CN112473651A - 一种具有光催化活性的石墨烯气凝胶及其制备方法 - Google Patents
一种具有光催化活性的石墨烯气凝胶及其制备方法 Download PDFInfo
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Abstract
本发明属于石墨烯制备及应用领域，具体涉及一种具有光催化活性的石墨烯气凝胶及其制备方法；该复合材料由三维多孔结构的石墨烯和负载于所述石墨烯表面的Bi2WO6微米颗粒组成；其中,Bi2WO6微米颗粒的直径为3～5μm。制备方法如下：首先将Bi(NO3)3溶液与氧化石墨烯溶液混合均匀,进而将其与Na2WO4混合进行水热反应,制得钨酸铋‑石墨烯复合材料。本发明的钨酸铋‑石墨烯复合材料比表面积大,带隙可达2.96eV,对可见光的吸收性强,可以有效提高光生载流子的分离和降低载流子的复合率,与其单一相相比，表现出更优异的光催化性能。而且，本方法新颖,颗粒均匀、设备操作要求低、工艺简单且过程条件容易控制。
Description
技术领域
本发明属于石墨烯制备及应用领域，具体涉及一种具有光催化活性的石墨烯气凝胶及其制备方法。
背景技术
能源短缺和环境污染是实现社会可持续发展迫切需要解决的问题。在各种污染处理技术中，可见光催化技术可直接利用可见光降解甚至矿化污染物质，在环境保护和新能源开发方面具有良好的应用前景。其中，铋系可见光光催化剂以其独特的电子结构和优良的可见光吸收能力，引起研究者的极大兴趣。常见的铋系光催化剂包括铋氧化物、钛酸铋、钒酸铋、钼酸铋、钨酸铋、铁酸铋等。其中钨酸铋(Bi2WO6)作为一种优异的n型半导体功能材料，不仅带隙能较窄可对可见光进行吸收，同时光化学性质稳定、环境友好，已被广泛用于环境催化领域。
在Bi2WO6材料的研究过程中，研究人员发现，单一Bi2WO6纳米材料存在光谱响应范围窄(<450nm)、光生电子空穴复合速度过快等问题，从而进行了大量基于Bi2WO6材料的研究。研究表明，将石墨烯和半导体光催化材料复合，可提高半导体的可见光催化性能。如将铁酸铋和石墨烯复合后光催化性能有较大的提高，表明石墨烯的复合可改善原材料的光生电子与空穴间的复合作用，使光生电子和空穴能更好的分离。此外，石墨烯较大的比表面积对吸附性能的改善，亦可进一步提高材料的可见光催化性能。
因此，结合钨酸铋和石墨烯材料的各自优势，利用简单易控的一步水热法制备出铁酸铋-石墨烯复合气凝胶。将该气凝胶用于可见光催化降解亚甲基蓝，可取得良好的催化降解效果，对可见光催化技术的发展具有重要的意义。
发明内容
本发明的目的：为解决上述技术问题，提供了一种具有光催化活性的石墨烯气凝胶。
本发明技术方案：一种具有光催化活性的石墨烯气凝胶，其特征在于，所述石墨烯气凝胶中钨酸铋的质量分数为70～95％，石墨烯的质量分数为5～30％。
上述石墨烯气凝胶采用以下步骤制备：
(1)将Bi(NO3)3溶于乙二醇，超声处理；
(2)采用超声处理，将氧化石墨烯分散于去离子水中；
(3)将步骤(1)制得的溶液加入步骤(2)制得的溶液中，搅拌混合；
(4)向步骤(3)制得的溶液中加入Na2WO4，持续搅拌混合，转移至反应釜进行水热反应；
(5)使用去离子水浸泡清洗步骤(4)所得产物，冷冻干燥后得到石墨烯气凝胶。
步骤(1)中Bi(NO3)3浓度为0.001～0.2M，超声处理时间为10～30min；
步骤(2)中氧化石墨烯溶液的浓度为1～20g/L，超声处理时间为30～60min；
步骤(3)中搅拌时间为15～30min；
步骤(4)中Bi(NO3)3与Na2WO4的摩尔比为2:1,持续搅拌混合15～30min，在反应釜进行水热反应的条件为180～200℃，24h；
步骤(5)中的浸泡清洗为2～3天，冷冻干燥-30℃冷冻干燥60～72h。
将上述制备方法制得的石墨烯气凝胶用于处理环境中的污染物。
该发明的有益效果为：本发明提供一种合成钨酸铋-石墨烯复合气凝胶的制备方法，该方法可以一步合成具有光催化活性的石墨烯气凝胶，同时完成氧化石墨烯的还原和钨酸铋-石墨烯的复合。将所得气凝胶用于亚甲基蓝和二氯苯酚的可见光催化降解，催化活性优异。
附图说明
