CN112844372B - 一种含氧空位的钼酸铋热催化剂及其制备方法和应用 - Google Patents
一种含氧空位的钼酸铋热催化剂及其制备方法和应用 Download PDFInfo
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- DKUYEPUUXLQPPX-UHFFFAOYSA-N dibismuth;molybdenum;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Mo].[Mo].[Bi+3].[Bi+3] DKUYEPUUXLQPPX-UHFFFAOYSA-N 0.000 title claims abstract description 39
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000001301 oxygen Substances 0.000 title claims abstract description 34
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 34
- 239000003054 catalyst Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001257 hydrogen Substances 0.000 claims abstract description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 13
- 238000001354 calcination Methods 0.000 claims abstract description 12
- 230000003197 catalytic effect Effects 0.000 claims abstract description 11
- 150000001621 bismuth Chemical class 0.000 claims abstract description 10
- 239000002243 precursor Substances 0.000 claims abstract description 10
- 150000002751 molybdenum Chemical class 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 4
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 29
- 239000007789 gas Substances 0.000 claims description 11
- 230000015556 catabolic process Effects 0.000 claims description 8
- 238000006731 degradation reaction Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000003344 environmental pollutant Substances 0.000 claims description 5
- 231100000719 pollutant Toxicity 0.000 claims description 5
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical group [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 4
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 4
- 239000011609 ammonium molybdate Substances 0.000 claims description 4
- 229940010552 ammonium molybdate Drugs 0.000 claims description 4
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical group O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- QYIGOGBGVKONDY-UHFFFAOYSA-N 1-(2-bromo-5-chlorophenyl)-3-methylpyrazole Chemical compound N1=C(C)C=CN1C1=CC(Cl)=CC=C1Br QYIGOGBGVKONDY-UHFFFAOYSA-N 0.000 claims description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 2
