CN110227489A - 一种纳米级高量子转化率光催化剂及其制备工艺 - Google Patents
一种纳米级高量子转化率光催化剂及其制备工艺 Download PDFInfo
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Abstract
本发明涉及光催化剂的加工技术,具体的说涉及一种纳米级高量子转化率光催化剂及其制备工艺。由按照质量百分比数的如下原料加工而成:10‑15%钛酸四丁酯,0.05‑0.1%硝酸铂或氯铂酸钾,0.05‑0.1%硝酸铁或氢氧化铁,0.05‑0.1%硝酸银或氯化银,余量为无水乙醇,原料的总和为100%。本发明的有益效果是:该光催化剂呈纳米级粒径(≤10nm),比表面积大,通过适量加入贵金属的方式降低电子与空穴复合几率,生成大量羟基自由基(OH),提高量子转化率;通过适量加入金属离子的方式使光激发区范围由紫外光区扩展至可见光区,使适用环境更广、降低能耗。
Description
技术领域
本发明涉及光催化剂的加工技术,具体的说涉及一种纳米级高量子转化率光催化剂及其制备工艺。
背景技术
光催化剂是一种被国际社会公认的无毒无害不产生二次污染的静态环保治理材料,被广泛应用于室内空气净化、工业废气、生活污水、工业污水等环保治理领域,其治理成果获得普遍的认可。但目前,国内尚缺乏对光催化理论的深入研究,及用于实施该项技术的核心高效光催化剂。现有光催化剂的光响应范围窄(<380nm),量子转换效率低(≤30%),可见光利用率低,浪费能耗,是目前困扰国内光催化氧化技术发展的主要问题。
发明内容
本发明的目的之一为解决可见光下光催化剂产生的光生电子(e-)和光生空穴(h+)快速复合及光催化剂基材受限于禁带宽度(Eg≤3.2ev)的问题,提供一种纳米级高量子转化率光催化剂,该光催化剂呈纳米级粒径(≤10nm),比表面积大,通过适量加入贵金属的方式降低电子与空穴复合几率,生成大量羟基自由基(OH),提高量子转化率;通过适量加入金属离子的方式使光激发区范围由紫外光区扩展至可见光区,使适用环境更广、降低能耗。
本发明的目的之二在于提供一种纳米级高量子转化率光催化剂的制备工艺。该工艺设计合理,光催化剂品质可控。
本发明解决其技术问题所采用的技术方案是:
一种纳米级高量子转化率光催化剂,由按照质量百分比数的如下原料加工而成:10-15%钛酸四丁酯,0.05-0.1%硝酸铂或氯铂酸钾,0.05-0.1%硝酸铁或氢氧化铁,0.05-0.1%硝酸银或氯化银,余量为无水乙醇,原料的总和为100%。
作为优选,纳米级高量子转化率光催化剂由按照质量百分比数的如下原料加工而成:12%钛酸四丁酯,0.075%硝酸铂或氯铂酸钾,0.075%硝酸铁或氢氧化铁,0.075%硝酸银或氯化银,余量为无水乙醇。
优选的,硝酸铂或氯铂酸钾、硝酸铁或氢氧化铁和硝酸银或氯化银的纯度为99.99%以上。
优选的,所述光催化剂其粒径≤10nm,比表面积大于等于400m2,光激发范围包括紫外光区(<380nm)和可见光区(400-600nm)。
一种纳米级高量子转化率光催化剂的制备工艺,包括以下步骤:
步骤S1,首先将配方量的钛酸四丁酯与无水乙醇混合,形成A液;
步骤S2,配置0.05M氨水,加热至60-70℃,形成B液;
步骤S3,将步骤S1的A液加热至60-70℃,缓慢加入B液中,恒温维持10-20min,然后离心分离,获得胶状物C;
步骤S4,备置配方量的硝酸铂或氯铂酸钾、硝酸铁或氢氧化铁和硝酸银或氯化银,加入步骤S3获得的胶装物C中,脱水处理;
步骤S5,脱水处理后,离心分离;
步骤S6,在400-550℃烘干处理4-6h;
