CN113351223A - 一种零价Pd/Cu改性毛竹遗态复合材料的制备方法及应用 - Google Patents
一种零价Pd/Cu改性毛竹遗态复合材料的制备方法及应用 Download PDFInfo
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Abstract
本发明公开了一种零价Pd/Cu改性毛竹遗态复合材料的制备方法及应用。将切成条状的毛竹用去离子水洗涤，干燥后置于氮气氛围的管式炉中于600℃煅烧4h，经冷却、研磨和过筛制得毛竹碳；称取不同质量比的PdCl2和CuCl2于100mL具塞玻璃瓶中，用50mL去离子水溶解，称取0.5600g毛竹碳加入玻璃瓶中，塞上密封塞，通入氮气20min，随后超声1h；称取过量NaBH4于20mL去离子水中溶解，使用滴管逐滴加入，再以130rpm的转速震荡30min，随后用无水乙醇和去离子水反复清洗，抽滤后于40℃烘箱中烘干得到零价Pd/Cu改性毛竹遗态复合材料。本发明制备工艺简单，成本低廉，对水中的硝酸盐具有良好的去除效果，电催化还原反应后的材料能通过抽滤进行循环再利用，且利用效果高。
Description
技术领域
本发明属于废物资源化利用和水处理技术领域，特别涉及一种零价Pd/Cu改性毛竹遗态复合材料的制备方法及应用。
背景技术
随着我国社会生产的发展和生活水平的提高，生活污水和工业废水进入自然环境的排放量迅速增加，当前我国很多城市和地区的地下水和地表水源均受到不同程度的NO3-N污染，严重威胁着用水人群的身体健康。硝酸盐也是地表水和地下水中常见的污染物，自然界中硝酸盐的积累主要是由于化石燃料的燃烧、富氮化肥的过度使用、生活工业污废水的排放等人为活动引起的，为去除饮用水源中的NO3-N盐，保障饮用水卫生安全，多种技术被相继提出。
当前脱除水体中硝酸盐的工艺方法主要包括生物处理技术和物理化学处理技术两大技术。物理过程，如反渗透、电渗析和接触过滤法具有成本高的缺点；生物法主要是利用聚磷菌的“好氧摄磷，厌氧释磷”的生理生化活动，再通过排放剩余污泥来实现除P目的，但除P效率较为有限。其中，多相催化还原法因反应迅速、无二次污染等被视为最有发展前景的脱氮技术。但其相关研究尚不成熟，运行效能目前无法满足净水工程上的应用需求。现阶段，基于解决催化剂的催化活性和选择性之间的统一问题，设计和研发出具有高催化活性和N2选择性的催化剂，是推动该技术发展和实际应用的关键途径。
中国是世界上的最大产竹国，竹类资源丰富。毛竹在我国栽培面积大，特别是广西地区，毛竹产量久居全国前列。竹类的开采、加工和利用过程中会产生大量低价值的竹类废弃物，竹类废弃物如被随意丢弃，或腐烂、或掩埋和或焚烧，都会对环境造成污染，也是对竹类资源的一种浪费。毛竹其自身具有不同尺度范围的有序多孔特殊解剖结构、发达的微孔构造和较大比表面积，常被用于制备吸附材料。如果能有效利用毛竹废弃物资源，不仅可以使其变废为宝，而且能达到较好的经济效益和社会效益，这对促进全国毛竹产业的可持续发展具有重要意义。
采用具有高效、高选择性、易回收等优势的钯、铜为原料，通过遗态改性技术制备出Pd/Cu复合材料，对其载体基材选择、载体改性以及其表面结构修饰、催化还原条件等方面开展毛竹生物碳材料的制备及表面定向修饰，结合材料表征结果，分析材料中Pd和Cu的形态组成、载体修饰结构设计等影响机制，不仅可以提高毛竹废弃物资源的利用率，还可以为实现水中硝酸盐氮的处理提供一条绿色可靠高效的途径。
发明内容
本发明涉及零价Pd/Cu改性毛竹遗态复合材料的制备及应用。该方法通过在不同质量比的PdCl2和CuCl2的混合液中，加入一定质量煅烧后的毛竹碳，在NaBH4作用下还原制备零价Pd/Cu改性毛竹遗态复合材料，通过控制改性条件，合成的复合材料既保留天然生物炭丰富的多孔形态结构，又具有更高的比表面积。对其物相特征、结构和成分以及形貌进行表征，并应用于水体中硝酸盐氮的去除。
1.一种零价Pd/Cu改性毛竹遗态复合材料的制备方法及应用，其特征在于具体步骤为：
