十六烷基三甲基四硫代钼酸铵的合成与表征

SYNTHESIS AND CHARACTERIZATION OF CETYLTRIMETHYLAMMIONIUM TETRATHIOMOLYBDATES

以四硫代钼酸铵(ATTM)和十六烷基三甲基溴化铵(CTABr)为原料,在水溶液中合成了十六烷基三甲基四硫代钼酸铵(CTMATTM)。采用XRD、元素分析、TG DTA、FT IR和UV Vis等手段表征了产物。结果表明,产物CTMATTM具有较好的结晶纯度,烷基的引入使Mo—S键的IR振动峰向波数较低的方向移动,TG DTA中的失重主要是由C16H33N(CH3)2的生成引起的,UV Vis发现CTMATTM中MoS42-的吸收发生蓝移。CTMATTM于N2气流中进行了分解。结果表明,CTMATTM在N2气流中热分解可以得到比表面积为254.51m2/g,孔容为0.14cm3/g,平均孔径为2.15nm的多孔MoS2固体。

A novel alkyl tetrathiomolybdate, cetyltrimethylammionium tetrathiomolybdate(CTMATTM), was synthesized in aqueous solution using ammonium tetrathiomolybdates(ATTM) and cetyltrimethyl ammonium bromide(CTABr) as reactants. The as-synthesized sample was characterized by XRD, elemental analysis, TG-DTA, FT-IR and UV-Vis techniques. The analysis results showed that the synthesized product CTMATTM had good crystallinity, the introduction of alkyls resulted in the shift of IR peak of Mo—S bond to position of the lower wavenumber. The formation of C_16H_33N(CH_3)_2 was the reason of weight loss in the TG-DTA curve. The absorbence of MoS_4~2- of CTMATTM in UV-Vis spectrum showed blue shift. Furthermore, CTMATTM was thermally decomposed under N_2 flow and the solid product MoS_2 had a surface area of 254.51 m^2/g, a pore volume of 0.14 cm^3/g and an average pore diameter of 2.15 nm, which was formed from thermal decomposition of CTMATTM.