甲醇羰基化催化剂的合成、表征及溶解性研究

SYNTHESIS, CHARACTERIZATION AND SOLUBILITY OF METHANOL CARBONYLATION CATALYST Cu(OCH_3)Cl

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。

Cupric methoxychloride is synthesized by CuCl, CH_3OH and air at ambient condition, and the conversion of CuCl is 945% at 55*#℃, reaction time is 8h and W_ MeOH∶[WTB1X]W_ CuCl=40∶1 The solubility of cupric methoxychloride is 123% at 18*#℃ in HCl/CH_3OH solution, in which the concentration of HCl is 53% The cupric methoxychloride was characterized by FTIR, TGA and XRD IR spectrum show that the bands at 2*#936*#cm -1 and 2*#826*#cm -1 could be assigned to the vibration of OCH_3 and CH_3 in the CuOCH_3Cl molecule, and the bands at 517*#cm -1 and 465*#cm -1 could be assigned to the CuO vibration XRD result show that CuOCH_3Cl has three strong bands at 2θ=119°, 286° and 475° respectively, although CuCl has the same bands at 286° and 475° The product CuOCH_3Cl will decompose above 180*#℃ with the loss ratio of weight 175%, which is quite in agreement with the result of calculation of formula 177%