(1)将毛竹切成条状块体，用去离子水反复洗涤去除表面杂质，干燥后置于氮气氛围的管式炉中，在600℃温度下煅烧4h，经冷却、研磨和过筛(18目)获得实验所需的毛竹碳材料；
(2)分别称取0.5097g、0.3185g、0.1272g的PdCl2和0.1600g、0.4000g、0.6390g的CuCl2于100mL具塞玻璃瓶中，加入50mL去离子水使其充分溶解；
(3)称取0.5600g的毛竹碳于玻璃瓶中，塞上橡胶密封塞，利用两个长短不一的16号不锈钢针穿过塞子，一根针连接N2气体供应，另一根针作为排气口，持续通入氮气20min排出瓶中及溶液中的氧气，随后超声1h，使毛竹碳均匀分布散于溶液中；
(4)称取过量NaBH4于20mL去离子水中溶解，使用滴管逐滴加入上述玻璃瓶中，再以130rpm的转速震荡30min使BH4 -与Cu2+、Pd2+充分反应。
(5)完全反应后静置至固体颗粒与液体分层，用针管抽去液体，用无水乙醇和去离子水反复清洗多次固体颗粒，抽滤后置于40℃烘箱中烘干，得到纳米零价钯和纳米零价铜质量比分别为4:1，1:1，1:4的零价Pd/Cu改性毛竹遗态复合材料。
2.根据权利要求1中所述的一种零价Pd/Cu改性毛竹遗态复合材料的制备方法，其特征是步骤(2)中所述的不同质量比的PdCl2和CuCl2以1:4质量比为最优。
3.根据权利要求1中所述的一种零价Pd/Cu改性毛竹遗态复合材料的制备方法，其特征是步骤(4)中所述的NaBH4为2mol/L。
4.根据权利要求1中所述的一种零价Pd/Cu改性毛竹遗态复合材料的制备方法，其特征是步骤(5)中用无水乙醇和去离子水反复清洗次数为3次。
5.根据权利要求1、2、3或4中所述方法制备的一种零价Pd/Cu改性毛竹遗态复合材料的应用，其特征在于该零价Pd/Cu改性毛竹遗态复合材料应用于对地表水和地下水中硝酸盐氮的电催化分解。
本发明的优点在于：制备的以毛竹生物炭为载体基材的零价纳米Pd/Cu改性遗态复合材料对水中硝酸盐氮具有很好的净化去除效果，反应后的催化材料能够通过抽滤方式进行重复利用。本发明制备的复合材料是一种低成本、操作简易的高效绿色材料，为毛竹碳的改性利用方法探索了一条新的道路，对解决环境污染、促进废物二次利用具有重要意义。
附图说明
图1为本发明实施案例所制备的零价Pd/Cu改性毛竹遗态复合材料的SEM谱图。
图2为本发明实施案例所制备的零价Pd/Cu改性毛竹遗态复合材料的FT-IR谱图。
图3为本发明实施案例所制备的零价Pd/Cu改性毛竹遗态复合材料的XRD谱图。
图4为本发明所制备的零价Pd/Cu改性毛竹遗态复合材料对水中NO3-N的去除效果图。
具体实施方式
实施例零价Pd/Cu改性毛竹遗态复合材料：
(1)将毛竹切成条状块体，用去离子水反复洗涤去除表面杂质，干燥后置于氮气氛围的管式炉中，在600℃温度下煅烧4h，经冷却、研磨和过筛(18目)获得实验所需的毛竹碳材料；
(2)分别称取0.1272g的PdCl2和0.6390g的CuCl2于100mL具塞玻璃瓶中，加入50mL去离子水使其充分溶解；
(3)称取0.5600g的毛竹碳于玻璃瓶中，塞上橡胶密封塞，利用两个长短不一的16号不锈钢针穿过塞子，一根针连接N2气体供应，另一根针作为排气口，持续通入氮气20min排出瓶中及溶液中的氧气，随后超声1h，使毛竹碳均匀分布散于溶液中；
(4)称取过量NaBH4于20mL去离子水中溶解，使用滴管逐滴加入上述玻璃瓶中，再以130rmp的转速震荡30min使BH4 -与Cu2+、Pd2+充分反应。
(5)完全反应后静置至固体颗粒与液体分层，用针管抽去液体，用无水乙醇和去离子水反复清洗多次固体颗粒，抽滤后置于40℃烘箱中烘干，得到纳米零价钯和纳米零价铜质量比分别为1:4的零价Pd/Cu改性毛竹遗态复合材料。
将本实施例制备得到的零价Pd/Cu改性毛竹遗态复合材料应用到对水中NO3-N盐的去除实验。
