河北大学学报(自然科学版) >

2022 , Vol. 42 >Issue 3: 265 - 272

DOI: https://doi.org/10.3969/j.issn.1000-1565.2022.03.007

季铵盐阳离子的Waugh型化合物的合成与表征

  • 刘雪梅 ,
  • 郭珂欣 ,
  • 李金环 ,
  • 李慧敏 ,
  • 胡若晖
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刘雪梅(1976—),女,陕西西安人,西安石油大学副教授,博士.主要从事杂多化合物方向的研究.
E-mail: lxm2503@163.com

收稿日期: 2021-09-21

  网络出版日期: 2022-06-16

基金资助

陕西省自然科学基础研究计划项目(2016JQ2037);国家级大学生创新创业训练计划项目(S202010705018);西安石油大学研究生创新与实践能力培养项目(YCS20211018)

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Synthesis and characterization of Waugh-type compounds containing quaternary ammonium cations

  • LIU Xuemei ,
  • GUO Kexin ,
  • LI Jinhuan ,
  • LI Huimin ,
  • HU Ruohui
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  • College of Chemistry and Chemical Engineering, Xian Shiyou University, Xian 710065, China

Received date: 2021-09-21

  Online published: 2022-06-16

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摘要

以(NH4)6［MnMo9O32］为前体原料,采用常规的水溶液法与四甲(乙)氯化铵反应制备了2种含有混合阳离子的Waugh型钼酸盐(NH4)4［N(CH3)4］2［MnMo9O32］·9H2O(化合物1)和(NH4)4［N(CH2CH3)4］2［MnMo9O32］·7H2O(化合物2),用元素分析、红外光谱、热重分析对其进行了表征,并对化合物1进行了单晶结构测定,化合物1属于单斜晶系,C2/c空间群,a=2.379(11)nm,b=1.186(5)nm,c=1.600(7)nm,β=102.308(4)°,V=4.413(3)nm3,Z=4,Dc=2.460 g/cm3,R1=0.041 8,wR2=0.117 5(I>2σ),GOF=1.058.对化合物的形成规律探索发现:季铵盐与(NH4)6MnMo9O32的物质的量之比为3∶1,易形成单晶.对化合物1和2光催化降解亚甲基蓝模拟废水进行了探索,光催化90 min和180 min时脱色率分别达到95.96%和85.64%,表明化合物1和2对亚甲基蓝染料废水均具有良好的光催化活性.

关键词： Waugh结构; 季铵盐; 晶体结构; 表征; 光催化

本文引用格式

刘雪梅 , 郭珂欣 , 李金环 , 李慧敏 , 胡若晖 . 季铵盐阳离子的Waugh型化合物的合成与表征[J]. 河北大学学报(自然科学版), 2022 , 42(3) : 265 -272 . DOI: 10.3969/j.issn.1000-1565.2022.03.007

