橡胶防老剂双酚F的清洁化合成工艺研究

研究了橡胶防老剂双酚F2,2'-亚乙基双(4,6-二叔丁基苯酚)]的清洁化生产工艺方法。以2,4-二叔丁基苯酚、三聚乙醛为反应原料,水乳化液为反应溶剂,其中含有表面活性剂、分散剂、硫酸催化剂,经缩合反应制备2,2'-亚乙基双(4,6-二叔丁基苯酚)。当n(2,4-二叔丁基苯酚):n(三聚乙醛)=2:1.2,m(2,4-二叔丁基苯酚):m(硫酸催化剂):m(乳化剂)=1:0.1:0.05,反应温度92～93℃,反应时间6.0h时,得到产品双酚F的收率为96.6%。经液相色谱分析,产品质量分数99.66%,熔点164.6～165.2℃。反应母液可循环使用,解决了传统生产工艺中所产生的含酚废水处理问题。

Study on cleaning synthetic technology of rubber antioxidant bisphenol F

The cleaning production technology for 2,2＇-ethylene bis（4,6-di-t-butylphenol） （Referred to as bisphenol F） was studied. Using 2,4-di-t-butylphenol and trimeric acetaldehyde as raw materials, dispersing agent and surfactant as reaction solvent, bisphenol F was synthesized. The optimum conditions of synthesis are as follows, the molar ratio of 2,4-di-t-butylphenol and trimeric acetaldehyde is 2 ： 1.2, the mass ratio of 2,4- di-t-butylphenol,sulfuric acid and the emulsifier is 1 ： 0.1 ： 0.05, reaction temperature is 92-93℃ and the reaction time is 6. Oh. Under the above optimum conditions, the yield of the product is over 96.6% with the purity of 99. 66% by HPLC and the melting point of 164.6-165.2℃. This technology is adopted to recycle the raw reaction solvent again and again, and also resolve the problem of pollution of sewage of traditional production technol- ogy including phenol .