CN107349926A - 单分子层钼酸铋纳米片及其在光催化氧化苄醇到醛的应用 - Google Patents
单分子层钼酸铋纳米片及其在光催化氧化苄醇到醛的应用 Download PDFInfo
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- 239000002356 single layer Substances 0.000 title claims abstract description 38
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 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 16
- 235000019445 benzyl alcohol Nutrition 0.000 title claims abstract description 13
- 229960004217 benzyl alcohol Drugs 0.000 title claims abstract description 13
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- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 13
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 title claims 2
- 230000003197 catalytic effect Effects 0.000 title abstract description 7
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- 238000002360 preparation method Methods 0.000 claims abstract description 14
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- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 9
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- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical compound [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 claims description 4
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Abstract
本发明公开了一种单分子层钼酸铋纳米片及其在光催化氧化苄醇到醛的应用,属于光催化材料的制备领域。单层Bi2MoO6纳米片是以Bi(NO3)3·5H2O和Na2MoO4·2H2O为原料,通过CTAB表面活性剂辅助的自下而上温和的水热方法制备而成。该单分子层纳米片在光催化选择性氧化苄醇到相应的醛具有较高的活性,解决了传统钼酸铋材料在制备苯甲醛及其衍生物时反应时间久、选择性低、转化率低等问题。本发明工艺简单,制备周期短,环保绿色,选择性高,能耗低,转化率高,符合实际生产需要,具有较大的应用潜力。
Description
技术领域
本发明属于光催化材料领域,具体涉及到一种单分子层钼酸铋纳米片及其在光催化氧化苄醇到醛的应用。
背景技术
在工业生产中,选择性氧化苯甲醇是一个基本的有机转化反应,对应生成的产物——羰基复合物,醛或者酮在药物的合成和精细化工中都起到重要的作用。随着社会现代化发展的需要,苯甲醛的用途不断扩大,苯甲醛是最简单的和工业上最常使用的芳香醛,用于制月桂醛、月桂酸、苯乙醛和苯甲酸苄酯等,也用作香料。目前常用于生产苯甲醛的方法有甲苯氯化再水解法,甲苯直接氧化法以及苯甲醇氧化法。然而这些制备苯甲醛的方法存在着能耗高,成本高,副产物多,步骤繁杂,反应速率慢,毒性大,效率低等问题。因此为了解决这些缺点以满足社会发展进步的需要和经济环境的要求,开发清洁、环保、高效的苯甲醛生产方法具有非常重大的意义。如何实现这一要求引起各国科研工作者们的广泛关注。到目前为止,很多半导体催化剂特别是具有可见光响应半导体催化剂以及具有不同的结构形态催化剂被开发利用,它们为促进苯甲醇的氧化制备苯甲醛提供了新思路和方法。然而这些体相的催化剂大多具有光生载流子分离效率低下的缺点,不利于光生电子和空穴的分离。进一步说,光生电子和空穴的有效分离才能更好的转化苯甲醇到苯甲醛。此外,层状催化剂的空间维度对催化活性起至关重要的作用。如果能将这些催化剂的维度从多层降低到单层并且催化剂的用量也极大地降低,这将极大的有利于不可再生能源的节约和环境污染的降低。
