熔融法制取不溶性硫黄新技术研究

发布时间：2018-05-16 03:40

本文选题：不溶性硫黄 + 熔融法　；参考：《华东理工大学》2015年硕士论文

【摘要】：不溶性硫黄(简称IS)是性能优良、应用广泛的橡胶硫化剂。本论文对熔融法制取不溶性硫黄新技术进行了研究。首先考察了硫黄原料对熔融法反应合成IS的影响,结果表明：以普光气田硫黄反应合成的IS转化率为37.9%,120℃热稳定性相对较高,达13.2%。其次,对反应产物IS萃取提浓技术进行考察。采用动态平衡法测定硫黄在氯苯中的溶解度,结果表明：随着温度的升高,氯苯对硫黄的溶解能力明显提升,在80。C时氯苯对硫黄的溶解能力为17.8g/100g,超过文献[61]报道的萃取剂1,1,1-三氯乙烷/四氯乙烯混合液对硫黄的溶解能力。在上述基础上,对氯苯一级平衡萃取提高IS含量的工艺进行优化,结果表明：在萃取温度为80。C,溶剂比为10：1,萃取时间为30min的条件下,新鲜氯苯对Is的萃取率为98.10%,高于萃取剂1,1,1-三氯乙烷/四氯乙烯混合液的萃取率85.08%。经六次循环回收利用的氯苯对IS的萃取率为93.40%,略低于新鲜氯苯。氯苯的萃取效果接近二硫化碳(C82),且安全、低毒、环保。最后,对填充油的基属、充油稳定剂和充油方式进行考察优选,结果表明：以环烷基油作为填充油,以0.5%的六氯丁二烯作为稳定剂,以石油醚分散填充油对含量达97.2%、120。C热稳定性为38.1%的IS进行充油,充油IS的120℃热稳定性为43%,较充油前提高了4.9%,接近Crystex-OT20产品。
[Abstract]:Insoluble sulfur (IS) is a rubber vulcanizing agent with excellent properties and wide application.
The effect of sulfur raw materials on the synthesis of IS by melting reaction was investigated. The results showed that the conversion rate of IS was 37.9%, and the thermal stability was relatively high at 120 C, reaching 13.2%..
Secondly, the extraction concentration technology of the reaction product IS extraction was investigated. The solubility of sulfur in chlorobenzene was determined by dynamic equilibrium method. The results showed that the solubility of chlorobenzene to sulfur was obviously improved with the increase of temperature, and the solubility of chlorobenzene to sulfur was 17.8g/100g at 80.C, which was more than that of 1,1,1- three chloroethane, an extractant reported in [61]. / dissolving capacity of four chloroethylene mixture on sulphur.
On the basis of the above basis, the process of improving the content of IS by the first class equilibrium extraction of chlorobenzene was optimized. The results showed that the extraction rate of fresh chlorobenzene to Is was 98.10% under the conditions of 80.C, 10:1 and 30min, which was higher than that of the extractant 1,1,1- three chloroethane / four chloroethylene mixture. The extraction rate of 85.08%. was followed by six times. The extraction rate of chlorobenzene recycled by ring is 93.40%, slightly lower than that of fresh chlorobenzene. The extraction effect of chlorobenzene is close to carbon disulfide (C82), and is safe, low toxic and environmental friendly. IS
Finally, the base genera, oil filling stabilizers and oil filling methods were investigated and optimized. The results showed that the naphthenic oil was used as filling oil and 0.5% hexahchlorbutadiene was used as stabilizer. The oil filled oil was 97.2% and the thermal stability of 120.C was 38.1%. The thermal stability of the oil filled IS was 43%, and the oil filled oil was 43%, and the oil filled oil was 43%. The previous increase was 4.9%, close to the Crystex-OT20 product.

【学位授予单位】：华东理工大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TQ125.116

【参考文献】