Kolbe-Schmitt Synthesis

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Volker Hessel - One of the best experts on this subject based on the ideXlab platform.

  • Agile green process design for the intensified Kolbe-Schmitt Synthesis by accompanying (simplified) life cycle assessment.
    Environmental science & technology, 2013
    Co-Authors: Sabine Kressirer, Annegret Stark, Dana Kralisch, Ulrich Krtschil, Volker Hessel
    Abstract:

    In order to investigate the potential for process intensification, various reaction conditions were applied to the Kolbe–Schmitt Synthesis starting from resorcinol. Different CO2 precursors such as aqueous potassium hydrogencarbonate, hydrogencarbonate-based ionic liquids, DIMCARB, or sc-CO2, the application of microwave irradiation for fast volumetric heating of the reaction mixture, and the effect of harsh reaction conditions were investigated. The experiments, carried out in conventional batch-wise as well as in continuously operated microstructured reactors, aimed at the development of an environmentally benign process for the preparation of 2,4-dihydroxybenzoic acid. To provide decision support toward a green process design, a research-accompanying simplified life cycle assessment (SLCA) was performed throughout the whole investigation. Following this approach, it was found that convective heating methods such as oil bath or electrical heating were more beneficial than the application of microwave ir...

  • Kolbe‐Schmitt Flow Synthesis in Aqueous Solution – From Lab Capillary Reactor to Pilot Plant
    Chemical Engineering & Technology, 2013
    Co-Authors: Ulrich Krtschil, Volker Hessel, Hans-joachim Kost, D Reinhard
    Abstract:

    Significant process intensification was achieved for the continuously operated Kolbe-Schmitt Synthesis of 2,4-dihydroxybenzoic acid (β-resorcylic acid) on laboratory scale by using different approaches opening novel process windows. The results of the optimal process variant, both from the economic and ecological view, were scaled up to the pilot scale. In a first step, the Synthesis from resorcinol in aqueous potassium hydrogen carbonate solution was transferred from the capillary reactor to a tailor-made electrically heated microstructured reactor comprising 40 microchannels and enabling a 25-fold increase of the capacity. In a second step, a pilot plant comprising three of such reactors operated in parallel was built and successfully tested with the same reaction.

  • Agile Green Process Design for the Intensified Kolbe–Schmitt Synthesis by Accompanying (Simplified) Life Cycle Assessment
    2013
    Co-Authors: Sabine Kressirer, Annegret Stark, Dana Kralisch, Ulrich Krtschil, Volker Hessel
    Abstract:

    In order to investigate the potential for process intensification, various reaction conditions were applied to the Kolbe–Schmitt Synthesis starting from resorcinol. Different CO2 precursors such as aqueous potassium hydrogencarbonate, hydrogencarbonate-based ionic liquids, DIMCARB, or sc-CO2, the application of microwave irradiation for fast volumetric heating of the reaction mixture, and the effect of harsh reaction conditions were investigated. The experiments, carried out in conventional batch-wise as well as in continuously operated microstructured reactors, aimed at the development of an environmentally benign process for the preparation of 2,4-dihydroxybenzoic acid. To provide decision support toward a green process design, a research-accompanying simplified life cycle assessment (SLCA) was performed throughout the whole investigation. Following this approach, it was found that convective heating methods such as oil bath or electrical heating were more beneficial than the application of microwave irradiation. Furthermore, the consideration of workup procedures was crucial for a holistic view on the environmental burdens

  • Tailor-made microdevices for maximizing process intensification and productivity through advanced heating
    Chemical Engineering Journal, 2010
    Co-Authors: Ulrich Krtschil, Volker Hessel, Patrick Löb, D Reinhard, S Hübschmann, Dana Kralisch
    Abstract:

    For the Kolbe–Schmitt Synthesis from resorcinol, large process intensification was achieved recently, using a simple continuous set-up comprising a capillary reactor. However, the productivity of such capillary is low and the design less convenient for scale-up to the pilot or even production scale. Consequently, a tailor-made electrically heated microdevice was developed and successfully tested for the pilot scale using the internal numbering-up approach and enabling external numbering-up. For the Kolbe–Schmitt Synthesis in aqueous potassium hydrogen carbonate solution, a productivity of 225 kg/h at 4 s residence time and 32% yield was achieved, corresponding to a space-time yield of 38,250 kg/(m3 h). As alternative heating approach, continuous microwave heating applying both multi-mode and single-mode devices and using capillary reactors of different dimensions and shapes was investigated and revealed the benefits of a compact design with respect to microwave absorption and of small dimensions for higher space-time yields up to 32,550 kg/(m3 h). The first attempt of developing a microstructured plate reactor made of PEEK for continuous microwave heating did not lead to the expected performance. The detected reasons are discussed.