而近几十年来人们对于清洁能源的探索从未停止,全球能源危机和消耗急切的要求化学制造业朝着最小的能源消耗和催化剂用量方向发展,可见光捕获的反应或许能够替代传统的以热为基的化学过程,这为当今化学工业中大幅度的减少能源消耗提供了极大的可能性。光催化剂的研究是最重要的研究热点之一,到目前为止已经有很多光催化剂被开发出来,其中二维材料由于其本身的独特结构成为近年研究的热点之一。
无机二维(2D)片状纳米材料是一类分子或原子厚度并具有各向异性的片状结构,是一种纳米级的特殊材料。同时在重要的功能材料扮演着重要的角色,其特殊的结构使之在催化,吸附,活化等方面有着重要的应用。近年来,具有单分子层形貌的纳米片得到极大的关注,与其体相材料相比,单层的纳米片具有更大的比表面积,超快的电荷分离效率以及更多的反应活性位。进一步说,如果把层状纳米片的维度降低到单层,那么单层纳米片的优点强力的支持其在多相催化反应中表现出优越的性能和诱人的前景。光催化是多相催化的一种,作为一种可利用清洁可再生的太阳能来实现化学反应的具有巨大潜力的技术,它具有绿色环保,无二次污染的特点,因此受到了国内外科学家的高度关注。如果能结合具有单分子层形貌纳米片的优点,将其应用到苯甲醇氧化成苯甲醛反应中,这将为清洁能源的开发以及降低苯甲醛生产成本带来新希望。
发明内容
本发明的目的在于针对现有技术的不足,提供单分子层钼酸铋纳米片及其在光催化氧化苄醇到醛的应用。本发明制得的单层的Bi2MoO6纳米材料可作为催化剂用于光催化反应,该催化剂高效,无毒,制备方法简单,选择性高,操作简单,成本低廉,具有广阔的应用前景,并且可以扩展到其它层状材料到单分子层材料的制备。
为实现上述目的,本发明采用如下技术方案:
一种单分子层钼酸铋纳米片的制备方法,以Bi(NO3)3·5H2O和Na2MoO4·2H2O为主要原料,以CTAB为模板调节剂,以去离子水为溶剂,搅拌均匀后得混合溶液,经一步水热合成得到单分子层钼酸铋纳米片;其中,CTAB在混合溶液中的浓度为0.01 mol·L-1;水热合成的温度为180 ℃,时间为16 h。Bi(NO3)3·5H2O和Na2MoO4·2H2O的摩尔比为2:1。
更具体的,将Bi(NO3)3·5H2O和Na2MoO4·2H2O以及CTAB( 十六烷基三甲基溴化铵)溶解在80 ml去离子水,搅拌40 min,然后转移到100 ml聚四氟乙烯内衬,用钢套拧紧,180℃下水热合成16 h,待其自然冷却到室温后,所得产品收集离心,经过去离子水和乙醇洗涤,在60 ℃烘箱中干燥即可得到。
一种如上所述的制备方法制得的单分子层钼酸铋纳米片,厚度为0.82-1 nm。
如上制备的单分子层钼酸铋纳米片可作为光催化剂,在可见光的条件下光催化选择性氧化苄醇或苄醇的衍生物到相应的醛。
本发明的显著优点在于:
(1)本发明制得的单分子层Bi2MoO6纳米片可作为催化剂用于光催化反应,该催化剂高效,无毒,制备方法简单,选择性高,操作简单,成本低廉,具有广阔的应用前景;
(2)本发明的单分子层纳米片用于可见光下选择性氧化苯甲醇制得苯甲醛。较于传统的体相光催化剂用于此反应,具有较好的活性以及好的稳定性以及催化剂的用量少,节约能耗,降低环境污染,节约成本;
(3)本发明的单分子层纳米片作为催化剂时,实验操作方法简单,易于操作,有利于大规模的推广使用。
附图说明
图1是本发明的催化剂单分子层Bi2MoO6和体相Bi2MoO6的X射线衍射(XRD)图;
图2是本发明的催化剂单分子层Bi2MoO6的原子力显微镜(AFM)图和对应的高度剖面图;
图3是本发明的单分子层Bi2MoO6和体相Bi2MoO6为催化剂在光诱导下催化苯甲醇生成苯甲醛的转化率和选择性图;
图4是本发明的单分子层Bi2MoO6和体相Bi2MoO6的紫外-可见漫反射图。
具体实施方式
为了使本发明所述的内容更加便于理解,下面结合具体实施方式对本发明所述的技术方案做进一步的说明,但是本发明不仅限于此。
实施例1
单分子层Bi2MoO6纳米片的制备:
