Novel process windows – Concept, proposition and evaluation methodology, and intensified superheated processing

Hessel, Volker; Cortese, B.; Croon, M.H.J.M. de

doi:10.1016/j.ces.2010.08.018

Cited by 162 publications

(93 citation statements)

References 106 publications

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“…For these reasons, the chemical industry has started to explore different means of so-called " process intensifi cation " technologies, which demand abrupt changes in traditional processing and a search for game-changing improvements [1 -5] . The idea to deliberately explore harsh or otherwise very unusual process conditions for process intensifi cation of chemical reactions is a recent concept termed " novel process windows " [1,6] . Here, the general notion is to operate at conditions that considerably increase reaction rates while maintaining selectivity.…”

Section: Introductionmentioning

confidence: 99%

“…Here, the general notion is to operate at conditions that considerably increase reaction rates while maintaining selectivity. One key principle in this area is to operate chemical transformations in a high-temperature/high-pressure (high-T/p) process window, taking advantage of often dramatic rate increases based on the Arrhenius relationship [ k = A exp(-E a /R T )] [6] .…”

Section: Introductionmentioning

confidence: 99%

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Microwave-assisted continuous flow synthesis on industrial scale

Morschhäuser

Krull

Kayser

et al. 2012

Green Processing and Synthesis

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A continuous fl ow microwave system based on a transmission line short-circuited waveguide reactor concept is described. The continuous fl ow reactor is capable of operating in a genuine high-temperature/high-pressure process window (310 ° C/60 bar), applying a microwave transparent and chemical resistant cylindrical γ -Al 2 O 3 tube as reaction zone. The system can be operated in an extremely energy effi cient manner, utilizing 0.6 -6 kW microwave power (2.45 GHz). The application of the reactor for processing four chemical transformations in a high-temperature/high-pressure regime with a throughout of 3.5 -6.0 l/h is demonstrated.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Microwave-assisted continuous flow synthesis on industrial scale

Morschhäuser

Krull

Kayser

et al. 2012

Green Processing and Synthesis

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“…29,30 Novel Process Windows is focused on enabling chemical intensification by using high temperatures, pressures, and/or concentrations to remove the limitations artificially added to chemistry. The Moffatt-Swern oxidation is generally performed at very low temperatures (<−50°C) in batch reactors.…”

Section: Etcmentioning

confidence: 99%

Highly efficient synthesis of cyclic carbonate with CO₂catalyzed by ionic liquid in a microreactor

et al. 2013

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The development of highly efficient processes for the cycloaddition of CO 2 with epoxides to produce five-membered cyclic carbonates is a very attractive topic. In this work, the cycloaddition of propylene oxide (PO) and CO 2 to give propylene carbonate (PC) is studied in a microreactor using a HETBAB ionic liquid catalyst. The microreactor performance is evaluated by studying the effects of different operating conditions, including reaction temperature, operating pressure, residence time, molar ratio of CO 2 /PO, and the catalyst concentration in PO. The process characteristics of the reaction concerning the gas-liquid mass transfer and the intrinsic kinetics perspectives are discussed. The results show that the residence time can be dramatically reduced from several hours in a conventional stirred reactor to about 10 s in a microreactor. The yield of PC at 3.5 MPa can reach 99.8% at a residence time of 14 s. The turnover frequency (TOF) value varies in the range of 3000 to 14 000 h −1 compared to 60 h −1 in the conventional stirred reactor. The space time yield (STY) or the overall reaction rate ranges from 650 to 4500 g prod. (g cat. h) −1 , which is much larger than the value [ca. 19 g prod. (g cat. h) −1 ] for the conventional stirred reactor. To some extent, the present study has also demonstrated the concept of 'Novel Process Windows'.

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“…Kappe and co-workers reported work on combined microwaves and flow systems using meso-scale reactors and microwave heating [21]. The authors employed the concepts of "Novel Process Windows", as introduced by Hessel et al, and discussed the multiple opportunities for operating and controlling organic reactions at elevated temperatures and pressures [22,23]. Organ and co-workers also contributed to state-of-art microwave-assisted capillary-type flow-reactors for metal-catalyzed organic reactions [24,25].…”

Section: Introductionmentioning

confidence: 99%

Microwave-assisted Cu-catalyzed Ullmann ether synthesis in a continuous-flow milli-plant

Benaskar

Patil

Engels

et al. 2012

Chemical Engineering Journal

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The combination of milli-scale processing and microwave heating has been investigated for the Cu-catalyzed Ullmann etherification in fine-chemical synthesis, providing improved catalytic activity and selective catalyst heating. Wall-coated and fixed-bed milli-reactors were designed and applied in the Cu-catalyzed Ullmann-type C-O coupling of phenol and 4-chloropyridine. In a batch reactor the results show clearly increased yields for the microwave heated process at low microwave powers, whereas high powers and catalyst loadings reduced the benefits of microwave heating. Slightly higher yields were found in the Cu/ZnO wallcoated as compared to the Cu/TiO 2 fixed-bed flow-reactor. The benefit here is that the reaction occurs at the surface of the metal nanoparticles confined within a support film making the nano-copper equally accessible. Catalyst deactivation was mainly caused by Cu oxidation and coke formation; however, at longer process times leaching played a significant role. Catalyst 2 activity could partially be recovered by removal of deposited by-product by means of calcination. After 6 h on-stream the reactor productivities were 28.3 and 55.1 kg prod /(m R 3 •hr)for the fresh Cu/ZnO wall-coated and Cu/TiO 2 fixed-bed reactor, respectively. Comparison of single-and multimode microwaves showed a three-fold yield increase for single-mode microwaves. Control of nanoparticles size and loading allows to avoid high temperatures in a single-mode microwave field and provides a novel solution to a major problem for combining metal catalysis and microwave heating. Catalyst stability appeared to be more important and provided two-fold yield increase for the CuZn/TiO 2 catalyst as compared to the Cu/TiO 2 catalyst due to stabilized copper by preferential oxidation of the zinc. For this catalyst a threefold yield increase was observed in single-mode microwaves which, to the best of our knowledge, led to a not yet reported productivity of 172 kg prod /(m R 3 •hr) for the microwave and flow Ullmann C-O coupling.

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Novel process windows – Concept, proposition and evaluation methodology, and intensified superheated processing

Cited by 162 publications

References 106 publications

Microwave-assisted continuous flow synthesis on industrial scale

Microwave-assisted continuous flow synthesis on industrial scale

Highly efficient synthesis of cyclic carbonate with CO₂catalyzed by ionic liquid in a microreactor

Microwave-assisted Cu-catalyzed Ullmann ether synthesis in a continuous-flow milli-plant

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Novel process windows – Concept, proposition and evaluation methodology, and intensified superheated processing

Cited by 162 publications

References 106 publications

Microwave-assisted continuous flow synthesis on industrial scale

Microwave-assisted continuous flow synthesis on industrial scale

Highly efficient synthesis of cyclic carbonate with CO2catalyzed by ionic liquid in a microreactor

Microwave-assisted Cu-catalyzed Ullmann ether synthesis in a continuous-flow milli-plant

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Product

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Highly efficient synthesis of cyclic carbonate with CO₂catalyzed by ionic liquid in a microreactor