步骤S7,对步骤S6烘干的块状物料研磨后即得。
优选的,步骤S3中分离采用离心分离,离心机的转速为1000-5000rpm。
优选的,步骤S4中,脱水处理的设备为负压釜,脱水处理的压力为-1000~-2000pa,脱水处理的温度为80-100℃。
优选的,步骤S7中研磨采用纳米粉碎机进行粉碎研磨后按比例与去离子水混合,获得的光催化剂90%的粒径为6-10nm。
本发明的有益效果是:该光催化剂呈纳米级粒径(≤10nm),比表面积大,通过适量加入贵金属的方式降低电子与空穴复合几率,生成大量羟基自由基(OH),提高量子转化率;通过适量加入金属离子的方式使光激发区范围由紫外光区扩展至可见光区,使适用环境更广、降低能耗。
具体实施方式
下面通过具体实施例,对本发明的技术方案作进一步的具体说明。
实施例1:
一种纳米级高量子转化率光催化剂,所述光催化剂其粒径≤10nm,比表面积大于等于400m2,光激发范围包括紫外光区(<380nm)和可见光区(400-600nm),由按照质量百分比数的如下原料加工而成:10%钛酸四丁酯,0.05%硝酸铂,0.05%硝酸铁,0.05%硝酸银,余量为无水乙醇,原料的总和为100%。
本实施例中,硝酸铂、硝酸铁和硝酸银的纯度为99.99%。
实施例1的纳米级高量子转化率光催化剂的制备工艺,包括以下步骤:
步骤S1,首先将配方量的钛酸四丁酯与无水乙醇混合,形成A液;
步骤S2,配置0.05M氨水,加热至65℃,形成B液;
步骤S3,将步骤S1的A液加热至65℃,缓慢加入B液中,恒温维持10min,然后离心分离,获得胶状物C;
步骤S4,备置配方量的硝酸铂、硝酸铁和硝酸银,加入步骤S3获得的胶装物C中,脱水处理;
步骤S5,脱水处理后,离心分离;
步骤S6,在400℃烘干处理6h;
步骤S7,对步骤S6烘干的块状物料研磨后即得。
具体的说,步骤S3中分离采用离心分离,离心机的转速为1000rpm,步骤S4中,脱水处理的设备为负压釜,脱水处理的压力为-1000pa,脱水处理的温度为80℃,步骤S7中研磨采用纳米粉碎机进行粉碎研磨,获得的光催化剂90%的粒径为6-10nm。
实施例2
一种纳米级高量子转化率光催化剂,所述光催化剂其粒径≤10nm,比表面积大于等于400m2,光激发范围包括紫外光区(<380nm)和可见光区(400-600nm),由按照质量百分比数的如下原料加工而成:15%钛酸四丁酯,0.1%氯铂酸钾,0.1%氢氧化铁,0.1%氯化银,余量为无水乙醇,原料的总和为100%。
本实施例中,氯铂酸钾、氢氧化铁和氯化银的纯度为99.99%。
实施例2的纳米级高量子转化率光催化剂的制备工艺,包括以下步骤:
步骤S1,首先将配方量的钛酸正丁酯与无水乙醇混合,形成A液;
步骤S2,配置0.05M氨水,加热至70℃,形成B液;
步骤S3,将步骤S1的A液加热至70℃,缓慢加入B液中,恒温维持15min,然后离心分离,获得胶状物C;
步骤S4,备置配方量的氯铂酸钾、氢氧化铁和氯化银,加入步骤S3获得的胶装物C中,脱水处理;
步骤S5,脱水处理后,离心分离;
步骤S6,在450℃烘干处理5h;
步骤S7,对步骤S6烘干的块状物料研磨后即得。
本实施例中,步骤S3中分离采用离心分离,离心机的转速为5000rpm,步骤S4中,脱水处理的设备为负压釜,脱水处理的压力为-1500pa,脱水处理的温度为90℃,步骤S7中研磨采用纳米粉碎机进行粉碎研磨,获得的光催化剂90%的粒径为6-10nm。
实施例3
