非均相催化剂羰基合成醋酐工艺研究

Process of No-Homogeneous Catalyst Carbonylation Synthesizing for Acetic Anhydride

以醋酸甲酯、甲醇和一氧化碳为原料，选用铑系催化剂，碘甲烷、醋酸锂为助催化剂，选用高压釜，非均相羰基合成醋酐，为进一步研究中试放大，对羰基合成小试工艺进行研究。对小试提供的最佳工艺条件进行研究考核，结果表明：在温度190～200℃下，压力5～5．5 MPa，催化剂质量分数20％～25％，碘甲烷浓度3mol／L，醋酸锂浓度1mol／L，反应时间80-100min的工艺条件下，按醋酐选择性为96％，CO转化率为97％，羰基产物醋酐收率为94％，醋酐的时空收率为460molAc_2O／（molRh·h）。此工艺数据的可以指导中试放大，并为工业化生产提供基础数据。

The small - scaletest of no - homogeneous carbonyl synthesis was made of acetic anhydride, for which methyl acetate, methanol and carbon monoxide were selected as feed stock, and choosing autoclave, rhodium as a main catalyst and methyl iodide and lithium acetace as promoter. A pilot plant was built to examine and qualify for the optimum technological conditions which were provided by the small -scale test. The results showed that under the reaction conditions of 190 ～ 200 ℃, pressure 5 - 5.5 MPa, catalyst mass fraction 20% - 25% , methyl liodide 3 mol/L and lithium acetace 1 mol/L and residence time 80 ～ 100 min, the selectivity of acetic anhydride was 96%, the conversion rate of CO was 97% and the acetic anhydride product yield was 94%, the space - time yield of acetic anhydride was 460 mol Ac20/（molRh· h）. The parameters of such process can preliminary guide the pilot and provide the basic data for industrialization.