  • Intensification of the Capillary-Based Kolbe−Schmitt Synthesis from Resorcinol by Reactive Ionic Liquids, Microwave Heating, or a Combination Thereof
    Organic Process Research & Development, 2009
    Co-Authors: F. Benaskar, Volker Hessel, Ulrich Krtschil, Patrick Löb, Annegret Stark
    Abstract:

    The continuous Kolbe−Schmitt Synthesis of 2,4-dihydroxybenzoic acid from resorcinol was carried out using a setup with a capillary reactor of mm-internals and a micro heat exchanger. The process intensification potential of microwave irradiation for heating up the reactant solution and/or of using ionic liquids as carbonating reactants was evaluated. For the Microwave assisted Aqueous Kolbe−Schmitt Synthesis (MAKS), power-to-temperature graphs were calibrated with water and real-case (ion-containing) solutions, revealing several features relevant for process control. Due to higher mean reaction temperatures inside the reactor thanks to faster heating, the yields of all MAKS experiments were higher as compared to the Conventionally Heated (oil bath) aqueous Kolbe−Schmitt Synthesis (CHKS) without use of microwave irradiation. The highest yield (before isolation and purification) obtained by MAKS was 52% (at 160 °C, 8 bar, 1 L/h, 90 s), exceeding the yield of CHKS by 5% (at 140 °C, 40 bar, 84 mL/h, 390 s) at...

Ulrich Krtschil - One of the best experts on this subject based on the ideXlab platform.

  • Agile green process design for the intensified Kolbe-Schmitt Synthesis by accompanying (simplified) life cycle assessment.
    Environmental science & technology, 2013
    Co-Authors: Sabine Kressirer, Annegret Stark, Dana Kralisch, Ulrich Krtschil, Volker Hessel
    Abstract:

    In order to investigate the potential for process intensification, various reaction conditions were applied to the Kolbe–Schmitt Synthesis starting from resorcinol. Different CO2 precursors such as aqueous potassium hydrogencarbonate, hydrogencarbonate-based ionic liquids, DIMCARB, or sc-CO2, the application of microwave irradiation for fast volumetric heating of the reaction mixture, and the effect of harsh reaction conditions were investigated. The experiments, carried out in conventional batch-wise as well as in continuously operated microstructured reactors, aimed at the development of an environmentally benign process for the preparation of 2,4-dihydroxybenzoic acid. To provide decision support toward a green process design, a research-accompanying simplified life cycle assessment (SLCA) was performed throughout the whole investigation. Following this approach, it was found that convective heating methods such as oil bath or electrical heating were more beneficial than the application of microwave ir...

  • Kolbe‐Schmitt Flow Synthesis in Aqueous Solution – From Lab Capillary Reactor to Pilot Plant
    Chemical Engineering & Technology, 2013
    Co-Authors: Ulrich Krtschil, Volker Hessel, Hans-joachim Kost, D Reinhard
    Abstract:

    Significant process intensification was achieved for the continuously operated Kolbe-Schmitt Synthesis of 2,4-dihydroxybenzoic acid (β-resorcylic acid) on laboratory scale by using different approaches opening novel process windows. The results of the optimal process variant, both from the economic and ecological view, were scaled up to the pilot scale. In a first step, the Synthesis from resorcinol in aqueous potassium hydrogen carbonate solution was transferred from the capillary reactor to a tailor-made electrically heated microstructured reactor comprising 40 microchannels and enabling a 25-fold increase of the capacity. In a second step, a pilot plant comprising three of such reactors operated in parallel was built and successfully tested with the same reaction.

