摘要
受阻胺光稳定剂744的合成以苯甲酸甲酯和2,2,6,6-四甲基-4-哌啶醇为原料,在催化剂钛酸四异丙酯作用下,以石油醚(120℃～140℃)为溶剂进行酯交换反应后,用甲醇水溶液结晶,过滤、干燥而得。通过正交实验取得较佳的合成条件:反应时间为9 h,催化剂用量为2,2,6,6-四甲基-4-哌啶醇质量的10%,n(苯甲酸甲酯):n(2,2,6,6-四甲基-4-哌啶醇)=1.1:1,合成收率为96.5%(以2,2,6,6-四甲基-4-哌啶醇计)。结晶溶剂为30%(v/v)甲醇水溶液,用量为初产物质量的3倍,结晶的最终温度为20℃,结晶收率为96.0%。在此条件下合成的产品质量符合标准,总收率为92.7%。
The hindered amine light stabilizer（HALS） 744 was synthesized with methyl benzoate and 2,2,6, 6-tetramethyl-4-piperidinol with tetraisopropyl titanate as catalyst, petroleum ether（ 120 ~C-140 ~C） as solvent, via the crystallization in solution with methanol（30%）, filtration and desiccation. The optimum reaction condition were found as follow： reaction time 9 h,mole ratio of 2,2,6,6-tetramethyl-4-piperidinol to methyl benzoate 1.1：1 and tetraisopropyl titanate dosage 10% of the mass of 2,2,6,6-tetramethyl-4-piperidinol. The yield was 96.5%. The crystallization solvent （30%v/v） was 3 times the mass of early product. The final crystallization temperature was 20 ~C. The yield of crystallization was 96.0%. Under the optimum condition the total yield of HALS744 was up to 92.7%. The quality of HALS744 conforms standards.
出处
《浙江化工》
CAS
2011年第5期15-17,共3页
Zhejiang Chemical Industry
