CN108525696A - 一种宽光谱吸收富氧缺碘异质光催化材料TaON/BiO1.2I0.6的制备方法 - Google Patents
一种宽光谱吸收富氧缺碘异质光催化材料TaON/BiO1.2I0.6的制备方法 Download PDFInfo
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- 229910003071 TaON Inorganic materials 0.000 title claims abstract description 77
- 239000000463 material Substances 0.000 title claims abstract description 24
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 17
- 239000001301 oxygen Substances 0.000 title claims abstract description 17
- 238000001228 spectrum Methods 0.000 title claims abstract description 17
- 238000007210 heterogeneous catalysis Methods 0.000 title claims abstract description 12
- 206010067997 Iodine deficiency Diseases 0.000 title claims description 7
- 235000006479 iodine deficiency Nutrition 0.000 title claims description 7
- 238000000034 method Methods 0.000 title claims description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000012855 volatile organic compound Substances 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052740 iodine Inorganic materials 0.000 claims abstract description 10
- 239000011630 iodine Substances 0.000 claims abstract description 10
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 239000002131 composite material Substances 0.000 claims abstract description 5
- 239000011941 photocatalyst Substances 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 4
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000013019 agitation Methods 0.000 claims abstract description 3
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims abstract description 3
- 206010013786 Dry skin Diseases 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 7
- 238000010521 absorption reaction Methods 0.000 claims description 3
- 229910000069 nitrogen hydride Inorganic materials 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- 238000006555 catalytic reaction Methods 0.000 claims description 2
- 238000005121 nitriding Methods 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- YXFVVABEGXRONW-UHFFFAOYSA-N toluene Substances CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 abstract description 29
- 230000001699 photocatalysis Effects 0.000 abstract description 9
- 238000007146 photocatalysis Methods 0.000 abstract description 7