图1是本发明实施例1、2、3与对比例1不同石墨烯含量的钨酸铋-石墨烯复合气凝胶的X射线衍射图(XRD)。(a为对比例1Bi2WO6；b为实施例1Bi2WO6-10％石墨烯气凝胶；c为实施例2Bi2WO6-20％石墨烯气凝胶；d为实施例3Bi2WO6-30％石墨烯气凝胶)
图2是本发明实施例2中Bi2WO6-20％石墨烯对亚甲基蓝的可见光催化效果图。
图3是本发明实施例1、2、3与对比例1中不同石墨烯含量的钨酸铋-石墨烯复合气凝胶对亚甲基蓝的可见光催化效果对比。
具体实施方式
下面将结合附图及具体实施例对本发明的技术方案进行清楚、完整地描述，但是本领域技术人员将会理解，下列所描述的实施例是本发明一部分实施例，而不是全部的实施例，仅用于说明本发明，而不应视为限制本发明的范围。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。实施例中未注明具体条件者，按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者，均为可以通过市售购买获得的常规产品。
实施例1：Bi2WO6-10％石墨烯气凝胶的制备
(1)将0.5mmol Bi(NO3)3溶于20ml乙二醇，超声处理10min；
(2)将氧化石墨烯分散于去离子水中，制得20mL溶液，浓度为1g/L，超声处理40min；
(3)将(1)制得的溶液加入(2)中，搅拌混合15min；
(4)向(3)中加入0.25mmol Na2WO4，持续搅拌混合15min，转移至反应釜进行水热反应，条件为180℃，24h；
(5)使用去离子水浸泡清洗(4)所得产物3天，-30℃冷冻干燥72h后得到石墨烯气凝胶。
(6)以所制得的钨酸铋-石墨烯气凝胶为光催化剂，可见光催化降解亚甲基蓝。亚甲基蓝的初始浓度为40mg/L，气凝胶加入量为0.5g/L，温度为25℃。
由图1b的XRD测试结果可以看出，一步水热法所制得的钨酸铋-石墨烯气凝胶中钨酸铋为Bi2WO6。氧化石墨烯的特征峰完全消失，表明氧化石墨烯在水热过程中完全还原，该材料为Bi2WO6-10％石墨烯气凝胶。
将Bi2WO6-10％石墨烯气凝胶用于可见光催化亚甲基蓝效果较好。由图2可知，亚甲基蓝浓度随光照时间增长而不断降低，光催化3h后，亚甲基蓝去除效率为65％。
对比例1：单一相Bi2WO6的制备
对比例1与实施例1相比，制备过程中不加入氧化石墨烯，其他步骤如上述实施例1，制得单一相钨酸铋材料。由图1a的XRD测试结果可知，所制得钨酸铋为Bi2WO6。
由图2可知，单一相Bi2WO6的光催化活性相对较弱，光催化3h后，亚甲基蓝的去除效率为31％。
实施例2：Bi2WO6-20％石墨烯气凝胶的制备
(1)将0.5mmol Bi(NO3)3溶于20ml乙二醇，超声处理10min；
(2)将氧化石墨烯分散于去离子水中，制得10mL溶液，浓度为5g/L，超声处理40min；
(3)将(1)制得的溶液加入(2)中，搅拌混合15min；
(4)向(3)中加入0.25mmol Na2WO4，持续搅拌混合15min，转移至反应釜进行水热反应，条件为180℃，24h；
(5)使用去离子水浸泡清洗(4)所得产物3天，-30℃冷冻干燥72h后得到石墨烯气凝胶。
(6)以所制得的钨酸铋-石墨烯气凝胶为光催化剂，可见光催化降解亚甲基蓝。亚甲基蓝的初始浓度为40mg/L，气凝胶加入量为0.5g/L，温度为25℃。
由图1c的XRD测试结果可以看出，一步水热法所制得的钨酸铋-石墨烯气凝胶中钨酸铋为Bi2WO6，与实施例1的结果一致。因此，石墨烯加入量的变化不会影响气凝胶中铁酸铋的晶型结构。
将Bi2WO6-20％石墨烯气凝胶用于可见光催化亚甲基蓝降解。由图2可知，亚甲基蓝浓度随光照时间增长而不断降低，光催化3h后，亚甲基蓝去除效率为73％。可见，复合气凝胶中石墨烯含量的增加有利于亚甲基蓝的降解。
实施例3：Bi2WO6-30％石墨烯气凝胶的制备
(1)将0.5mmol Bi(NO3)3溶于20ml乙二醇，超声处理10min；
(2)将氧化石墨烯分散于去离子水中，制得5mL溶液，浓度为17g/L，超声处理40min；
(3)将(1)制得的溶液加入(2)中，搅拌混合15min；
