高纯度甲缩醛的制备方法研究

Preparation Methods of methylal with High Purity

摘要:

采用实验室常用仪器搭建的反应精馏装置，在硫酸催化甲醇与多聚甲醛制备甲缩醛的过程中，考查了原料配比、加热温度、催化剂用量、反应时间等对甲醇转化率、甲醇选择性及制备出甲缩醛的纯度的影响，并通过正交实验得出了最优甲缩醛制备条件：n（甲醇）：n（多聚甲醛）=1.9，加热温度为70℃，反应时间为2.75h，催化剂加入体积为甲醇体积的3.5%时，甲醇转化率达99.32%，甲醇的选择性99.88%，所制得甲缩醛的纯度为96.88%，甲醇含量为3.11%，含水量小于0.01%。

Abstract:

Effects of material ratio, heating temperature, dosage of catalyst and reaction time on the conversation rate of methanol ,selectivity of methanol and purification of methylal were investigated in the process of preparing methylal with methanol , paraformaldehyde as materials and sulfuric acid as catalyst. The optimal preparation conditions were obtained by orthogonal experiment with results as follows: n(methanol):n(paraformaldehyde)=1.9, heating temperature 70℃, reaction time 2.75h, v(sulfuric acid):v(methanol) =3.5:100 and conversation rate 99.32%, selectivity of methanol 99.88%, mass fraction of methylal is 96.88%(content of methanol 3.11%, content of water less than 0.01% ).