CN108404924A - 一种具有可见光响应的复合光催化剂制备方法 - Google Patents
一种具有可见光响应的复合光催化剂制备方法 Download PDFInfo
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Abstract
本发明公开了一种具有可见光响应的复合光催化剂制备方法。该方法包括:步骤1:将钛源、硼源与二元醇混合,得到溶液A;步骤2:将铁盐、镧盐、柠檬酸溶于水,得到溶液B;步骤3:在搅拌条件下将溶液B缓慢滴加至溶液A中,滴加完毕后,再加入三乙醇胺与N‑甲基吡咯烷酮的混合液,搅拌回流,之后在室温下密封陈化,得到复合凝胶;步骤4:复合凝胶干燥后研磨成粉,经过阶段煅烧,得到复合光催化剂。本发明方法制备过程简单,制备条件要求低,原料易得,可进行工业化应用,得到的复合光催化剂对可见光具有良好响应,具有较高的可见光催化水分解效率,吸附率高。
Description
技术领域
本发明属于新材料技术领域,涉及一种无机光催化材料领域,具体涉及一种具有可见光响应的复合光催化剂制备方法。
背景技术
随着石油、天然气等化石能源的枯竭,全球环境污染问题日益严重,新能源开发和环境污染治理成为当前科学研究的热点话题,人们急切需要开发新能源及成本低的绿色环保的环境污染物处理技术,而光催化材料在光解水制氢开发新能源及污水处理领域展现出了广泛的应用前景。
利用半导体及复合半导体光催化降解有机污染物,近年来在环境污染治理中取得较好的研究效果。TiO2作为光催化剂,具有良好的化学稳定性、低成本、无毒、原料易获得,而且能直接利用太阳光中的可见光作为激发光源来进行催化氧化,无二次污染。但TiO2光催化剂量子效率低,且光谱响应范围在紫外光区,太阳光谱中可见光部分不能有效利用,限制了其工业应用。例如专利201410146893.0《一种钙钛矿/多糖复合光催化剂降解甲基橙的方法》公开了采用凝胶-溶胶法制备钙钛矿氧化物,再将钙钛矿与壳聚糖复合,该复合光催化剂制备繁琐,且降解甲基橙是需要在紫外光照射下470-490min,且第一次的降解效率不超过70%。专利201510373800.2《一种含铁活性物的微生物合成法及其在甲基橙降解催化领域的应用》,该催化剂包括含铁活性物73%,柠檬酸20%和二氧化钛7%,其中利用氧化亚铁杆菌与硫酸亚铁反应得到的含铁活性物,该催化剂利用含铁活性物在水中产生活性较高的Fe(OH)2+、Fe2(OH)2 4+,这些物质在有机酸、氧气作用下与二氧化钛协同产生强氧化性的含氧自由基,该催化剂需要生物培养1-3天,对氧化亚铁杆菌活性有一定要求,且现有生物培养的产率要远低于化学合成方法。
鉴于太阳光中仅含约4%的紫外光,而可见光约占45%,因此开发对可见光相应的光催化剂更具有使用价值和应用前景。
发明内容
针对现有光催化剂存在的不足,本发明提供一种具有良好催化性能,且具有可见光响应的复合光催化剂。
为了实现本发明的目的,通过大量试验研究并不懈努力,最终获得如下技术方案:一种具有可见光响应的复合光催化剂制备方法,包括如下步骤:
步骤1:将钛源、硼源与二元醇混合,得到溶液A,其中钛、硼的摩尔比为1:(0.04-0.12),钛源与二元醇的体积比为1:(5-10);
步骤2:将铁盐、镧盐、柠檬酸溶于水,得到溶液B,其中铁、镧、柠檬酸的摩尔比为1:(1.005-1.025):(2-4);
步骤3:在搅拌条件下将溶液B缓慢滴加至溶液A中,其中钛与铁的摩尔比为1:(1.3-3.0),滴加完毕后,再加入三乙醇胺与N-甲基吡咯烷酮的混合液,混合液体积是二元醇体积的10%-25%,其中三乙醇胺与N-甲基吡咯烷酮的体积比为1:(0.5-1.5),最后在60-80℃下搅拌回流,之后在室温下密封陈化,得到复合凝胶;