称取10-18目的100mg本实施例制得到的零价Pd/Cu改性毛竹遗态复合材料置于125mL含硝酸钠浓度为100mg/L的溶液中。在以Na2SO4为支撑电解质，钛辽网为电极，电极板间距为1.5cm，电流密度为100mA，初始pH为7，温度为25℃，转速为900rpm的条件下，进行电催化还原实验，每隔30min取样1mL至比色管中，取样180min。随后定容至50mL，用紫外分光光度仪测定溶液中的硝酸盐氮的浓度，以考察材料的电催化还原能力，结果如图4所示，可以看出，本发明制备得到的零价Pd/Cu改性毛竹遗态复合材料在Pd/Cu质量比为1:4的条件下对硝酸盐氮具有更良好的去除能力。
Claims (5)
1.一种零价Pd/Cu改性毛竹遗态复合材料的制备方法及应用，其特征在于具体步骤为：
(1)将毛竹切成条状块体，用去离子水反复洗涤去除表面杂质，干燥后置于氮气氛围的管式炉中，在600℃温度下煅烧4h，经冷却、研磨和过筛(18目)获得实验所需的毛竹碳BC；
(2)分别称取0.5097g、0.3185g、0.1272g的PdCl2和0.1600g、0.4000g、0.6390g的CuCl2于100mL具塞玻璃瓶中，加入50mL去离子水使其充分溶解；
(3)称取0.5600g的毛竹碳于玻璃瓶中，塞上橡胶密封塞，利用两个长短不一的16号不锈钢针穿过塞子，一根针连接N2气体供应，另一根针作为排气口，持续通入氮气20min排出瓶中及溶液中的氧气，随后超声1h，使毛竹碳均匀分布散于溶液中；
(4)称取过量NaBH4于20mL去离子水中溶解，使用滴管逐滴加入上述玻璃瓶中，再以130rpm的转速震荡30min使BH4 -充分还原Cu2+、Pd2+为零价Pd和零价Cu；
(5)完全反应后静置至固体颗粒与液体分层，用针管抽去液体，用无水乙醇和去离子水反复清洗多次固体颗粒，抽滤后置于40℃烘箱中烘干，得到纳米零价钯和纳米零价铜质量比分别为4:1，1:1，1:4的零价Pd/Cu改性毛竹遗态复合材料。
2.根据权利要求1中所述的一种零价Pd/Cu改性毛竹遗态复合材料的制备方法，其特征是步骤(2)中所述的不同质量比的PdCl2和CuCl2以1:4质量比为最优。
3.根据权利要求1中所述的一种零价Pd/Cu改性毛竹遗态复合材料的制备方法，其特征是步骤(4)中所述的过量的NaBH4为2mol/L。
4.根据权利要求1中所述的一种零价Pd/Cu改性毛竹遗态复合材料的制备方法，其特征是步骤(5)中用无水乙醇和去离子水反复清洗次数为3次。
5.如权利要求1、2、3或4中所述方法制备的一种零价Pd/Cu改性毛竹遗态复合材料的应用，其特征在于该零价Pd/Cu改性毛竹遗态复合材料应用于对地表水和地下水中硝酸盐氮的净化去除。
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| CN114538567A (zh) * | 2022-01-25 | 2022-05-27 | 桂林理工大学 | 一种生物碳基单原子钯铜催化剂的制备及应用方法 |
| CN115078498A (zh) * | 2022-06-13 | 2022-09-20 | 山西大学 | 一种生物质碳材料负载金属纳米颗粒催化剂及其制备方法 |
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| CN114538567A (zh) * | 2022-01-25 | 2022-05-27 | 桂林理工大学 | 一种生物碳基单原子钯铜催化剂的制备及应用方法 |
| CN114538567B (zh) * | 2022-01-25 | 2023-08-11 | 桂林理工大学 | 一种生物碳基单原子钯铜催化剂的制备及应用方法 |
| CN115078498A (zh) * | 2022-06-13 | 2022-09-20 | 山西大学 | 一种生物质碳材料负载金属纳米颗粒催化剂及其制备方法 |
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