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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-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-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。
In a 50L glass stirred autoclave, a pilot-scale test of antioxidant YS-1330 was carried out at low temperature using sulfuric acid as a catalyst, mesitylene and an intermediate methylene chloride solution as raw materials. In the above reaction system, the 45 ° trefoil-blade turbine was finally selected by the non-geometrically similar amplification-overall flow rate method and considering the dispersion and suspension performance and energy consumption. , Stirring rate of 4 to 5 levels. At the same time, the effects of feeding mode and reactor shape on liquid-liquid dispersion were analyzed. And were carried out 1L reactor 40 times, 30 times and 25.5 times the pilot scale up test. The test results show that the stirring rate of 4 to 5, the separation rate of the reaction is above 80%, with good repeatability. In the experiment, the temperature of the reaction kettle was monitored and recorded every 5 min. It was found that the reaction was continuously exothermic during the entire dropping of the raw materials and the most exothermic heat was generated within 15 min of the start of the reaction. With the passage of time, The temperature dropped continuously until equal to the external bath temperature, indicating that the reaction occurred mainly in the dropping phase of the feedstock and the catalyst sulfuric acid.