研究了以3,5-二叔丁基-4-羟基-苯甲酸和2,4-二叔丁基苯酚为原料,SOCl2为酰化试剂,一锅法合成光稳定剂3,5-二叔丁基-4-羟基-苯甲酸-2,4-二叔丁基苯基酯的工艺.通过实验考察了投料比、温度及酰化试剂用量对反应的影响,确定了较佳的工艺条...研究了以3,5-二叔丁基-4-羟基-苯甲酸和2,4-二叔丁基苯酚为原料,SOCl2为酰化试剂,一锅法合成光稳定剂3,5-二叔丁基-4-羟基-苯甲酸-2,4-二叔丁基苯基酯的工艺.通过实验考察了投料比、温度及酰化试剂用量对反应的影响,确定了较佳的工艺条件:3,5-二叔丁基-4-羟基-苯甲酸与2,4-二叔丁基苯酚的物质的量比为1∶1.1;酰化剂SOCl2与3,5-二叔丁基-4-羟基-苯甲酸的物质的量比为1.2∶1;反应温度为70℃;反应时间为11 h.还考察了结晶溶剂的种类、用量和温度对产品质量和收率的影响,得到了较佳的结晶工艺条件:V(正丁醇)/m(初产物)为1.4 m L/g;结晶温度为25℃.产品总收率可达83.0%.展开更多
以联苯为原料,经傅克酰化、溴代、格氏和氧化反应,制备了4-(4-乙酰基苯基)苯甲酸;以苯甲醚为原料经傅克酰化,醚解制备了4-乙酰基苯酚;两者再经酯化、还原、脱水反应,合成了一种新型的双官能团聚合物材料单体4-(4-乙烯基)苯基苯甲酸-(4-...以联苯为原料,经傅克酰化、溴代、格氏和氧化反应,制备了4-(4-乙酰基苯基)苯甲酸;以苯甲醚为原料经傅克酰化,醚解制备了4-乙酰基苯酚;两者再经酯化、还原、脱水反应,合成了一种新型的双官能团聚合物材料单体4-(4-乙烯基)苯基苯甲酸-(4-乙烯基)苯酯,基于联苯的总收率为7%～10%,其结构经1 H NMR和FT-IR确认,并用偏光显微镜和差示扫描量热仪对其液晶性进行了研究。展开更多
Two kinds of organic-inorganic comp osite luminescent material were pre pared through sol-gel route,by dopi ng o-amino-benzoic acid(ABA)or N-phenylanthranilic acid(N-PA)into SiO 2 xerogels.Fluorescence properties and ...Two kinds of organic-inorganic comp osite luminescent material were pre pared through sol-gel route,by dopi ng o-amino-benzoic acid(ABA)or N-phenylanthranilic acid(N-PA)into SiO 2 xerogels.Fluorescence properties and thermal properties of ABA and N-PA in SiO 2 xerogels were studied.The relation ship between the fluorescence properties and the preparative cond ition was also studied.The results s howed that the ABA was easy to form dim er of non-luminescence among the molec ules.The quenching concentration o f the ABA was obviously increased owi ng to the shield of silica network.The f luorescence intensity of the composite material prepared at the acid con dition was decreased,and a red shift for the fluorescence peak appeared.With th e increasing of the pH value,the flu-orescence peak blue shifted and the i ntensity was increased.However,th e fluorescent intensity of N-PA /SiO 2 was increasing due to the concentration of N-PA was increased.The thermal stability of ABA and N-PA in the composite material was also improved.But,when the temperature continued to incre ase,the collapse of the silica netwo rk made the organic molecules escape fr om the pore of the silica network,the decomposition of escaping molecule s decreased the intensity of emission spectrum.展开更多
文摘研究了以3,5-二叔丁基-4-羟基-苯甲酸和2,4-二叔丁基苯酚为原料,SOCl2为酰化试剂,一锅法合成光稳定剂3,5-二叔丁基-4-羟基-苯甲酸-2,4-二叔丁基苯基酯的工艺.通过实验考察了投料比、温度及酰化试剂用量对反应的影响,确定了较佳的工艺条件:3,5-二叔丁基-4-羟基-苯甲酸与2,4-二叔丁基苯酚的物质的量比为1∶1.1;酰化剂SOCl2与3,5-二叔丁基-4-羟基-苯甲酸的物质的量比为1.2∶1;反应温度为70℃;反应时间为11 h.还考察了结晶溶剂的种类、用量和温度对产品质量和收率的影响,得到了较佳的结晶工艺条件:V(正丁醇)/m(初产物)为1.4 m L/g;结晶温度为25℃.产品总收率可达83.0%.
文摘以联苯为原料,经傅克酰化、溴代、格氏和氧化反应,制备了4-(4-乙酰基苯基)苯甲酸;以苯甲醚为原料经傅克酰化,醚解制备了4-乙酰基苯酚;两者再经酯化、还原、脱水反应,合成了一种新型的双官能团聚合物材料单体4-(4-乙烯基)苯基苯甲酸-(4-乙烯基)苯酯,基于联苯的总收率为7%～10%,其结构经1 H NMR和FT-IR确认,并用偏光显微镜和差示扫描量热仪对其液晶性进行了研究。
文摘Two kinds of organic-inorganic comp osite luminescent material were pre pared through sol-gel route,by dopi ng o-amino-benzoic acid(ABA)or N-phenylanthranilic acid(N-PA)into SiO 2 xerogels.Fluorescence properties and thermal properties of ABA and N-PA in SiO 2 xerogels were studied.The relation ship between the fluorescence properties and the preparative cond ition was also studied.The results s howed that the ABA was easy to form dim er of non-luminescence among the molec ules.The quenching concentration o f the ABA was obviously increased owi ng to the shield of silica network.The f luorescence intensity of the composite material prepared at the acid con dition was decreased,and a red shift for the fluorescence peak appeared.With th e increasing of the pH value,the flu-orescence peak blue shifted and the i ntensity was increased.However,th e fluorescent intensity of N-PA /SiO 2 was increasing due to the concentration of N-PA was increased.The thermal stability of ABA and N-PA in the composite material was also improved.But,when the temperature continued to incre ase,the collapse of the silica netwo rk made the organic molecules escape fr om the pore of the silica network,the decomposition of escaping molecule s decreased the intensity of emission spectrum.
