路感染。⑺痢疾杆菌或沙门氏菌属引起的痢疾或肠炎。
四环素易溶于水。现该药品已经禁用于人体治病。但常被偷偷用于动物饲料中。四环素随动物的排泄物进入水中，污染水源。对无病的人体造成危害，如(1)胃肠道症状如恶心、呕吐、上腹不适、腹胀、腹泻等。(2)该品可致肝毒性。(3)变态反应：多为斑丘疹和红斑等，偶有过敏性休克和哮喘发生。(4)偶可引起溶血性贫血、血小板减少、中性粒细胞减少和嗜酸粒细胞减少。(5)中枢神经系统：偶可致良性颅内压增高，可表现为头痛、呕吐、视神经乳头水肿等。(6)肾毒性：原有显著肾功能损害的患者可能发生氮质血症加重、高磷酸血症和酸中毒。(7)二重感染：长期应用该品可发生耐药金黄色葡萄球菌、革兰阴性杆菌和真菌等引起的消化道、呼吸道和尿路感染，严重者可致败血症。(8)四环素类的应用可使人体内正常菌群减少，导致维生素B缺乏、真菌繁殖，出现口干、咽炎、口角炎、舌炎、舌苔色暗或变色等。(9)出现四环素牙。
因此，需要对含有四环素的水进行处理。由于水体量大，如果用化学方法降解工程量巨大，且成本很高。
近年来有人用氧化铜(CuO)对四环素进行光催化降解，几个小时的时间能达到80-85％的降解率。要应用氧化铜降解四环素，还需要提高光催化降解的速率和降解率。
发明内容
本发明的目的在于考虑上述问题而提供一种高效降解四环素的混合物粉末的简易制备方法，本发明的制备方法将氧化铜处理成高速率、高效率降解四环素的掺碳、氮、氯的氧化铜、氧化亚铜、铜的混合物粉末；该粉末能在2分钟之内将四环素完全光催化降解。
本发明的技术方案是：高效降解四环素的混合物粉末的简易制备方法，包括有如下步骤：
1)将氧化铜与尿素、盐酸胍按照1：x:y(x＝0.1-5；y＝0.01-0.5) 的比例混合置于设有盖体的陶瓷容器中；
2)将上述陶瓷容器置于马弗炉中进行热处理0.5‐3小时，得到所需要的粉末样品，该粉末含有CuO、Cu2O、Cu的晶相，有C、N、Cl 的掺入。
上述步骤2)将陶瓷容器中置于马弗炉中加热的温度范围为 400-550℃。
本发明的制备方法将氧化铜处理成高速率、高效率降解四环素的氧化铜、氧化亚铜、铜的混合物粉末；该粉末具有比较高的比表面积, 能在2分钟之内将四环素完全降解。本发明是一种结构简单，方便实用的高效降解四环素的混合物粉末制备方法。
附图说明
图1为本发明制得的样品做电子衍射能谱(EDS)示意图，得到的元素含有Cu、O、C、N、Cl；
图2为本发明实施例1制备的粉末的XRD示意图，其中有CuO和 Cu2O的相；
图3为本发明实施例1制备的粉末的光催化曲线图；
图 4为本发明实施例2制备的粉末的XRD示意图；
图5为本发明实施例2制备的粉末的“光降解-时间”曲线 (Ed-t)。
图6为本发明实施例3制备的粉末的XRD示意图；
图7为本发明实施例3制备的粉末的“光降解-时间”曲线 (Ed-t)。
图8为本发明实施例4制备的粉末的XRD示意图；
图9为本发明实施例4制备的粉末的“光降解-时间”曲线 (Ed-t)；
图10为本发明实施例5制备的粉末的XRD示意图；
图11为本发明实施例5制备的粉末的“光降解-时间”曲线 (Ed-t)。
具体实施方式
本发明的高效降解四环素的混合物粉末的简易制备方法,包括有如下步骤：
1)将氧化铜与尿素、盐酸胍按照1：x:y(x＝0.1-5；y＝0.01-0.5) 的比例混合置于设有盖体的陶瓷容器中；
2)将上述陶瓷容器置于马弗炉中进行热处理0.5-3小时，得到所需要的粉末样品，该粉末含有CuO、Cu2O、Cu的晶相，有C、N、Cl 的掺入。
上述氧化铜是商业氧化铜。步骤2)将陶瓷容器中置于马弗炉中加热的温度范围为400-550℃。
上述步骤2)得到的粉末样品具有比表面积为1.114-1.468m2/g，能在1分10秒-2分钟将四环素完全降解。
制得样品其中一个做电子衍射能谱(EDS)如图1所示，得到的元素含有Cu、O、C、N、Cl。其含量如表1.
