CN112079389A - 一种棒状偏钒酸锰粉末的制备方法及其用途 - Google Patents
一种棒状偏钒酸锰粉末的制备方法及其用途 Download PDFInfo
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- 239000011572 manganese Substances 0.000 title claims abstract description 56
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 37
- ALTWGIIQPLQAAM-UHFFFAOYSA-N metavanadate Chemical compound [O-][V](=O)=O ALTWGIIQPLQAAM-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 239000000843 powder Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000003756 stirring Methods 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
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- 229910000357 manganese(II) sulfate Inorganic materials 0.000 claims abstract description 9
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims abstract description 8
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 8
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
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Abstract
本发明公开了一种棒状偏钒酸锰粉末的制备方法,将MnSO4·H2O溶解于去离子水中,磁力搅拌形成均匀溶液;再将钒源溶于去离子水中,搅拌,得到橙黄色溶液,将此溶液缓慢滴入到MnSO4溶液中,加入过程中不断磁力搅拌,得到棕色沉淀物后继续搅拌8‑15分钟,将其移入聚四氟乙烯内衬高压反应釜中加热反应,冷却后,经过洗涤、干燥得到棒状的Mn(VO3)2样品。本发明可以在无需添加表面活性剂的情况下制备出具有均一形貌的棒状的偏钒酸锰,并使用K2(H2O)10H2V10O28·4H2O做钒源,且制备工艺简单,周期短,生产过程安全,生产效率高,制得的棒状偏钒酸锰可以在紫外光下较好地降解亚甲基蓝、罗丹明B等有机染料。
Description
技术领域
本发明涉及无机微纳米功能材料技术领域,尤其涉及一种棒状偏钒酸锰粉末的制备方法及其用途。
背景技术
研究发现,半导体作为光催化材料,光催化降解和消除有害有机物是一种治理环境污染的重要的技术之一,而且半导体材料还可以用作电极的负极材料,并具有优良的性能。目前,偏钒酸锰Mn(VO3)2凭其独有的结构拥有良好的光学和电化学性能,在光学器件、光催化以及锂离子电池领域拥有良好的应用前景。通过高温固相反应法、沉淀法、水热法以及聚合物辅助合成法可以合成出不同形貌的偏钒酸锰粉末,材料的尺寸和形态对物理、化学性质有着决定性的作用。因此合成出具有一定形貌制备出特殊形态的偏钒酸锰对于其应用具有重要意义。根据文献报道,具有不同形貌结构的偏钒酸锰材料已经被成功地合成出来,比如最早E. andrukaitis (J. Power Sources, 1997, 68(2):652-655.)