利用副产甲基硫酸钠合成苯甲醚的方法

Synthesis of anisole from phenol and sodium methyl sulfate,a byproduct from synthesis of medicine intermediates

以苯酚和甲基硫酸钠废渣为原料,在氢氧化钠条件下,以水为溶剂,常压下进行连续蒸馏回流反应合成苯甲醚。考察了反应温度、原料摩尔比、回流时间、氢氧化钠含量、回流方式等条件对反应的影响。实验结果表明,在氢氧化钠含量20%(w),苯酚、氢氧化钠、甲基硫酸钠的摩尔比为1.0∶1.2∶1.3,反应温度(105±5)℃的条件下,采用连续蒸馏回流方式回流反应6 h,苯酚转化率为98.98%,苯甲醚收率95.54%;反应后的无机相加入50%(φ)的甲醇进行析晶,得到无水硫酸钠产品,硫酸钠的析晶率达94.06%,硫酸钠含量为99.80%(w)。

Anisole was synthesized from phenol and sodium methyl sulfate, a byproduct from the synthesis of medicine intermediates, through continuous distillation and refluxing under normal pressure in the presence of sodium hydrate with water as solvent. The effects of reaction temperature, molar ratio of raw materials, sodium hydrate dosage, refluxing time and refluxing modes on the synthesis were investigated. It was showed that, under the optimal conditions of n（phenol） ： n（ sodium hydroxide） ： n（sodium methyl sulfate） 1.0 ： 1.2 ： 1.3, continuous distillation and refluxing for 6 h, sodium hydrate concentration 20%（w） and temperature 105 ± 5 ℃, the conversion of phenol and the yield of anisole were 98.98% and 95.54%, respectively. After the reaction, the sodium sulfate was separated by adding 50%（φ） methanol to the inorganic phase and crystallization. And the crystallization rate of sodium sulfate and its content in the crystal reached 94.06% and 99.80%（w）, respectively.