CN111085196B - 含碳固体废弃物制备含金属单质颗粒复合光催化剂的方法 - Google Patents
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Abstract
本发明公开一种含碳固体废弃物制备含金属单质颗粒复合光催化剂的方法，具体步骤为：将含碳量为2%~98%的固体废弃物与金属前驱体固态原料按照总固液比为1:10~30加入到pH值为1~6的水溶液中，均匀混合；在20~90℃的温度条件下连续搅拌1~24 h后，过滤，烘干，并制成粉状颗粒；在通有保护气体的条件下，高温反应10~1440 min得到含金属单质颗粒的复合光催化剂。制备过程简单，易实施操作，充分利用了含碳固废的特有性质，制备出的复合光催化剂应用于有机废水处理上效果显著。
Description
技术领域
本发明涉及固体废弃物资源化利用领域，具体涉及一种含碳固体废弃物制备含金属单质颗粒复合光催化剂的方法。
背景技术
含碳固体废弃物主要来源于污水处理厂含碳污泥、工业生产中产生的有机废渣以及生活垃圾等。含碳固体废弃物在一定条件下会发生物性变化，并通过生物圈以及自然力扩散传播污染环境，进而危害动植物体的健康。目前处理含碳固体废弃物的常用方法包括堆肥发酵法、填埋及填海法、二次资源循环再生法、焚烧发电法等。但现有的处理方法通常存在二次污染、能量消耗高或社会效益低等问题，这些问题限制了该类方法的进一步扩大化应用。
解立平等人（城市固体有机废弃物制备中孔活性碳[J]. 过程工程学报, 2002, 2(5): 465-469）以固体有机废弃物热解后的产物为原料制备中孔活性碳，实验表明用木类、纸张和塑料这3种固体有机废弃物热解后的产物为原料可制得中孔发达的活性碳。黄海涛等人（下吸式气化炉处理有机废弃物[J]. 过程工程学报, 2003, 3(5): 477-480）利用热解气化技术将有机固体废弃物转化为气体燃料。潘嘉芬等人（利用河道淤泥等固体废弃物制备水处理多孔陶粒滤料试验研究[J]. 2010, 33(6): 68-71）利用河道淤泥为实验原料，制备多孔陶粒滤料，实验结果表明用河道淤泥制备的陶粒处理含油废水的效果比砂粒的处理效果好。此外，牛花朋等人（粉煤灰与若干有机固体废弃物配施改良土壤的研究进展[J].地球与环境, 2006, 34(2): 27-34）将粉煤灰与若干有机固体废弃物混合投施来改良土壤性质。李谦盛等人（利用工农业有机废弃物生产优质无土栽培基质[J]. 自然资源学报,2002, 17(4): 515-519）利用有机废弃物制造无土栽培中的有机基质，在多种实验作物上取得较好的效果。
以上这些方式虽然开辟了较好的含碳固体废弃物资源化利用的新途径，但是仍然存在一些问题，由于含碳固体废弃物中或多或少的存在重金属物质，会对实验样品产生一定的毒性污染；此外，利用热解法资源化利用含碳固体废弃物所产生的灰烬处理不当也会造成二次污染，无法进行更好的循环再利用。
为了能充分发挥含碳固体废弃物本身的独特性能，并避免现有处理方法带来的一些后续问题，有必要研究一种新的含碳固体废弃物资源化利用方式。
发明内容
针对现有技术中存在的问题，本发明公开一种含碳固体废弃物制备含金属单质颗粒复合光催化剂的方法，充分利用含碳固体废物物中的含碳物质可在高温无氧条件下形成还原性物质的性质，将金属前驱体固态原料引入其中，通过还原性物质与金属离子反应来产生含金属单质颗粒的新型复合光催化剂，所制备的复合光催化剂具有较好的有机废水处理效果。
本发明的技术方案为：一种含碳固体废弃物制备含金属单质颗粒复合光催化剂的方法，具体步骤为：
（1）将含碳量为2%~98%的固体废弃物与金属前驱体固态原料按照总固液比为1:10~30加入到pH值为1~6的水溶液中，均匀混合；
（2）在20~90℃的温度条件下连续搅拌1~24 h后，过滤，洗涤，烘干，并制成粉状颗粒；
