摘要
在液相法制备不溶性硫(IS)的过程中,以无机卤化物KCl、KBr、KI作为稳定剂,采用单因素法确定了适宜的稳定剂用量、反应温度和反应时间。实验结果表明,稳定剂KCl的适宜用量为0.6%,反应时间1h,反应温度260℃,IS收率为17.09%;稳定剂KBr适宜用量为0.8%,反应时间90min,反应温度280℃,IS收率为28.5%;稳定剂KI适宜用量为0.6%,反应时间1h,反应温度240℃,IS收率为29.30%。在研究IS热稳定性的过程中,对用三种稳定剂所制备的IS进行充环烷油、脂肪烃油、芳烃油处理,比较了工艺油的品种和稳定剂的协同作用对IS的受热影响。在105℃下15min内,三种工艺油中,以IS充芳烃油的热稳定性为最高;三种稳定剂中,以KI制备的IS充油后的热稳定性最好;以KCl、KBr、KI为稳定剂所制备的IS充芳烃油的热稳定性顺序依次为76.3%、87.5%、96.0%,同时初步讨论了工艺油种类和无机卤化物对抑制IS还原的作用机理。
The insoluble sulfur （IS） was prepared by the liquid phase method with the halides KCl, KBr and KI as stabilizer, respectively. The favorable reaction conditions for IS preparation, such as the amount of stabilizer used, the reaction temperature and the reaction time, were determined by the single factor method. The experimental results show that the favorable stabilizer amount, reaction temperature and reaction time is 0.6%, 260 ℃ and 60min respectively when the KCl is used as stabilizer; is 0.8%, 280℃ and 90min with the KBr as stabilizer and is 0.6%, 240℃ and 60min with Kl as stabilizer, and under above conditions, the yields oflS are 17.09%, 28.5% and 29.3%, respectively. The thermal stabilities of the IS treated by different oils, such as the naphthenic oil, paraffinic oil and arene oil, were studied separately, and the synergistic effects of processing oil types and stabilizers on the thermal stability were compared. The results show that among the three types of processing oil mentioned above, the IS treated with arene oil has the highest thermal stability, moreover, when the same processing oil is used, the treated IS prepared with Kl as stabilizer has the highest thermal stability. After treating with the arene oil at 105℃ for 15 minutes, the thermal stabilities of IS prepared with KCl, KBr and KI separately are 76.3%, 87.5% and 96%, correspondingly. The working mechanisms of processing oil types and halide stabilizer for inhibiting IS from reversion were discussed preliminarily.
出处
《高校化学工程学报》
EI
CAS
CSCD
北大核心
2006年第3期356-361,共6页
Journal of Chemical Engineering of Chinese Universities
基金
江苏省高校自然科学基金资助(04KJB530050)。
关键词
卤化物稳定剂
不溶性硫
热稳定性
工艺油
halide stabilizer
insoluble sulfur
thermal stability
processing oil
