松香树脂酸和甲醛的Prins反应研究

Study on the Prins reaction of rosin acids and paraformaldehyde

研究了以松香和多聚甲醛为原料,甲苯为溶剂进行的Prins反应(羟甲基化)。采用单因素实验和正交实验方法考察了催化剂种类、用量、反应温度和时间对羟甲基化程度的影响,以红外光谱表征了产物结构,并优化出合成羟甲基松香的最佳工艺条件:甲醛与松香物质的量比为3∶1,以对甲苯磺酸为催化剂,用量为松香质量的0.8%,反应温度为100℃,反应时间为6 h。产物的羟值(KOH)为236 mg/g,原料转化率为80.56%。

The Prins reaction（hydroxymethylation）between rosin resin acids and paraformaldehyde using methylbenzene as solvent was studied.The effects of catalyst type,amount,reaction temperature and time on the degree of hydroxymethylation were studied by single-factor experiment and orthogonal test method.The structure of the product was characterized by FTIR.The optimum synthesis conditions of hydroxymethyl rosin were as followed： molar ratio of formaldehyde to rosin 3∶1,using 0.8% p-toluenesulfonic acid（based on the mass of rosin）as catalyst,reaction temperature 100 ℃ and reaction time 6 h.The hydroxyl value（KOH） of the product was 236 mg/g and the conversion was 80.56%.