一种纳米级高量子转化率光催化剂,所述光催化剂其粒径≤10nm,比表面积大于等于400m2,光激发范围包括紫外光区(<380nm)和可见光区(400-600nm),由按照质量百分比数的如下原料加工而成:12%钛酸四丁酯,0.075%硝酸铂,0.075%硝酸铁,0.075%硝酸银,余量为无水乙醇。
具体的说,硝酸铂、硝酸铁和硝酸银的纯度为99.999%。
实施例3的纳米级高量子转化率光催化剂的制备工艺,包括以下步骤:
步骤S1,首先将配方量的钛酸正丁酯与无水乙醇混合,形成A液;
步骤S2,配置0.05M氨水,加热至60℃,形成B液;
步骤S3,将步骤S1的A液加热至60℃,缓慢加入B液中,恒温维持20min,然后离心分离,获得胶状物C;
步骤S4,配方量的硝酸铂、硝酸铁和硝酸银,加入步骤S3获得的胶装物C中,脱水处理;
步骤S5,脱水处理后,离心分离;
步骤S6,在550℃烘干处理4h;
步骤S7,对步骤S6烘干的块状物料研磨后即得。
本实施例中,步骤S3中分离采用离心分离,离心机的转速为3000rpm,步骤S4中,脱水处理的设备为负压釜,脱水处理的压力为-2000pa,脱水处理的温度为100℃,步骤S7中研磨采用纳米粉碎机进行粉碎研磨,获得的光催化剂90%的粒径为6-10nm。
以上所述的实施例只是本发明的一种较佳的方案,并非对本发明作任何形式上的限制,在不超出权利要求所记载的技术方案的前提下还有其它的变体及改型。
Claims (8)
1.一种纳米级高量子转化率光催化剂,其特征在于,由如下质量百分比的原料加工而成:10-15%钛酸四丁酯,0.05-0.1%硝酸铂或氯铂酸钾,0.05-0.1%硝酸铁或氢氧化铁,0.05-0.1%硝酸银或氯化银,余量为无水乙醇,原料的总和为100%。
2.根据权利要求1所述的纳米级高量子转化率光催化剂,其特征在于,由如下质量百分比的原料加工而成:12%钛酸四丁酯,0.075%硝酸铂,0.075%硝酸铁,0.075%硝酸银,余量为无水乙醇。
3.根据权利要求1所述的纳米级高量子转化率光催化剂,其特征在于,所述硝酸铂、氯铂酸钾、硝酸铁、氢氧化铁、硝酸银和氯化银的纯度纯为99.99%以上。
4.根据权利要求1所述的纳米级高量子转化率光催化剂,其特征在于,所述光催化剂其粒径≤10nm,比表面积大于等于400m2/g,光激发范围包括紫外光区和可见光区。
5.一种权利要求1-4任意一项所述纳米级高量子转化率光催化剂的制备工艺,其特征在于,包括以下步骤:
步骤S1,首先将配方量的钛酸四丁酯与无水乙醇混合,形成A液;
步骤S2,配置0.05M氨水,加热至60-70℃,形成B液;
步骤S3,将步骤S1的A液加热至60-70℃,缓慢加入B液中,恒温维持10-20min,然后离心分离,获得胶状物C;
步骤S4,备置配方量的硝酸铂或氯铂酸钾、硝酸铁或氢氧化铁和硝酸银或氯化银,加入步骤S3获得的胶装物C中,脱水处理;
步骤S5,脱水处理后,离心分离;
步骤S6,在400-550℃烘干处理4-6h;
步骤S7,对步骤S6烘干的块状物料研磨后即得制成品。
6.根据权利要求5所述的纳米级高量子转化率光催化剂的制备工艺,其特征在于,步骤S3中分离采用离心分离,离心机的转速为1000-5000rpm。
7.根据权利要求5所述的纳米级高量子转化率光催化剂的制备工艺,其特征在于,步骤S4中,脱水处理的设备为负压釜,脱水处理的压力为-1000~-2000pa,脱水处理的温度为80-100℃。
8.根据权利要求5所述的纳米级高量子转化率光催化剂的制备工艺,其特征在于,步骤S7中研磨采用纳米粉碎机进行粉碎研磨,获得的光催化剂90%的粒径为6-10nm。
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