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作 者:袁国卿[1] 钱庆利[1] 闫芳[1] 邵守言[2] 凌晨[2] 曹宏兵[2]
机构地区:[1]中国科学院化学研究所,北京100080 [2]江苏索普(集团)有限公司,江苏镇江212006
出 处:《精细化工原料及中间体》2010年第1期5-7,共3页Fine Chemical Industrial Raw Materials & Intermediates
摘 要:甲醇羰基化反应制醋酸,是一个重要的化学反应[1],无论在实验室或在工业生产上,其反应过程的监测均是以色谱为分析手段[2,3]。由于该反应产物的组分多(甲醇、水、碘甲烷、乙酸甲酯、醋酸),通常采用色谱程序升温的方法才可达到各组分的分离[4],这种方法由于存在分析周期长和由于反应物在色谱柱中的保留时间长而发生变化影响了定量的准确性的缺点,给对该反应进行的快速、准确的监测带来诸多不便。The porous polymer beads of styrene divinylbenzene copolymer (GDX203) were nitrated by different proportion of HNO3 (65%)-H2SO4 (98% ) mixture at room temperature.The nitrogen content and nitro-group were confirmed with elementary analysis and IR spectrum. The modified GDX203 was used as chromatographic stationary phase for analysis of carbonylation products of methanol. The optimum gas chromatographic stationary phase was selected from modified GDX203 of different nitrogenous contents. The results showed that by using a modified column of proper nitrogen content all components in the reaction medium were separated at constant chromatographic temperature. Especially CH3COOCH3 and CH3I can be separated completely. The gas chromatographic analysis of five components was accomplished in 6 minutes.
关 键 词:GDX203 NITRATION Gas CHROMATOGRAPHIC STATIONARY phase METHANOL CARBONYLATION
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