CN110550661A - 一种钨酸铋可见光催化剂的制备方法及钨酸铋可见光催化剂的应用 - Google Patents
一种钨酸铋可见光催化剂的制备方法及钨酸铋可见光催化剂的应用 Download PDFInfo
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- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 26
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 26
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 claims abstract description 63
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 235000019445 benzyl alcohol Nutrition 0.000 claims abstract description 21
- 239000003054 catalyst Substances 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002244 precipitate Substances 0.000 claims abstract description 15
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 13
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- 239000000413 hydrolysate Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 12
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound 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 abstract description 11
- 239000000047 product Substances 0.000 claims abstract description 10
- 239000006185 dispersion Substances 0.000 claims abstract description 9
- QWMFKVNJIYNWII-UHFFFAOYSA-N 5-bromo-2-(2,5-dimethylpyrrol-1-yl)pyridine Chemical compound CC1=CC=C(C)N1C1=CC=C(Br)C=N1 QWMFKVNJIYNWII-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000007062 hydrolysis Effects 0.000 claims abstract description 8
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 6
- 230000001590 oxidative effect Effects 0.000 claims abstract description 6
- 238000001291 vacuum drying Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 abstract description 5
- 230000001699 photocatalysis Effects 0.000 abstract description 5
- 239000004065 semiconductor Substances 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 description 9
- 238000007254 oxidation reaction Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
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- 230000002349 favourable effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- LBSANEJBGMCTBH-UHFFFAOYSA-N manganate Chemical compound [O-][Mn]([O-])(=O)=O LBSANEJBGMCTBH-UHFFFAOYSA-N 0.000 description 1
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- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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Abstract
本发明涉及半导体光催化材料技术领域。目的是提供一种工艺简单、成本低廉的钨酸铋可见光催化剂,并将该可见光催化剂应用于苯甲醇选择性氧化为苯甲醛的反应中。技术方案是:一种钨酸铋可见光催化剂的制备方法,按如下步骤进行:1)将五水硝酸铋分散在25‑40℃的水中发生水解,20min后离心洗涤水解产物备用;2)将步骤1)得到的水解产物和定量的二水钨酸钠在去离子水中混合均匀,获得分散液,之后用0.1mol/L硝酸溶液调节体系pH到4;3)将步骤2)得到的分散液转移到水热反应釜中,经过160‑180℃水热反应20‑24h得到沉淀物,再用去离子水洗涤数次后在真空干燥箱中60℃干燥12h,得到催化剂产品。
Description
技术领域
本发明涉及半导体光催化材料技术领域。具体涉及一种钨酸铋(Bi2WO6)光催化剂制备方法及钨酸铋光催化剂在苯甲醇氧化为苯甲醇的反应中的应用。
背景技术
随着人们对环境保护意识的日益加强和能源危机的日益紧张。现急需要利用清洁能源替代传统能源,太阳能是一种可再生清洁能源。因此充分利用太阳能为人类的生产活动提供了必要的拓展。自从TiO2光催化剂的诞生,光催化剂得到了快速的发展,如半导体光催化剂催化分解水产H2、降解有机污染物、光催化促进有机合成反应等。