(4)向(3)中加入0.25mmol Na2WO4，持续搅拌混合15min，转移至反应釜进行水热反应，条件为180℃，24h；
(5)使用去离子水浸泡清洗(4)所得产物3天，-30℃冷冻干燥72h后得到石墨烯气凝胶。
(6)以所制得的钨酸铋-石墨烯气凝胶为光催化剂，可见光催化降解亚甲基蓝。亚甲基蓝的初始浓度为40mg/L，气凝胶加入量为0.5g/L，温度为25℃。
由图1b的XRD测试结果可以看出，一步水热法所制得的钨酸铋-石墨烯气凝胶中钨酸铋为Bi2WO6，与实施例1的结果一致。因此，石墨烯加入量的变化不会影响气凝胶中铁酸铋的晶型结构。
将Bi2WO6-30％石墨烯气凝胶用于可见光催化亚甲基蓝降解。由图3可知，光催化3h后，亚甲基蓝去除效率为97％，高于实施例1和实施例2。可见，复合气凝胶中石墨烯含量的进一步增加仍有利于亚甲基蓝的降解。
最后应说明的是：以上各实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述各实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分或者全部技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的范围。
Claims (8)
1.一种具有光催化活性的石墨烯气凝胶，其特征在于，所述石墨烯气凝胶中钨酸铋的质量分数为70～95％，石墨烯的质量分数为5～30％。
2.如权利要求1所述的具有光催化活性的石墨烯气凝胶的制备方法，其特征在于，包括以下步骤：
(1)将Bi(NO3)3溶于乙二醇，超声处理；
(2)采用超声处理，将氧化石墨烯分散于去离子水中；
(3)将步骤(1)制得的溶液加入步骤(2)制得的溶液中，搅拌混合；
(4)向步骤(3)制得的溶液中加入Na2WO4，持续搅拌混合，转移至反应釜进行水热反应；
(5)使用去离子水浸泡清洗步骤(4)所得产物，冷冻干燥后得到石墨烯气凝胶。
3.如权利要求1所述的具有光催化活性的石墨烯气凝胶的制备方法，其特征在于，步骤(1)中Bi(NO3)3浓度为0.001～0.2M，超声处理时间为10～30min。
4.如权利要求1所述的具有光催化活性的石墨烯气凝胶的制备方法，其特征在于，步骤(2)中氧化石墨烯溶液的浓度为1～20g/L，超声处理时间为30～60min。
5.如权利要求1所述的具有光催化活性的石墨烯气凝胶的制备方法，其特征在于，步骤(3)中搅拌时间为15～30min。
6.如权利要求1所述的具有光催化活性的石墨烯气凝胶的制备方法，其特征在于，步骤(4)中Bi(NO3)3与Na2WO4的摩尔比为2:1,持续搅拌混合15～30min，在反应釜进行水热反应的条件为180～200℃，24h。
7.如权利要求1所述的具有光催化活性的石墨烯气凝胶的制备方法，其特征在于，步骤(5)中的浸泡清洗为2～3天。
8.如权利要求1所述的具有光催化活性的石墨烯气凝胶的制备方法，其特征在于，步骤(5)中的冷冻干燥-30℃冷冻干燥60～72h。
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| CN106512987A (zh) * | 2016-11-24 | 2017-03-22 | 河南师范大学 | 钨酸铋/石墨烯气凝胶复合可见光催化剂及其制备方法 |
| CN108579727A (zh) * | 2018-01-11 | 2018-09-28 | 湘潭大学 | 一种石墨烯量子点-钨酸铋复合光催化剂及其制备方法 |
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| CN106512987A (zh) * | 2016-11-24 | 2017-03-22 | 河南师范大学 | 钨酸铋/石墨烯气凝胶复合可见光催化剂及其制备方法 |
| CN108579727A (zh) * | 2018-01-11 | 2018-09-28 | 湘潭大学 | 一种石墨烯量子点-钨酸铋复合光催化剂及其制备方法 |
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