步骤4:将复合凝胶干燥后研磨成粉,粉体先以3-5℃/min速率升温至180-220℃下保温1-1.5h,再以8-15℃/min速率升温至450-600℃下焙烧2-3h,得到复合光催化剂。
优选地,如上所述具有可见光响应的复合光催化剂制备方法,包括如下步骤:
步骤1:将钛源、硼源与二元醇混合,得到溶液A,其中钛、硼的摩尔比为1:(0.08-0.10),钛源与二元醇的体积比为1:(5-10);
步骤2:将铁盐、镧盐、柠檬酸溶于水,得到溶液B,其中铁、镧、柠檬酸的摩尔比为1:(1.010-1.015):(2.6-3.5);
步骤3:在搅拌条件下将溶液B缓慢滴加至溶液A中,其中钛与铁摩尔比为1:(1.8-2.5),滴加完毕后,再加入三乙醇胺与N-甲基吡咯烷酮的混合液,混合液体积是二元醇体积的15%-20%,其中三乙醇胺与N-甲基吡咯烷酮的体积比为1:(0.8-1.1),最后在60-80℃下搅拌回流3-5h,之后室温下密封陈化12-20h,得到复合凝胶;
步骤4:将复合凝胶干燥后研磨成粉,粉体先以5℃/min速率升温至200℃下保温1.2h,再以12℃/min速率升温至550℃下焙烧2.5h,得到复合光催化剂。
优选地,如上所述具有可见光响应的复合光催化剂制备方法,其中步骤1中所述钛源为四氯化钛、三氯化钛或钛酸四丁酯中任意一种。
优选地,如上所述具有可见光响应的复合光催化剂制备方法,其中步骤1中所述硼源为硼酸或硼酸三正丁酯。
优选地,如上所述具有可见光响应的复合光催化剂制备方法,其中步骤1中所述二元醇为乙二醇。
优选地,如上所述具有可见光响应的复合光催化剂制备方法,其中步骤2中所述铁盐为硝酸铁、氯化铁或硫酸铁中任意一种。
优选地,如上所述具有可见光响应的复合光催化剂制备方法,其中步骤2中所述镧盐为硝酸镧、氯化镧或硫酸镧中任意一种。
优选地,如上所述具有可见光响应的复合光催化剂制备方法,其中步骤4中复合凝胶干燥温度为60-80℃。
本发明相对于现有技术,具有如下技术效果:
本发明方法得到的复合光催化剂对可见光具有良好响应,催化性能高,在可见光照射下,制氢速率达到1325.8umol/h·g,具有较高的可见光催化水分解效率,对浓度在100mg/L以下的甲基橙废水在可见光下进行吸附处理,吸附率达到96.7%以上。总之,本发明方法制备过程简单,制备条件要求低,原料易得,可进行工业化应用。
具体实施方式
下面结合实施例对本发明的技术方案进行清楚、完整地描述,下列实施例仅用于说明本发明,而不应视为限定本发明的保护范围。另外,实施例中未注明具体技术操作步骤或条件者,均按照本领域内的文献所描述的技术或条件或者按照产品说明书进行。所用试剂或仪器未注明生产厂商者,均为可以通过市购获得的常规产品。
实施例1具有可见光响应的复合光催化剂制备:
(1)量取钛酸四丁酯10ml(9.96g、0.0293mol)、硼酸0.09g(0.001456),将其溶于60ml乙二醇中,得到溶液A;
(2)称取硝酸铁9.92g(0.041)、六水硝酸镧17.87g(0.04127)、柠檬酸15.77g(0.082),溶于80ml去离子水中,得到溶液B;
(3)在搅拌条件下将溶液B缓慢滴加至溶液A中,滴加完毕后,再加入6ml三乙醇胺与N-甲基吡咯烷酮的混合液,其中三乙醇胺与N-甲基吡咯烷酮的体积比为1:0.5,将混合液在60℃下搅拌回流5h,之后在室温下密封陈化20h,得到复合凝胶;
(4)将复合凝胶在70℃下干燥,之后研磨成粉,粉体在马弗炉中先以3℃/min速率升温至180℃下保温1.5h,再以8℃/min速率升温至600℃下焙烧3h,得到复合光催化剂。
实施例2具有可见光响应的复合光催化剂制备:
(1)量取钛酸四丁酯10ml、硼酸0.21g,将其溶于100ml乙二醇中,得到溶液A;
(2)称取硝酸铁21.25g、六水硝酸镧38.82g、柠檬酸67.55g,溶于200ml去离子水中,得到溶液B;