  • Agile Green Process Design for the Intensified Kolbe–Schmitt Synthesis by Accompanying (Simplified) Life Cycle Assessment
    2013
    Co-Authors: Sabine Kressirer, Annegret Stark, Dana Kralisch, Ulrich Krtschil, Volker Hessel
    Abstract:

    In order to investigate the potential for process intensification, various reaction conditions were applied to the Kolbe–Schmitt Synthesis starting from resorcinol. Different CO2 precursors such as aqueous potassium hydrogencarbonate, hydrogencarbonate-based ionic liquids, DIMCARB, or sc-CO2, the application of microwave irradiation for fast volumetric heating of the reaction mixture, and the effect of harsh reaction conditions were investigated. The experiments, carried out in conventional batch-wise as well as in continuously operated microstructured reactors, aimed at the development of an environmentally benign process for the preparation of 2,4-dihydroxybenzoic acid. To provide decision support toward a green process design, a research-accompanying simplified life cycle assessment (SLCA) was performed throughout the whole investigation. Following this approach, it was found that convective heating methods such as oil bath or electrical heating were more beneficial than the application of microwave irradiation. Furthermore, the consideration of workup procedures was crucial for a holistic view on the environmental burdens

  • Tailor-made microdevices for maximizing process intensification and productivity through advanced heating
    Chemical Engineering Journal, 2010
    Co-Authors: Ulrich Krtschil, Volker Hessel, Patrick Löb, D Reinhard, S Hübschmann, Dana Kralisch
    Abstract:

    For the Kolbe–Schmitt Synthesis from resorcinol, large process intensification was achieved recently, using a simple continuous set-up comprising a capillary reactor. However, the productivity of such capillary is low and the design less convenient for scale-up to the pilot or even production scale. Consequently, a tailor-made electrically heated microdevice was developed and successfully tested for the pilot scale using the internal numbering-up approach and enabling external numbering-up. For the Kolbe–Schmitt Synthesis in aqueous potassium hydrogen carbonate solution, a productivity of 225 kg/h at 4 s residence time and 32% yield was achieved, corresponding to a space-time yield of 38,250 kg/(m3 h). As alternative heating approach, continuous microwave heating applying both multi-mode and single-mode devices and using capillary reactors of different dimensions and shapes was investigated and revealed the benefits of a compact design with respect to microwave absorption and of small dimensions for higher space-time yields up to 32,550 kg/(m3 h). The first attempt of developing a microstructured plate reactor made of PEEK for continuous microwave heating did not lead to the expected performance. The detected reasons are discussed.

  • Intensification of the Capillary-Based Kolbe−Schmitt Synthesis from Resorcinol by Reactive Ionic Liquids, Microwave Heating, or a Combination Thereof
    Organic Process Research & Development, 2009
    Co-Authors: F. Benaskar, Volker Hessel, Ulrich Krtschil, Patrick Löb, Annegret Stark
    Abstract:

    The continuous Kolbe−Schmitt Synthesis of 2,4-dihydroxybenzoic acid from resorcinol was carried out using a setup with a capillary reactor of mm-internals and a micro heat exchanger. The process intensification potential of microwave irradiation for heating up the reactant solution and/or of using ionic liquids as carbonating reactants was evaluated. For the Microwave assisted Aqueous Kolbe−Schmitt Synthesis (MAKS), power-to-temperature graphs were calibrated with water and real-case (ion-containing) solutions, revealing several features relevant for process control. Due to higher mean reaction temperatures inside the reactor thanks to faster heating, the yields of all MAKS experiments were higher as compared to the Conventionally Heated (oil bath) aqueous Kolbe−Schmitt Synthesis (CHKS) without use of microwave irradiation. The highest yield (before isolation and purification) obtained by MAKS was 52% (at 160 °C, 8 bar, 1 L/h, 90 s), exceeding the yield of CHKS by 5% (at 140 °C, 40 bar, 84 mL/h, 390 s) at...

Annegret Stark - One of the best experts on this subject based on the ideXlab platform.

  • Agile green process design for the intensified Kolbe-Schmitt Synthesis by accompanying (simplified) life cycle assessment.
    Environmental science & technology, 2013
    Co-Authors: Sabine Kressirer, Annegret Stark, Dana Kralisch, Ulrich Krtschil, Volker Hessel
    Abstract:

    In order to investigate the potential for process intensification, various reaction conditions were applied to the Kolbe–Schmitt Synthesis starting from resorcinol. Different CO2 precursors such as aqueous potassium hydrogencarbonate, hydrogencarbonate-based ionic liquids, DIMCARB, or sc-CO2, the application of microwave irradiation for fast volumetric heating of the reaction mixture, and the effect of harsh reaction conditions were investigated. The experiments, carried out in conventional batch-wise as well as in continuously operated microstructured reactors, aimed at the development of an environmentally benign process for the preparation of 2,4-dihydroxybenzoic acid. To provide decision support toward a green process design, a research-accompanying simplified life cycle assessment (SLCA) was performed throughout the whole investigation. Following this approach, it was found that convective heating methods such as oil bath or electrical heating were more beneficial than the application of microwave ir...

