CN109012672A - 一种利用废汞触媒制备复合光催化剂的方法 - Google Patents
一种利用废汞触媒制备复合光催化剂的方法 Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C02F2305/00—Use of specific compounds during water treatment
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Abstract
本发明涉及一种利用废汞触媒制备复合光催化剂的方法,属于资源综合利用以及化工技术领域。将废汞触媒经振动筛除去粒度为5~10目的残渣,剩余的破碎至80~120目,用去离子水和乙醇洗涤至中性,真空干燥得到废汞触媒活性炭原料;将得到的废汞触媒活性炭原料加入到硝酸铁溶液中搅拌12h,过滤并干燥得到浸渍物;将浸渍物微波焙烧制备得到Fe/AC;将得到的Fe/AC分散到水中,然后加入硝酸铜溶液,再按照与Fe/AC质量比为3~8:5加入葡萄糖混合均匀,在汞灯辐射下照射60min,将得到的混合液过滤干燥,制备得到Fe/AC‑Cu复合光催化剂。该方法做到了变废为宝,实现了废弃物的循环利用,有利于缓解资源与环境的压力,具有优越的经济和生态效益。
Description
技术领域
本发明涉及一种利用废汞触媒制备复合光催化剂的方法,属于资源综合利用以及化工技术领域。
背景技术
目前,工业制备聚氯乙烯一般采用乙炔法,然而在制备过程中常用活性炭汞触媒催化以降低成本。活性炭汞触媒是指以优质活性炭作为载体,上面附着少量的汞。经过使用后,活性炭汞触媒催化剂的汞逐渐失效,活性逐渐降低,所以在工业生产中会产生大量的活性炭废汞触媒。然而,汞是一种有害的物质,具有挥发性并且能溶于水,活性炭废汞触媒易对环境造成污染,引起安全隐患。目前,对废汞触媒的回收方法主要有“复盐法”、“高温法”两种,这两种方法存在回收效率低,对设备要求高等缺点。存在活性炭废汞催化剂中的汞难以回收,所以可以考虑将基体活性炭进行回收。因此,高效回收利用活性炭废汞触媒,既可以防止汞破坏环境以及对人身体有伤害,又可以减少经济支出。
近年来,水中有机化合物的污染对人体健康影响引起了全世界的广泛关注,大力开展有机废水的治理研究,是保护环境的重要任务。纺织染料和其他工业染料占据了有机成分的一大部分,这些有机成分对环境造成了巨大的危害,水中残留的染料不经过处理直接排放到江河湖泊中,对人体健康和水生态环境具有直接和间接的影响,给当地的水域带来了一系列严重的负面影响。一般染料较难以降解,然而活性炭被证明是最有效吸附降解染料的材料。
如何制备吸附降解染料最优的活性炭是个难题。
发明内容
针对上述现有技术存在的问题及不足,本发明提供一种利用废汞触媒制备复合光催化剂的方法。本方法以废汞触媒为原料,采用负载焙烧结合的方式制备得到载铁活性炭,再利用葡萄糖作为还原剂,利用光化学沉积法制备Fe/AC-Cu。该方法做到了变废为宝,实现了废弃物的循环利用,有利于缓解资源与环境的压力,具有优越的经济和生态效益。本发明通过以下技术方案实现。
一种利用废汞触媒制备复合光催化剂的方法,其具体步骤如下:
步骤1、将废汞触媒经振动筛除去粒度为5~10目的残渣,剩余的破碎至80~120目,用去离子水和乙醇洗涤至中性,真空干燥得到废汞触媒活性炭原料;
步骤2、将步骤1得到的废汞触媒活性炭原料按照固液比为30~50:60~100g/mL加入到浓度为0.8~1.2mol/L的硝酸铁溶液中搅拌12h,过滤并干燥得到浸渍物;
步骤3、将步骤2得到的浸渍物在温度为300℃~600℃下微波焙烧10~30min制备得到Fe/AC;
步骤4、将步骤3得到的Fe/AC按照固液比为5:100~200g/mL分散到水中,然后按照与水的体积比为100~150:100~200加入浓度为0.1mol/L~0.25mol/L的硝酸铜溶液,再按照与Fe/AC质量比为3~8:5加入葡萄糖混合均匀,在汞灯辐射下照射60min,将得到的混合液过滤干燥,制备得到Fe/AC-Cu复合光催化剂。
所述步骤3微波焙烧微波功率为300~800W。
