CN110465287A - 一种钼酸铋-凹凸棒复合材料及其制备方法 - Google Patents
一种钼酸铋-凹凸棒复合材料及其制备方法 Download PDFInfo
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- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 20
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 239000002131 composite material Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 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 claims abstract description 19
- 239000002105 nanoparticle Substances 0.000 claims abstract description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 27
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 14
- 239000011684 sodium molybdate Substances 0.000 claims description 10
- 235000015393 sodium molybdate Nutrition 0.000 claims description 10
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical class [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
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- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000003760 magnetic stirring Methods 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 1
- 229910017604 nitric acid Inorganic materials 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 11
- 238000007146 photocatalysis Methods 0.000 abstract description 7
- 239000003054 catalyst Substances 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 4
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 abstract description 4
- 229940043267 rhodamine b Drugs 0.000 abstract description 4
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 239000006185 dispersion Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 6
- 229910002900 Bi2MoO6 Inorganic materials 0.000 description 5
- 238000000034 method Methods 0.000 description 4
- 238000000643 oven drying Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- -1 bismuthino Chemical group 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 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 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
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- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000003504 photosensitizing agent Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052604 silicate mineral Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 230000003612 virological effect Effects 0.000 description 1
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Abstract
本发明公开了一种钼酸铋‑凹凸棒复合材料及其制备方法。钼酸铋在为纳米颗粒,部分呈片状,一维的凹凸棒(ATP)是一种优良的载体、分散剂,将钼酸铋与凹凸棒复合,得到具有分散性好,活性位点多的催化剂,在光催化降解罗丹明B方面表现出良好的催化活性。钼酸铋和凹凸棒的最佳质量比为1:0.5,180分钟即可将罗丹明B降解掉约94%,其性能是纯钼酸铋的3.7倍。光催化性能的提升,得益于钼酸铋与凹凸棒的紧密结合,增强了催化剂的吸附性和分散性,从而提升了光催化性能。
Description
技术领域
本发明涉及一种钼酸铋-凹凸棒复合材料及其制备方法,属于纳米材料制备领域。
背景技术
环境污染和能源短缺是当今世界的两大焦点问题,光催化技术是解决能源短缺和环境问题的理想技术,利用许多材料的光催化性能将太阳能转化为化学能,得到包括氢和碳氢化合物等有效益的材料,去除污染物和细菌等。光催化剂因其光利用率低、光生电子复合率高、表面活性位点少等因素限制了其应用。
为提升光催化剂的光催化性能,将对其进行改性,途径包括贵金属掺杂,半导体复合,引入缺陷或杂原子,加光敏化剂等。典型的光催化半导体有TiO2,ZnO,铋基半导体等,Bi2MoO6是奥利维里斯相铋系三元化合物,无毒,属于n型直接半导体,禁带宽度2.70-2.80eV,可吸收波长小于460nm的可见光,克服了TiO2等仅对紫外光响应的缺点而备受研究;凹凸棒是一种铝镁硅酸盐矿物,棒状结构,价廉易得,储存丰富。Fu,F.等利用Fe对含氧空位的Bi2MoO6进行改性,提升了其对苯酚的光催化降解能力[Fu,F.,et al.(2019)."Synergistic effect of surface oxygen vacancies and interfacial chargetransfer on Fe(III)/Bi2MoO6 for efficient photocatalysis."Applied Catalysis B:Environmental 247:150-162.],Zhang,G.等将Bi2MoO6与ZnO复合,提升了其光催化还原Cr(VI)的能力[Zhang,G.,et al.(2019)."Fabrication of Bi2MoO6/ZnO hierarchicalheterostructures with enhanced visible-light photocatalytic activity."AppliedCatalysis B:Environmental 250:313-324.],Hu,T.等将Bi2MoO6与In(OH)3复合提升了其光催化降解罗丹明B的能力[Hu,T.,et al.(2019)."Facile synthesis of indiumhydroxide nanosheet/bismuth molybdate hierarchical microsphere heterojunctionwith enhanced photocatalytic performance."J Colloid Interface Sci 545:301-310.]。上述改性方式制备成本较高,含金属元素(稀土元素),性能一般,因此需要研究一种成本低,不含金属元素改性,操作简单的方法。
发明内容
本发明的目的在于提供一种钼酸铋-凹凸棒复合材料及其制备方法。
实现本发明目的的技术解决方案为:
钼酸铋-凹凸棒复合材料,凹凸棒具有一维棒状结构,钼酸铋纳米颗粒与凹凸棒棒状结构按1-5:1的质量比紧密结合。
进一步的,钼酸铋纳米颗粒的尺寸为10nm的凹凸棒棒状的尺寸为50nm。
一种钼酸铋-凹凸棒复合材料的制备方法,包括以下步骤:
第一步,将凹凸棒与盐酸混合,放在磁力搅拌器上搅拌3h以上,离心洗涤后烘干;
第二步,分别将第一步样品、五水硝酸铋、钼酸钠分别分散于乙二醇溶液中超声搅拌1h以上后,混合,再搅拌0.5h;
第三步,第二步所得溶液转移至100mL聚四氟乙烯反应釜中,溶剂热18h后取出自然冷却;
第四步,第三步所得样品离心洗涤,烘干,制得钼酸铋-凹凸棒复合材料。
进一步的,第一步中,盐酸浓度为3mol/L,烘干温度为60℃。
进一步的,第三步中,溶剂热的温度为180℃。
进一步的,第四步中,离心转速为9000r/min,离心时间为1min,烘干温度为60℃。
进一步的,第一步和第二步中凹凸棒与五水硝酸铋、钼酸钠的质量比为0.4-2:4:1。