- 238000000354 decomposition reaction Methods 0.000 abstract description 5
- 238000012986 modification Methods 0.000 abstract description 3
- 238000002336 sorption--desorption measurement Methods 0.000 description 8
- 239000011148 porous material Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000000985 reflectance spectrum Methods 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- URVGHPZOLQFKJZ-UHFFFAOYSA-N [Bi]=O.[I] Chemical compound [Bi]=O.[I] URVGHPZOLQFKJZ-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000013335 mesoporous material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007592 spray painting technique Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公布了一种宽光谱吸收富氧缺碘异质光催化材料TaON/BiO1.2I0.6的制备方法,首先以Ta2O5为原料制备TaON,然后将TaON加入含有硝酸铋的乙二醇溶液中,磁力搅拌0.5‑1h,滴入含碘化钾的乙二醇溶液,反应后转入高压反应釜,反应后获得TaON/BiOI复合光催化材料;转入管式炉中,以5‑10℃/min的升温速率加热至350‑450℃,焙烧3‑6h,获得宽光谱吸收富氧缺碘异质光催化材料TaON/BiO1.2I0.6。将TaON/BiO1.2I0.6应用于VOCs净化中,经过TaON修饰的BiO1.2I0.6光催化分解典型VOCs甲苯的效率比BiO1.2I0.6提高了约1.4倍。
Description
技术领域
本发明涉及有机污染物降解催化材料技术领域,尤其是一种富氧缺碘异质光催化材料TaON/BiO1.2I0.6的制备及其在VOCs净化中的应用。
背景技术
VOCs是挥发性有机化合物(volatile organic compounds)的 英文缩写,它通常是指沸点在250℃以内、室温下饱和蒸汽压超过 133Kpa的一类有机化合物。VOCs种类较多,包括的物质超过100多 种,主要来源于石油化工、燃料燃烧、交通运输、涂料、喷漆、印 刷等行业。近年来,随着我国社会经济的高速发展,排放到大气中 的VOCs种类和浓度也在逐年增加。进入空气中的VOCs,即使在浓 度很低的情况下,其危害程度也非常之大,它被喻为人类健康的 “隐形杀手”。因此,VOCs治理将接力脱硫、脱硝、除尘。
采用半导体光催化技术净化VOCs,具有可以利用太阳能、能够在大范围内实施,反应条件温和、在常温常压下即可进行,所需设备简单,能深度破坏VOCs结构等优点,引起了研究人员广泛的关注。然而,缺少宽光谱吸收高效光催化材料是该技术治理VOCs所面临的关键技术问题。
近年来,一种宽光谱吸收的催化剂铋氧碘(BiOI),在降解有机污染物方面显示出了较高的催化活性。BiOI带隙约为1.8eV,吸收可以覆盖从紫外线到可见光的很宽的光谱范围,光生电子与空穴数较多。 BiOI晶体是由双I-离子层和[Bi2O2]2+层交替排列成的 -I-Bi-O-O-Bi-I-层状结构。这种层状结构可以使双I-离子层和 [Bi2O2]2+层之间产生内建电场,促进光生电子-空穴分离和转移,从而使得BiOI展现出较高的光催化活性。为了进一步提高BiOI的光催化活性,研究人员近来又开发出了氧富余、碘缺少的BixOyIz,如Bi7O9I3、Bi4O5I2、Bi5O7I。BiOI的价带主要由O2p和I5p轨道组成,与O2p轨道相比,I5p轨道更接近价带边,其价带边电位较高约为2.3V,具有很强的氧化能力。而氧富余、碘缺少的BixOyIz价带中O2p轨道的贡献增加,I5p轨道的贡献下降,这意味着BixOyIz价带边的位置将下移,其氧化能力得到进一步增强。此外,O2-离子半径小于I-离子半径,氧取代了少量碘,将减小O2-离子层和[Bi2O2]2+离子层间距,增强内建电场,抑制光生电子-空穴复合,这进一步增强了它的光催化活性。但是BixOyIz载流子的分离效率仍然较低,且还存在一个严重的缺点是其导带边电位较高约为0.5V,因此其还原能力较弱。
发明内容
为解决现有技术中BixOyIz载流子的分离效率低及还原能力较弱的缺陷,本发明提供一种宽光谱吸收富氧缺碘异质光催化材料 TaON/BiO1.2I0.6的制备方法。
一种宽光谱吸收富氧缺碘异质光催化材料TaON/BiO1.2I0.6的制备方法,包括以下步骤:
1)、以Ta2O5为原料,以50-100mL/min流量通入NH3,并以5-10℃/min的升温速率加热至700-900℃,氮化6-10h,保持同样流量持续通入NH3,冷却至室温,获得土黄色TaON;
