新型橡胶氯化剂的合成与表征  

Synthesis and characterization of a novel chlorinating agent used in unsaturated rubber

作　　者：李艳丽[1] 石淑先[1] 夏宇正[1] 焦书科[1] 

机构地区：[1]北京化工大学材料科学与工程学院,北京100029

出　　处：《北京化工大学学报（自然科学版）》2004年第4期45-49,共5页Journal of Beijing University of Chemical Technology(Natural Science Edition)

基　　金：中国石油化工股份有限公司资助课题 (X0 5 0 999)

摘　　要：文中以次氯酸钠、叔丁醇和冰醋酸为原料制备次氯酸叔丁酯 ,考查了反应温度、反应物配比、投料方式、反应时间对产物的收率及纯度的影响 ;产物放置时间对其储存稳定性的影响 ;并用色谱 -质谱对其纯度、杂质含量及产物结构进行了表征。结果表明 ,次氯酸叔丁酯合成最佳工艺条件为 :次氯酸钠与冰醋酸摩尔比 1∶1 ,次氯酸钠与叔丁醇摩尔比 1 4∶1 ,叔丁醇和冰醋酸一次性投料 ,反应温度 0℃ ,反应 3min ,产物收率达 72 2 % ,纯度达 92 %。产物纯度随存放时间的延长下降 ,杂质叔丁醇含量增加。将次氯酸叔丁酯用于镍系顺丁橡胶的氯化 ,1 H NMR和FTIR结果表明 ,此氯化反应系加成反应 。T butyl hypochlorite is a chlorination agent used in unsaturated rubber. The synthesis of t butyl hypochlorite with sodium hypochlorite and t butanol in the presence of glacial acetic acid were studied in detail. The effects of reaction temperature, ratio of reagents and addition pattern on purity and yield of t butyl hypochlorite were investigated and the optimum technical condition was confirmed. The reaction system of t butyl hypochlorite were characterized by gas chromatogram mass spectrum. The results show that the content of t butyl hypochlorite is decrease and the content of impurity of tert butanol is increase with the time of storage. Studies on the chlorination reaction of the agent with nickel polybutadiene were also carried out. It can be confirmed that the reaction is an addition reaction, and the chlorinated polybutadiene was synthesized.

关 键 词：橡胶氯化试剂 次氯酸叔丁酯 氯化顺丁橡胶 

分 类 号：O623.12[理学—有机化学]