不溶性硫黄的制备技术

以普通硫黄为原料,考察了低温熔融法工艺条件、稳定剂的加入、填充油和萃取剂的选择对不溶性硫黄(IS)含量、收率及产品稳定性的影响.结果表明,适宜的聚合工艺条件为:聚合温度为260℃,聚合时间为1h,室温去离子水作为淬冷液,固化温度为60℃,固化时间为4h,硫黄聚合转化为IS可达40%以上;聚合产品的固化过程、提高萃取温度以及在淬冷、萃取、充油过程中稳定剂的加入能较显著提高产品的稳定性;溶剂SL可以替代二硫化碳成为新的萃取剂并确定了其相应的萃取工艺条件.确定了淬冷液、萃取剂、填充油中适宜的稳定剂及其添加量,最终IS产品120℃、15min时的热稳定性达到49%以上,居同类工艺领先水平.

Preparation of insoluble sulfur

Low temperature melting method was used to produce insoluble sulfur (IS) from normal sulfur. The effects of polymerization conditions,addition of stabilizer,selections of treatment oil and extractant on content and yield of IS and on high temperature stability were studied. The proper polymerization conditions were:reaction temperature 260℃,reaction time 1h,deionized water at room temperature as quenching solvent,solidifying temperature 60℃,solidifying time 4h. In this case,IS content in polymerization product reached more than 40%. Solidification of polymerization product,higher extraction temperature,oil-treatment,and addition of stabilizer in the quenching and oil-treating processes were beneficial to improving stability of the products. Stabilizers added to quenching solvent,extractant and treatment oil and their addition amounts were determined respectively. As a result,high temperature stability of IS product at 120℃ was more than 49%,at domestic leading level in the same processes.