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在高压反应釜中考察了操作方式、催化剂配比及用量、溶剂用量、反应压力、反应温度及添加水对Co-Mn-Br液相催化氧化β-甲基萘制β-萘甲酸反应的影响。结果表明,恒压操作方式优于分步恒压操作方式。甲基萘催化氧化体系存在明显的诱导期,时间长短与催化剂组成和反应条件有关。催化剂中Co、Br的量多时氧化反应快,但Br的量增多导致产物颜色加深。水对氧化反应有抑制作用,添加水量达到7%时严重阻止了氧化反应的进行。采用Co-Mn-Br原子比为1∶1∶2的催化剂和恒压操作方式,较适宜的工艺反应参数为催化剂用量1%,120℃,0.6MPa。在此条件下,β-萘甲酸收率达93.7%。
The effects of operating mode, catalyst ratio and amount, solvent amount, reaction pressure, reaction temperature and addition of water on the reaction of β-methyl naphthalene β-naphthoic acid catalyzed by Co-Mn-Br in liquid phase were investigated in high pressure reactor . The results show that the constant pressure operation method is better than the stepwise constant pressure operation method. Methylnaphthalene catalytic oxidation system there is a clear induction period, the length of time and catalyst composition and reaction conditions. When the amount of Co and Br in the catalyst is large, the oxidation reaction is quick, but the amount of Br increases and the color of the product is deepened. Water has an inhibitory effect on the oxidation reaction. When the amount of water added reaches 7%, the oxidation reaction is seriously prevented. The optimum reaction parameters were 1% of catalyst, 120 ℃ and 0.6MPa, using the catalyst with Co-Mn-Br atomic ratio of 1: 1: 2 and constant pressure operation. Under this condition, the yield of β-naphthoic acid reached 93.7%.