Samuel Struzek, Tim Delrieux, Florian Maurer, Danielle Santos Gonçalves, Sarina-Lena Heck, Linda Klag, Joachim Czechowsky, Anna Zimina and Jan-Dierk Grunwaldt
{"title":"Role of powders and coatings for relating catalytic activity and structure of Pt in emission control catalysis†","authors":"Samuel Struzek, Tim Delrieux, Florian Maurer, Danielle Santos Gonçalves, Sarina-Lena Heck, Linda Klag, Joachim Czechowsky, Anna Zimina and Jan-Dierk Grunwaldt","doi":"10.1039/D4RE00262H","DOIUrl":"https://doi.org/10.1039/D4RE00262H","url":null,"abstract":"<p >Packed powder beds and coatings are two relevant forms of catalysts, applied in industrial heterogeneous catalysis and multiple fundamental studies including <em>operando</em> spectroscopy. Both types have their individual advantages and disadvantages in regard to the performance and characterisation causing some complexity in the resulting flow patterns, possible temperature inhomogeneities in the reactor and the dynamic evolution of chemical state of the noble metal during the reaction along the catalytic bed. The well-known CO oxidation reaction over Pt/Al<small><sub>2</sub></small>O<small><sub>3</sub></small> catalysts was used in this study to uncover the influence of the gas phase compositions and the temperature on the evolution of the electronic structure of Pt for powdered and coated catalysts at comparable length scales. Advanced <em>operando</em> investigations were used to demonstrate the influence of spatial gradients in the gas phase for washcoats in contrast to packed powder beds. Additionally, transient gradients in the chemical state of Pt, which occurred more pronounced for packed powder beds than for coated monoliths were followed and traced back to heat and mass transfer effects. Finally, the catalytic activity can be linked to the temperature distributions for both types of samples. These findings will be valuable for planning and evaluating future combinations of spectroscopic and catalytic experiments on industrially relevant systems.</p>","PeriodicalId":101,"journal":{"name":"Reaction Chemistry & Engineering","volume":" 6","pages":" 1233-1243"},"PeriodicalIF":3.4,"publicationDate":"2025-03-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://pubs.rsc.org/en/content/articlepdf/2025/re/d4re00262h?page=search","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144148237","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Zahra Bazyar, Fatemeh Zeraatpisheh and Nastaran Moalemiyan
{"title":"Selective photocatalytic oxidation of (hetero)aryl alcohols to aldehydes and ketones by visible-light-absorbing three-dimensional Ni/ZnO nanoparticles†","authors":"Zahra Bazyar, Fatemeh Zeraatpisheh and Nastaran Moalemiyan","doi":"10.1039/D5RE00035A","DOIUrl":"https://doi.org/10.1039/D5RE00035A","url":null,"abstract":"<p >Heterogeneous photocatalysis offers a promising avenue for green oxidation processes in organic synthesis. In this study, we developed a three-dimensional Ni/ZnO photocatalyst for the selective oxidation of (hetero)aryl alcohols to aldehydes and ketones using molecular oxygen as a green and cost-effective oxidant. The results indicated that the three-dimensional Ni/ZnO catalyst, with a nickel loading of 2.92 wt%, exhibited exceptional performance, achieving a conversion rate of 95% and a selectivity of 97%. Moreover, the Ni/ZnO photocatalyst could be easily separated from the crude reaction mixture and reused for several cycles without a significant decrease in reaction efficiency. This highlights its potential for industrial application in large scale synthesis.</p>","PeriodicalId":101,"journal":{"name":"Reaction Chemistry & Engineering","volume":" 6","pages":" 1365-1377"},"PeriodicalIF":3.4,"publicationDate":"2025-03-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144148230","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Johannes Luibl, Markus Hegelmann, Stephan Schwarzinger, Wolfgang Korth, Mirza Cokoja and Andreas Jess