2)、将TaON加入含有硝酸铋的乙二醇溶液中,磁力搅拌0.5-1h,
然后向上述溶液中滴入含碘化钾的乙二醇溶液,继续搅拌反应 0.5-1h后,将反应液转入高压反应釜,140-180℃反应8-12h,自然冷却至室温,过滤、洗涤、80℃干燥后获得TaON/BiOI复合光催化材料;
3)、以TaON/BiOI复合光催化材料为前驱体,并将其置于管式炉中,以5-10℃/min的升温速率加热至350-450℃,焙烧3-6h,自然冷却至室温称重,获得宽光谱吸收富氧缺碘异质光催化材料 TaON/BiO1.2I0.6。
进一步的,所述步骤1)的氮化温度是850℃,氮化时间是10h,氨气流量80mL/min。
进一步的,所述步骤2)中高压反应釜内的反应温度160℃,反应时间12h。
进一步的,所述步骤3)中焙烧温度400℃,焙烧时间5h,升温速率5℃/min。
有益效果:
TaON的导带边电位约为-0.3V,还原能力较强,利用TaON修饰 BixOyIz,不仅将体系的还原能力显著增强,而且TaON的价带边电位 (约2.1V)又比BixOyIz小,可以和BixOyIz构成异质结体系。将本发明所得的TaON/BiO1.2I0.6应用于VOCs净化中,经过TaON修饰的BiO1.2I0.6光催化分解典型VOCs甲苯的效率比BiO1.2I0.6提高了约1.4倍。
附图说明
附图用来提供对本发明的进一步理解,并且构成说明书的一部分,与本发明的实施例一起用于解释本发明,并不构成对本发明的限制。在附图中:
图1为TaON、TaON/BiO1.2I0.6、BiO1.2I0.6的X射线衍射图;
图2是TaON、TaON/BiO1.2I0.6、BiO1.2I0.6紫外-可见漫反射光谱;
图3为TaON的N2吸附-脱附等温线及孔径分布曲线;
图4为5wt%TaON/BiO1.2I0.6的N2吸附-脱附等温线及孔径分布曲线;
图5为为BiO1.2I0.6的N2吸附-脱附等温线及孔径分布曲线;
图6是TaON、TaON/BiO1.2I0.6和BiO1.2I0.6光催化分解甲苯的结果;
图7为5wt%TaON/BiO1.2I0.6循环3次运行降解甲苯的结果。
具体实施方式
以下结合附图对本发明的优选实施例进行说明,应当理解,此处所描述的优选实施例仅用于说明和解释本发明,并不用于限定本发明。
实施例1
以Ta2O5为原料,以80mL/min流量通入NH3,并以5-10℃/min的升温速率加热至850℃,氮化10h,保持同样流量持续通入NH3,冷却至室温,获得土黄色TaON;
称取0.05gTaON,将其加入40mL含1.51gBi(NO3)3·5H2O乙二醇溶液中,磁搅拌0.5h后,向其中滴入40mL含0.52gKI的乙二醇溶液,继续磁搅拌反应0.5h。接着,将其转入100mL高压反应釜并置于烘箱中,160℃反应12h。自然冷却至室温,样品经过滤、洗涤、80℃干燥后放入坩埚,并将其置于管式炉中,以5℃/min的升温速率加热至400℃,焙烧5h,自然冷却至室温,获得5wt%TaON/BiO1.2I0.6。
比较例1
称取0.01gTaON,将其加入40mL含1.58gBi(NO3)3·5H2O乙二醇溶液中,磁搅拌0.5h后,向其中滴入40mL含0.54gKI的乙二醇溶液,继续磁搅拌反应0.5h。接着,将其转入100mL高压反应釜并置于烘箱中,160℃反应12h。自然冷却至室温,样品经过滤、洗涤、80℃干燥后放入坩埚,并将其置于管式炉中,以5℃/min的升温速率加热至400℃,焙烧5h,自然冷却至室温,获得1wt%TaON/BiO1.2I0.6。
比较例2
称取0.03gTaON,将其加入40mL含1.54gBi(NO3)3·5H2O乙二醇溶液中,磁搅拌0.5h后,向其中滴入40mL含0.53gKI的乙二醇溶液,继续磁搅拌反应0.5h。接着,将其转入100mL高压反应釜并置于烘箱中,160℃反应12h。自然冷却至室温,样品经过滤、洗涤、80℃干燥后放入坩埚,并将其置于管式炉中,以5℃/min的升温速率加热至400℃,焙烧5h,自然冷却至室温,获得3wt%TaON/BiO1.2I0.6。
比较例3
称取0.07gTaON,将其加入40mL含1.48gBi(NO3)3·5H2O乙二醇溶液中,磁搅拌0.5h后,向其中滴入40mL含0.51gKI的乙二醇溶液,继续磁搅拌反应0.5h。接着,将其转入100mL高压反应釜并置于烘箱中,160℃反应12h。自然冷却至室温,样品经过滤、洗涤、80℃干燥后放入坩埚,并将其置于管式炉中,以5℃/min的升温速率加热至400℃,焙烧5h,自然冷却至室温,获得7wt%TaON/BiO1.2I0.6。
比较例4
称取0.09gTaON,将其加入40mL含1.45gBi(NO3)3·5H2O乙二醇溶液中,磁搅拌0.5h后,向其中滴入40mL含0.50gKI的乙二醇溶液,继续磁搅拌反应0.5h。接着,将其转入100mL高压反应釜并置于烘箱中,160℃反应12h。自然冷却至室温,样品经过滤、洗涤、80℃干燥后放入坩埚,并将其置于管式炉中,以5℃/min的升温速率加热至400℃,焙烧5h,自然冷却至室温,获得9wt%TaON/BiO1.2I0.6。
比较例5
称取1gTa2O5放入坩埚,并将其置于管式炉中,以80mL/min流量通入NH3,并以10℃/min的升温速率加热至850℃,并将温度保持在 850℃氮化10h,保持流量不变通入NH3,冷却至室温,获得土黄色TaON。
