An Automated Continuous Synthesis and Isolation for the Scalable Production of Aryl Sulfonyl Chlorides
In this work, a continuous system to produce multi-hundred-gram quantities of aryl sulfonyl chlorides is described. The scheme employs multiple continuous stirred-tank reactors (CSTRs) and a continuous filtration system and incorporates an automated process control scheme. The experimental process o...
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| Format: | Article |
| Language: | English |
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MDPI AG
2023-05-01
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| Series: | Molecules |
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| Online Access: | https://www.mdpi.com/1420-3049/28/10/4213 |
| _version_ | 1797598874338066432 |
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| author | Matthew Glace Cameron Armstrong Nathan Puryear Colin Bailey Roudabeh Sadat Moazeni-Pourasil Drew Scott Sherif Abdelwahed Thomas. D. Roper |
| author_facet | Matthew Glace Cameron Armstrong Nathan Puryear Colin Bailey Roudabeh Sadat Moazeni-Pourasil Drew Scott Sherif Abdelwahed Thomas. D. Roper |
| author_sort | Matthew Glace |
| collection | DOAJ |
| description | In this work, a continuous system to produce multi-hundred-gram quantities of aryl sulfonyl chlorides is described. The scheme employs multiple continuous stirred-tank reactors (CSTRs) and a continuous filtration system and incorporates an automated process control scheme. The experimental process outlined is intended to safely produce the desired sulfonyl chloride at laboratory scale. Suitable reaction conditions were first determined using a batch-chemistry design of experiments (DOE) and several isolation methods. The hazards and incompatibilities of the heated chlorosulfonic acid reaction mixture were addressed by careful equipment selection, process monitoring, and automation. The approximations of the CSTR fill levels and pumping performance were measured by real-time data from gravimetric balances, ultimately leading to the incorporation of feedback controllers. The introduction of process automation demonstrated in this work resulted in significant improvements in process setpoint consistency, reliability, and spacetime yield, as demonstrated in medium- and large-scale continuous manufacturing runs. |
| first_indexed | 2024-03-11T03:26:45Z |
| format | Article |
| id | doaj.art-c47eecde8d954146866e25520e95d673 |
| institution | Directory Open Access Journal |
| issn | 1420-3049 |
| language | English |
| last_indexed | 2024-03-11T03:26:45Z |
| publishDate | 2023-05-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Molecules |
| spelling | doaj.art-c47eecde8d954146866e25520e95d6732023-11-18T02:40:58ZengMDPI AGMolecules1420-30492023-05-012810421310.3390/molecules28104213An Automated Continuous Synthesis and Isolation for the Scalable Production of Aryl Sulfonyl ChloridesMatthew Glace0Cameron Armstrong1Nathan Puryear2Colin Bailey3Roudabeh Sadat Moazeni-Pourasil4Drew Scott5Sherif Abdelwahed6Thomas. D. Roper7Department of Chemical and Life Sciences Engineering, Virginia Commonwealth University, Richmond, VA 23284, USADepartment of Chemical and Life Sciences Engineering, Virginia Commonwealth University, Richmond, VA 23284, USADepartment of Electrical and Computer Engineering, Virginia Commonwealth University, Richmond, VA 23284, USADepartment of Chemical and Life Sciences Engineering, Virginia Commonwealth University, Richmond, VA 23284, USADepartment of Chemical and Life Sciences Engineering, Virginia Commonwealth University, Richmond, VA 23284, USADepartment of Chemical and Life Sciences Engineering, Virginia Commonwealth University, Richmond, VA 23284, USADepartment of Electrical and Computer Engineering, Virginia Commonwealth University, Richmond, VA 23284, USADepartment of Chemical and Life Sciences Engineering, Virginia Commonwealth University, Richmond, VA 23284, USAIn this work, a continuous system to produce multi-hundred-gram quantities of aryl sulfonyl chlorides is described. The scheme employs multiple continuous stirred-tank reactors (CSTRs) and a continuous filtration system and incorporates an automated process control scheme. The experimental process outlined is intended to safely produce the desired sulfonyl chloride at laboratory scale. Suitable reaction conditions were first determined using a batch-chemistry design of experiments (DOE) and several isolation methods. The hazards and incompatibilities of the heated chlorosulfonic acid reaction mixture were addressed by careful equipment selection, process monitoring, and automation. The approximations of the CSTR fill levels and pumping performance were measured by real-time data from gravimetric balances, ultimately leading to the incorporation of feedback controllers. The introduction of process automation demonstrated in this work resulted in significant improvements in process setpoint consistency, reliability, and spacetime yield, as demonstrated in medium- and large-scale continuous manufacturing runs.https://www.mdpi.com/1420-3049/28/10/4213flow chemistrychlorosulfonationprocess automationpump control systemcontinuous manufacturingbatch design |
| spellingShingle | Matthew Glace Cameron Armstrong Nathan Puryear Colin Bailey Roudabeh Sadat Moazeni-Pourasil Drew Scott Sherif Abdelwahed Thomas. D. Roper An Automated Continuous Synthesis and Isolation for the Scalable Production of Aryl Sulfonyl Chlorides Molecules flow chemistry chlorosulfonation process automation pump control system continuous manufacturing batch design |
| title | An Automated Continuous Synthesis and Isolation for the Scalable Production of Aryl Sulfonyl Chlorides |
| title_full | An Automated Continuous Synthesis and Isolation for the Scalable Production of Aryl Sulfonyl Chlorides |
| title_fullStr | An Automated Continuous Synthesis and Isolation for the Scalable Production of Aryl Sulfonyl Chlorides |
| title_full_unstemmed | An Automated Continuous Synthesis and Isolation for the Scalable Production of Aryl Sulfonyl Chlorides |
| title_short | An Automated Continuous Synthesis and Isolation for the Scalable Production of Aryl Sulfonyl Chlorides |
| title_sort | automated continuous synthesis and isolation for the scalable production of aryl sulfonyl chlorides |
| topic | flow chemistry chlorosulfonation process automation pump control system continuous manufacturing batch design |
| url | https://www.mdpi.com/1420-3049/28/10/4213 |
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