{"title":"Amphiphobic surface-active ionic liquids as dynamic micellar phase-transfer catalysts for biphasic epoxidations†","authors":"Johannes Luibl, Markus Hegelmann, Stephan Schwarzinger, Wolfgang Korth, Mirza Cokoja and Andreas Jess","doi":"10.1039/D4RE00616J","DOIUrl":"https://doi.org/10.1039/D4RE00616J","url":null,"abstract":"<p >We report on the synthesis of amphiphobic surface-active ionic liquids (FSAILs) containing fluorinated anions. The solubility and aggregation behavior of the FSAILs was determined in both aqueous hydrogen peroxide and in organic media. The FSAILs were applied as temperature-controlled micellar and phase transfer epoxidation catalysts by mixing the FSAIL with sodium tungstate in aqueous H<small><sub>2</sub></small>O<small><sub>2</sub></small> solution. The epoxidation of <em>cis</em>-cyclooctene with aqueous hydrogen peroxide was studied in terms of catalyst activity, phase behavior and recycling. To deepen insights recycability and phase transfer, especially of the catalytically active species, characteristics of the micellar catalysis were investigated in detail over different reaction time periods. High-resolution <small><sup>1</sup></small>H-qNMR reveals a quantitative phase transfer of the FSAILs into the organic phase, while the additive remains in the aqueous phase. Additionally, the present tungsten species also remain fully in the aqueous phase as shown by ICP-MS analysis.</p>","PeriodicalId":101,"journal":{"name":"Reaction Chemistry & Engineering","volume":" 6","pages":" 1350-1358"},"PeriodicalIF":3.4,"publicationDate":"2025-03-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://pubs.rsc.org/en/content/articlepdf/2025/re/d4re00616j?page=search","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144148228","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Wenwen Song, Haodong Xie, Li Liu, Xiang Ni, Yuan Xue, Yan Liu, Junwen Chen, Lei Wang and Hongjun Zhu
{"title":"Iron-loaded pure silica -SVR zeolite for the hydroxylation of phenol†","authors":"Wenwen Song, Haodong Xie, Li Liu, Xiang Ni, Yuan Xue, Yan Liu, Junwen Chen, Lei Wang and Hongjun Zhu","doi":"10.1039/D5RE00013K","DOIUrl":"https://doi.org/10.1039/D5RE00013K","url":null,"abstract":"<p >Dihydroxybenzene compounds are a type of crucial fine chemicals used in daily life, but their production process is severely constrained by contamination and relatively low efficiency. In this work, the iron-containing pure silica <strong>-SVR</strong> zeolite was successfully developed and proven to be an efficient catalyst in the conversion of phenol into dihydroxybenzene compounds in a green way. Notably, in the presence of hydroperoxide, the heterogeneous-mediated oxidative process achieved a record-high conversion of 37% and selectivity of 99%. Combining physicochemical analysis and multiple spectroscopic techniques, the active species was confirmed to be the trivalent iron sites confined within the <strong>-SVR</strong> voids. Moreover, the accessible ordered silanol defects confined within the <strong>-SVR</strong> channel system are abundant, providing anchor points for grafting iron sites. The highly active iron species initiates the free radical-mediated reaction pathway, significantly facilitating the oxidative reaction process. As unveiled by the catalytic kinetics, the iron-containing zeotype catalyst affords a TON of 861 and TOF of 430.5 h<small><sup>−1</sup></small>, and the apparent active energy <em>E</em><small><sub>a</sub></small> was determined as 26 kJ mol<small><sup>−1</sup></small>. Overall, these results not only provide a highly effective heterogeneous catalyst for the conversion of phenol into dihydroxybenzene compounds in an eco-friendly manner but also open up new horizons for the effective utilization of pure silica zeolites listed in the IZA database.</p>","PeriodicalId":101,"journal":{"name":"Reaction Chemistry & Engineering","volume":" 6","pages":" 1259-1267"},"PeriodicalIF":3.4,"publicationDate":"2025-03-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144148239","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Ziliang Yuan, Xi Wang, Yuxin Liu, Peng Zhou, Renjie Huang, Jie Lv, Yimeng Yang, Yanrong Ren, Zehui Zhang and Bing Liu
{"title":"Efficient one-pot hydrogenation and acetylation of 4-nitrophenol for selective synthesis of 4-aminophenol and paracetamol with a reusable Ni catalyst†","authors":"Ziliang Yuan, Xi Wang, Yuxin Liu, Peng Zhou, Renjie Huang, Jie Lv, Yimeng Yang, Yanrong Ren, Zehui Zhang and Bing Liu","doi":"10.1039/D5RE00016E","DOIUrl":"https://doi.org/10.1039/D5RE00016E","url":null,"abstract":"<p >Paracetamol, a widely used analgesic and antipyretic, is in high demand globally, necessitating its large-scale synthesis. Herein, carbon supported earth-abundant Ni nanoparticles were prepared using the impregnation and reduction method. The Ni nanoparticle catalyst exhibited excellent catalytic activity in the one-pot hydrogenation and acetylation of 4-nitrophenol for the synthesis of 4-aminophenol and paracetamol at 80 °C under 10 bar H<small><sub>2</sub></small>. Compared to previous methods, this protocol enables the selective synthesis of amide drug molecules to be more cost-effective, efficient, and stable, offering significant potential value. These advancements provide an alternative to traditional paracetamol synthesis techniques burdened by environmental challenges.