比较例6
称取1.55gBi(NO3)3·5H2O,将其加入40mL乙二醇溶液中,磁搅拌 0.5h后,向其中滴入40mL含0.55gKI的乙二醇溶液,继续磁搅拌反应0.5h。接着,将其转入100mL高压反应釜并置于烘箱中,160℃反应12h。自然冷却至室温,样品经过滤、洗涤、80℃干燥后放入坩埚,并将其置于管式炉中,以5℃/min的升温速率加热至400℃,焙烧5h,自然冷却至室温,获得黄色BiO1.2I0.6。
图1为TaON、TaON/BiO1.2I0.6、BiO1.2I0.6的X射线衍射图,从图1 可见BiO1.2I0.6分别在2θ为28.1°、28.8°、31.1°、33.0°、35.5°、46.0°、47.8°处出现显著的衍射峰。TaON的衍射峰与其单斜相 (PDF#70-1193)一致。对于TaON/BiO1.2I0.6,在2θ为28.8°处出现了TaON的特征衍射峰,表明TaON/BiO1.2I0.6异质材料中含有TaON。
从图2为TaON、TaON/BiO1.2I0.6、BiO1.2I0.6的紫外-可见漫反射光谱。由图2可知TaON是光吸收范围很宽的催化剂,其最大吸收波长为600nm,BiO1.2I0.6也是一种光吸收范围良好的材料,能够吸收波长小于525nm的光。TaON/BiO1.2I0.6最大光吸收范围在525nm-600nm之间,证实TaON/BiO1.2I0.6是一种宽光谱吸收的异质材料。
图3为TaON的N2吸附-脱附等温线及孔径分布曲线;图4为 5wt%TaON/BiO1.2I0.6的N2吸附-脱附等温线及孔径分布曲线;图5为为 BiO1.2I0.6的N2吸附-脱附等温线及孔径分布曲线;
由图3-5可以看出TaON、5wt%TaON/BiO1.2I0.6、BiO1.2I0.6吸附-脱附等温线与IV型等温线一致,均有明显的滞后环,说明TaON、 5wt%TaON/BiO1.2I0.6、BiO1.2I0.6为介孔材料。BJH孔径分析显示,TaON、 5wt%TaON/BiO1.2I0.6、BiO1.2I0.6的平均孔径分别为32nm、35.3nm、42.2nm,这与吸附-脱附等温线一致。BET分析显示,TaON、5wt%TaON/BiO1.2I0.6、 BiO1.2I0.6的比表面积分别为4.3m2/g、16.3m2/g、19.5m2/g。
图6为TaON、TaON/BiO1.2I0.6、BiO1.2I0.6光催化分解甲苯活性的结果。其反应器体积为250mL、光源300W氙灯、催化剂量0.2g、甲苯初始浓度3000ppm、H2O 5μL。
由图6可以看出,TaON/BiO1.2I0.6的光催化分解甲苯活性高于 BiO1.2I0.6和TaON,其中5wt%TaON/BiO1.2I0.6展示出最高的光催化活性。经过24h照射,TaON仅可将50%的甲苯降解,BiO1.2I0.6降解了54%的甲苯,而在同样的条件下,5wt%TaON/BiO1.2I0.6能够将74%的甲苯降解。
图7为5wt%TaON/BiO1.2I0.6循环3次运行降解甲苯的活性。图7 显示,5wt%TaON/BiO1.2I0.6循环使用3次,其降解甲苯的活性并没有明显下降,表明5wt%TaON/BiO1.2I0.6具有良好的稳定性。
最后应说明的是:以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (5)
1.一种宽光谱吸收富氧缺碘异质光催化材料TaON/BiO1.2I0.6的制备方法,其特征在于,包括以下步骤:
1)、以Ta2O5为原料,以50-100mL/min流量通入NH3,并以5-10℃/min的升温速率加热至700-900℃,氮化6-10h,保持同样流量持续通入NH3,冷却至室温,获得土黄色TaON;
2)、将TaON加入含有硝酸铋的乙二醇溶液中,磁力搅拌0.5-1h,然后向上述溶液中滴入含碘化钾的乙二醇溶液,继续搅拌反应0.5-1h后,将反应液转入高压反应釜,140-180℃反应8-12h,自然冷却至室温,过滤、洗涤、80℃干燥后获得TaON/BiOI复合光催化材料;
3)、以TaON/BiOI复合光催化材料为前驱体,并将其置于管式炉中,以5-10℃/min的升温速率加热至350-450℃,焙烧3-6h,自然冷却至室温称重,获得宽光谱吸收富氧缺碘异质光催化材料TaON/BiO1.2I0.6。
2.如权利要求1所述的宽光谱吸收富氧缺碘异质光催化材料TaON/BiO1.2I0.6的制备方法,其特征在于,所述步骤1)的氮化温度是850℃,氮化时间是10h,氨气流量80mL/min。
3.如权利要求1所述的宽光谱吸收富氧缺碘异质光催化材料TaON/BiO1.2I0.6的制备方法,其特征在于,所述步骤2)中高压反应釜内的反应温度160℃,反应时间12h。
4.如权利要求1所述的宽光谱吸收富氧缺碘异质光催化材料TaON/BiO1.2I0.6的制备方法,其特征在于,所述步骤3)中焙烧温度400℃,焙烧时间5h,升温速率5℃/min。
5.一种权利要去1所述的宽光谱吸收富氧缺碘异质光催化材料TaON/BiO1.2I0.6在VOCs净化中的应用。
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