利用沉淀法合成出了带有结晶水的Mn(VO3)2·yH2O 用作锂离子电池的负极材料,Tan等利用路线流变相法并将前躯体高温热解成功合成出了不同粒径的Mn(VO3)2粉末(Inorganic Materials,2010, 46(2):201-205),以及后来Michio Inagaki等人用水热法合成出来具有棒状结构的Mn(VO3)2(Solid State Ionics, 2003, 156, 275-282),还有刘奕,钱奕太等人合成出了单晶Mn(VO3)2纳米带(Journal of Crystal Growth, 2005, 133(2):117-120)以及Huang等采用多步水热法合成出了具有带状结构的钒酸锰纳米带(Journal of Alloys andCompounds, 2010, 41(26):185-188),尽管上述文献报道合成出了具有各种独特形貌的偏钒酸锰材料,但上述研究工作都是针对于锂离子电池电极材料的,还没有对其在光催化方面展开相关的研究,而且这些制备方法大多比较繁琐,要么就是产品的结晶度较差,形貌不易控制,因此,寻求一种条件温和、成本低廉、操作简单、环境友好而且能够控制偏钒酸锰材料的尺寸、形貌以及特殊结构的合成路线具有重要的意义。
发明内容
基于背景技术存在的技术问题,本发明提出了一种棒状偏钒酸锰Mn(VO3)2粉末的制备方法,可以在无需添加表面活性剂的情况下,利用K2(H2O)10H2V10O28·4H2O作为钒源,制备出具有均一形貌的棒状偏钒酸锰,且制备工艺简单,反应时间短,制得的纳米粉体可以在紫外光下降解罗丹明B和亚甲基蓝。
本发明的技术方案如下:
一种棒状偏钒酸锰粉末的制备方法,包括以下步骤:
第一步,将3-8mmol 的MnSO4·H2O 溶解于25 mL去离子水中,搅拌15-25min,得到无色溶液;
第二步,0.3-0.8mmol的钒源溶于25mL去离子水中,搅拌15-25min,得到的橙黄色溶液;
第三步,将第二步配制的橙黄色溶液缓慢滴入到第一步得到的无色溶液中,用盐酸调pH=2.5-5.0,并继续搅拌8-15min得到棕色悬浊液;
第四步,将第三步得到的棕色悬浊液转移到聚四氟乙烯内衬高压反应釜中,然后把反应釜放入鼓风干燥箱中170-200℃下反应20-30h;
第五步,将产品离心、洗涤,然后在真空干燥箱中65-75℃干燥18-24h,得到棕色的棒状偏钒酸锰Mn(VO3)2粉末。
优选的,所述的步骤二中的钒源为K2(H2O)10H2V10O28·4H2O。
优选的,所述第五步中的洗涤是指将冷却后的产物用去离子水和无水乙醇各洗涤3 次。
优选的,本发明制备的棒状偏钒酸锰Mn(VO3)2粉末作为催化剂,可以在紫外光下高效地降解罗丹明B和亚甲基蓝。
本发明的有益之处在于:
(1)采用K2(H2O)10H2V10O28·4H2O作为反应物,提供钒源;
(2)方法简便,易于操作,反应条件温和;
(3)制备周期短,24h即可制备出样品;
(4)制得的棒状偏钒酸锰Mn(VO3)2经光催化实验验证可以在紫外光下高效地降解罗丹明B和亚甲基蓝;
(5)无需添加任何表面活性剂的情况下制备出具有均一形貌的棒状偏钒酸锰Mn(VO3)2。
附图说明
图1是本发明实施例一制备的棒状Mn(VO3)2的XRD图。
图2是本发明实施例五制备的棒状Mn(VO3)2的SEM图,放大倍数1500倍。
图3分别是本发明实施例一制备的棒状Mn(VO3)2的SEM图,放大倍数30000倍和TEM图。
图4是本发明实施例一制备的棒状Mn(VO3)2在紫外光催化下罗丹明B降解量随着光照时间变化的关系图。
具体实施方式
实施例1
第一步,将5mmol 的MnSO4·H2O溶解于25 mL去离子水中,搅拌20min,得到透明溶液;
第二步,0.5mmol的K2(H2O)10H2V10O28·4H2O溶于25mL去离子水中,搅拌20min,得到的橙黄色溶液;
第三步,将第二步配制的K2(H2O)10H2V10O28·4H2O溶液缓慢滴入到第一步得到的MnSO4溶液中,用HCl调pH=3.0,并继续搅拌10min得到悬浊液;
第四步,将第三步得到的棕色悬浊液转移到聚四氟乙烯内衬高压反应釜中,然后把反应釜放入鼓风干燥箱中180℃下反应24h。
第五步,将产品离心、洗涤,然后在真空干燥箱中70℃干燥20h,得到棒状偏钒酸锰Mn(VO3)2粉末。
如附图1所示,为本实施例制备的棒状偏钒酸锰的XRD图,可以看出其纯度高,结晶度好。
如附图3所示,左图为本实施例制备的棒状偏钒酸锰纳米粉体的SEM图,放大倍数30000 倍;右图为实施例制备的棒状偏钒酸锰纳米粉体的TEM图。
可以看出本实施例1制备的棒状偏钒酸锰为明显的单晶棒状。
实施例2
第一步,将3mmol 的MnSO4·H2O溶解于25 mL去离子水中,搅拌15min,得到透明溶液;
第二步,0.8mmol的K2(H2O)10H2V10O28·4H2O溶于25mL去离子水中,搅拌25min,得到的橙黄色溶液;