</p>","PeriodicalId":101,"journal":{"name":"Reaction Chemistry & Engineering","volume":" 5","pages":" 953-958"},"PeriodicalIF":3.4,"publicationDate":"2025-03-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143888508","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Wenjun Huang, Xuanyu Chen, Qianjiang Lv, Xiaolan Cai, Wei Tan and Yanxiong Fang
{"title":"Rapid preparation of waterborne polyurethane dispersions using continuous-flow microreaction technology†","authors":"Wenjun Huang, Xuanyu Chen, Qianjiang Lv, Xiaolan Cai, Wei Tan and Yanxiong Fang","doi":"10.1039/D5RE00015G","DOIUrl":"https://doi.org/10.1039/D5RE00015G","url":null,"abstract":"<p >This paper provides a strategy for the preparation of waterborne polyurethane (WPU) dispersions by continuous-flow microreaction technology. The strategy starts with the preparation of polyurethane prepolymers in a continuous-flow reactor, followed by emulsification and post-chain expansion reaction in a high-speed disperser to produce M-WPU. Compared with B-WPU preparation in a traditional batch reactor, the continuous-flow microreaction technology can shorten the polymerization time from several hours to several minutes, which greatly improves the production efficiency. Meanwhile, the optimal process conditions were determined by investigating the effects of solvent dosage, catalyst type and dosage, reaction temperature, reaction residence time, total flow rate, and reactor configuration on the extent of reaction of polyurethane prepolymers as well as the effects of neutralization residence time and neutralization temperature on the particle size of WPU. Finally, the films of M-WPU and B-WPU were characterized and tested, and it was found that the M-WPU film exhibited higher molecular weight, tensile strength, hardness, larger water contact angle, better heat resistance, and lower water absorption compared with the B-WPU film prepared by the traditional batch process. This suggests that the continuous-flow microreactor process provides an efficient and promising method for the preparation of WPU.</p>","PeriodicalId":101,"journal":{"name":"Reaction Chemistry & Engineering","volume":" 6","pages":" 1326-1336"},"PeriodicalIF":3.4,"publicationDate":"2025-03-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144148244","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Fei Wang, Yulong Jin, Yue Zhang, Xuan Liang, Zihao Tong, Xuejiao Wei, Yihu Ke, Jie Xu and Bing Xue
{"title":"Oxygen vacancy-enriched MOF-derived Mn2O3 catalysts for high-efficiency direct synthesis of ethylene urea from CO2†","authors":"Fei Wang, Yulong Jin, Yue Zhang, Xuan Liang, Zihao Tong, Xuejiao Wei, Yihu Ke, Jie Xu and Bing Xue","doi":"10.1039/D5RE00061K","DOIUrl":"https://doi.org/10.1039/D5RE00061K","url":null,"abstract":"<p >The direct reaction of CO<small><sub>2</sub></small> with ethylene diamine (EDA) to produce ethylene urea (EU) provides significant potential for the resourceful utilization of CO<small><sub>2</sub></small>. Herein, we systematically synthesized a series of Mn<small><sub>2</sub></small>O<small><sub>3</sub></small> catalysts by pyrolyzing the corresponding metal–organic framework (MOF) precursor with different calcination temperatures to evaluate their catalytic activity in the synthesis of EU from CO<small><sub>2</sub></small>. Among them, MnBDC-400 exhibited the highest reactivity for EU formation, which reached 96% EDA conversion and 98% EU selectivity, even at a lower temperature (120 °C). This result was superior to all previously reported catalysts. The excellent activity benefited from more surface oxygen vacancies and Mn<small><sup>3+</sup></small> species on the surface of MnBDC-400, which facilitated the formation of ethylenediamine carbamate (EDA-CA) intermediates, leading to improved EU yields. This work has a certain guiding significance for the preparation of highly active MOF-derived oxide catalysts for CO<small><sub>2</sub></small> conversion.</p>","PeriodicalId":101,"journal":{"name":"Reaction Chemistry & Engineering","volume":" 6","pages":" 1399-1407"},"PeriodicalIF":3.4,"publicationDate":"2025-03-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144148247","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Yinkun Li, Dongxue Wang, Xixi Liu, Guoqiang She, Peng Zhou, Yanxi Zhao, Zehui Zhang and Bing Liu
