CN109603760A - 一种吸附盐酸四环素的磁性纳米材料NiFe2O4@ N–C的制备方法 - Google Patents

一种吸附盐酸四环素的磁性纳米材料NiFe2O4@ N–C的制备方法 Download PDF

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CN109603760A
CN109603760A CN201910073847.5A CN201910073847A CN109603760A CN 109603760 A CN109603760 A CN 109603760A CN 201910073847 A CN201910073847 A CN 201910073847A CN 109603760 A CN109603760 A CN 109603760A
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陈哲
陈�峰
刘风磊
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Abstract

本发明提供了一种中空球形NiFe2O4@N‑C的制备方法和应用，属于吸附材料领域。本发明以该产品是以NCHSs（N‑doped carbon composite hollow spheres）为模板，将Ni(NO3)2.6H2O、Fe(NO3)3.9H2O、柠檬酸钠、NH4F、尿素为原料与NCHSs复合在一起制备得到了由纳米片聚集而成的具有中空结构的NiFe2O4@N‑C纳米球，直径为200‑300 nm。本发明提供的中空结构的NiFe2O4@N‑C纳米球结晶度高，晶型完好，能够有效吸附盐酸四环素；另外，本发明提供的中空结构的NiFe2O4@N–C纳米球具有优异的磁性性能，能够反复回收使用。由实施例试验结果可知，将所述材料作为吸附材料吸附盐酸四环素，最大吸附量为271.739mg/g；同时由循环实验可知，该吸附剂具有良好的循环再利用能力，稳定性良好，具有实际应用价值。

Description

一种吸附盐酸四环素的磁性纳米材料NiFe2O4@ N–C的制备 方法
技术领域
本发明涉及吸附技术领域，具体涉及到一种中空球NiFe2O4@ N–C的制备方法，此材料可应用于盐酸四环素的吸附。
背景技术
几十年来，学者们发展了一些去除水环境中传统污染物(金属和有机污染物)的高效方法，如吸附、混凝/絮凝、光催化、化学氧化、离子交换和生物降解，但抗生素污染的环境污染物没有得到有效去除。传统的物理法、化学法和生物法已被用于处理含抗生素废水，如吸附、光催化、絮凝/混凝、膜过滤、真菌处理和氧化。在这些技术中，吸附技术以其操作简单、效率高、能耗低、成本低、易于回收和再利用等优点而成为最方便、最普遍、最有发展前景的技术之一。此外，这一过程不会产生二次污染物。
近年来，掺氮空心碳球(NCHSs)作为一种优良的前驱体越来越受到人们的关注，它具有大的比表面积、多孔结构、良好的机械强度、良好的循环稳定性和导电性。本发明用一种简单、温和、生态化的方法在N掺杂空心碳球(NCHSs)上生长多孔NiFe2O4纳米片继而形成NiFe2O4@ N–C复合材料。
本发明（NiFe2O4@ N–C复合材料）既具有掺氮空心碳球(NCHSs)大的比表面积、多孔结构、良好的机械强度、良好的循环稳定性和导电性等优点，也具有NiFe2O4的多孔材料的优点。从而具有吸附材料所具有的特点，可以用于吸附水体中难以除去的盐酸四环素，同时本发明提供的中空结构的NiFe2O4@ N–C 纳米球具有优异的磁性性能，能够反复回收使用，且本发明提供的制备方法操作简单，适宜工业化生产。
发明内容
本发明的目的是制备一种中空球NiFe2O4@ N–C的吸附材料方法。
为实现上述发明目的，本发明提供以下技术方案：
NCHSs的合成：用量筒称取乙醇溶于水中，混合均匀，向其中滴入 NH3.H2O（25%），磁力搅拌后，再滴入TEOS（正硅酸乙酯），继续搅拌，而后滴入多巴胺（多巴胺分散溶于H2O中），搅拌32 h之后离心、洗涤、干燥。所得黑色粉末转移到瓷舟中，在管式炉中以氮气为保护气，5℃/min程序升温至800℃保持煅烧3h，得到黑色固体粉末，即得NHCS球，备用。
NiFe2O4@ N–C的合成：称取少量NHCS球溶于60ml水中，超声分散，然后向所得混合溶液中逐次加入Ni(NO3)2.6H2O、Fe(NO3)3.9H2O、柠檬酸钠、NH4F、尿素。边加边搅拌，混合均匀后入釜，之后水洗、乙醇洗、干燥。所得样品氧气条件下，以2℃/min的程序升温至400℃保持煅烧3h即得实验所用样品。
优选地，所述氨水的体积为1~3 mL，乙醇的体积为10~15 mL，再滴入TEOS（正硅酸乙酯）体积为0.5~1mL，多巴胺（50 mg/mL）体积为7~9 mL，即得NHCS球。
优选地，所述Ni(NO3)2.6H2O 的浓度为0.2-0.6 mmol, Fe(NO3)3.9H2O的浓度为0.4-1.2 mmol, 且Ni(NO3)2.6H2O：Fe(NO3)3.9H2O的摩尔比为1:2；柠檬酸钠（0.35-0.4mmol）、NH4F（1-3 mmol）、尿素（5-10 mmol）。
本发明还提供了上述方案所述中空NiFe2O4@ N–C材料在吸附盐酸四环素中的应用。所述材料能够吸附盐酸四环素，最大吸附量为271.739mg/g；同时由循环实验可知，该吸附剂具有良好的循环再利用能力，稳定性良好，具有实际应用价值。
附图说明：
图1.本发明中空NiFe2O4@ N–C材料扫描和透射电镜图
图2. 本发明吸附性能图
图3. 本发明吸附性能与前者们的对比图
图4. 本发明循环性能图
具体实施方式：
下面结合实施例对本发明的技术方案及效果作进一步描述。但是，所使用的具体方法、配方、和说明并不是对本发明的限制。
实施例1：NCHSs的合成：用量筒称取12 mL 的乙醇溶于水中，混合均匀后向其中滴入 1 mL NH3.H20（25%），室温磁力搅拌后，再缓慢滴入0.5 mL TEOS（正硅酸乙酯），继续搅拌，而后滴入8 mL多巴胺（50 mg/mL），搅拌32 h之后离心、洗涤、干燥。所得黑色粉末转移到瓷舟中，在管式炉中以氮气为保护气，5℃/min程序升温至800℃保持煅烧3h，得到黑色固体粉末，即得NHCS球，备用。
NiFe2O4@ N–C的合成：称取少量NHCS球溶于60ml水中，超声分散，然后向所得混合溶液中逐次加入0.2 mmol Ni(NO3)2.6H2O、0.4 mmol Fe(NO3)3.9H2O、0.38 mmol 柠檬酸钠、1 mmol NH4F、5 mmol 尿素,边搅拌边加，混合均匀后入釜150℃, 36 h。冷却后水洗、乙醇洗、干燥。所得样品氧气条件下，以2℃/min的程序升温至400℃保持煅烧3h即得实验所用样品。
实施例2：实施例1中的制备NHCS球所述氨水的体积为1~3 mL，乙醇的体积为10~15mL，再滴入TEOS（正硅酸乙酯）体积为0.5~1mL，多巴胺（50 mg/mL）体积为7~9 mL。
实施例3：实施例1中所述NHCS球，煅烧温度为600-800℃, 升温速度为5-10℃/min。
实施例3：实施例1中的制备中空NiFe2O4@ N–C纳米球所述Ni(NO3)2.6H2O 的浓度为0.2-0.6 mmol, Fe(NO3)3.9H2O的浓度为0.4-1.2 mmol, 且Ni(NO3)2.6H2O：Fe(NO3)3.9H2O的摩尔比为1:2；柠檬酸钠（0.35-0.4 mmol）、NH4F（1-3 mmol）、尿素（5-10 mmol）。
实施例4：实施例1中所述中空NiFe2O4@ N–C纳米球，水热反应的温度为150-200℃，时间为24-36 h；煅烧温度为400-800℃，时间为2-4小时，升温速度为5-10℃/min。
实施例5：NiFe2O4@ N–C吸附剂的吸附性能与前者们相比展现出了更好的吸附性能（ACS Sustainable Chem. Eng. 5 (2017) 10298−10306; J. Colloid Interface Sci.368 (2012) (1),540; Chem. Engineering Journal 225 (2013) 679; ChemicalEngineering Journal 178 (2011) 26 .Bioresour. Technol. 151 (2014) 428），如附图表2, 3所示。
实施例6：实施例1中所述中空NiFe2O4@ N–C纳米球，具有优异的磁性性能，也可以反复回收使用，且具有较高的稳定性，如图4所示。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。