(3)在搅拌条件下将溶液B缓慢滴加至溶液A中,滴加完毕后,再加入25ml三乙醇胺与N-甲基吡咯烷酮的混合液,其中三乙醇胺与N-甲基吡咯烷酮的体积比为1:1.5,将混合液在80℃下搅拌回流3h,之后在室温下密封陈化13h,得到复合凝胶;
(4)将复合凝胶在70℃下干燥,之后研磨成粉,粉体在马弗炉中先以5℃/min速率升温至220℃下保温1.2h,再以15℃/min速率升温至600℃下焙烧2h,得到复合光催化剂。
实施例3具有可见光响应的复合光催化剂制备:氯化铁、四氯化钛
(1)量取四氯化钛10ml、硼酸0.45g,将其溶于80ml乙二醇中,得到溶液A;
(2)称取氯化铁26.57g、六水硝酸镧71.63g、柠檬酸81.83g,溶于200ml去离子水中,得到溶液B;
(3)在搅拌条件下将溶液B缓慢滴加至溶液A中,滴加完毕后,再加入12ml三乙醇胺与N-甲基吡咯烷酮的混合液,其中三乙醇胺与N-甲基吡咯烷酮的体积比为1:0.8,将混合液在80℃下搅拌回流3h,之后在室温下密封陈化13h,得到复合凝胶;
(4)将复合凝胶在70℃下干燥,之后研磨成粉,粉体在马弗炉中先以5℃/min速率升温至200℃下保温1.2h,再以12℃/min速率升温至550℃下焙烧2.5h,得到复合光催化剂。
实施例4具有可见光响应的复合光催化剂制备:
(1)量取四氯化钛10ml、硼酸0.56g,将其溶于100ml乙二醇中,得到溶液A;
(2)称取氯化铁36.9g、六水硝酸镧99.98g、柠檬酸152.99g,溶于250ml去离子水中,得到溶液B;
(3)在搅拌条件下将溶液B缓慢滴加至溶液A中,滴加完毕后,再加入20ml三乙醇胺与N-甲基吡咯烷酮的混合液,其中三乙醇胺与N-甲基吡咯烷酮的体积比为1:1,将混合液在80℃下搅拌回流3h,之后在室温下密封陈化13h,得到复合凝胶;
(4)将复合凝胶在80℃下干燥,之后研磨成粉,粉体在马弗炉中先以5℃/min速率升温至200℃下保温1.5h,再以15℃/min速率升温至600℃下焙烧2h,得到复合光催化剂。
实施例5
对实施例1-4制备得到的复合光催化剂进行光催化水分解制氢试验,具体过程如下:
使用密闭循环光催化系统进行测量,复合光催化剂的加入量为1g/L,超声分散至形成均匀的悬浊液,整个体系的总体积(含反应器)为700ml,进行实验前先抽真空30min,体系的相对真空度保持在-0.1MPa。催化系统的光源选用300W疝灯,配合可见光反射片,光源在使用前先开机预热,保证光波稳定,实验温度为室温,实时采集反应一段时间的气体样品,然后经过体积为3.14ml的取样管定容后,导入气相色谱中测定产氢含量,从而计算产氢速率。
试验结果得到实施例1-4制备得到的复合光催化剂的制氢速率分别为1359.2umol·h-1·g、1325.8umol·h-1·g、1521.7umol·h-1·g和1487.3umol·h-1·g。
实施例6甲基橙吸附效果检测
取实施例1-4制备得到的复合光催化剂各0.5g,放入100ml锥形瓶,加入100ml50mg/L的甲基橙溶液,放在磁力搅拌器上,常温缓慢搅拌1h(模拟污水处理厂中流水速度),吸附完成后将溶液过滤,随后将滤液用紫外可见分光光度计在波长463nm处测其吸光度,按照吸光度-浓度工作曲线换算成吸附平衡时的甲基橙溶液浓度,进而计算出甲基橙的吸附率R%。
R%={(Co-Ct)/Co}×100,其中Co—甲基橙的初始浓度(mg/L),Ct—1h后甲基橙浓度(mg/L)。
表1 不同复合光催化剂吸附甲基橙
实施例7
称取实施例3得到的复合光催化剂,将其加入甲基橙溶液中,其它步骤与实施例6的相同,改变甲基橙溶液浓度为25mg/L、50mg/L、75mg/L、100mg/L,考察其吸附率,得到如表2所示结果。