{"title":"Efficient selective hydrogenation of benzonitrile over TiO2-supported nickel catalysts†","authors":"Yinkun Li, Dongxue Wang, Xixi Liu, Guoqiang She, Peng Zhou, Yanxi Zhao, Zehui Zhang and Bing Liu","doi":"10.1039/D5RE00024F","DOIUrl":"https://doi.org/10.1039/D5RE00024F","url":null,"abstract":"<p >Secondary amines are important organic compounds, given their frequent application in medicine. This work reported efficient TiO<small><sub>2</sub></small>-supported nickel catalysts (Ni/TiO<small><sub>2</sub></small>-T) for synthesizing secondary amines <em>via</em> catalytic hydrogenation of broad-scope nitriles under mild conditions and represents a promising method for producing high-value dibenzylamines with cost-effective catalysts.</p>","PeriodicalId":101,"journal":{"name":"Reaction Chemistry & Engineering","volume":" 5","pages":" 970-974"},"PeriodicalIF":3.4,"publicationDate":"2025-03-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143888511","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Yuesu Chen, Cassian Desmons, Martin Cattoen and Jean-Christophe M. Monbaliu
{"title":"Open-source fraction collector for flash column chromatography and continuous flow reactions†","authors":"Yuesu Chen, Cassian Desmons, Martin Cattoen and Jean-Christophe M. Monbaliu","doi":"10.1039/D5RE00070J","DOIUrl":"https://doi.org/10.1039/D5RE00070J","url":null,"abstract":"<p >The design and construction of an open-source fraction collector and its applications in flash column chromatography are described. With the collection vials arranged in a circular array, the outlet of the flash column is guided by an arm to stay above each vial over a defined interval of time, liberating the chemists from the manual labor of swapping vials in high frequency. The assembly is constructed with flow reactor components (plunger pump, tubing, and valves) and optional 3D printed parts (vial holders and arm). The applicability of such a device is demonstrated through relevant examples from the daily work of a chemist, including the purification of crude products, the separation of a reaction mixture, and the fractional collection of effluents from continuous flow reactors.</p>","PeriodicalId":101,"journal":{"name":"Reaction Chemistry & Engineering","volume":" 6","pages":" 1408-1416"},"PeriodicalIF":3.4,"publicationDate":"2025-03-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144148248","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Is it reliable to determine the stoichiometry of extraction complexes using the classic slope analysis model in acidic extraction systems?†","authors":"Qi Zhao, Shuai Wang and Kaimin Shih","doi":"10.1039/D4RE00596A","DOIUrl":"https://doi.org/10.1039/D4RE00596A","url":null,"abstract":"<p >Although the classic slope analysis model has become a standard tool for determining the stoichiometry of extraction complexes in acidic extraction systems, its application limitation has not been taken seriously yet. Specifically, this model simplifies the activity coefficients to 1 and constant extractant contents—these assumptions may fail under certain conditions. In this study, a general modified fitting model applicable to acidic extractants was proposed, incorporating corrections for activity coefficients and extractant mass balance. Results reveal that the stoichiometries determined by both the slope analysis model and the modified fitting model align closely for high extractant-to-metal ratios. However, at low extractant-to-metal ratios, the slope analysis model tends to overestimate the stoichiometry (extractant–metal ratio) in the extraction complex relative to the modified fitting model. This discrepancy highlights the need to carefully review the applicability and reliability of the slope analysis model in extraction experiments.</p>","PeriodicalId":101,"journal":{"name":"Reaction Chemistry & Engineering","volume":" 6","pages":" 1378-1385"},"PeriodicalIF":3.4,"publicationDate":"2025-03-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144148231","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}