金属铁具有铁磁性,氧化铁和氧化亚铜属于N型半导体,常被用于光催化剂中,将金属负载到活性炭表面能够提高活性炭的吸附性能。用葡萄糖(HOCH2(CHOH)4CHO)作为还原剂,主要可以发生以下反应:
在紫外或可见光的照射下,氧化铁或氧化亚铜会产生自由基物质可引起氧化或还原反应,反应方程式如下:
Fe2O3/Cu2O (hVB +) + H2O →Fe2O3/Cu2O+ H+ + HO•
Fe2O3/Cu2O (hVB +) + OH-→Fe2O3/Cu2O+ HO•
Fe2O3/Cu2O (eCB -) + O2→Fe2O3/Cu2O+ O2•-
Fe2O3/Cu2O (eCB -) + H+→Fe2O3/Cu2O+ H•
本发明的有益效果是:
(1)本方法以废汞触媒为原料,减少了废弃物的排放和对环境污染,实现了废弃物的资源综合利用。
(2)本方法生产工艺非常简单,操作简单,能耗低,成本低廉且无污染。
(3)本方法充分利用光源制备复合材料,降低了生产成本。
(4)本方法制备的复合光催化剂具有较大的比表面积,可达859.3m2/g,不仅对亚甲基蓝有非常好的吸附效果,亚甲基蓝吸附值可达165mg/g,而且还能光催化降解罗丹明B染料,降解效率可达89.97%。
(5)本方法制备的复合光催化剂在被利用后,可利用吸铁石对活性炭中的铁回收以便多次循环使用。
附图说明
图1是本发明实施例1制备得到的Fe/AC-Cu复合光催化剂的SEM图。
图2是本发明实施例1制备得到的Fe/AC-Cu复合光催化剂的EDS图。
图3是本发明实施例1制备得到的Fe/AC-Cu复合光催化剂的XRD图。
图4是本发明实施例1制备得到的Fe/AC-Cu复合光催化剂光催化降解罗丹明B染料的UV-vis图。
图5是本发明实施例1制备得到的Fe/AC-Cu复合光催化剂吸附亚甲基蓝后用磁铁回收铁图。
具体实施方式
下面结合附图和具体实施方式,对本发明作进一步说明。
下面实施例中实验中比表面积采用全自动物理化学吸附仪(Autosorb-1-C,康塔公司)测定,亚甲基蓝吸附值根据国家标准GBT12496.10-1999测定,光催化降解波长变化图采用紫外分光光度计(UV-2600,岛津)测定。
实施例1
该利用废汞触媒制备复合光催化剂的方法,其具体步骤如下:
步骤1、将废汞触媒经振动筛除去粒度为5目的残渣,剩余的破碎至120目,用去离子水和乙醇洗涤至中性,真空干燥6h得到废汞触媒活性炭原料;
步骤2、将步骤1得到的30g废汞触媒活性炭原料按照固液比为30:100g/mL加入到浓度为0.8mol/L的硝酸铁溶液中搅拌12h,过滤并干燥得到浸渍物;
步骤3、将步骤2得到的浸渍物在温度为600℃下微波焙烧(微波功率为300W)30min制备得到Fe/AC;
步骤4、将步骤3得到的5gFe/AC按照固液比为5:120g/mL分散到水中,然后按照与水的体积比为150:120加入浓度为0.25mol/L的硝酸铜溶液,再按照与Fe/AC质量比为3:5加入葡萄糖混合均匀,在汞灯辐射下(辐射波长为200nm)照射60min,将得到的混合液过滤干燥,制备得到Fe/AC-Cu复合光催化剂。
本实施例中制备得到的Fe/AC-Cu复合光催化剂扫描电镜图(SEM图)如图1所示,从图1中可以看出活性炭基体表面负载了大量的金属颗粒,说明负载效果较为明显。本实施例制备得到的Fe/AC-Cu复合光催化剂的EDS图如图2所述,从图中可以看出复合材料中主要含有C、O、Fe、Cu元素,其中Al为废汞触媒原本包含的杂质,说明此种方法成功地将Fe和Cu负载到活性炭表面上。本实施例制备得到的Fe/AC-Cu复合光催化剂XRD图如图3所示,从图3中可以看出Fe/AC-Cu复合光催化剂主要含有C、Fe2O3,Cu2O,Fe3O4物质,说明经过焙烧后硝酸铁分解成了Fe3O4,Fe2O3,在光化学沉积反应下,葡萄糖将硝酸铜还原成Cu2O。
将本实施例制备得到的Fe/AC-Cu复合光催化剂光催化降解罗丹明B染料得到的UV-vis图如图4所示,从图4中可以看出,在黑暗条件-60min-0min时,染料的去除主要依靠活性炭的吸附,染料几乎不能够被吸附,在紫外灯辐射0-140min时,染料吸光度明显降低,说明复合光催化剂中的Fe2O3和Cu2O具有光催化的性能。
