【作者】 侯文杰；

【导师】 欧阳福生；

【作者基本信息】 华东理工大学 ， 化学工艺， 2012， 硕士

【摘要】 本论文对不溶性硫磺的发展前景及其生产技术进行了较全面的综述。考察了低温熔融法制备不溶性硫磺的反应条件以及引发剂和稳定剂的加入对硫磺聚合转化率的影响。结果表明,低温熔融法聚合工艺的适宜反应温度为260℃、反应时间为60min；引发剂的加入可以提高不溶性硫磺收率,适宜的引发剂为Na2S2O8/FeCl2组成的复合引发剂,其用量为0.5%,最佳配比为4：1；聚合过程中的适宜稳定剂为KI,其用量为0.2%,制得的IS收率可达44.54%。通过不同溶剂对普通硫磺溶解度的考察,筛选出由四氯乙烯和1,1,1-三氯乙烷按1：1体积比组成的混合溶剂作为萃取剂能取得较为理想的萃取效果。其适宜的萃取条件为：萃取时间15min,萃取温度55℃,剂硫比12：1。与CS2相比,该萃取剂毒性小、安全性高,有望成为不溶性硫磺新型萃取剂。考察了不溶性硫磺填充油的种类以及充油稳定剂SN-1和SN-2对热稳定率的影响,结果表明环烷基橡胶油的效果最好,当稳定剂的添加量分别为0.1%和0.08%时,不溶性硫磺的热稳定率均可达90%以上,达到了HG/T2525-93的要求。更多还原

【Abstract】 This paper gave a relatively comprehensive review in technical progress and development prospects of insoluble sulfur (IS). Based on the low temperature molten method for insoluble sulfur production, effects of polymerization conditions, initiators, stabilizers on IS yield were investigated. The results show that the suitable conditions for sulfur polymerization are at reaction temperature 260℃, reaction time 60min. Addition of initiator into polymerization system can increase IS yield in product and the proper initiator added into polymerization system is Na2S2O8/FeCl2 (mass ratio 4:1 and 0.5m%). The appropriate stabilizer added in the system is KI (0.2%). In this case, IS content in polymerization product can reach 44.54%. Based on measuring solubility of a few solvents, the mixture with tetrachloroethylene and 1,1,1-trichloroethane (1:1 volume ratio) was screen out as extractan for IS and have both good solvency and extraction effect for sulfur. The proper extraction conditions are at 55℃of temperature,15min of extraction time,12:1 of solvent ratio. Compared with CS2, the extractant has low toxicity and simple recovery method. Therefore it is hopeful to replace carbon disulfur. Effct of different treating oils and SN-1, SN-2 stabilizers for IS on thermal stability of IS product was investigated. The results show that naphthenic rubber oil is the best choice. The thermal stability can reach more than 90% and can fully meet the requirements of HG/T2525-93 when SN-1, SN-2 are added in the IS product by 0.1% and 0.08% respectively during treating oil for IS product.更多还原