CN110152649A - 一种正方相氧化铋活性炭光催化剂的制备方法及应用 - Google Patents
一种正方相氧化铋活性炭光催化剂的制备方法及应用 Download PDFInfo
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Abstract
本发明涉及一种正方相氧化铋活性炭光催化剂的制备方法及应用，属于光催化剂技术领域。本发明将失活的活性炭置于微波功率为800~1000 W、温度为600~900℃条件下恒温反应10~30 min得到再生活性炭；将再生活性炭与赖氨酸溶液、硝酸铋溶液混合均匀并在搅拌条件下浸渍反应120~240 min，然后再置于微波功率为500~1000W、温度300~900℃条件下微波焙烧10~30min即得正方相Bi2O3‑AC光催化剂。本发明将失活活性炭作为金属氧化物的载体，制备正方相氧化铋活性炭光催化剂提高吸附能力并且在可见/紫外光的照射下可降解染料废水中的染料。
Description
技术领域
本发明涉及一种正方相氧化铋活性炭光催化剂的制备方法及应用，属于光催化剂技术领域。
背景技术
活性炭具有孔结构发达、高比表面积、可循环利用等优异性能，是一种良好的吸附剂可广泛用于处理工业废水，在使用一段时间后由于活性炭失活产生大量的失活活性炭。失活活性炭若不能高效利用将对环境和人体健康造成严重影响，因此失活活性炭的处理成了必然趋势。
氧化铋(Bi2O3)为P型半导体材料，包括的晶型有单斜晶型的α-Bi2O3，正方晶型的β-Bi2O3，立方晶型的γ- Bi2O3和δ-Bi2O3。Bi2O3被认为是安全、无毒和无致癌的光催化剂，其带隙较窄为2.8 eV。Bi2O3具有光生载流子分离能力强、高活性、无毒、低成本等优点，受到人们更多的关注，在电子陶瓷材料、光伏电池、燃料电池、光电子器件和催化剂材料方面均有应用。
随着纺织工业的迅速发展，印染类的工业废水排放量也逐年增加。据有关数据统计，全球每年染料废水的排放量达到了6万吨。染料排放到水资源中会对水生生物和食物网造成干扰，也会对人体引起过敏性皮炎和皮肤刺激，其中一些已被报道为致癌物。因此，用高效、经济的技术处理废水中的染料是当务之急。
现有技术中光催化水处理的催化剂一般采用TiO2负载金属氧化物催化剂，但是其带隙为3.2 ev，只能吸收紫外光，未能吸收可见光，因此需要研究出一种可同时吸收紫外和可见光的水处理光催化剂。
发明内容
本发明针对现有技术存在的问题，提供一种正方相氧化铋活性炭光催化剂的制备方法，本发明将失活活性炭作为金属氧化物的载体，制备正方相氧化铋活性炭光催化剂提高吸附能力并且在可见/紫外光的照射下可降解染料废水中的刚果红。
一种正方相氧化铋活性炭光催化剂的制备方法，具体步骤如下：
（1）将失活的活性炭置于微波功率为800~1000 W、温度为600~900℃条件下恒温反应10~30 min得到再生活性炭；
（2）将步骤（1）再生活性炭与赖氨酸溶液、硝酸铋溶液混合均匀并在搅拌条件下浸渍反应 120~240 min，然后再置于微波功率为500~1000W、温度300~900℃条件下微波焙烧10~30min即得正方相Bi2O3-AC光催化剂。
所述步骤（1）失活的活性炭的粒径为180~300目，亚甲基蓝吸附值为30~60mg/g（亚甲基蓝吸附值根据国家标准GB/T12496.10-1999测定）。
进一步地，所述失活的活性炭为处理过蒽醌的失活活性炭；
所述步骤（2）赖氨酸溶液的浓度为0.5~1.5 g/L，硝酸铋溶液的浓度为0.10~0.25mol/L。
进一步地，所述再生活性炭与赖氨酸溶液、硝酸铋溶液的固液比g:mL:mL为1:1:5。
所述正方相氧化铋活性炭光催化剂用于降解去除染料废水中的染料。
优选的，所述正方相氧化铋活性炭光催化剂用于降解去除染料废水中的刚果红。
本发明的有益效果是：
（1）本发明将处理过蒽醌的失活活性炭进行微波再生改性处理，微波辅助失活活性炭再生改性所需能耗低，加热速率快，失活活性炭再生改性处理避免了有害固体废物的二次污染，实现了有用资源的循环利用；