将本实施例制备得到的Fe/AC-Cu复合光催化剂用于吸附甲基蓝后用磁铁回收铁图如图5所示,从图5中可以看出磁铁能够很好地将铁的氧化物与其他物质分离。
经上述方法制备得到的Fe/AC-Cu复合光催化剂的BET比表面积达到859.3m2/g,亚甲基蓝吸附值可达165mg/g,光催化降解罗丹明B染料,降解效率可达89.97%。
实施例2
该利用废汞触媒制备复合光催化剂的方法,其具体步骤如下:
步骤1、将废汞触媒经振动筛除去粒度为10目的残渣,剩余的破碎至80目,用去离子水和乙醇洗涤至中性,真空干燥6h得到废汞触媒活性炭原料;
步骤2、将步骤1得到的50g废汞触媒活性炭原料按照固液比为50:60g/mL加入到浓度为1.2mol/L的硝酸铁溶液中搅拌12h,过滤并干燥得到浸渍物;
步骤3、将步骤2得到的浸渍物在温度为300℃下微波焙烧(微波功率为800W)10min制备得到Fe/AC;
步骤4、将步骤3得到的5gFe/AC按照固液比为5:200g/mL分散到水中,然后按照与水的体积比为100:200加入浓度为0.1mol/L的硝酸铜溶液,再按照与Fe/AC质量比为8:5加入葡萄糖混合均匀,在汞灯辐射下(辐射波长为200nm)照射60min,将得到的混合液过滤干燥,制备得到Fe/AC-Cu复合光催化剂。
经上述方法制备得到的Fe/AC-Cu复合光催化剂的BET比表面积达到837.12m2/g,亚甲基蓝吸附值可达154mg/g,光催化降解罗丹明B染料,降解效率可达83.43%。
实施例3
该利用废汞触媒制备复合光催化剂的方法,其具体步骤如下:
步骤1、将废汞触媒经振动筛除去粒度为6目的残渣,剩余的破碎至100目,用去离子水和乙醇洗涤至中性,真空干燥6h得到废汞触媒活性炭原料;
步骤2、将步骤1得到的40g废汞触媒活性炭原料按照固液比为40:90g/mL加入到浓度为1.0mol/L的硝酸铁溶液中搅拌12h,过滤并干燥得到浸渍物;
步骤3、将步骤2得到的浸渍物在温度为400℃下微波焙烧(微波功率为500W)20min制备得到Fe/AC;
步骤4、将步骤3得到的5gFe/AC按照固液比为5:100g/mL分散到水中,然后按照与水的体积比为80:100加入浓度为0.15mol/L的硝酸铜溶液,再按照与Fe/AC质量比为5:5加入葡萄糖混合均匀,在汞灯辐射下(辐射波长为200nm)照射60min,将得到的混合液过滤干燥,制备得到Fe/AC-Cu复合光催化剂。
经上述方法制备得到的Fe/AC-Cu复合光催化剂的BET比表面积达到845.32m2/g,亚甲基蓝吸附值可达159mg/g,光催化降解罗丹明B染料,降解效率可达85.66%。
以上结合附图对本发明的具体实施方式作了详细说明,但是本发明并不限于上述实施方式,在本领域普通技术人员所具备的知识范围内,还可以在不脱离本发明宗旨的前提下作出各种变化。
Claims (2)
1.一种利用废汞触媒制备复合光催化剂的方法,其特征在于具体步骤如下:
步骤1、将废汞触媒经振动筛除去粒度为5~10目的残渣,剩余的破碎至80~120目,用去离子水和乙醇洗涤至中性,真空干燥得到废汞触媒活性炭原料;
步骤2、将步骤1得到的废汞触媒活性炭原料按照固液比为30~50:60~100 g/mL加入到浓度为0.8~1.2mol/L的硝酸铁溶液中搅拌12h,过滤并干燥得到浸渍物;
步骤3、将步骤2得到的浸渍物在温度为300℃~600℃下微波焙烧10~30min制备得到Fe/AC;
步骤4、将步骤3得到的Fe/AC按照固液比为5:100~200g/mL分散到水中,然后按照与水的体积比为100~150:100~200加入浓度为0.1mol/L~0.25mol/L的硝酸铜溶液,再按照与Fe/AC质量比为3~8:5加入葡萄糖混合均匀,在汞灯辐射下照射60min,将得到的混合液过滤干燥,制备得到Fe/AC-Cu复合光催化剂。
2.根据权利要求1所述的利用废汞触媒制备复合光催化剂的方法,其特征在于:所述步骤3微波焙烧微波功率为300~800W。
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