3-甲基-2-噻唑硫酮合成及性质

Synthesis and Properties of 3-Methylthiazolidine-2-Thione

本研究首先采用一步法合成出了3-甲基-2-噻唑硫酮(MTT),通过FT-IR、TG-DTA、1HNMR、HPLC-MS对其进行检测和表征,揭示了MTT的微观结构和内在规律性。FT-IR揭示了MTT分子内部各元素之间的化学键键型。TG-DTA表明MTT的相变温度、分解温度分别为76.3、309.8℃,MTT的分解温度偏高。1HNMR从化学位移角度,揭示了MTT分子中,氢质子的数目及其在碳链上的位置,氢原子数目为7,和其分子式C4H7NS2相吻合。HPLC-MS分析确定了MTT分子量为133,与C4H7NS2化学计算的分子量相同。该研究为企业MTT工业化生产进行跟踪检测,评判MTT的产品性能指标,提供了基础实验数据。

In the study, rubber accelerator 3-methylthiazolidine-2-thione （MTT） was synthesized by one-step method firstly. MTT was detected and characterized by FT-IR, TG-DTA,1HNMR, HPLC-MS. The micro-structure and intrinsic regularity were revealed. Chemical bond types into MTT molecule were revealed by FT-IR. MTT phase composition and structure were given by crystallographic data from XRD detecting such as cell parameters, crystal face index. The phase composition and qualitative identification of MTT structure were completed. Two kinds of information were detected by TG-DTA as quality change and thermal effect. MTT phase transition and decomposition temperature were 76.3, 306.9℃ respectively. The decomposition temperature of MTT was very high. Hydrogen protons in the MTT molecule and its position on the carbon chain were revealed by 1HNMR from the chemical displacement angle. The number of hydrogen atoms is 7, consistent with its molecular CaHTNS2. MTT analysis by liquid chromatography mass spectrometry （HPLC-MS） confirmed that the molecular weight of MTT was 133, which was the same as chemical calculation of C4H7NS2. This study can provide the basis experimental data on the enterprises to designate the working standard tracing detection of MTT industrialized production. Performance index of MTT was judged.