  • Agile Green Process Design for the Intensified Kolbe–Schmitt Synthesis by Accompanying (Simplified) Life Cycle Assessment
    2013
    Co-Authors: Sabine Kressirer, Annegret Stark, Dana Kralisch, Ulrich Krtschil, Volker Hessel
    Abstract:

    In order to investigate the potential for process intensification, various reaction conditions were applied to the Kolbe–Schmitt Synthesis starting from resorcinol. Different CO2 precursors such as aqueous potassium hydrogencarbonate, hydrogencarbonate-based ionic liquids, DIMCARB, or sc-CO2, the application of microwave irradiation for fast volumetric heating of the reaction mixture, and the effect of harsh reaction conditions were investigated. The experiments, carried out in conventional batch-wise as well as in continuously operated microstructured reactors, aimed at the development of an environmentally benign process for the preparation of 2,4-dihydroxybenzoic acid. To provide decision support toward a green process design, a research-accompanying simplified life cycle assessment (SLCA) was performed throughout the whole investigation. Following this approach, it was found that convective heating methods such as oil bath or electrical heating were more beneficial than the application of microwave irradiation. Furthermore, the consideration of workup procedures was crucial for a holistic view on the environmental burdens

  • Microwave‐Assisted Kolbe‐Schmitt Synthesis Using Ionic Liquids or Dimcarb as Reactive Solvents
    Chemical Engineering & Technology, 2009
    Co-Authors: Annegret Stark, Sabine Huebschmann, Martin Sellin, Dana Kralisch, Ronald Trotzki, Bernd Ondruschka
    Abstract:

    The activation of relatively inert carbon dioxide as a building block for organic products is of interest from both ecological and chemical points of view. One of the few industrially relevant processes using CO 2 is the Kolbe-Schmitt Synthesis. Two strategies to obtain the carboxylated product 2,4-dihydroxybenzoic acid from resorcinol are presented: both Dimcarb and hydrogencarbonate- or methyl-carbonate-based ionic liquids are employed as reactive solvents in a microwave-assisted reaction. Reaction optimization shows that the ionic liquids are more reactive than Dimcarb. However, Dimcarb offers advantages with regard to ecological aspects, such as the Global Warming and Human Toxicity Potential and the Cumulative Energy Demand, which were assessed as part of the process development.

  • Intensification of the Capillary-Based Kolbe−Schmitt Synthesis from Resorcinol by Reactive Ionic Liquids, Microwave Heating, or a Combination Thereof
    Organic Process Research & Development, 2009
    Co-Authors: F. Benaskar, Volker Hessel, Ulrich Krtschil, Patrick Löb, Annegret Stark
    Abstract:

    The continuous Kolbe−Schmitt Synthesis of 2,4-dihydroxybenzoic acid from resorcinol was carried out using a setup with a capillary reactor of mm-internals and a micro heat exchanger. The process intensification potential of microwave irradiation for heating up the reactant solution and/or of using ionic liquids as carbonating reactants was evaluated. For the Microwave assisted Aqueous Kolbe−Schmitt Synthesis (MAKS), power-to-temperature graphs were calibrated with water and real-case (ion-containing) solutions, revealing several features relevant for process control. Due to higher mean reaction temperatures inside the reactor thanks to faster heating, the yields of all MAKS experiments were higher as compared to the Conventionally Heated (oil bath) aqueous Kolbe−Schmitt Synthesis (CHKS) without use of microwave irradiation. The highest yield (before isolation and purification) obtained by MAKS was 52% (at 160 °C, 8 bar, 1 L/h, 90 s), exceeding the yield of CHKS by 5% (at 140 °C, 40 bar, 84 mL/h, 390 s) at...

