摘要
在50L玻璃搅拌反应釜中，以硫酸为催化剂、均三甲苯和中间体的二氯甲烷溶液作为原料，在低温下进行抗氧剂YS-1330的中试试验。抗氧剂YS-1330中试合成体系的搅拌放大试验采用非几何相似放大一整体流速法，并综合考虑分散悬浮性能和能耗的影响，以上反应体系中，最终选择了45。三折叶涡轮，搅拌速率为4～5级。同时，分析了加料方式、反应釜形状对液一液分散性能的影响。并分别进行了1L反应釜40倍、30倍和25．5倍的中试放大试验。试验结果表明，搅拌速率选择4～5级，反应的分离收率都在80％以上，具有较好的重复性。试验中，对反应釜温度进行监控．每隔5min记录一次，发现在整个原料滴加过程中反应在持续放热，在反应开始的15min内放热最为剧烈，随着时间的推移，反应体系的温度不断下降，直至与外部浴温相等，表明反应主要发生在原料及催化剂硫酸的滴加阶段。
Technicians conducted a pilot test on the synthesis of antioxidant YS1330 in a 50L glass stirred tank reactor under low temperatures,using sulfuric acid as catalyst and dichloromethane solution containing mesitylene and intermediates as feedstock.The nongeometric scaleup overall flow method was used for the mixing scaleup experiment for the YS1330 antioxidant pilotscale synthesis system,having regard to the effect of dispersion and suspension properties and energy efficiency.In the above reaction system,45~three pitched blade turbines were adopted,with the stirring rate being 45 grades.Based on an analysis of the ef fect of feeding method and the shape of the reactor kettle on liquidliquid dispersion properties,they con ducted 40times,30times and 25.5times pilotscale scaleup experiments on a 1L reactor kettle.Experimen tal results show that when the stirring rates were grades 45 ,the separation yields of all reactions exceeded 80% and good repeatability could be achieved.During the experiments,the temperature in the reactor kettle was monitored and recorded every five minutes.The reactions were continuously releasing heat throughout the feedstock adding process.Heat release was the most intense within the first 15 minutes after the start of re action and the temperature of the reaction system declined over time until it reached the external bath tem perature.These phenomena suggests that reactions primarily took place in the stage where feedstock and cata lyst sulfuric acid were added.
出处
《中外能源》
CAS
2013年第12期85-89,共5页
Sino-Global Energy
