季戊四醇硬脂酸酯的合成与提纯

Synthesis and Purification of Pentaerythritol stearate

以对甲苯磺酸(TsOH)为催化剂,季戊四醇和硬脂酸为反应物催化合成了季戊四醇硬脂酸酯.通过单因子法研究产物的合成与提纯工艺条件;采用FTIR表征产物的结构,并检测产物的部分理化性能.结果表明:TsOH对产物合成具有良好的催化活性,优化合成条件下:催化剂TsOH 1.0 g(相对0.01 mol季戊四醇)、酸醇物质的量比4.3:1、带水剂甲苯20 mL、反应时间90 min,酯化率可达96.5%;优化提纯条件下:25 mL丙酮(相对粗产物2.5 g)、加热回流30 min,产率可达80.4%以上;经提纯产物的酸值、熔点和皂化值分别为0.4 mg KOH/g、66℃和186.1 mg KOH/g.

With p-toluenesulfonic acid（ TsOH） as the catalyst,pentaerythritol stearate was synthesized by esterification of pentaerythritol and stearic acid. The process conditions to synthesize and purify the esterification product were optimized by single factor method. The chemical structure of the esterification product was confirmed by FTIR,and some of its physicochemical properties were determined through China＇s National Standards. The experimental results showed that TsOH has excellent catalytic activity for the synthesis of pentaerythritol stearate with esterification rate of 96. 5% under the optimized synthesis conditions： catalyst dosage（ TsOH） of 1. 0 g（ based on pentaerythritol of 0.01 mol）,mole ratio of stearic acid to pentaerythritol of 4. 3∶ 1,water entrainer（ toluene） of 20 mL and refluxing time of 90 min. The yield of purified product can reach more than 80. 4%under the optimized purification conditions： acetone of 25 mL（ based on initial product of 2. 5 g）,refluxing time of 30 min; and the acid value, melting point and saponification value of the purified products were0. 4 mg KOH /g,66℃ and 186. 1 mg KOH /g,respectively.