An automated multi-stage continuous reaction system with in-line PATs for a high viscosity reactive crystallization process was developed in the present study. Data acquisition (DAQ) hardware and Labview software were used as the local control system. A “forward-backward” burst pumping strategy was developed to smoothly transfer the highly viscous hot slurry from one vessel to the next. In addition, a comparative analysis between a plug flow reactor (PFR) and continuous stirred-tank reactors (CSTRs) in series revealed that to achieve the same conversion, the latter would require more volume than the former, but less than a single CSTR. For a second-order reaction, the value of the Damköhler number necessary to achieve conversion of 90.0% in a single CSTR is 90. Thus, it is reasonable to approximate a PFR using CSTRs in series to obtain a high yield with a smaller reaction volume (compared with a single CSTR). As the probes could not be positioned in the hot slurry due to fouling issues, in-line focused beam reflectance measurement (FBRM) and React IR were used to monitor the crystal size and reactant concentration in the vessel containing the cold slurry. E-factors of batch and continuous processes were also compared and the continuous reaction could obtain a lower E-factor because less waste was generated.

中文翻译：

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开发具有在线PAT的自动化多级连续反应结晶系统，用于高粘度工艺†

在本研究中，开发了具有在线PATs的自动化多级连续反应系统，用于高粘度反应结晶过程。数据采集​​（DAQ）硬件和Labview软件被用作本地控制系统。制定了“向前-向后”爆破泵送策略，以将高粘度热浆从一个容器顺利转移到另一个容器。另外，在串联的活塞流反应器（PFR）和连续搅拌釜反应器（CSTR）之间进行的比较分析表明，要实现相同的转化率，后者将比前者需要更多的体积，但少于单个CSTR。对于二阶反应，在单个CSTR中实现90.0％转化所必需的Damköhler数的值为90。因此，因此，合理的方法是串联使用CSTR来近似PFR，以获得高收率和较小的反应体积（与单个CSTR相比）。由于探针由于结垢问题而无法放置在热浆液中，因此使用在线聚焦光束反射率测量（FBRM）和React IR来监测包含冷浆液的容器中的晶体尺寸和反应物浓度。E-因素分批和连续过程也进行了比较，该连续反应可以得到较低的E-因子因为产生更少的废物。