本发明与现有技术相比,其优点在于:(1)采用一步溶剂热法制得钼酸铋-凹凸棒复合材料,反应条件温和,操作简单;(2)原料凹凸棒资源丰富,价廉易得,预处理方式简单;(3)该材料用于光催化降解罗丹明B,表现出优异的催化性能。
附图说明
图1是本发明的合成机理图。
图2是本发明实施例2所制备的钼酸铋-凹凸棒复合材料的透射电镜图(其中A为较低放大倍数下的透射电镜,粒径约10nm的BMO和半径约50nm的凹凸棒,B为高分辨透射电镜图)。
图3是本发明实施例2,对比例1所制备材料的XRD衍射谱图。
图4是本发明实施例1-3,和对比例1制备的钼酸铋-凹凸棒的催化性能图。
具体实施方式
下面结合附图对本发明作进一步说明
图1是本发明的合成机理图,凹凸棒用盐酸预处理后,分散于乙二醇溶剂中;五水合硝酸铋,钼酸钠分别分散于乙二醇中。将上述溶液混合,转移至聚四氟乙烯反应釜中,溶剂热一定时间后取出,离心洗涤干燥得到钼酸铋-凹凸棒复合材料。
本发明制备的钼酸铋-凹凸棒复合材料作为光催化剂有优异的光催化性能,这主要归因于钼酸铋在凹凸棒上良好的分散性以及凹凸棒与钼酸铋紧密的结合程度,使得催化反应的有效比表面积增加,活性位点增多,提升了催化活性。
本发明的钼酸铋-凹凸棒复合材料光催化剂通过以下步骤制备:
第一步,将凹凸棒与盐酸混合,放在磁力搅拌器上搅拌3h以上,离心洗涤后放入烘箱烘干;
第二步,分别将第一步所得样品、五水硝酸铋、钼酸钠分别分散于乙二醇溶液中超声搅拌1h以上后,混合,再搅拌0.5h;
第三步,第二步所得溶液转移至100mL聚四氟乙烯反应釜中,于烘箱中溶剂热18h;
第四步,第三步所的样品离心洗涤,烘箱烘干,制得钼酸铋-凹凸棒复合材料。
实施例1
第一步,将凹凸棒与3mol/L盐酸混合,放在磁力搅拌器上搅拌3h以上,离心洗涤后放入烘箱烘干12h;
第二步,称取第一步中的样品、五水硝酸铋、钼酸钠(质量比2:4:1)分别分散于20mL乙二醇溶液中超声搅拌1h以上后,混合,再搅拌0.5h;
第三步,第二步所得溶液转移至聚四氟乙烯反应釜中,于180℃烘箱中溶剂热18h后取出;
第四步,第三步所的样品离心洗涤,60℃烘箱烘干12h,制得钼酸铋-凹凸棒1:1复合材料。
实施例2
第一步,将凹凸棒与3mol/L盐酸混合,放在磁力搅拌器上搅拌3h以上,离心洗涤后放入烘箱烘干12h;
第二步,称取第一步中的样品、五水硝酸铋、钼酸钠(质量比1:4:1)分别分散于20mL乙二醇溶液中超声搅拌1h以上后,混合,再搅拌0.5h;
第三步,第二步所得溶液转移至聚四氟乙烯反应釜中,于180℃烘箱中溶剂热18h后取出;
第四步,第三步所的样品离心洗涤,60℃烘箱烘干12h,制得钼酸铋-凹凸棒2:1复合材料。
实施例3
第一步,将凹凸棒与3mol/L盐酸混合,放在磁力搅拌器上搅拌3h以上,离心洗涤后放入烘箱烘干12h;
第二步,称取第一步中的样品、五水硝酸铋、钼酸钠(质量比0.4:4:1)分别分散于20mL乙二醇溶液中超声搅拌1h以上后,混合,再搅拌0.5h;
第三步,第二步所得溶液转移至聚四氟乙烯反应釜中,于180℃烘箱中溶剂热18h后取出;
第四步,第三步所的样品离心洗涤,60℃烘12h,制得钼酸铋-凹凸棒5:1复合材料。
对比例1
第一步,将五水硝酸铋、钼酸钠(质量比4:1)分散于20mL乙二醇溶液中,超声搅拌1h以上后,混合,再搅拌0.5h;
第二步,第一步所得溶液转移至聚四氟乙烯反应釜中,于烘箱中溶剂热18h;
第三步,第三步所得样品离心洗涤,烘干,制得纯钼酸铋(BMO)样品。
Claims (7)
1.钼酸铋-凹凸棒复合材料,其特征在于,所述的凹凸棒具有一维棒状结构,约10nm的钼酸铋纳米颗粒与50nm的凹凸棒棒状结构按1-5:1的质量比紧密结合。
2.根据权利要求1所述的钼酸铋-凹凸棒复合材料,其特征在于,所述的钼酸铋纳米颗粒的尺寸为10nm的凹凸棒棒状的尺寸为50nm。
3.一种钼酸铋-凹凸棒复合材料的制备方法,其特征在于,包括以下步骤:
第一步,将凹凸棒与盐酸混合,放在磁力搅拌器上搅拌3h以上,离心洗涤后烘干;
第二步,分别将第一步样品、五水硝酸铋、钼酸钠分别分散于乙二醇溶液中超声搅拌1h以上后,混合,再搅拌0.5h;
第三步,第二步所得溶液转移至100mL聚四氟乙烯反应釜中,溶剂热18h后取出自然冷却;
第四步,第三步所得样品离心洗涤,烘干,制得钼酸铋-凹凸棒复合材料。
4.如权利要求3所述的制备方法,其特征在于,第一步中,盐酸浓度为3mol/L,烘干温度为60℃。
5.如权利要求3所述的制备方法,其特征在于,第三步中,溶剂热的温度为180℃。
6.如权利要求3所述的制备方法,其特征在于,第四步中,离心转速为9000r/min,离心时间为1min,烘干温度为60℃。
7.如权利要求3所述的制备方法,其特征在于,第一步和第二步中凹凸棒与五水硝酸铋、钼酸钠的质量比为0.4-2:4:1。
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