甲醇与甲醛合成乙二醇的研究

Study on Synthesis of Ethylene Glycol Using Methanol and Formaldehyde

以甲醇与甲醛为原料,选择二叔丁基过氧化物(DTBP)和过氧化二异丙苯(DCP)分别作为引发剂进行缩合反应,制得乙二醇。考察了引发剂用量、反应温度、反应时间、甲醇与甲醛质量比、引发剂加入速度对反应产物的影响,优化了合成线路,使过程简单可行,产率提高。同时对DTBP的合成进行改进,达到了降低成本,清洁生产的目的。确定了以DCP为引发剂合成乙二醇的最佳工艺条件:DCP用量2%,甲醇与甲醛质量比10:1,反应温度145℃,反应时间3 h。以DTBP为引发剂合成乙二醇的最佳工艺条件:反应温度145℃,反应时间4 h,甲醇与甲醛质量比8:1,DTBP用量2.5%,引发剂加入速度0.05 mL/min,在此条件下产物中乙二醇含量可达9.65%。

Ethylene glycol was prepared by condensation reaction using methanol and formaldehyde as raw materials and di - tert - butyl peroxide （DTBP） and dicumyl peroxide （DCP） as initiators respectively. The effects of initiator amount, reaction temperature, reaction time, mass ratio of methanol to formaldehyde, adding speed of initiator on the reaction product were investigated. The synthetic routes were optimized so that the processes were simple and feasible and rates of production were raised. At the same time, the synthesis of DTBP was modified. The producing cost was lowered and the productive process was clean. The optimal process conditions for synthesizing ethylene glycol using DCP as initiator were determined as follows： dosage of DCP was 2%, the mass ratio of methanol to formaldehyde was 10：1 ,reaction temperature was 145 ℃ and reaction time was 3 h. The optimal process condition for synthesizing ethylene glycol using DTBP as initiator was as follows： reaction temperature was 145 ℃, reaction time was 4 h, the mass ratio of methanol to formaldehyde was 8：1 ,dosage of DTBP was 2.5 %, adding speed of initiator was 0.05 mL/min. Under this condition, the ethylene glycol content in the product could reach 9.65%.