Abstract

The new Waugh compounds(NH4)4［N(CH3)4］2［MnMo9O32］·9H2O(1)and(NH4)4［N(CH2CH3)4］2［MnMo9O32］·7H2O(2)containing quaternary ammonium cations were obtained by reacting of(NH4)6MnMo9O32 and tetramethyl ammonium chloride or tetraethyl ammonium chloride in aqueous solution, and properties were characterized by elemental analysis, IR and TG. The structure of the compound 1 was determined by single crystal X-ray diffraction. The chemical formula of the compound 1 belongs to monoclinic system with space group C2/c, a=2.379(11)nm,b=1.186(5)nm,c=1.600(7)nm,β=102.308(4)°,V=4.413(3)nm3, Z=4, Dc=2.460 g/cm3, R1=0.041 8, wR2=0.117 5(I>2σ), GOF=1.058. Exploring the formation rules of the compounds 1 and 2 revealed that the optimal ratio of the amount of［N(CH3)4］Cl or［N(C2H5)4］Cl to(NH4)6MnMo9O32·9H2O is equal to 3∶1, and that single crystals of title compounds were easily formed. Methylene blue simulated dye wastewater for photocatalytic degradation by compounds 1 and 2 was explored, the decolorization of methylene blue solutions at 90 min and 180 min reached 95.96% and 85.64%, respectively. The photocatalytic results show- DOI:10.3969/j.issn.1000-1565.2022.03.007季铵盐阳离子的Waugh型化合物的合成与表征刘雪梅,郭珂欣,李金环,李慧敏,胡若晖( 西安石油大学 化学化工学院,陕西 西安 710065)摘 要:以(NH4)6［MnMo9O32］为前体原料,采用常规的水溶液法与四甲(乙)氯化铵反应制备了2种含有混合阳离子的Waugh型钼酸盐(NH4)4［N(CH3)4］2［MnMo9O32］·9H2O(化合物1)和(NH4)4［N(CH2CH3)4］2［MnMo9O32］·7H2O(化合物2),用元素分析、红外光谱、热重分析对其进行了表征,并对化合物1进行了单晶结构测定,化合物1属于单斜晶系,C2/c空间群,a=2.379(11)nm,b=1.186(5)nm,c=1.600(7)nm,β=102.308(4)°,V=4.413(3)nm3,Z=4,Dc=2.460 g/cm3,R1=0.041 8,wR2=0.117 5(I>2σ),GOF=1.058.对化合物的形成规律探索发现:季铵盐与(NH4)6MnMo9O32的物质的量之比为3∶1,易形成单晶.对化合物1和2光催化降解亚甲基蓝模拟废水进行了探索,光催化90 min和180 min时脱色率分别达到95.96%和85.64%,表明化合物1和2对亚甲基蓝染料废水均具有良好的光催化活性.关键词:Waugh结构;季铵盐;晶体结构;表征;光催化 中图分类号:O611.2 文献标志码:A 文章编号:1000-1565(2022)03-0265-08Synthesis and characterization of Waugh-type compounds containing quaternary ammonium cationsLIU Xuemei, GUO Kexin, LI Jinhuan, LI Huimin, HU Ruohui( College of Chemistry and Chemical Engineering, Xian Shiyou University, Xian 710065, China )Abstract: The new Waugh compounds(NH4)4［N(CH3)4］2［MnMo9O32］·9H2O(1)and(NH4)4［N(CH2CH3)4］2［MnMo9O32］·7H2O(2)containing quaternary ammonium cations were obtained by reacting of(NH4)6MnMo9O32 and tetramethyl ammonium chloride or tetraethyl ammonium chloride in aqueous solution, and properties were characterized by elemental analysis, IR and TG. The structure of the compound 1 was determined by single crystal X-ray diffraction. The chemical formula of the compound 1 belongs to monoclinic system with space group C2/c, a=2.379(11)nm,b=1.186(5)nm,c=1.600(7)nm,β=102.308(4)°,V=4.413(3)nm3, Z=4, Dc=2.460 g/cm3, R1=0.041 8, wR2=0.117 5(I>2σ), GOF=1.058. Exploring the formation rules of the compounds 1 and 2 revealed that the optimal ratio of the amount of［N(CH3)4］Cl or［N(C2H5)4］Cl to(NH4)6MnMo9O32·9H2O is equal to 3∶1, and that single crystals of title compounds were easily formed. Methylene blue simulated dye wastewater for photocatalytic degradation by compounds 1 and 2 was explored, the decolorization of methylene blue solutions at 90 min and 180 min reached 95.96% and 85.64%, respectively. The photocatalytic results show- 收稿日期:2021-09-21 基金项目:陕西省自然科学基础研究计划项目(2016JQ2037);国家级大学生创新创业训练计划项目(S202010705018);西安石油大学研究生创新与实践能力培养项目(YCS20211018) 第一作者:刘雪梅(1976—),女,陕西西安人,西安石油大学副教授,博士.主要从事杂多化合物方向的研究.E-mail: lxm2503@163.com第3期刘雪梅等:季铵盐阳离子的Waugh型化合物的合成与表征that both compounds 1 and 2 have good photocatalytic activity against methylene blue simulated dye wastewater.

Key words： Waugh structure; quaternary ammonium; crystal structure; characterization; photocatalysis

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