CN110152687A - 一种利用天然黄铁矿制备复合光催化剂的方法 - Google Patents
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Abstract
本发明涉及一种利用天然黄铁矿制备复合光催化剂的方法,属于光催化剂技术领域。本发明将天然黄铁矿进行球磨研磨20~30 min得到天然黄铁矿粉;将得到的天然黄铁矿粉过筛,然后匀速升温至温度为200~600℃并恒温煅烧2~2.5 h,随炉冷却即得复合光催化剂。本发明复合光催化剂可应用于光催化降解卡马西平和/或双氯芬酸钠。本发明的复合光催化剂活性高,用于光催化降解卡马西平和/或双氯芬酸钠废水,在室温模拟太阳光条件下具有优于纯Fe2S催化剂的光催化活性,降解率可提高35~36%。
Description
技术领域
本发明涉及一种利用天然黄铁矿制备复合光催化剂的方法,属于光催化剂技术领域。
背景技术
药品和个人护理用品(PPCPs)是指包括人和动物使用的各种药品和日常护理品在内的多种化学物质的总称,常见的有消炎药、抗生素、镇静剂、抗癫痫药、降压药等。该类污染物是继除草剂、杀虫剂之后发现的在水体中普遍存在的痕量有机污染物,其与人类的生产活动紧密相关。虽然它们在环境中的浓度较低,但由于其极性较强以及具有较强的生物活性,并且当这类污染物长期存在于环境中时很难被降解,从而表现出一定的毒性效应和干扰效应等,不仅会对环境造成污染,也会对人类身体健康带来影响。其中卡马西平(CBZ)和双氯芬酸钠(DCF)是这类污染物的典型代表,卡马西平是一种典型的抗癫痫药物,而双氯芬酸钠是一种起效较快的抗炎药。这些污染物能够长期作用于水环境,对水生态系统产生潜在威胁,同时造成水体污染,进而直接或间接对饮用水质量造成影响,危害人体健康。因此,开发针对这类污染物的去除技术,对预防大量药品和个人护理用品污染物进入环境具有重要意义。
光催化技术因其成本低、操作简单、降解效率高等特点,在污染物的降解方面显示出了巨大的优势,它主要是利用半导体催化材料吸收光产生的电子-空穴对诱发氧化与还原反应,从而降解污染物。黄铁矿是自然界分布最广泛的铁硫化物半导体,其价带上的电子易受外部能量的激发而跳跃到导电带,从而表现出良好的半导体性能和光学性。但目前国内外研究者对黄铁矿的研究主要集中于黄铁矿的吸附、交换以及矿物学属性的研究,对其光催化性能关注和研究较少。
发明内容
本发明针对现有技术存在的问题,提供一种利用天然黄铁矿制备复合光催化剂的方法,本发明通过热处理过程,使得天然黄铁矿的结构转变并且形成的不同物相结构组分之间有紧密接触的界面,有利于电荷传输;利用热处理促使天然黄铁矿结构转变制备得到的光催化剂具有较好的光催化性能,在室温模拟太阳光条件下对卡马西平和双氯芬酸钠废水的光催化降解率得到了明显的改善,具有良好的应用前景。
一种利用天然黄铁矿制备复合光催化剂的方法,具体步骤如下:
(1)将天然黄铁矿进行球磨研磨20~25 min得到天然黄铁矿粉;
(2)将步骤(1)的天然黄铁矿粉过筛,然后匀速升温至温度为200~800 ℃并恒温煅烧2~2.5 h,随炉冷却即得复合光催化剂。
所述匀速升温速率为5~ 6 ℃/min。
所述复合光催化剂在光催化降解卡马西平和/或双氯芬酸钠中的应用。
所述复合光催化剂在光催化降解卡马西平和/或双氯芬酸钠中的应用方法,具体步骤为:
(1)将复合光催化剂加入到含有卡马西平和/或双氯芬酸钠的溶液中混合均匀并吸附至平衡状态得到体系A;
(2)在室温、光照条件下,体系A中卡马西平和/或双氯芬酸钠进行光催化降解反应,利用紫外-可见分光光度法测量卡马西平和/或双氯芬酸钠溶液的吸光度并计算其转化率。
所述含有卡马西平和/或双氯芬酸钠的溶液中卡马西平的浓度为2.5~ 12.5 mg/L,双氯芬酸钠的浓度为10~20 mg/L;
所述体系A中复合光催化剂的浓度为0.8~ 1.6 g/L。
本发明的有益效果是:
(1)本发明的复合光催化剂活性高,用于光催化降解卡马西平和/或双氯芬酸钠废水,在室温模拟太阳光条件下具有优于纯Fe2S催化剂的光催化活性,降解率可提高35~36%;
