萃取剂对不溶性硫制备的影响及工艺条件优化

摘要

以升华硫为原料采用熔融法制备了不溶性硫(IS),考察了不同萃取剂对IS的萃取效果并与CS2的萃取效果进行了比较,同时,以硬脂酸钙为稳定剂优化了IS的聚合条件,比较了不同急冷方式对IS收率的影响.实验结果表明,环己烷为萃取剂可得到与CS2接近的萃取效果.以硬脂酸钙为稳定剂时适宜的聚合条件为:聚合温度250℃,聚合时间60 min,硬脂酸钙用量为0.2％(w),稳定剂在体系中的停留时间60 min,在此条件下可得到最高IS收率为37％.高距离垂撒的急冷方式可以提高IS的收率.%The insoluble sulfur(IS) was prepared by rapid cooling of sulfur melts using sublimed sulfur as raw material.The effects of different extraction agents on the extraction efficiency of IS were investigated and compared with the extraction effect of CS2.Meanwhile,the polymerization conditions of IS were optimized with calcium stearate as stabilizer,and the effects of different quenching methods on IS yield were compared.The results showed that,when cyclohexane was used as the extraction agent,the extraction efficiency was close to that of CS2 under the optimum extraction conditions.The optimum conditions were as follows:polymerization temperature 250 ℃,polymerization time 60 min,the amount of calcium stearate stabilizer 0.2％(w) and the residence time of the stabilizer in the reaction system 60 min.Under these conditions,the highest yield of IS is 37％.The results of the quenching method showed that the high-range dispersion could obviously improve the yield of IS.