第三步,将第二步配制的K2(H2O)10H2V10O28·4H2O溶液缓慢滴入到第一步得到的MnSO4溶液中,用HCl调pH=5.0,并继续搅拌15min得到悬浊液;
第四步,将第三步得到的棕色悬浊液转移到聚四氟乙烯内衬高压反应釜中,然后把反应釜放入鼓风干燥箱中170℃下反应30h。
第五步,将产品离心、洗涤,然后在真空干燥箱中65℃干燥24h,得到偏钒酸锰Mn(VO3)2粉末。
实施例3
第一步,将8mmol 的MnSO4·H2O 溶解于25 mL去离子水中,搅拌25min,得到透明溶液;
第二步,0.3mmol的K2(H2O)10H2V10O28·4H2O溶于25mL去离子水中,搅拌15min,得到的橙黄色溶液;
第三步,将第二步配制的K2(H2O)10H2V10O28·4H2O溶液缓慢滴入到第一步得到的MnSO4溶液中,用HCl调pH=2.5,并继续搅拌25min得到悬浊液;
第四步,将第三步得到的棕色悬浊液转移到聚四氟乙烯内衬高压反应釜中,然后把反应釜放入鼓风干燥箱中200℃下反应20h;
第五步,将产品离心、洗涤,然后在真空干燥箱中75℃干燥18h,得到片状偏钒酸锰Mn(VO3)2粉末。
实施例4
第一步,将4.5mmol 的MnSO4·H2O溶解于25 mL去离子水中,搅拌20min,得到透明溶液;
第二步,0.55mmol的K2(H2O)10H2V10O28·4H2O溶于25mL去离子水中,搅拌25min,得到的橙黄色溶液;
第三步,将第二步配制的K2(H2O)10H2V10O28·4H2O溶液缓慢滴入到第一步得到的MnSO4溶液中,用HCl调pH=4.5,并继续搅拌20min得到悬浊液;
第四步,将第三步得到的棕色悬浊液转移到聚四氟乙烯内衬高压反应釜中,然后把反应釜放入鼓风干燥箱中185℃下反应24h;
第五步,将产品离心、洗涤,然后在真空干燥箱中75℃干燥20h,得到转子状偏钒酸锰Mn(VO3)2粉末。
实施例5
第一步,将3.5mmol 的MnSO4·H2O溶解于25 mL去离子水中,搅拌20min,得到透明溶液;
第二步,0.65mmol的K2(H2O)10H2V10O28·4H2O溶于25mL去离子水中,搅拌20min,得到的橙黄色溶液;
第三步,将第二步配制的K2(H2O)10H2V10O28·4H2O溶液缓慢滴入到第一步得到的MnSO4溶液中,用HCl调pH=3.5,并继续搅拌22min得到悬浊液;
第四步,将第三步得到的棕色悬浊液转移到聚四氟乙烯内衬的高压反应釜中,然后把反应釜放入鼓风干燥箱中185℃下反应24h;
第五步,将产品离心、洗涤,然后在真空干燥箱中75℃下干燥20h,得到棒状偏钒酸锰Mn(VO3)2粉末。
如附图2所示,为本实施例制备的棒状偏钒酸锰的SEM图,放大倍数1500 倍;
可以看出本实施例5制备的棒状偏钒酸锰为明显的棒状。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (4)
1.一种棒状偏钒酸锰粉末的制备方法,其特征在于,包括以下步骤:
第一步,将3-8mmol 的MnSO4·H2O 溶解于25 mL去离子水中,搅拌15-25min,得到无色溶液;
第二步,0.3-0.8mmol的钒源溶于25mL去离子水中,搅拌15-25min,得到的橙黄色溶液;
第三步,将第二步配制的橙黄色溶液缓慢滴入到第一步得到的无色溶液中,用盐酸调pH=2.5-5.0,并继续搅拌8-15min得到棕色悬浊液;
第四步,将第三步得到的棕色悬浊液转移到聚四氟乙烯内衬高压反应釜中,然后把反应釜放入鼓风干燥箱中170-200℃下反应20-30h;
第五步,将产品离心、洗涤,然后在真空干燥箱中65-75℃干燥18-24h,得到棕色的棒状偏钒酸锰Mn(VO3)2粉末。
2.如权利要求1所述的棒状偏钒酸锰粉末的制备方法,其特征在于,所述的步骤二中的钒源为K2(H2O)10H2V10O28·4H2O。
3. 如权利要求1所述的棒状偏钒酸锰粉末的制备方法,其特征在于,所述第五步中的洗涤是指将冷却后的产物用去离子水和无水乙醇各洗涤3 次。
4.如权利要求1所述的棒状偏钒酸锰粉末的制备方法,其特征在于,该方法制备的棒状偏钒酸锰粉末作为催化剂,可以在紫外光下高效地降解罗丹明B和亚甲基蓝。
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