表3 不同浓度甲基橙溶液吸附率率
从表2数据可知,本发明得到的复合光催化剂对浓度低于100mg/L的甲基橙废水处理效果均显著,去除率可以达到96.7%以上。
实施例8
(1)量取钛酸四丁酯10ml、硼酸0.036g,将其溶于50ml乙二醇中,得到溶液A;
(2)称取硝酸铁7.08g、六水硝酸镧12.68g、柠檬酸60g,溶于100ml去离子水中,得到溶液B;
(3)在搅拌条件下将溶液B缓慢滴加至溶液A中,滴加完毕后,加入再加入6ml三乙醇胺与N-甲基吡咯烷酮的混合液,其中三乙醇胺与N-甲基吡咯烷酮的体积比为1:0.5,在80℃下搅拌回流3h,之后在室温下密封陈化13h,得到复合凝胶;
(4)将复合凝胶在70℃下干燥,之后研磨成粉,粉体在马弗炉中先以5℃/min速率升温至220℃下保温1.2h,再以15℃/min速率升温至600℃下焙烧2h,得到复合光催化剂。
对其按照实施例5和6的方法进行检测,结果发现制氢速率为927.6umol·h-1·g,50mg/L的甲基橙溶液中对甲基橙吸附率为78.4%。
实施例9
(1)量取钛酸四丁酯10ml、硼酸0.35g,将其溶于60ml乙二醇中,得到溶液A;
(2)称取硝酸铁25.0g、六水硝酸镧46.1g、柠檬酸70g,溶于150ml去离子水中,得到溶液B;
(3)在搅拌条件下将溶液B缓慢滴加至溶液A中,滴加完毕后,加入加入再加入6ml三乙醇胺与N-甲基吡咯烷酮的混合液,其中三乙醇胺与N-甲基吡咯烷酮的体积比为1:0.5,在80℃下搅拌回流3h,之后在室温下密封陈化13h,得到复合凝胶;
(4)将复合凝胶在70℃下干燥,之后研磨成粉,粉体在马弗炉中先以5℃/min速率升温至220℃下保温1.2h,再以15℃/min速率升温至600℃下焙烧2h,得到复合光催化剂。
对其按照实施例5和6的方法进行检测,结果发现制氢速率为728.4umol·h-1·g,50mg/L的甲基橙溶液中对甲基橙吸附率为69.7%。
实施例10
(1)量取钛酸四丁酯10ml、硼酸0.09g,将其溶于60ml乙二醇中,得到溶液A;
(2)称取硝酸铁9.92g、六水硝酸镧17.87g、柠檬酸15.77g,溶于80ml去离子水中,得到溶液B;
(3)在搅拌条件下将溶液B缓慢滴加至溶液A中,滴加完毕后,再加入20ml三乙醇胺与N-甲基吡咯烷酮的混合液,三乙醇胺与N-甲基吡咯烷酮的体积比为1:0.5,将混合液在60℃下搅拌回流5h,之后在室温下密封陈化20h,得到复合凝胶;
(4)将复合凝胶在70℃下干燥,之后研磨成粉,粉体在马弗炉中先以3℃/min速率升温至180℃下保温1.5h,再以8℃/min速率升温至600℃下焙烧3h,得到复合光催化剂。
对其按照实施例5和6的方法进行检测,结果发现制氢速率为1157.3umol·h-1·g,50mg/L的甲基橙溶液中对甲基橙吸附率为83.7%。
实施例11
(1)量取钛酸四丁酯10ml、硼酸0.09g,将其溶于60ml乙二醇中,得到溶液A;
(2)称取硝酸铁9.92g、六水硝酸镧17.87g、柠檬酸15.77g,溶于80ml去离子水中,得到溶液B;
(3)在搅拌条件下将溶液B缓慢滴加至溶液A中,滴加完毕后,再加入6ml三乙醇胺,将混合液在60℃下搅拌回流5h,之后在室温下密封陈化20h,得到复合凝胶;
(4)将复合凝胶在70℃下干燥,之后研磨成粉,粉体在马弗炉中先以3℃/min速率升温至180℃下保温1.5h,再以8℃/min速率升温至600℃下焙烧3h,得到复合光催化剂。
对其按照实施例5和6的方法进行检测,结果发现制氢速率为1157.3umol·h-1·g,50mg/L的甲基橙溶液中对甲基橙吸附率为87.8%。
实施例12
(1)量取钛酸四丁酯10ml、硼酸0.09g,将其溶于60ml乙二醇中,得到溶液A;
