CN107213911A - CQDs/TNS和SiQDs/TNS复合光催化剂的制备方法 - Google Patents
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Abstract
本发明涉及一种具有可见光活性的CQDs/TNS和SiQDs/TNS复合光催化剂的制备方法。本发明步骤为(1)采用明胶为碳源,3‑氨基,丙基‑三甲氧基硅烷为硅源,水热法处理分别得到碳量子点(CQDs)和硅量子点(SiQDs)溶液;(2)将初始得到的CQDs溶液经过聚乙二醇回流修饰得到分散均匀的碳量子点;(3)采用钛酸四丁酯为钛源,在HF水溶液中经水热处理得到TNS;(4)将CQDs和SiQDs分别与TNS以不同质量比在乙醇溶液中混合,用HCl调pH为3‑4,回流处理5h,然后洗涤,烘干,得到CQDs/TNS和SiQDs/TNS复合光催化剂。本发明得到的复合可见光催化剂对罗丹明B具有较强的可见光催化降解活性,而且可以多次循环利用。该催化剂制备工艺简单易调控,原料易得,生产成本低。
Description
技术领域
本发明涉及一种具有可见光活性的IV族量子点(C、Si)与TiO2纳米片(TNS)复合光催化剂的制备方法。属于光催化技术领域。
背景技术
与传统的II-IV族和III-V量子点相比,IV族的碳量子点(CQDs)、硅量子点(SiQDs)等,有良好的光稳定性,低毒性、独特的上转换荧光性能和光诱导电子转移性能,且碳、硅量子点的制备原料来源广泛,制备方法多种多样,在生物标记、光催化等领域都受到广泛关注。
在光催化方面,量子点与许多其它材料的复合光催化剂被广泛研究。由于CQDs的上转换性能和在可见光范围的强吸收,使CQDs/TNS复合光催化剂在可见光下实现对多种染料的快速降解。硅是一种窄带半导体,在可见光范围有明显吸收,而SiQDs/TNS复合光催化剂也具有很好的光催化性能,由于TNS表面暴露有更多高反应活性的{001}晶面,因此它要比一般TiO2具有更高的光催化活性。
实际应用中,催化剂的分离回收和可循环利用性能是制约其实用化的瓶颈问题。本专利以廉价易得的碳源和硅源采用水热法制备碳量子点和硅量子点,通过与TNS醇溶液回流使CQDs与SiQDs稳定的复合到TNS表面,得到高分散型的CQDs/TNS和SiQDs/TNS复合催化剂。在以罗丹明B作为探针分子的光催化评价反应中,复合光催化剂显示出了高效的可见光催化降解活性。
发明内容
本发明解决以上问题,采用的方案是:复合催化剂的制备方法,其特征在于包括以下步骤:
(1)将碳源或硅源,经过180-240℃,3-26h,水热反应得到初始CQDs溶液或SiQDs溶液;
(2)将初始得到的CQDs溶液经过聚乙二醇回流修饰得到分散均匀的CQDs;
(3)将钛源在HF水溶液中160-200℃,水热反应18-24h得到TNS;
(4)将CQDs或SiQDs与TNS以不同质量比(2.5%-12.5%)在乙醇溶液中混合,用HCl调pH为3-4,回流处理5h,然后洗涤,烘干,得到CQDs/TNS或SiQDs/TNS复合光催化剂。
按上述方案,步骤(1)所述的碳源为明胶、柠檬酸或抗坏血酸,硅源为3-氨基,丙基-三甲氧基硅烷、3-丙烯酰胺丙基三甲氧基硅烷或其它硅烷偶联剂。
按上述方案,步骤(2)所述的聚乙二醇修饰CQDs时的质量比(PEG/CQDs)为1/5~1/3。
按上述方案,步骤(4)所述的钛源为钛酸四丁酯、钛酸异丙酯或其它钛酯。
所制备的CQDs/TNS或SiQDs/TNS复合可见光催化剂的光催化活性,是通过可见光下降解罗丹明B进行评价的。制得的光催化剂100mg加入到100mL10ppm的罗丹明B溶液中,磁力搅拌下,用氙灯模拟可见光光源,加滤光片滤掉紫外光,可见光照射,间隔固定时间取样,在罗丹明B分子的最大吸收波长处(λ=554nm)测得罗丹明B在光照过程中吸光度的变化,换算成浓度,绘制出相对浓度随时间变化的曲线C/C0~t和反应速率曲线ln(C0/C)~t。
本发明的优点:以明胶为原料合成的碳量子点或者以硅烷为原料合成的硅量子点,通过在乙醇溶液中的回流,得到量子点与TNS复合的复合光催化剂,在可见光下能够有效的降解罗丹明B染料。由于量子点与TNS之间形成稳定的C-O-Ti或Si-O-Ti化学键,使得复合光催化剂比较稳定,并且经多次循环测试评价,降解效果仍然很好。本方法制备工艺简单,生产成本较低。
