多组分一锅法合成抗氧剂3052

Synthesis of Antioxidant 3052 by Multi-component One-pot Reaction

为开发丙烯酸4-甲基-2-叔丁基-6-(4-甲基-3-叔丁基-2-羟基苯甲基)苯酯(抗氧剂3052)的合成新路线,通过以固体光气(双(三氯甲基)碳酸酯(BTC))为绿色酰氯化试剂,双酚A2246、丙烯酸为原料,滴加酰氯化试剂用一锅法合成了抗氧剂3052。设计正交试验,考察了熟化温度、物料摩尔比、加料方式、熟化时间对目标产物抗氧剂3052的影响。确立了优化工艺条件为:反应熟化温度40℃,物料比1:1.30,滴加方式为半交替,熟化时间60 min。并对优化工艺条件进行了放大中试实验,结果表明:目标产物的产率可达75%,纯度达98%。对目标产物在ABS树脂生产中进行应用评价,可以显著提升产品的耐黄变性能。

In order to develop a new route to prepare antioxidant 4-methyl-2-tert-butyl-6-(4-methyl-3-tert-butyl-2-hydroxyphenyl)phenyl acrylate(antioxidant 3052)synthesized by using solid phosgene(bis(trichloromethyl)carbonate BTC)as green acyl chlorination reagent,bisphenol A2246 and acrylic acid as substrates through drop-adding acyl chlorination reagent and one-pot method.To investigate the effects of curing temperature,molar ratio of materials,feeding method and curing time on the target product antioxidant 3052,orthogonal test is designed.Establishing the optimum reaction conditions as follows:reaction curing temperature(40℃),material ratio(1:1.30),dripping mode(semi-alternate),curing time(60 min).The pilot experiment showed that the yield and purity of the target product can reach 75%and 98%respectively.Applying the target product into the production of ABS resin can significantly improve the yellowing resistance.