传统苯甲醇氧化过程反应是在高温高压大量溶剂条件下进行,同时使用了大量的锰酸盐和铬酸盐作为催化剂,这给现代工业造成了大量的能耗和环境污染,为此光催化半导体材料在苯甲醇选择性氧化为苯甲醛的反应中,具有很好的应用前景。
虽然TiO2性质稳定,价格低廉,又具有众多独特的性能,但其只能在紫外光辐射下效果好;由于大量含Bi化合物具有较好的光催化苯甲醇氧化为苯甲醛的性能,同时其还具有特殊的层状结构,有利于光生载流子的分离和传导,Bi2WO6是典型Aurivillius型结构氧化物,具有合适的禁带宽度具有可见光下催化活性。但目前制备Bi2WO6光催化剂过程中基本上会使用一些表面活性剂,这对催化剂的纯度不利,并且制备方法都较复杂,不利于工业化生产。
发明内容
本发明的目的在于提供一种工艺简单、成本低廉的钨酸铋可见光催化剂,并将该可见光催化剂应用于苯甲醇选择性氧化为苯甲醛的反应中。
为了实现上述目的,将通过以下方案进行:
一种钨酸铋可见光催化剂的制备方法,按如下步骤进行:
1)将五水硝酸铋分散在25-40℃的水中发生水解,20min后离心洗涤水解产物备用;
2)将步骤1)得到的水解产物和定量的二水钨酸钠在去离子水中混合均匀,获得分散液,之后用0.1mol/L硝酸溶液调节体系pH到4;
3)将步骤2)得到的分散液转移到水热反应釜中,经过160-180℃水热反应20-24h得到沉淀物,再用去离子水洗涤数次后在真空干燥箱中60℃干燥12h,得到催化剂产品。
所述步骤1)中五水硝酸铋与水的摩尔比为6:11-12。
所述步骤2)中水解产物与二水钨酸钠的摩尔比为1:3-4。
所述钨酸铋可见光催化剂应用于苯甲醇氧化为苯甲醛的反应中。
本发明的有益效果是:本发明提供的方法,只需将三种原料混合、水热反应干燥后即成,工艺简单成本低廉,获得的钨酸铋(Bi2WO6)可见光催化剂晶相完好(经过XRD(X-射线粉末衍射仪)测定,材料各衍射峰均出现,峰强度强,同时没有任何杂质峰出现,与标准卡片JCPDS No.73-1126.卡片非常吻合;在具体光催化苯甲醇氧化为苯甲醛的应用实验中,苯甲醛选择性在99%,同时苯甲醇转化率也达到88%以上甚至达到93%。。
附图说明
图1为本发明实施例1制备的钨酸铋(Bi2WO6)的XRD图谱。
图2为本发明实施例1制备的钨酸铋光催化剂在催化苯甲醇为苯甲醛时的反应活性。
图3为本发明实施例1制备的钨酸铋光催化剂苯甲醇选择性氧化循环稳定性测试结果。
图4为本发明实施例2制备的钨酸铋光催化剂苯甲醇选择性氧化循环稳定性测试结果。
具体实施方式
以下是对本发明的进一步说明,而不是对本发明的限制。
实施例1:
将0.020mol五水硝酸铋分散在25℃、0.037mol的水中发生水解,20min后离心洗涤水解产物备用。然后将上述五水硝酸铋水解产物(0.0033mol)和0.010mol二水钨酸钠在30ml去离子水中充分搅拌均匀,用0.1mol/L硝酸溶液调节体系pH到4,最后将得到的分散液转移到水热反应釜中经过160℃水热反应20h,得到沉淀物用去离子水洗涤数次后在真空干燥箱中60℃干燥12h,得到钨酸铋(Bi2WO6)可见光催化剂产品。
实施例1得到钨酸铋(Bi2WO6)光催化剂,其XRD图谱如图1所示,Bi2WO6的衍射特征峰均存在,并且与JCPDS No.73-1126.卡片吻合,说明得到了晶相较好的Bi2WO6。
本实施例1的Bi2WO6在可见光下进行了苯甲醇催化氧化为苯甲醛的实验,结果如图2所示:反应10h苯甲醛选择性为99%,同时苯甲醇转化率也达到93%,对本实施例中的催化剂还进行了稳定性测试实验,结果如3所示:经过五次循环测试Bi2WO6仍具有非常高的活性,基本没有受到影响。因此该催化剂具有非常高的通过光催化将苯甲醇氧化为苯甲醛的活性。
实施例2:
将0.020mol五水硝酸铋分散在35℃、0.040mol的水中发生水解,20min后离心洗涤水解产物备用。然后将上述五水硝酸铋水解产物(0.0033mol)和0.010mol二水钨酸钠在30ml去离子水中充分搅拌均匀,用0.1mol/L硝酸溶液调节体系pH到4,最后将得到的分散液转移到水热反应釜中经过170℃水热反应24h,得到沉淀物用去离子水洗涤数次后在真空干燥箱中60℃干燥12h,得到钨酸铋(Bi2WO6)可见光催化剂产品;其XRD图谱也与图1相同。
本发明实施例的钨酸铋(Bi2WO6)在可见光下进行了苯甲醇催化氧化为甲醛的实验,结果如图2所示:反应10h苯甲醛选择性为99%,同时苯甲醇转化率也达到88%。同时对本实施例中的催化剂还进行了稳定性测试实验,结果如4所示:经过五次循环测试Bi2WO6仍具有非常高的活性,基本没有受到影响。
实施例3:
将0.02mol五水硝酸铋分散在40℃、0.037mol的水中发生水解,20min后离心洗涤水解产物备用。然后将五水硝酸铋水解产物(0.0033mol)和0.013mol二水钨酸钠在30ml去离子水中充分搅拌均匀,用0.1mol/L硝酸溶液调节体系pH到4,最后将得到的分散液转移到水热反应釜中经过180℃水热反应20h,得到沉淀物用去离子水洗涤数次后在真空干燥箱中60℃干燥12h,得到钨酸铋(Bi2WO6)可见光催化剂产品;其XRD图谱也与图1相同。
本发明实施例的Bi2WO6在可见光下进行了苯甲醇催化氧化为苯甲醛的实验,结果如图2所示:反应10h苯甲醛选择性为99%,同时苯甲醇转化率也达到90%。
以上实施例仅用以说明本发明的技术方案而非对本发明保护范围的限制,本领域的普通技术人员应当理解,可以对本发明的技术方案进行修改或者等同替换,而不脱离本发明技术方案的实质和范围。
Claims (4)
1.一种钨酸铋可见光催化剂的制备方法,按如下步骤进行:
1)将五水硝酸铋分散在25-40℃的水中发生水解,20min后离心洗涤水解产物备用;
2)将步骤1)得到的水解产物和定量的二水钨酸钠在去离子水中混合均匀,获得分散液,之后用0.1mol/L硝酸溶液调节体系pH到4;
3)将步骤2)得到的分散液转移到水热反应釜中,经过160-180℃水热反应20-24h得到沉淀物,再用去离子水洗涤数次后在真空干燥箱中60℃干燥12h,得到晶相较好催化剂产品。
2.根据权利要求1所述的钨酸铋可见光催化剂的制备方法,其特征在于:所述步骤1)中五水硝酸铋与水的摩尔比6:11-12。
3.根据权利要求1所述的钨酸铋可见光催化剂的制备方法,其特征在于:所述步骤2)中水解产物与二水钨酸钠的摩尔比为1:3-4。
4.权利要求1所述的钨酸铋可见光催化剂的制备方法,所述钨酸铋可见光催化剂应用于苯甲醇氧化为苯甲醛的反应中。
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