附图说明
图1为CQDs/TNS-7.5%和SiQDs/TNS复合光催化剂的XRD谱图
图2为SiQDs/TNS-7.5%和SiQDs/TNS复合光催化剂在可见光条件下对罗丹明B光催化降解的曲线图
具体实施方案
下面结合实施例对本发明做进一步详细说明,但本发明的保护范围并不局限于这些实施例。
实施例1
CQDs/TNS质量比为2.5%
(1)采用明胶为碳源,水热处理得到碳量子点溶液;
(2)将初始得到的CQDs溶液经过聚乙二醇回流修饰得到分散均匀的碳量子点;
(3)采用钛酸四丁酯为钛源,水热处理得到TNS;
(4)将CQDs与TNS以质量比为2.5%比例在乙醇溶液中混合,用HCl调pH为3-4,回流处理5h,然后洗涤,烘干,得到CQDs/TNS复合光催化剂。
实施例2
CQDs/TNS质量为7.5%
(1)采用明胶为碳源,水热处理得到碳量子点溶液;
(2)将初始得到的CQDs溶液经过聚乙二醇回流修饰得到分散均匀的碳量子点;
(3)采用钛酸四丁酯为钛源,水热处理得到TNS;
(4)将CQDs与TNS以质量比为7.5%比例在乙醇溶液中混合,用HCl调pH为3-4,回流处理5h,然后洗涤,烘干,得到CQDs/TNS复合光催化剂。其XRD图谱与和光催化活性曲线见说明书附图的图1和图2。
实施例3
CQDs/TNS质量比为12.5%
(1)采用明胶为碳源,水热处理得到碳量子点溶液;
(2)将初始得到的CQDs溶液经过聚乙二醇回流修饰得到分散均匀的碳量子点;
(3)采用钛酸四丁酯为钛源,水热处理得到TNS;
(4)将CQDs与TNS以质量比为12.5%比例在乙醇溶液中混合,用HCl调pH为3-4,回流处理5h,然后洗涤,烘干,得到CQDs/TNS复合光催化剂。
实施例4
SiQDs/TNS质量比为5%
(1)采用硅烷为硅源,水热处理得到硅量子点溶液;
(2)采用钛酸四丁酯为钛源,水热处理得到TNS;
(4)将SiQDs与TNS以质量比为5%比例在乙醇溶液中混合,用HCl调pH为3-4,回流处理5h,然后洗涤,烘干,得到SiQDs/TNS复合光催化剂。
实施例5
SiQDs/TNS质量比为7.5%
(1)采用硅烷为硅源,水热处理得到硅量子点溶液;
(2)采用钛酸四丁酯为钛源,水热处理得到TNS;
(4)将SiQDs与TNS以质量比为7.5%比例在乙醇溶液中混合,用HCl调pH为3-4,回流处理5h,然后洗涤,烘干,得到SiQDs/TNS复合光催化剂。其XRD图谱与光催化活性曲线见说明书附图的图1和图2。
实施例6
SiQDs/TNS质量比为10%
(1)采用硅烷为硅源,水热处理得到硅量子点溶液;
(2)采用钛酸四丁酯为钛源,水热处理得到TNS;
(4)将SiQDs与TNS以质量比为10%比例在乙醇溶液中混合,用HCl调pH为3-4,回流处理5h,然后洗涤,烘干,得到SiQDs/TNS复合光催化剂。
Claims (4)
1.CQDs/TNS和SiQDs/TNS复合光催化剂的制备,其特征在于以二氧化钛纳米片(TNS)为载体,以CQDs或SiQDs为光活性组分。包括以下步骤:
(1)将碳源或硅源,经过180-240℃,3-26h,水热反应得到初始CQDs或SiQDs溶液;
(2)将初始得到的CQDs溶液经过聚乙二醇回流修饰得到分散均匀的CQDs;
(3)将钛源在HF水溶液中保持160-200℃,水热反应18-24h得到TNS;
(4)将CQDs或SiQDs与TNS以不同质量比(2.5%-12.5%)在乙醇溶液中混合,用HCl调pH为3-4,回流处理若干小时,然后洗涤,烘干,得到CQDs/TNS或SiQDs/TNS复合光催化剂。
2.根据权利1所述的复合光催化剂的制备方法,其特征在于:碳源为明胶、柠檬酸或抗坏血酸;硅源为3-氨基,丙基-三甲氧基硅烷、3-丙烯酰胺丙基三甲氧基硅烷或其它硅烷偶联剂。
3.根据权利1所述的复合光催化剂的制备方法,其特征在于:聚乙二醇修饰CQDs时的质量比(PEG:CQDs)为1/5~1/3。
4.根据权利1所述的CQDs/TNS复合光催化剂的制备方法,其特征在于:采用的钛源为钛酸四丁酯、钛酸异丙酯或其它钛酯。
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