论文部分内容阅读
用CuCl、甲醇和空气为原料 ,合成了甲醇氧化羰基化反应催化剂甲氧基氯化铜 ,最佳的合成条件是 :5 5℃、8h、CuCl与甲醇的比为 1∶40 (重量比 ) ,甲氧基氯化铜的产率为 94 5 %。对甲氧基氯化铜的溶解性进行了讨论 ,18℃时 ,甲氧基氯化铜在 5 3%的氯化氢甲醇溶液中的溶解度为 12 3%。用IR、TGA和XRD对所合成的甲氧基氯化铜进行了表征 ,在IR图谱中发现了官能团 OCH3 , CH3 的特征吸收峰 ,证明所合成的产物为甲氧基氯化铜。XRD谱显示三个强峰 ,分别位于 2θ =11 9° ,2 8 6° ,47 5°处。根据TGA分析得知该化合物在高于 180℃时会分解 ,其失重率为17 5 % ,与理论值 17 7%相当。
The optimum conditions for the oxidative carbonylation of methanol with CuCl, methanol and air were as follows: the molar ratio of CuCl to methanol was 1:40 (weight ratio) at 5 5 ℃ for 8h, , The yield of methoxy cupric chloride was 94 5%. The solubility of methoxy cupric chloride is discussed. At 18 ° C, the solubility of methoxy cupric chloride in a 5 3% solution of hydrogen chloride in methanol is 123%. The synthesized methoxy cupric chloride was characterized by IR, TGA and XRD. The characteristic absorption peaks of OCH3 and CH3 were found in the IR spectrum, which proved that the synthesized product was methoxy cupric chloride. XRD spectra showed three strong peaks at 2θ = 11 9 °, 2 8 6 °, 47 5 °, respectively. According to TGA analysis, the compound decomposes above 180 ° C and has a weight loss rate of 17.5%, which is comparable to the theoretical value of 17.7%.