(2)称取硝酸铁9.92g、六水硝酸镧17.87g、柠檬酸15.77g,溶于80ml去离子水中,得到溶液B;
(3)在搅拌条件下将溶液B缓慢滴加至溶液A中,滴加完毕后,再加入6mlN-甲基吡咯烷酮,将混合液在60℃下搅拌回流5h,之后在室温下密封陈化20h,得到复合凝胶;
(4)将复合凝胶在70℃下干燥,之后研磨成粉,粉体在马弗炉中先以3℃/min速率升温至180℃下保温1.5h,再以8℃/min速率升温至600℃下焙烧3h,得到复合光催化剂。
对其按照实施例5和6的方法进行检测,结果发现制氢速率为875umol·h-1·g,50mg/L的甲基橙溶液中对甲基橙吸附率为73.5%。
Claims (9)
1.一种具有可见光响应的复合光催化剂制备方法,其特征在于包括如下步骤:
步骤1:将钛源、硼源与二元醇混合,得到溶液A,其中钛、硼的摩尔比为1:(0.04-0.12),钛源与二元醇的体积比为1:(5-10);
步骤2:将铁盐、镧盐、柠檬酸溶于水,得到溶液B,其中铁、镧、柠檬酸的摩尔比为1:(1.005-1.025):(2-4);
步骤3:在搅拌条件下将溶液B缓慢滴加至溶液A中,其中钛与铁的摩尔比为1:(1.3-3.0),滴加完毕后,再加入三乙醇胺与N-甲基吡咯烷酮的混合液,混合液体积是二元醇体积的10%-25%,其中三乙醇胺与N-甲基吡咯烷酮的体积比为1:(0.5-1.5),最后在60-80℃下搅拌回流,之后在室温下密封陈化,得到复合凝胶;
步骤4:将复合凝胶干燥后研磨成粉,粉体先以3-5℃/min速率升温至180-220℃下保温1-1.5h,再以8-15℃/min速率升温至450-600℃下焙烧2-3h,得到复合光催化剂。
2.根据权利要求1所述具有可见光响应的复合光催化剂制备方法,其特征在于包括如下步骤:
步骤1:将钛源、硼源与二元醇混合,得到溶液A,其中钛、硼的摩尔比为1:(0.08-0.10),钛源与二元醇的体积比为1:(5-10);
步骤2:将铁盐、镧盐、柠檬酸溶于水,得到溶液B,其中铁、镧、柠檬酸的摩尔比为1:(1.010-1.015):(2.6-3.5);
步骤3:在搅拌条件下将溶液B缓慢滴加至溶液A中,其中钛与铁摩尔比为1:(1.8-2.5),滴加完毕后,再加入三乙醇胺与N-甲基吡咯烷酮的混合液,混合液体积是二元醇体积的15%-20%,其中三乙醇胺与N-甲基吡咯烷酮的体积比为1:(0.8-1.1),最后在60-80℃下搅拌回流3-5h,之后室温下密封陈化12-20h,得到复合凝胶;
步骤4:将复合凝胶干燥后研磨成粉,粉体先以5℃/min速率升温至200℃下保温1.2h,再以12℃/min速率升温至550℃下焙烧2.5h,得到复合光催化剂。
3.根据权利要求1或2所述具有可见光响应的复合光催化剂制备方法,其特征在于,步骤1中所述钛源为四氯化钛、三氯化钛或钛酸四丁酯中任意一种。
4.根据权利要求1或2所述具有可见光响应的复合光催化剂制备方法,其特征在于,步骤1中所述硼源为硼酸。
5.根据权利要求1或2所述具有可见光响应的复合光催化剂制备方法,其特征在于,步骤1中所述二元醇为乙二醇。
6.根据权利要求1或2所述具有可见光响应的复合光催化剂制备方法,其特征在于,步骤2中所述铁盐为硝酸铁、氯化铁或硫酸铁中任意一种。
7.根据权利要求1或2所述具有可见光响应的复合光催化剂制备方法,其特征在于,步骤2中所述镧盐为硝酸镧、氯化镧或硫酸镧中任意一种。
8.根据权利要求1或2所述具有可见光响应的复合光催化剂制备方法,其特征在于,步骤4中复合凝胶干燥温度为60-80℃。
9.根据权利要求1或2所述具有可见光响应的复合光催化剂制备方法,其特征在于:步骤2中水为蒸馏水或去离子水。
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