（3）在通有保护气体的条件下，高温反应10~1440 min得到含金属单质颗粒的复合光催化剂。
步骤1中，含碳固体废弃物与金属前驱体固态原料的质量比为1: 0.1~5。
步骤1中，含碳固体废弃物包括城市生活污泥、动物粪便、作物废料、木炭废料、食品生产废料、工业有机废料、厨余垃圾中的一种或者多种。
步骤1中，金属前驱体固态原料包括含金属元素Pt、Pd、Au、Ag、Rh、Ru、Ti、Cr、Fe、Co、Ni、Zn、Al、Pb、Sn的一种或者多种化合物。
步骤1中，金属前驱体固态原料中，金属元素的含量为1%~90%。
步骤2中，制成粉状颗粒的方法为研磨、粉碎机粉碎、机械球磨中的一种或多种。
步骤3中，在通有保护气体的条件下，高温反应的温度为200~1000℃。温度较低，含碳固体废弃物中的有机物碳化程度较低或无法碳化，金属单质无法充分被还原出来或根本还原不出来；温度较高，耗能较高且复合光催化剂的光催化性能会发生降低。
制备得到的复合光催化剂的BET在80~2000m2/g，这是由于在复合光催化剂的制备过程中，蛋白质、糖类等有机物高温碳化形成BET比较大的孔隙结构导致的，这也使制备得到的金属单质颗粒复合光催化剂在处理有机废水的过程中能够对有机物进行充分的吸附和光催化降解。
本发明的有益效果为：
1. 本发明公开的制备方法简单，易于操作实施，是含碳固体废弃物资源化利用的一种新型高效方式，充分利用了含碳固体废弃物本身固有的性质，制备出的复合光催化剂光催化性能优异，其BET在80~2000 m2/g，在处理有机废水的过程中能够对有机物进行充分的吸附和光催化降解；
2. 本发明采用湿法处理的方式混合含碳固体废弃物和金属前驱体固态原料，调节pH后可使金属单质颗粒均匀地分散到含碳固体废弃物表面；
3. 烘干后将固体粉碎成固态颗粒，能够保证后续的焙烧过程中固体物质受热更加均匀，并使得制备得到的金属单质复合光催化剂在后期使用中更为便利。
附图说明
图1为实施例1制备的含Au单质纳米颗粒复合光催化剂在全光谱照射1 h内对甲基橙的降解效率图；
图2为实施例3制备的含Cr单质纳米颗粒复合光催化剂在全光谱照射1 h内对水杨酸的降解效率图。
具体实施方式
以下实施例进一步说明本发明的内容，但不应理解为对本发明的限制。在不背离本发明实质的情况下，对本发明方法、步骤或条件所作的修改和替换，均属于本发明的范围。
实施例1
基于城市生活污泥制备含Au单质纳米颗粒复合光催化剂
在城市污水处理厂获取含碳污泥，测定湿污泥含碳率为2%。取5 g湿污泥和0.5 gAuCl3·HCl·4H2O按照1:10的固液比加入到装有蒸馏水的烧杯中，蒸馏水的pH值预先调为1。将混合后的溶液在90℃水浴加热搅拌6 h，之后离心得到固体沉淀；用乙醇-水混合溶液清洗三次后将沉淀烘干并研磨成粉，将研磨后的粉状颗粒放进坩埚中，在氩气保护下，用管式炉于500℃煅烧100min，得到基于污泥活性碳的含Au单质颗粒的复合光催化剂。所得污泥活性炭-Au单质颗粒复合光催化剂的BET达到500 m2/g，并且在全光谱照射1h内对甲基橙的降解效率达到98%（如图1所示）。
实施例2
基于木屑制备含Ag单质纳米颗粒复合光催化剂
在木材加工厂获取木屑，测定木屑含碳率为98%。取2 g木屑和0.2 g AgNO3按照1:20的固液比加入到装有蒸馏水的烧杯中，蒸馏水的pH值预先调为2。将混合后的溶液在90℃水浴加热搅拌1 h，之后离心得到固体沉淀；用乙醇-水混合溶液清洗三次后将沉淀烘干，将烘干后的沉淀放进坩埚中，在氩气保护下用管式炉于1000℃煅烧10 min，得到基于木屑的含Ag单质颗粒的复合光催化剂。所得木屑-Ag单质颗粒复合光催化剂的BET达到1800 m2/g，并且在全光谱照射1 h内对甲基橙的降解效率达到100%。
实施例3
