两步法合成高环氧值低黏度聚丙二醇缩水甘油醚的研究

Study on synthesis of high epoxy value low viscosity polypropylene glycol glycidyl ether by two-step method

以氢氟酸为催化剂，环氧氯丙烷（ZCH）、相对分子质量为400的聚丙二醇（PPG）为基体，采用两步法合成低黏度聚丙二醇缩水甘油醚。通过对产物环氧值和产率分析，研究了开环原料配比、催化剂用量、温度、时间以及闭环原料比、温度、时间对合成的影响。实验结果表明：催化剂、原料配比、开环反应、闭环反应均对产物环氧值和产率有较大影响。最优反应条件为埘（催化剂）：m（PPG）=0．15％、m（PPG）：m（ECH）=1：2．4、开环温度60～65℃、闭环温度50～55℃，此时环氧值为3．23mmol／g，收率为95．49％，旋转黏度为36～60mPa．S。

Using hydrofluoric acid as catalyst, epichlorohydrin （ECH） and polypropylene glycol （PPG） with 400 relative molecular mass as matrixes, the polypropylene glycol glycidyl ether with low viscosity was synthesized by two-step method. By investigating the epoxy value and yield of the product, the influence of ratio of raw materials, catalyst amount, temperature and time during ring-opening reaction, as well as the ratio of raw materials, temperature and time during ring-closing reaction on synthesis was studied. The experimental results show that the catalyst, ratio of raw materials, ring-opening reaction and ring-closing reaction possess significant influence on the epoxy value and yield of the product. The optimized reaction conditions are as follows： m（catalyst）：m（PPG） is 0.15%, m（PPG）：m（ECH）=1：2.4, ring-opening temperature is 60-65℃, ring-closing temperature is 50-55℃. Under such conditions, the epoxy value is 3.23 mmol/g, the yield is 95.49%, the rotational viscosity is 36-60 mPaos.