（2）本发明以硝酸铋为前驱体，赖氨酸为分散剂，通过微波辅助对失活活性炭进行再生改性处理制备得到正方相氧化铋活性炭Bi2O3-AC；赖氨酸通过电荷排斥和高分子位阻效应，使活性炭与硝酸铋均匀并稳定地悬浮在溶剂中结合微波快速分解硝酸铋使Bi2O3负载在活性炭表面，可实现工业化生产；
（3）本发明制备的正方相Bi2O3-AC光催化剂相比于失活活性炭，经过微波与分散剂结合处理后增大了活性炭的比表面积，提高了吸附性能，负载正方相Bi2O3的正方相Bi2O3-AC光催化剂具有光催化降解染料废水的优良性能；
（4）本发明操作简单，成本低，吸附降解染料废水效果显著，有利于实现工业化生产。
附图说明
图1为实施例3 正方相氧化铋活性炭光催化剂Bi2O3-AC的XRD图；
图2为实施例3 正方相氧化铋活性炭光催化剂Bi2O3-AC的扫描电镜图；
图3为实施例3 正方相氧化铋活性炭光催化剂Bi2O3-AC扫描电镜图的能谱图；
图4为实施例3正方相氧化铋活性炭光催化剂Bi2O3-AC在可见/紫外光照射下光催化不同时间的刚果红溶液染料的降解效果图。
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1：一种正方相氧化铋活性炭光催化剂的制备方法，具体步骤如下：
（1）将失活的活性炭置于微波功率为800W、温度为600℃条件下恒温反应30 min得到再生活性炭；其中失活的活性炭为处理过蒽醌的失活活性炭，失活的活性炭的粒径为180目，亚甲基蓝吸附值为30mg/g；
（2）将步骤（1）再生活性炭与赖氨酸溶液、硝酸铋溶液混合均匀并在搅拌条件下浸渍反应180 min，然后再置于微波功率为700W、温度500℃条件下微波焙烧10min即得正方相Bi2O3-AC光催化剂；其中赖氨酸溶液的浓度为0.5 g/L，硝酸铋溶液的浓度为0.20mol/L，再生活性炭与赖氨酸溶液、硝酸铋溶液的固液比g:mL:mL为1:1:5；
本实施例正方相Bi2O3-AC光催化剂的亚甲基蓝吸附值为160mg/g，取50 mg的正方相Bi2O3-AC光催化剂对200 mL初始浓度为150mg/L的刚果红溶液在可见光照射下催化降解反应，在180 min内刚果红的去除率为80.47%，取50 mg的正方相Bi2O3-AC光催化剂对200 mL初始浓度为150mg/L的刚果红溶液在紫外光照射下催化降解反应，在180 min内刚果红的去除率为89.6%。
实施例2：一种正方相氧化铋活性炭光催化剂的制备方法，具体步骤如下：
（1）将失活的活性炭置于微波功率为1000 W、温度为900℃条件下恒温反应10 min得到再生活性炭；其中失活的活性炭为处理过蒽醌的失活活性炭，失活的活性炭的粒径为200目，亚甲基蓝吸附值为45mg/g；
（2）将步骤（1）再生活性炭与赖氨酸溶液、硝酸铋溶液混合均匀并在搅拌条件下浸渍反应 120 min，然后再置于微波功率为500W、温度300℃条件下微波焙烧30min即得正方相Bi2O3-AC光催化剂；其中赖氨酸溶液的浓度为0.1 g/L，硝酸铋溶液的浓度为0.10mol/L，再生活性炭与赖氨酸溶液、硝酸铋溶液的固液比g:mL:mL为1:1:5；
本实施例正方相Bi2O3-AC光催化剂的亚甲基蓝吸附值为130mg/g，取50 mg的正方相Bi2O3-AC光催化剂对200 mL初始浓度为150mg/L的刚果红溶液在可见光照射下催化降解反应，在 180 min内刚果红的去除率为76.4%，取50 mg的正方相Bi2O3-AC光催化剂对200 mL初始浓度为150mg/L的刚果红溶液在紫外光照射下催化降解反应，在180 min内刚果红的去除率为84.6%。
实施例3：一种正方相氧化铋活性炭光催化剂的制备方法，具体步骤如下：
（1）将失活的活性炭置于微波功率为1000W、温度为800℃条件下恒温反应20min得到再生活性炭；其中失活的活性炭为处理过蒽醌的失活活性炭，失活的活性炭的粒径为200目，亚甲基蓝吸附值为45mg/g；
（2）将步骤（1）再生活性炭与赖氨酸溶液、硝酸铋溶液混合均匀并在搅拌条件下浸渍反应160 min，然后再置于微波功率为1000W、温度900℃条件下微波焙烧20min即得正方相Bi2O3-AC光催化剂；其中赖氨酸溶液的浓度为0.1 g/L，硝酸铋溶液的浓度为0.15mol/L，再生活性炭与赖氨酸溶液、硝酸铋溶液的固液比g:mL:mL为1:1:5；
