Continuous flow semi-hydrogenation of alkynes using 3D printed catalytic static mixers

Kundra, Milan; Sultan, Borhan Bin Mohamad; Ng, Derrick Wing Kwan; Wang, Yaxi; Alexánder, David; Nguyen, Xuan; Xie, Zongli; Hornung, Christian H.

doi:10.1016/j.cep.2020.108018

Cited by 24 publications

(18 citation statements)

References 29 publications

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“…Therefore, the detected contaminants of these metals can also result from the reactor walls. The observation is in strong agreement with all of our previous leaching tests with CSMs containing either electroplated, cold-sprayed or wash coated catalyst layers, 12,[27][28][29]31,32 where Fe was always the major contaminant. Aside from soluble metal impurities, measured by ICP-OES, CSMs can sometimes also produce insoluble metal particles that flake off the catalyst surface during use.…”

Section: Catalyst Performancesupporting

confidence: 91%

“…CSMs), which are 3D-printed metal mixer scaffolds, coated with an active catalyst layer, that can be inserted into a continuous flow reactor. Over the past years we have used CSMs for a range of different hydrogenation applications, such as the reduction of nitro groups [28][29][30] which are commonly used in API manufacture, the hydrogenation of alkenes and carbonyls for the production of flavourings and fragrances, 27 the reduction of fatty acids, 31 the semihydrogenation of alkynes 12 and in reductive aminations. 32 In all these cases the CSMs were manufactured in two steps: 1) 3D printing of mixer scaffold, 2) deposition of a catalytically active layer by means of electroplating, metal cold-spraying or wash-coating.…”

Section: Introductionmentioning

confidence: 99%

“…Hurt et al, 4 Rossi et al, 5 and Parra-Cabrera et al 6 have presented reviews of 3D-printed catalysts for reactions used in the manufacture of pharmaceuticals, fine and bulk chemicals, food products and others, and we have further referenced recent additions to the field in our latest publications. 12,27 Our work on 3D printed structured catalysts has focused on the use in catalytic hydrogenations. For this we have investigated the performance of catalytic static mixers (abbr.…”

Section: Introductionmentioning

confidence: 99%

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3D printed nickel catalytic static mixers made by corrosive chemical treatment for use in continuous flow hydrogenation

et al. 2022

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Section: Catalyst Performancesupporting

confidence: 91%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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3D printed nickel catalytic static mixers made by corrosive chemical treatment for use in continuous flow hydrogenation

et al. 2022

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“…To capitalize on this, we have designed, manufactured, and studied − catalytic static mixers ( abbr . CSMs), which are 3D-printed metal scaffolds coated with an active catalyst layer that can be inserted into a continuous flow reactor.…”

Section: Introductionmentioning

confidence: 99%

Continuous Flow Hydrogenation of Flavorings and Fragrances Using 3D-Printed Catalytic Static Mixers

Kundra

Grall

et al. 2021

Ind. Eng. Chem. Res.

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A new type of additively manufactured catalytic static mixer, coated with alumina-supported metal catalysts, has been used for the hydrogenation of various model compounds commonly employed in the flavoring and fragrance industries. These heterogeneous catalytic reactions were performed inside an intensified tubular flow reactor housing several catalytic static mixers. In addition to electroplated and cold-sprayed catalyst coatings, which were presented by our group in earlier work, we herein demonstrate a series of alumina-supported metal catalysts for the first time, namely Pd, Pt, Ru, and Ni, supported on alumina and deposited on stainless-steel static mixers. The continuous flow hydrogenation of (−)-isopulegol at 24 bar and 130 °C produced the high value product (−)-menthol at full conversion with a 98.8% purity and a space-time yield of 2.66 kg L −1 h −1 .

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“…As mentioned above, 3D printed reactors are widely used in flow chemistry, and many reviews can be found on this topic [1,10,[12][13][14]. Nevertheless, the use of 3D printing to realize supports and internals for structured reactors is more recent and still limited to few applications [15,16]. In industry, packed bed reactors filled with heterogenous catalyst powder are still preferred due to the facile utilization and the high surface area available for mass transfer.…”

Section: Introductionmentioning

confidence: 99%

3D printed ceramics as solid supports for enzyme immobilization: an automated DoE approach for applications in continuous flow

et al. 2021

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In recent years, 3D printing has emerged in the field of chemical engineering as a powerful manufacturing technique to rapidly design and produce tailor-made reaction equipment. In fact, reactors with complex internal geometries can be easily fabricated, optimized and interchanged in order to respond to precise process needs, such as improved mixing and increased surface area. These advantages make them interesting especially for catalytic applications, since customized structured bed reactors can be easily produced. 3D printing applications are not limited to reactor design, it is also possible to realize functional low cost alternatives to analytical equipment that can be used to increase the level of process understanding while keeping the investment costs low. In this work, in-house designed ceramic structured inserts printed via vat photopolymerization (VPP) are presented and characterized. The flow behavior inside these inserts was determined with residence time distribution (RTD) experiments enabled by in-house designed and 3D printed inline photometric flow cells. As a proof of concept, these structured inserts were fitted in an HPLC column to serve as solid inorganic supports for the immobilization of the enzyme Phenolic acid Decarboxylase (bsPAD), which catalyzes the decarboxylation of cinnamic acids. The conversion of coumaric acid to vinylphenol was chosen as a model system to prove the implementation of these engineered inserts in a continuous biocatalytic application with high product yield and process stability. The setup was further automated in order to quickly identify the optimum operating conditions via a Design of Experiments (DoE) approach. The use of a systematic optimization, together with the adaptability of 3D printed equipment to the process requirements, render the presented approach highly promising for a more feasible implementation of biocatalysts in continuous industrial processes.

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Continuous flow semi-hydrogenation of alkynes using 3D printed catalytic static mixers

Cited by 24 publications

References 29 publications

3D printed nickel catalytic static mixers made by corrosive chemical treatment for use in continuous flow hydrogenation

3D printed nickel catalytic static mixers made by corrosive chemical treatment for use in continuous flow hydrogenation

Continuous Flow Hydrogenation of Flavorings and Fragrances Using 3D-Printed Catalytic Static Mixers

3D printed ceramics as solid supports for enzyme immobilization: an automated DoE approach for applications in continuous flow

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