(2)本发明复合光催化剂实现了资源利用化,不仅实现了黄铁矿的资源化利用,同时可解决PPCPs污染问题;
(3)本发明方法的工艺简单,并且涉及的原料价廉易得,无危险和昂贵的化学药品,制备过程安全性能高且成本低。
附图说明
图1为实施例1复合光催化剂的XRD图;
图2为实施例1复合光催化剂对卡马西平的活性图;
图3为实施例1复合光催化剂对双氯芬酸钠的活性图。
具体实施方式
下面结合具体实施方式对本发明作进一步详细说明,但本发明的保护范围并不限于所述内容。
实施例1:一种利用天然黄铁矿制备复合光催化剂的方法,具体步骤如下:
(1)将天然黄铁矿进行球磨研磨20min得到天然黄铁矿粉;
(2)将步骤(1)的天然黄铁矿粉过筛,然后匀速升温至温度为400℃并恒温煅烧2h,随炉冷却即得复合光催化剂;其中匀速升温速率为5℃/min;
本实施例复合光催化剂的XRD图见图1,从图1可知,黄铁矿经过热处理后其晶体结构发生了明显变化,成功制得了复合光催化剂;
所述复合光催化剂在光催化降解卡马西平中的应用方法,具体步骤为:
(1)将复合光催化剂加入到含有卡马西平的溶液中混合均匀并吸附至平衡状态得到体系A;其中含有卡马西平的溶液中卡马西平的浓度为2.5 mg/L;体系A中复合光催化剂的浓度为0.8g/L;
(2)在室温、模拟太阳光氙灯的照射条件下,体系A中卡马西平进行光催化降解反应30min,每间隔5min取样,利用紫外-可见分光光度法测量卡马西平溶液的吸光度并计算其转化率;
本实施例复合光催化剂对卡马西平的活性图见图2,从图2可知,所制得的复合光催化剂可成功诱导卡马西平光催化降解;
纯Fe2S催化剂在30min内无法对卡马西平实现光催化降解,而本实施例复合光催化剂在30min对卡马西平的光催化降解率为36%;
所述复合光催化剂在光催化降解双氯芬酸钠中的应用方法,具体步骤为:
(1)将复合光催化剂加入到含有双氯芬酸钠的溶液中混合均匀并吸附至平衡状态得到体系A;其中含有双氯芬酸钠的溶液中双氯芬酸钠的浓度为10 mg/L;体系A中复合光催化剂的浓度为0.8g/L;
(2)在室温、模拟太阳光氙灯的照射条件下,体系A中双氯芬酸钠进行光催化降解反应30min,每间隔5min取样,利用紫外-可见分光光度法测量双氯芬酸钠溶液的吸光度并计算其转化率;
本实施例复合光催化剂对双氯芬酸钠的活性图见图3,从图3可知,所制得的复合光催化剂可成功诱导双芬酸钠光催化降解;
纯Fe2S催化剂在30min无法对双氯芬酸钠实现光催化降解,本实施例复合光催化剂在30min对双氯芬酸钠的催化降解率为35%。
实施例2:一种利用天然黄铁矿制备复合光催化剂的方法,具体步骤如下:
(1)将天然黄铁矿进行球磨研磨25 min得到天然黄铁矿粉;
(2)将步骤(1)的天然黄铁矿粉过筛,然后匀速升温至温度为200℃并恒温煅烧2.5 h,随炉冷却即得复合光催化剂;其中匀速升温速率为5℃/min;
所述复合光催化剂在光催化降解卡马西平中的应用方法,具体步骤为:
(1)将复合光催化剂加入到含有卡马西平的溶液中混合均匀并吸附至平衡状态得到体系A;其中含有卡马西平的溶液中卡马西平的浓度为2.5 mg/L;体系A中复合光催化剂的浓度为 1.6 g/L;
(2)在室温、模拟太阳光氙灯的照射条件下,体系A中卡马西平进行光催化降解反应30min,每间隔5min取样,利用紫外-可见分光光度法测量卡马西平溶液的吸光度并计算其转化率;
纯Fe2S催化剂在30min内无法对卡马西平实现光催化降解,而本实施例复合光催化剂在30min对卡马西平的光催化降解率为28%;
所述复合光催化剂在光催化降解双氯芬酸钠中的应用方法,具体步骤为:
(1)将复合光催化剂加入到含有双氯芬酸钠的溶液中混合均匀并吸附至平衡状态得到体系A;其中含有双氯芬酸钠的溶液中双氯芬酸钠的浓度为10 mg/L;体系A中复合光催化剂的浓度为 1.6 g/L;
(2)在室温、模拟太阳光氙灯的照射条件下,体系A中双氯芬酸钠进行光催化降解反应30min,每间隔5min取样,利用紫外-可见分光光度法测量双氯芬酸钠溶液的吸光度并计算其转化率;
