| 张天永,刘茜,李彬,张国玲,陈松,安静,王树华.化学通报,2016,79(3):259-263,237. |
| 双酚S合成过程脱水控制和精制工艺研究 |
| Research on water removal control of bisphenol S synthesis and its purification |
| 投稿时间：2015-07-01 修订日期：2015-09-14 |
| DOI： |
| 中文关键词: 双酚S 精制 醇 均三甲苯 |
| 英文关键词:Bisphenol S Purification Alcohol Mesitylene |
| 基金项目:国家自然科学基金(21276187),教育部高等学校博士学科点专项科研基金(20110032120011),天津市应用基础与前沿技术研究计划 (13JCQNJC05800) |
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| 中文摘要: |
| 双酚S合成过程研究了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%。双酚S精制过程分别研究了单一醇-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：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%。 |
| 英文摘要: |
| In the synthesis of bisphenol S, the effects of different refluxing and water removal time are studied when a 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 alcohol-mesitylene and mixed alcohol-mesitylene system are studied. 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 decolorants, the activated carbon for sugar is much better. The preferred conditions of a single alcohol-mesitylene system are as follows: 11.1g crude wet product is dissolved in 44.4g isopropanol. After 66.6g mesitylene and 1.11g activated carbon for sugar are added, the whole system is stirred and decolored under 60℃ for 1h. 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 1g activated carbon are added, the whole system is stirred and decolored under 60℃ for 1h. The final yield is 90.6% and the mass fraction of bisphenol S is 99.87%. |
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