双酚S合成过程脱水控制和精制工艺研究

Study on Water Removal Control in Synthesis and Purification of Bisphenol S

研究了双酚S合成过程中一套和两套分水器时不同回流脱水时间的影响,安装两套分水器能显著提高分水效率,缩短回流反应时间,提高产品粗收率。较佳条件为:492.5g苯酚、500g均三甲苯及25g 2,6-萘二磺酸混合,滴加256g浓硫酸,回流6.5h,粗收率可达99%以上,粗品中双酚S质量分数为96.69%。分别研究了双酚S精制过程中单一醇-均三甲苯和混合醇-均三甲苯体系对粗品的精制。从产品成本、收率、色度等方面综合考虑,异丙醇和异戊醇的混合醇溶剂比单一异丙醇溶剂精制效果更好。在脱色剂的选择上,糖用活性炭效果较好。单一醇-均三甲苯体系精制的较佳条件为,粗品湿品11.1g,用44.4g异丙醇全溶,加入66.6g均三甲苯和1.11g活性炭,60℃搅拌脱色1h,精制收率为97.0%,双酚S质量分数为99.89%。混合醇-均三甲苯体系精制较佳条件为,粗品10g,用40g混合醇(异丙醇∶异戊醇=1∶1)全溶,加入60g均三甲苯和1g活性炭,60℃搅拌脱色1h,精制收率为90.6%,双酚S质量分数为99.87%。

The effects of different refluxing and water removal time on the synthesis of bisphenol S are studied when one water distributor or two water distributors are installed. The water removal efficiency can be significantly improved with two water distributors. The refluxing time can be reduced and the crude yield can also be increased： The preferred conditions are as follows： 492. 5g phenol, 500g mesitylene and 25g 2,6-naphthalene disulfonic acid are mixed, then 256g concentrated sulfuric acid is dropped, after which refluxing is kept for 6.5h. The crude yield is more than 99% and the mass fraction of bisphenol S is 96.69%. In the purification of bisphenol S, a single al^ohol- mesitylene and mixed alcohol-mesitylene system are compared. Taking the cost, yield, color and other aspects into accounts, the mixed alcohol including isopropanol and isoamyl alcohol is better than a single isopropanol. In the selection of the deeolorants, the activated carbon for sugar is much better. The preferred conditions of a single aleohol-mesitylene system are as follows： 11. lg crude wet product is dissolved in 44.4g isopropanol, after 66.6g mesitylene and 1. 11 g activated carbon for sugar are added, the whole system is stirred and decolored under 60℃ for 1 h. The yield is 97.0% and the mass fraction of bisphenol S is 99.89%. The preferred conditions of mixed alcohol- mesitylene system are as follows ： 10g crude product is dissolved in 40g mixed alcohol （ isopropanol： isoamyl alcohol = 1 ： 1 ） , after 60g mesitylene and lg activated carbon are added, the whole system is stirred and decolored under 60℃ for I h. The final yield is 90. 6% and the mass fraction of bisphenol S is 99. 87%.