纯Fe2S催化剂在30min无法对双氯芬酸钠实现光催化降解,本实施例复合光催化剂在30min对双氯芬酸钠的催化降解率为26%。
实施例3:一种利用天然黄铁矿制备复合光催化剂的方法,具体步骤如下:
(1)将天然黄铁矿进行球磨研磨20 min得到天然黄铁矿粉;
(2)将步骤(1)的天然黄铁矿粉过筛,然后匀速升温至温度为600℃并恒温煅烧2 h,随炉冷却即得复合光催化剂;其中匀速升温速率为6℃/min;
所述复合光催化剂在光催化降解卡马西平中的应用方法,具体步骤为:
(1)将复合光催化剂加入到含有卡马西平的溶液中混合均匀并吸附至平衡状态得到体系A;其中含有卡马西平的溶液中卡马西平的浓度为2.5 mg/L;体系A中复合光催化剂的浓度为 0.8 g/L;
(2)在室温、模拟太阳光氙灯的照射条件下,体系A中卡马西平进行光催化降解反应30min,每间隔5min取样,利用紫外-可见分光光度法测量卡马西平溶液的吸光度并计算其转化率;
纯Fe2S催化剂在30min内无法对卡马西平实现光催化降解,而本实施例复合光催化剂在30min对卡马西平的光催化降解率为25%;
所述复合光催化剂在光催化降解双氯芬酸钠中的应用方法,具体步骤为:
(1)将复合光催化剂加入到含有双氯芬酸钠的溶液中混合均匀并吸附至平衡状态得到体系A;其中含有双氯芬酸钠的溶液中双氯芬酸钠的浓度为10 mg/L;体系A中复合光催化剂的浓度为 0.8 g/L;
(2)在室温、模拟太阳光氙灯的照射条件下,体系A中双氯芬酸钠进行光催化降解反应30min,每间隔5min取样,利用紫外-可见分光光度法测量双氯芬酸钠溶液的吸光度并计算其转化率;
纯Fe2S催化剂在30min无法对双氯芬酸钠实现光催化降解,本实施例复合光催化剂在30min对双氯芬酸钠的催化降解率为24%。
实施例4:一种利用天然黄铁矿制备复合光催化剂的方法,具体步骤如下:
(1)将天然黄铁矿进行球磨研磨20 min得到天然黄铁矿粉;
(2)将步骤(1)的天然黄铁矿粉过筛,然后匀速升温至温度为800℃并恒温煅烧2 h,随炉冷却即得复合光催化剂;其中匀速升温速率为5℃/min;
所述复合光催化剂在光催化降解卡马西平中的应用方法,具体步骤为:
(1)将复合光催化剂加入到含有卡马西平的溶液中混合均匀并吸附至平衡状态得到体系A;其中含有卡马西平的溶液中卡马西平的浓度为2.5 mg/L;体系A中复合光催化剂的浓度为 0.8 g/L;
(2)在室温、模拟太阳光氙灯的照射条件下,体系A中卡马西平进行光催化降解反应30min,每间隔5min取样,利用紫外-可见分光光度法测量卡马西平溶液的吸光度并计算其转化率;
纯Fe2S催化剂在30min内无法对卡马西平实现光催化降解,而本实施例复合光催化剂在30min对卡马西平的光催化降解率为28%;
所述复合光催化剂在光催化降解双氯芬酸钠中的应用方法,具体步骤为:
(1)将复合光催化剂加入到含有双氯芬酸钠的溶液中混合均匀并吸附至平衡状态得到体系A;其中含有双氯芬酸钠的溶液中双氯芬酸钠的浓度为10 mg/L;体系A中复合光催化剂的浓度为 0.8 g/L;
(2)在室温、模拟太阳光氙灯的照射条件下,体系A中双氯芬酸钠进行光催化降解反应30min,每间隔5min取样,利用紫外-可见分光光度法测量双氯芬酸钠溶液的吸光度并计算其转化率;
纯Fe2S催化剂在30min无法对双氯芬酸钠实现光催化降解,本实施例复合光催化剂在30min对双氯芬酸钠的催化降解率为25%。
Claims (3)
1.一种利用天然黄铁矿制备复合光催化剂的方法,其特征在于,具体步骤如下:
(1)将天然黄铁矿进行球磨研磨20~25 min得到天然黄铁矿粉;
(2)将步骤(1)的天然黄铁矿粉过筛,然后匀速升温至温度为200~800 ℃并恒温煅烧2~2.5 h,随炉冷却即得复合光催化剂。
2.根据权利要求1所述利用天然黄铁矿制备复合光催化剂的方法,其特征在于:匀速升温速率为5~6 ℃/min。
3.权利要求1所述利用天然黄铁矿制备复合光催化剂的方法所制备的复合光催化剂在光催化降解卡马西平和/或双氯芬酸钠中的应用。
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