四甘醇二甲醚提纯三甲基镓的研究

Study on purification of trimethylgallium by using tetraethylene glycol dimethyl ether

采用加合物提纯法(又称配合物提纯法)提纯三甲基镓(TMG),筛选出四甘醇二甲醚(TGDE)作为加和物,得到最佳的加合物配比和解配条件。结果表明,TMG·TGDE加合物中TMG与TGDE的最佳物质的量比为1∶0.2,且在解配条件t=120℃、p=10kPa时,解配产率y高达94%,产品TMG纯度可达6N。通过质谱、红外、元素分析方法表征了不同物质的量比的TMG·TGDE加合物,提出了加合反应与解配反应的机理。

The adduct purification method(complex purification method) has been used to purify trimethylgallium(TMG).Tetraethylene glycol dimethyl ether(TGDE) was chosen to form adducts with TMG.Two-step experiments varying the TMG to TGDE ratios have been performed in order to determine the optimal purification conditions.The results showed that when the ratio of TMG to TGDE in the adduct was 1∶ 0.2,the decomposition temperature was 120 ℃ and the decomposition pressure was 10 kPa,the highest yield of TMG(94%) was obtained with a purity of 6N(99.9999%).Mass spectrometry,Fourier transform infrared spectroscopy,and elemental analysis were used to characterize the TMG·TGDE adducts with different molar ratios.Reaction mechanisms for the synthesis and decomposition of the adducts have also been proposed.