本实施例正方相Bi2O3-AC光催化剂的XRD图如图1所示，图1中可知，Bi2O3-AC光催化剂具有较强且尖锐的衍射峰，表明具有较强的结晶程度；C峰主要出现在衍射角2θ = 22.3°，43.8°处；在衍射角2θ= 27.9°，31.7°，32.6°，46°，46.7°，54.2°，55.5°，57.6°，74.3°可以归类为Bi2O3；Bi2O3以四方相的β-Bi2O3呈现，Bi单质的出现是由于生成的Bi2O3被C还原；Bi2O3-AC光催化剂的扫描电镜图（见图2）与能谱图（见图3），从图2和3中可以看出呈蠕虫状的铋氧化物均匀的分布在活性炭表面，能谱图得到各种元素的分布，可知Bi2O3-AC光催化剂由碳、氧、铋组成；
本实施例正方相Bi2O3-AC光催化剂的亚甲基蓝吸附值为210mg/g，取50 mg的正方相Bi2O3-AC光催化剂对200 mL初始浓度为150mg/L的刚果红溶液在可见光照射下催化降解反应，在180 min内刚果红的去除率为96.4%，取50 mg的正方相Bi2O3-AC光催化剂对200 mL初始浓度为150mg/L的刚果红溶液在紫外光照射下催化降解反应，在180 min内刚果红的去除率为98.5%；
本实施例正方相Bi2O3-AC光催化剂在可见光/紫外光照射下催化降解刚果红的降解效果图见图4，从图中可知在黑暗条件下T=60 min和T=80 min时，刚果红染料去除率几乎不变，达到活性炭吸附平衡；T=100min时，可见光与紫外光照射下染料去除率明显提高，紫外光提升较大；在T=160min后，刚果红溶液在紫外光照射下去除率达98.5%，几乎为无色，说明制备的Bi2O3-AC具有较好的光催化性能。
实施例4：一种正方相氧化铋活性炭光催化剂的制备方法，具体步骤如下：
（1）将失活的活性炭置于微波功率为900 W、温度为800℃条件下恒温反应30 min得到再生活性炭；其中失活的活性炭为处理过蒽醌的失活活性炭，失活的活性炭的粒径为300目，亚甲基蓝吸附值为60mg/g；
（2）将步骤（1）再生活性炭与赖氨酸溶液、硝酸铋溶液混合均匀并在搅拌条件下浸渍反应 240 min，然后再置于微波功率为800W、温度700℃条件下微波焙烧20min即得正方相Bi2O3-AC光催化剂；其中赖氨酸溶液的浓度为0.15 g/L，硝酸铋溶液的浓度为0.25mol/L，再生活性炭与赖氨酸溶液、硝酸铋溶液的固液比g:mL:mL为1:1:5；
本实施例正方相Bi2O3-AC光催化剂的亚甲基蓝吸附值为180mg/g，取50 mg的正方相Bi2O3-AC光催化剂对200 mL初始浓度为150mg/L的刚果红溶液在可见光照射下催化降解反应，在 180 min内刚果红的去除率为82.8%，取50 mg的正方相Bi2O3-AC光催化剂对200 mL初始浓度为150mg/L的刚果红溶液在紫外光照射下催化降解反应，在180 min内刚果红的去除率为91.4%。
Claims (5)
1.一种正方相氧化铋活性炭光催化剂的制备方法，其特征在于，具体步骤如下：
（1）将失活的活性炭置于微波功率为800~1000W、温度为600~900℃条件下恒温反应10~30min得到再生活性炭；
（2）将步骤（1）再生活性炭与赖氨酸溶液、硝酸铋溶液混合均匀并在搅拌条件下浸渍反应120~240 min，然后再置于微波功率为500~1000W、温度300~900℃条件下微波焙烧10~30min即得正方相Bi2O3-AC光催化剂。
2.根据权利要求1所述正方相氧化铋活性炭光催化剂的制备方法，其特征在于：步骤（1）失活的活性炭的粒径为180~300目。
3.根据权利要求1所述正方相氧化铋活性炭光催化剂的制备方法，其特征在于：步骤（2）赖氨酸溶液的浓度为0.5~1.5 g/L，硝酸铋溶液的浓度为0.10~0.25mol/L。
4.根据权利要求3所述正方相氧化铋活性炭光催化剂的制备方法，其特征在于：再生活性炭与赖氨酸溶液、硝酸铋溶液的固液比g:mL:mL为1:1:5。
5.权利要求1所述正方相氧化铋活性炭光催化剂的制备方法所制备的正方相氧化铋活性炭光催化剂用于降解去除染料废水中的染料。
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