基于废弃树脂制备含Cr单质纳米颗粒复合光催化剂
在树脂生产厂获取废弃树脂，测定废弃树脂含碳率为60%。取3 g废弃树脂和15 gCr(NO3)3·9H2O按照1:30的固液比加入到装有蒸馏水的烧杯中，蒸馏水的pH值预先调为3。将混合后的溶液在室温20℃搅拌24 h，之后离心得到固体沉淀；用乙醇-水混合溶液清洗三次后将沉淀烘干，将烘干后的沉淀放进坩埚中，在氩气保护下用管式炉于200℃煅烧1440min，得到基于废弃树脂的含Cr单质颗粒的复合光催化剂。所得废弃树脂-Cr单质颗粒复合光催化剂的BET达到2000 m2/g，并且在全光谱照射1 h内对水杨酸的降解效率达到99%（如图2所示）。
实施例4
基于酒糟制备含Ni单质纳米颗粒复合光催化剂
在酒厂获取酒糟，测定酒糟含碳率为80%。取5 g酒糟和0.9 g Ni(NO3)2·6H2O按照1:15的固液比加入到装有蒸馏水的烧杯中，蒸馏水的pH值预先调为6。将混合后的溶液在80℃水浴加热搅拌6 h，之后离心得到固体沉淀；用乙醇-水混合溶液清洗三次后将沉淀烘干并研磨成粉，将研磨后的粉状颗粒放进坩埚中，在氩气保护下用管式炉于400℃煅烧240min，得到基于酒糟的含Ni单质颗粒的复合光催化剂。所得酒糟-Ni单质颗粒复合光催化剂的BET达到1850 m2/g，并且在全光谱照射1 h内对水杨酸的降解效率达到97%。
实施例5
基于玉米棒制备含Pt单质纳米颗粒复合光催化剂
在农产品加工处获取玉米棒，测定玉米棒含碳率为90%。取3 g玉米棒，将0.8 gH6N4O4Pt用硝酸溶解于烧杯中，将玉米棒和H6N4O4Pt按照1:10的固液比加入到装有蒸馏水的烧杯中，将混合后的溶液pH调为1。将混合后的溶液在80℃水浴加热搅拌8 h，之后离心得到固体沉淀；用乙醇-水混合溶液清洗三次后将沉淀烘干并研磨成粉，将研磨后的粉状颗粒放进坩埚中，在氩气保护下用管式炉于600℃煅烧240 min，得到基于玉米棒的含Pt单质颗粒的复合光催化剂。所得玉米棒-Pt单质颗粒复合光催化剂的BET达到1400 m2/g，并且在全光谱照射1 h内对环丙沙星的降解效率达到100%。
实施例6
基于鸡粪制备含Co单质纳米颗粒复合光催化剂
在养鸡场获取鸡粪，测定鸡粪含碳率为70%。取4 g鸡粪和0.9 g Co(NO3)2·6H2O按照1:20的固液比加入到装有蒸馏水的烧杯中，蒸馏水的pH值预先调为5。将混合后的溶液在90℃水浴加热搅拌6 h，之后离心得到固体沉淀；用乙醇-水混合溶液清洗三次后将沉淀烘干并研磨成粉，将研磨后的粉状颗粒放进坩埚中，在氩气保护下用管式炉于750℃煅烧120min，得到基于鸡粪的含Co单质颗粒的复合光催化剂。所得鸡粪-Co单质颗粒复合光催化剂的BET达到1200 m2/g，并且在全光谱照射1 h内对环丙沙星的降解效率达到97%。
以上显示和描述了本发明的基本原理、主要特征及优点。但是以上所述仅为本发明的具体实施例，本发明的技术特征并不局限于此，任何本领域的技术人员在不脱离本发明的技术方案下得出的其他实施方式均应涵盖在本发明的专利范围之中。
Claims (1)
1.一种含Cr单质颗粒复合光催化剂的制备方法，其特征在于，该复合光催化剂的BET达到2000 m2/g，在全光谱照射1 h内对水杨酸的降解效率达到99%；制备时首先从树脂生产厂获取废弃树脂，测定废弃树脂含碳率为60%；取3 g废弃树脂和15 g Cr(NO3)3·9H2O按照1:30的固液比加入到装有蒸馏水的烧杯中，蒸馏水的pH值预先调为3；将混合后液在20℃搅拌24 h，之后离心得到固体沉淀；用乙醇-水混合溶液清洗三次后将沉淀烘干，将烘干后的沉淀放进坩埚中，在氩气保护下用管式炉于200℃煅烧1440 min即得到含Cr单质颗粒复合光催化剂。
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