- 229910052797 bismuth Inorganic materials 0.000 claims description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 2
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 239000011733 molybdenum Substances 0.000 claims description 2
- 235000015393 sodium molybdate Nutrition 0.000 claims description 2
- 239000011684 sodium molybdate Substances 0.000 claims description 2
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 230000007704 transition Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910017299 Mo—O Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000006652 catabolic pathway Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/31—Chromium, molybdenum or tungsten combined with bismuth
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Abstract
本发明涉及一种含氧空位的钼酸铋热催化剂及其制备方法和应用。制备方法包括如下步骤:将钼盐和铋盐加入去离子水中,保持搅拌并使其充分溶解;加入聚乙二醇,继续搅拌,得到溶胶;将溶胶置于烘箱烘干,得前驱体;将所得前驱体研磨,在氢气环境下进行煅烧,得目标产物。本发明利用钼盐和铋盐制备出含氧空位的钼酸铋,其原料廉价易得,成本较低,环境友好。且合成的钼酸铋结构稳定,具有较高的热催化活性。本发明提供的含氧空位的钼酸铋热催化材料,氧空位能够在导带下形成施主能级,从而缩小带隙宽度,减少电子跃迁的能量,表现出良好的催化活性。
Description
技术领域
本发明属于热催化材料技术领域,具体涉及一种含氧空位的钼酸铋热催化剂及其制备方法和应用。
背景技术
随着社会的进步和经济发展,环境和能源问题愈加迫在眉睫,如何高效治理环境污染并寻找可替代化石燃料的清洁能源成为二十一世纪可持续发展的核心问题。催化技术在当今太阳能环境净化方面具有广阔的发展前景,有害的有机物和无机物的降解通常通过光催化、热催化、电催化降解等进行。其中,热催化是一种有效的降解途径,近年来,受到了科研工作者的广泛关注。
钼酸铋是一种新型的光催化材料,具有离子导电、介电性能、气体传感和催化活性等许多物理和化学性质。此物质具有纯度高和均匀性好等优点,合成后的钼酸铋具有较大的比表面积和丰富的氧空位。氧空位能够在导带下形成施主能级,从而缩小带隙宽度,减少电子跃迁的能量。然而,很少有人报道钼酸铋的热催化,通过研究,钼酸铋在热催化中具有良好的的催化活性,这也促进钼酸铋在降解气体污染物方面的应用。
发明内容
本发明的目的是提供一种含氧空位的钼酸铋热催化剂及其制备方法,该方法简单、方便、低成本、条件温和、有利于大规模生产。
本发明采用的技术方案为:一种含氧空位的钼酸铋热催化剂,制备方法包括如下步骤:
1)将钼盐和铋盐加入去离子水中,保持搅拌并使其充分溶解;
2)加入聚乙二醇,继续搅拌,得到溶胶;
3)将步骤2)所得溶胶置于烘箱烘干,得前驱体;
4)将步骤3)所得前驱体研磨,在氢气环境下进行煅烧,得目标产物。
优选地,上述的一种含氧空位的钼酸铋热催化剂,所述钼盐为钼酸铵或钼酸钠。
优选地,上述的一种含氧空位的钼酸铋热催化剂,所述铋盐为五水硝酸铋、氯化铋或乙酸铋。
优选地,上述的一种含氧空位的钼酸铋热催化剂,按元素摩尔比,铋:钼=2:1。
优选地,上述的一种含氧空位的钼酸铋热催化剂,步骤3)中,所述烘干,烘干温度为100-120℃。
优选地,上述的一种含氧空位的钼酸铋热催化剂,步骤4)中,所述煅烧,煅烧温度为300-700℃,煅烧时间为2h。
上述的一种含氧空位的钼酸铋热催化剂在热催化降解气体污染物中的应用。
优选地,上述的应用,所述气体污染物为异丙醇。
优选地,上述的应用,方法如下:于反应容器中,加入含氧空位的钼酸铋热催化剂,再加入异丙醇,在100℃-180℃下热催化降解。
本发明的有益效果是:
1.本发明利用钼盐和铋盐制备出含氧空位的钼酸铋,其原料廉价易得,成本较低,环境友好。且合成的钼酸铋结构稳定,具有良好的的热催化活性。