Claims (7)

1.一种吸附抗生素盐酸四环素的磁性纳米材料的制备方法，其特征在于，所述中空结构的NiFe2O4@ N–C 纳米球由以NCHSs（N-doped carbon composite hollow spheres）为模板，与Ni(NO3)2.6H2O、Fe(NO3)3.9H2O、柠檬酸钠、NH4F、尿素一起加入到水热釜后，离心，烘干、煅烧而成；所述NiFe2O4@ N–C的粒径为200~300nm，外表面由纳米片聚集而成。
2.根据权利要求1所述的NCHSs球，其特征在于，所述氨水的体积为1~3 mL，乙醇的体积为10~15 mL，再滴入TEOS（正硅酸乙酯）体积为0.5~1mL，多巴胺（50 mg/mL）体积为7~9 mL，即得NHCS球。
3.根据权利要求1所述的NCHSs纳米球，其特征在于， NHCS球煅烧温度为600-800℃,升温速度为5-10℃/min。
4.根据权利要求1所述的中空NiFe2O4@ N–C的制备方法，其特征在于Ni(NO3)2.6H2O（0.2-0.6 mmol）, Fe(NO3)3.9H2O（0.4-1.2 mmol）, 且Ni(NO3)2.6H2O：Fe(NO3)3.9H2O的摩尔比为1:2；柠檬酸钠（0.35-0.4 mmol）、NH4F（1-3 mmol）、尿素（5-10 mmol） 为原料。
5.根据权利要求1所述的中空NiFe2O4@ N–C制备方法，其特征在于，所述步骤水热反应的温度为150-200 ℃，时间为24-36 h；煅烧温度为400-800℃，时间为2-4小时，升温速度为5-10℃/min。
6.根据权利要求1所述的中空NiFe2O4@ N–C 纳米球，其特征在于，所述铁盐包括氯化铁/硫酸铁/硝酸铁；所述镍盐包括氯化镍/硝酸镍/醋酸镍。
7.根据权利要求1所述的中空NiFe2O4@ N–C 纳米球，其特征在于，所获得的产物用电子显微镜观测，其形貌是由纳米片聚集而成的纳米球，直径约为200-300 nm。
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CN112670499A (zh) * 2020-12-23 2021-04-16 浙江理工大学 一种多孔层状CoFe2O4/C纳米复合材料及其制备方法

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