季铵盐阳离子的Waugh型化合物的合成与表征  

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

作　　者：刘雪梅[1] 郭珂欣 李金环 李慧敏 胡若晖 LIU Xuemei;GUO Kexin;LI Jinhuan;LI Huimin;HU Ruohui(College of Chemistry and Chemical Engineering, Xi'an Shiyou University, Xi'an 710065, China)

机构地区：[1]西安石油大学化学化工学院,陕西西安710065

出　　处：《河北大学学报（自然科学版）》2022年第3期265-272,共8页Journal of Hebei University(Natural Science Edition)

基　　金：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)。

摘　　要：以(NH_(4))_(6)[MnMo_(9)O_(32)]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(CH_(3))_(4)]_(2)[MnMo_(9)O_(32)]·_(9)H_(2)O(化合物1)和(NH4)4[N(CH_(2)CH_(3))_(4)]_(2)[MnMo_(9)O_(32)]·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)nm^(3),Z=4,Dc=2.460 g/cm^(3),R_(1)=0.0418,wR_(2)=0.1175(I>2σ),GOF=1.058.对化合物的形成规律探索发现:季铵盐与(NH_(4))_(6)MnMo_(9)O_(32)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.The new Waugh compounds(NH_(4))_(4)[N(CH_(3))_(4)]_(2)[MnMo_(9)O_(32)]·9H_(2)O(1)and(NH4)4[N(CH_(2)CH_(3))_(4)]_(2)[MnMo_(9)O_(32)]·7H_(2)O(2)containing quaternary ammonium cations were obtained by reacting of(NH_(4))6MnMo_(9)O_(32)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/cm^(3),R1=0.0418,wR2=0.1175(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(CH_(3))_(4)]Cl or[N(C_(2)H_(5))_(4)]Cl to(NH_(4))6MnMo_(9)O_(32)·9H_(2)O 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 that both compounds 1 and 2 have good photocatalytic activity against methylene blue simulated dye wastewater.

关 键 词：WAUGH结构 季铵盐 晶体结构 表征 光催化 

分 类 号：O611.2[理学—无机化学]