表1，图1中各元素的含量。
本发明的具体实施例如下：
实施例1：将商业CuO与尿素、盐酸胍按照1：0.1：0.5的比例混合置于可盖盖的陶瓷容器中后于马弗炉中在一定的温度范围内400℃热处理3小时。得到所需要的粉末样品。该粉末含有氧化铜、氧化亚铜相，图2所示为制备粉末的XRD示意图，具有1.468m2/g 的比表面积，能2分钟之内将四环素完全光降解，图3所示为制备粉末的“光降解-时间”曲线(Ed-t)。
实施例2：商业氧化铜与尿素、盐酸胍按照1：5：0.5的比例混合置于可盖盖的陶瓷容器中后于马弗炉中在一定的温度范围内550℃热处理2小时。得到所需要的粉末样品。该粉末含有氧化铜、氧化亚铜、铜相，图4所示为制备粉末的XRD示意图，具有1.104m2/g的比表面积，能1分20秒之内将四环素完全光降解，图5所示为制备粉末的“光降解-时间”曲线(Ed-t)。
实施例3：将商业氧化铜与尿素、盐酸胍按照1：2:0.01的比例混合置于可盖盖的陶瓷容器中后于马弗炉中在一定的温度范围内 500℃热处理0.5小时。得到所需要的粉末样品。该粉末含有氧化铜、氧化亚铜、铜相，图6所示为制备粉末的XRD示意图，具有1.173m2/g的比表面积，能1分30秒之内将四环素完全光降解，图7所示为制备粉末的“光降解-时间”曲线(Ed-t)。
实施例4：将商业氧化铜与尿素、盐酸胍按照1：1:0.1的比例混合置于可盖盖的陶瓷容器中后于马弗炉中在一定的温度范围内450℃热处理1小时。得到所需要的粉末样品。该粉末含有氧化铜、氧化亚铜相，图8所示为制备粉末的XRD示意图，具有1.256m2/g的比表面积，能1分30秒之内将四环素完全光降解，图9所示为制备粉末的的“光降解-时间”曲线(Ed-t)。
实施例5：将商业氧化铜与尿素、盐酸胍按照1：3.5:0.3的比例混合置于可盖盖的陶瓷容器中后于马弗炉中在一定的温度范围内 475℃热处理0.75小时。得到所需要的粉末样品。该粉末含有氧化铜、氧化亚铜相，图10所示为制备粉末的XRD示意图，具有1.237m2/g的比表面积，能1分10秒之内将四环素完全光降解，图11所示为制备粉末的“光降解-时间”曲线(Ed-t)。
本发明四环素降解检测方法：将制备的粉末0.1g放入100mL的四环素溶液(10mg/L)中形成混合物。磁搅拌并光照，隔一段时间(时间间隔由光催化速率决定，催化速率快就时间间隔短一些，催化速率漫就可以时间间隔长一些)取出3mL溶液，离心后取上清液做紫外可见光谱。由于四环素在267nm和350nm附近各有一个特征吸收峰，对应四环素的功能团，吸收强度与浓度成正比；一般文献钟根据350nm 附近的峰来确定溶液中四环素的浓度。故我们根据350nm附近的峰的强度来确定溶液中四环素的浓度。降解率由如下公式1计算：
式中C0为四环素被光催化的起始浓度，C为光催化t时间后的四环素浓度；A0为350nm附近四环素吸收峰的强度，A为光催化t时间后350nm附近四环素吸收峰的强度。Ed为降解率。
光催化平衡时间：做Ed‐t曲线，Ed不再随时间变化的起始时间为光催化平衡时间。
Claims (2)
1.一种高效降解四环素的混合物粉末的简易制备方法,其特征在于包括有如下步骤：
1)将氧化铜与尿素、盐酸胍按照1：x：y，x＝0.1-5；y＝0.01-0.5的比例混合置于设有盖体的陶瓷容器中；
2)将上述陶瓷容器置于马弗炉中进行热处理0.5-3小时，得到所需要的粉末样品，该粉末含有CuO、Cu2O、Cu的晶相，有C、N、Cl的掺入；
上述步骤2)将陶瓷容器中置于马弗炉中加热的温度范围为400-550℃。
2.根据权利要求1所述的高效降解四环素的混合物粉末的简易制备方法,其特征在于上述步骤2)得到的粉末样品具有比表面积为1.114-1.468m2/g，能在1分10秒-2分钟将四环素完全降解。
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