将0.242 g Na2MoO4·2H2O放入磁力搅拌的聚四氟乙烯的内衬中,加入80 ml去离子水,搅拌至Na2MoO4·2H2O溶解,然后加入0.3 g CTAB,继续搅拌40 min至CTAB完全溶解。然后称取0.970 g Bi(NO3)3·5H2O,加入上述混合液中继续搅拌;等其混合均匀后,取出磁子,放入100 ml的钢套中,在180 ℃下保持16 h水热完成后,等其自然降至室温后,收集产品,离心并且用去离子水和乙醇清洗多遍,然后再60 ℃烘箱中保持10 h烘干产品,然后研磨成粉末状,即可得到单分子层的Bi2MoO6纳米片。
同样的合成体相Bi2MoO6,取0.242 g Na2MoO4·2H2O和0.970 g Bi(NO3)3·5H2O放入盛有80 ml去离子水中搅拌至其溶解,然后将混合液放入钢套中,在180 ℃下保持16 h水热完成后,等其自然降至室温后,收集产品。离心并且用去离子水和乙醇清洗多遍,然后在60 ℃烘箱中保持10 h烘干产品,然后研磨成粉末状,即可得到体相的Bi2MoO6样品。
图1展示了本发明的单分子层的Bi2MoO6纳米片催化剂和体相的Bi2MoO6的X射线衍射(XRD)图,从图中可以发现制备的单分子层的Bi2MoO6纳米片为纯相,并且他们的晶相保持一致;图2展示了本发明的催化剂单分子层的Bi2MoO6纳米片原子力显微镜(AFM)图和对应的高度剖面图,从图中可以看出通过此水热方法制备出平均厚度只有0.82 nm的高质量的单分子层Bi2MoO6纳米片。
应用实施例1
单分子层Bi2MoO6纳米片在光催化选择性氧化苯甲醇转化成苯甲醛。
将制备的单分子层Bi2MoO6纳米片用作催化剂在可见光光诱导下实现光催化氧化苯甲醇到苯甲醛。称取16 mg 单分子层Bi2MoO6纳米片放到反应器中,用移液枪量取1.5 ml通了0.5 h氧气的三氟甲苯溶液以及10.4 µl苯甲醇加入反应器中,超声5 min使其混合均匀,在氧气的气氛下,然后开启光源进行光催化反应,产物使用气相色谱检测;实验使用的光源为300 W氙灯;苯甲醇的转化率及和选择性的生成情况如图3所示,从图中可以看出在有催化剂时,苯甲醇在光照4 h后转化率达到26.5%,生成苯甲醛的选择性达到99 %以上。而在没有加催化剂或不光照或以体相的Bi2MoO6为催化剂的条件下,苯甲醇生成苯甲醛的转化率非常小,且没有苯甲醛的产生;因此,在可见光条件下,单分子层Bi2MoO6纳米片能高效地催化苯甲醇转化成苯甲醛。
应用实施例2
单分子层Bi2MoO6纳米片光催化选择性氧化苯甲醇衍生物到相应的醛。
称取16 mg单层纳米片放到反应器中,用移液枪分别量取1.5ml通了0.5h氧气的三氟甲苯溶液以及含有甲氧基,甲基,氟,氯和硝基不同取代基的苯甲醇加入不同的反应器中,超声5 min使其混合均匀,在氧气的气氛下,然后开启光源进行光催化反应,产物使用气相色谱检测;实验使用的光源为300 W氙灯;不同取代基的苯甲醇转化率和选择性表1所示。
表1 单分子层Bi2MoO6和体相Bi2MoO6在光催化选择性氧化苯甲醇及其衍生物到相应的醛的转化率和选择性。
[a] 反应温度; [b] λ ≥ 400 nm;[c] 体相 Bi2MoO6;[d] 单分子层 Bi2MoO6 纳米片。
以上所述仅为本发明的较佳实施例,凡依本发明申请专利范围所做的均等变化与修饰,皆应属本发明的涵盖范围。
Claims (6)
1.一种单分子层钼酸铋纳米片的制备方法,其特征在于:以Bi(NO3)3·5H2O和Na2MoO4·2H2O为主要原料,以CTAB为模板调节剂,以去离子水为溶剂,搅拌均匀后得混合溶液,经一步水热合成得到单分子层Bi2MoO6纳米片。
2.根据权利要求1所述的单分子层钼酸铋纳米片的制备方法,其特征在于:CTAB在混合溶液中的浓度:0.01 mol·L-1。
3.根据权利要求1所述的单分子层钼酸铋纳米片的制备方法,其特征在于:水热合成的温度为180 ℃,时间为16 h。
4.根据权利要求1所述的单分子层钼酸铋纳米片的制备方法,其特征在于:Bi(NO3)3·5H2O和Na2MoO4·2H2O的摩尔比为2:1。
5.一种如权利要求1-4任一项所述的制备方法制得的单分子层钼酸铋纳米片,其特征在于:单分子层Bi2MoO6纳米片的厚度为0.82-1 nm。
6.一种如权利要求5所述的单分子层钼酸铋纳米片的应用,其特征在于:作为光催化剂,在可见光的条件下光催化选择性氧化苄醇或苄醇的衍生物到相应的醛。
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CN113441132A (zh) * | 2021-06-10 | 2021-09-28 | 南昌航空大学 | 一种基于强界面相互作用的高活性钼酸铋/生物炭复合光催化剂的制备方法 |
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