2.本发明提供的含氧空位的钼酸铋热催化材料,氧空位能够在导带下形成施主能级,从而缩小带隙宽度,减少电子跃迁的能量,表现出良好的催化活性。
附图说明
图1为纯Bi2MoO6和本发明氢气下煅烧所得空位Bi2MoO6的XRD对比图。
图2为纯Bi2MoO6和本发明氢气下煅烧所得空位Bi2MoO6的FI-IT对比图。
图3为纯Bi2MoO6和本发明氢气下煅烧所得空位Bi2MoO6的UV-vis对比图。
图4a为纯Bi2MoO6的理论计算能带图。
图4b为本发明氢气下煅烧所得空位Bi2MoO6的理论计算能带图。
图5为纯Bi2MoO6和本发明氢气下煅烧所得空位Bi2MoO6的异丙醇转换率对比图。
具体实施方式
实施例1
(一)含氧空位的钼酸铋热催化材料
1)将4.85g五水硝酸铋和0.88g钼酸铵分别溶于50ml的去离子水中,搅拌0.5h,将五水硝酸铋的水溶液与钼酸铵的水溶液混合均匀。
2)称取2g聚乙二醇,溶于10mL的去离子水中,注入步骤1)所得的混合溶液中,搅拌均匀得到溶胶。
3)将步骤2)所得溶胶置于120℃鼓风干燥箱中干燥15-20h,得到前驱体。
4)将步骤3)所得前驱体充分研磨后置于管式炉中,分别在空气(流速10ml/min)氛围下或氢气(流速10ml/min)氛围下,于500℃焙烧2h,管式炉的升温速率控制在3℃/min,分别得空气氛围下获得的Bi2MoO6,标记为纯Bi2MoO6,和氢气氛围下获得的含氧空位的钼酸铋,标记为空位Bi2MoO6。
(二)检测
图1为Bi2MoO6标准卡与纯Bi2MoO6和空位Bi2MoO6的XRD对比图,由图1可见,样品与标准卡符合,证明成功合成钼酸铋纳米材料。
图2为纯Bi2MoO6和空位Bi2MoO6的FT-IT对比图,950-700cm-1带为Mo-O键的伸缩模式,600-400cm-1的带为Bi-O的伸缩和振动模式,1620和1358cm-1的峰为O-H的震动模式,与纯的钼酸铋相比峰发生很大变化这与对应氢气氛围下活性高相一致。
图3为纯Bi2MoO6和空位Bi2MoO6的uv-vis对比图,相比纯钼酸铋,在氢气下煅烧样品表现为往右偏移而且在700nm之后有拖尾峰呈现,说明在材料中存在氧缺陷,并且样品氢气煅烧下的热催化活性最高。
图4a为纯Bi2MoO6和图4b为本发明氢气下煅烧所得空位Bi2MoO6理论计算能带图。当把钼酸铋其中一个氧抠点以后会在0(eV)左侧形成一个新的峰值,表现为在施主能级和受主能级之间形成一个新的杂质能级,这有利于载流子的运输与传导与图5催化活性一致,而且和紫外数据结果一致。
实施例2含氧空位的钼酸铋热催化材料在降解异丙醇中的应用
分别将实施例1制备的纯Bi2MoO6和空位Bi2MoO6放于玻璃反应器顶部,连接仪器并检验装置的气密性。加热异丙醇到30℃,部分异丙醇液体可挥发成气体,调节好气体流量计,打开气体压缩机,异丙醇气体可流入玻璃反应器内,同时打开电阻器,通过加热催化剂,催化剂可将异丙醇分解成丙酮气体。加热到120℃-180℃,20min之后,抽取10mL气体对丙酮含量进行检测,对比进气口与出气口异丙醇的含量。用FID检测器(GC1690,捷道科技有限公司)对生成的丙酮进行气相色谱分析。
图5为纯Bi2MoO6和空位Bi2MoO6异丙醇气体转换率的对比图,Bi2MoO6和空位Bi2MoO6的异丙醇转化率可知含有空位的钼酸铋催化活性更高,在相同时间内污染物降解更加高效。氧空位作为最常见和最重要的晶体缺陷之一,对半导体热催化性能有着重要的影响。钼酸铋是一种典型的n型半导体,其氧空位会使一个或两个电子在其位置发生局域化,局域化的电子对钼酸铋的电子结构有直接的影响,即在钼酸铋导带以下产生施主能级。这些施主能级随着氧空位的增加而增加,如果氧空位浓度足够高,有时会与导带重叠,氧空位的引入降低了电子跃迁的能带宽度和能量。
Claims (6)
1.一种含氧空位的钼酸铋热催化剂在热催化降解气体污染物中的应用,其特征在于,所述气体污染物为异丙醇,方法如下:在反应容器中,加入一种含氧空位的钼酸铋热催化剂,再加入异丙醇,在100℃-180℃下热催化降解;所述含氧空位的钼酸铋热催化剂,制备方法包括如下步骤:
1)将钼盐和铋盐加入去离子水中,保持搅拌并使其充分溶解;
2)加入聚乙二醇,继续搅拌,得到溶胶;
3)将步骤2)所得溶胶置于烘箱中烘干,得前驱体;
4)将步骤3)所得前驱体研磨,在氢气环境下进行煅烧,得目标产物。
2.根据权利要求1所述的应用,其特征在于,所述钼盐为钼酸铵或钼酸钠。
3.根据权利要求1所述的应用,其特征在于,所述铋盐为五水硝酸铋、氯化铋或乙酸铋。
4.根据权利要求1所述的应用,其特征在于,按元素摩尔比,铋:钼=2:1。
5.根据权利要求1所述的应用,其特征在于,步骤3)中,所述烘干,烘干温度为100-120℃。
6.根据权利要求1所述的应用,其特征在于,步骤4)中,所述煅烧,煅烧温度为300-700℃,煅烧时间为2h。
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