不溶性硫磺的制备及热稳定性研究
发布时间:2018-02-15 08:54
本文关键词: 硫磺 不溶性硫磺 低温熔融法 热稳定性 出处:《华东理工大学》2015年硕士论文 论文类型:学位论文
【摘要】:本论文对国内外不溶性硫磺的研究进展进行了比较详细的综述。以工业硫磺为原料,采用低温熔融法工艺制备不溶性硫磺。通过正交实验设计考察工艺条件对硫磺聚合转化的影响,综合考虑硫磺聚合转化率、产品的热稳定性、萃取效果,不溶性硫磺制备工艺条件为:聚合温度280℃,聚合时间20min,升温速率4℃/min,淬冷液用室温下的去离子水,其用量与原料硫磺的质量比为10:1,固化温度60℃,固化时间2h,在淬冷液中添加0.6%的乙二醇作稳定剂,产品精制采用四氢萘作萃取剂,萃取温度70℃,剂硫比按7:1分两次萃取,每次萃取10min,由此硫磺聚合所得产品中不溶性硫磺的含量达43%左右,精制后产品纯度可达96%左右。萃取和充油过程稳定剂的加入均可显著提高产品热稳定性,但充油过程稳定剂的加入效果更好。萃取和充油阶段同时添加稳定剂能进一步提高产品的稳定性,当两阶段同时加入2%的酯类稳定剂C时效果最好,产品的热稳定性可达到50.45%。无论硫磺聚合转化率还是不溶性硫磺产品热稳定性均达到同类工艺的领先水平。
[Abstract]:In this paper, the research progress of insoluble sulfur at home and abroad is reviewed in detail. The insoluble sulfur was prepared by low temperature melting process. The effects of the process conditions on the conversion of sulfur polymerization were investigated by orthogonal experimental design. The conversion of sulfur polymerization, the thermal stability of the product and the extraction effect were considered synthetically. The preparation conditions of insoluble sulfur are as follows: polymerization temperature 280 鈩,
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