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Binary Solvent Swap Processing in a Bubble Column in Batch and Continuous Modes
Organic Process Research & Development ( IF 3.1 ) Pub Date : 2022-03-16 , DOI: 10.1021/acs.oprd.1c00455 Phillip Roche 1 , Roderick C Jones 1 , Brian Glennon 1 , Philip Donnellan 1
Organic Process Research & Development ( IF 3.1 ) Pub Date : 2022-03-16 , DOI: 10.1021/acs.oprd.1c00455 Phillip Roche 1 , Roderick C Jones 1 , Brian Glennon 1 , Philip Donnellan 1
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A lab-scale bubble column was investigated as an alternative means to achieve a low-temperature binary solvent swap of solutions containing pharmaceutical materials at atmospheric pressure, for batch and continuous configurations. The rate of solvent evaporation was predicted by first-principles vapor–liquid equilibrium (VLE) thermodynamic modeling and compared to experimentally achieved results. For batch configurations, evaporation rates of up to 5 g/min were achieved at gas flow rates up to 2.5 L/min (0.21 m/s superficial velocity) and temperatures up to 50 °C. This achieved 99 mol % purity of the desired solvent within three “put and take” evaporations from a 50:50 starting mixture. The evaporation rate profiles for the duration of the experiments were calculated, and the changing concentration profile was predicted within satisfactory error margins of <5%. Continuous process modeling explored a multistage equilibrium configuration and could predict the approach to attaining steady-state operation for various operating conditions. All rates of evaporation and resulting changes in solution concentration were measured, and direct comparison of model predictions fell within instrumentation error margins, as previously. This underlined the capability of the model to provide accurate representations of predicted evaporation rates and binary solution concentration changes during operation.
中文翻译：
以批处理和连续模式在气泡柱中进行二元溶剂交换处理
研究了实验室规模的气泡柱作为替代方法，以在大气压下实现含有药物材料的溶液的低温二元溶剂交换，用于批量和连续配置。通过第一性原理汽液平衡 (VLE) 热力学模型预测溶剂蒸发速率，并与实验获得的结果进行比较。对于批量配置，在高达 2.5 L/min（0.21 m/s 表观速度）的气体流速和高达 50 °C 的温度下，蒸发速率高达 5 g/min。这在 50:50 起始混合物的三个“放置和取出”蒸发过程中实现了 99 mol% 纯度的所需溶剂。计算了实验期间的蒸发速率曲线，并且在 <5% 的令人满意的误差范围内预测了不断变化的浓度分布。连续过程建模探索了多级平衡配置，并且可以预测在各种操作条件下实现稳态操作的方法。测量了所有蒸发率和溶液浓度的变化，模型预测的直接比较落在仪器误差范围内，如前所述。这强调了该模型能够准确表示运行期间预测的蒸发速率和二元溶液浓度变化。测量了所有蒸发率和溶液浓度的变化，模型预测的直接比较落在仪器误差范围内，如前所述。这强调了该模型能够准确表示运行期间预测的蒸发速率和二元溶液浓度变化。测量了所有蒸发率和溶液浓度的变化，模型预测的直接比较落在仪器误差范围内，如前所述。这强调了该模型能够准确表示运行期间预测的蒸发速率和二元溶液浓度变化。
更新日期：2022-03-16
中文翻译：
以批处理和连续模式在气泡柱中进行二元溶剂交换处理
研究了实验室规模的气泡柱作为替代方法，以在大气压下实现含有药物材料的溶液的低温二元溶剂交换，用于批量和连续配置。通过第一性原理汽液平衡 (VLE) 热力学模型预测溶剂蒸发速率，并与实验获得的结果进行比较。对于批量配置，在高达 2.5 L/min（0.21 m/s 表观速度）的气体流速和高达 50 °C 的温度下，蒸发速率高达 5 g/min。这在 50:50 起始混合物的三个“放置和取出”蒸发过程中实现了 99 mol% 纯度的所需溶剂。计算了实验期间的蒸发速率曲线，并且在 <5% 的令人满意的误差范围内预测了不断变化的浓度分布。连续过程建模探索了多级平衡配置，并且可以预测在各种操作条件下实现稳态操作的方法。测量了所有蒸发率和溶液浓度的变化，模型预测的直接比较落在仪器误差范围内，如前所述。这强调了该模型能够准确表示运行期间预测的蒸发速率和二元溶液浓度变化。测量了所有蒸发率和溶液浓度的变化，模型预测的直接比较落在仪器误差范围内，如前所述。这强调了该模型能够准确表示运行期间预测的蒸发速率和二元溶液浓度变化。测量了所有蒸发率和溶液浓度的变化，模型预测的直接比较落在仪器误差范围内，如前所述。这强调了该模型能够准确表示运行期间预测的蒸发速率和二元溶液浓度变化。
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