  • Flow Chemistry of the Kolbe‐Schmitt Synthesis from Resorcinol: Process Intensification by Alternative Solvents, New Reagents and Advanced Reactor Engineering
    Chemical Engineering & Technology, 2009
    Co-Authors: Ulrich Krtschil, Volker Hessel, D Reinhard, Annegret Stark
    Abstract:

    The Kolbe-Schmitt Synthesis from resorcinol was exemplarily investigated to figure out the process intensification potential of continuous processing in the milli and micro scale, alone and combined with additional intensification means like alternative solvents, new reagents and an advanced reactor design. The oil bath-heated Synthesis was investigated for capillary reactors of different dimensions, using aqueous solutions of KHCO3 and reactive ionic liquids. Already the first case led to space-time yields (STY) of 15,500 kg/(m3h) at 37 % yield. Synthesis with different CO2-donating salts showed that KHCO3 has the highest activity and that hydrogen carbonates are better than carbonates. The replacement of KHCO3 by reactive ionic liquids led to a substantial increase, both in yield (58 %) and STY (69,900 kg/(m3h)). The application of scCO2 did not significantly increase the yield despite an even more substantial change of the reaction medium. Using an electrically heated microstructured reactor resulted in a tenfold higher productivity (0.75 t/a) compared to the capillary reactor and does much better ensure scalability of the reaction.

D Reinhard - One of the best experts on this subject based on the ideXlab platform.

  • Kolbe‐Schmitt Flow Synthesis in Aqueous Solution – From Lab Capillary Reactor to Pilot Plant
    Chemical Engineering & Technology, 2013
    Co-Authors: Ulrich Krtschil, Volker Hessel, Hans-joachim Kost, D Reinhard
    Abstract:

    Significant process intensification was achieved for the continuously operated Kolbe-Schmitt Synthesis of 2,4-dihydroxybenzoic acid (β-resorcylic acid) on laboratory scale by using different approaches opening novel process windows. The results of the optimal process variant, both from the economic and ecological view, were scaled up to the pilot scale. In a first step, the Synthesis from resorcinol in aqueous potassium hydrogen carbonate solution was transferred from the capillary reactor to a tailor-made electrically heated microstructured reactor comprising 40 microchannels and enabling a 25-fold increase of the capacity. In a second step, a pilot plant comprising three of such reactors operated in parallel was built and successfully tested with the same reaction.

  • Tailor-made microdevices for maximizing process intensification and productivity through advanced heating
    Chemical Engineering Journal, 2010
    Co-Authors: Ulrich Krtschil, Volker Hessel, Patrick Löb, D Reinhard, S Hübschmann, Dana Kralisch
    Abstract:

    For the Kolbe–Schmitt Synthesis from resorcinol, large process intensification was achieved recently, using a simple continuous set-up comprising a capillary reactor. However, the productivity of such capillary is low and the design less convenient for scale-up to the pilot or even production scale. Consequently, a tailor-made electrically heated microdevice was developed and successfully tested for the pilot scale using the internal numbering-up approach and enabling external numbering-up. For the Kolbe–Schmitt Synthesis in aqueous potassium hydrogen carbonate solution, a productivity of 225 kg/h at 4 s residence time and 32% yield was achieved, corresponding to a space-time yield of 38,250 kg/(m3 h). As alternative heating approach, continuous microwave heating applying both multi-mode and single-mode devices and using capillary reactors of different dimensions and shapes was investigated and revealed the benefits of a compact design with respect to microwave absorption and of small dimensions for higher space-time yields up to 32,550 kg/(m3 h). The first attempt of developing a microstructured plate reactor made of PEEK for continuous microwave heating did not lead to the expected performance. The detected reasons are discussed.

  • Flow Chemistry of the Kolbe‐Schmitt Synthesis from Resorcinol: Process Intensification by Alternative Solvents, New Reagents and Advanced Reactor Engineering
    Chemical Engineering & Technology, 2009
    Co-Authors: Ulrich Krtschil, Volker Hessel, D Reinhard, Annegret Stark
    Abstract:

    The Kolbe-Schmitt Synthesis from resorcinol was exemplarily investigated to figure out the process intensification potential of continuous processing in the milli and micro scale, alone and combined with additional intensification means like alternative solvents, new reagents and an advanced reactor design. The oil bath-heated Synthesis was investigated for capillary reactors of different dimensions, using aqueous solutions of KHCO3 and reactive ionic liquids. Already the first case led to space-time yields (STY) of 15,500 kg/(m3h) at 37 % yield. Synthesis with different CO2-donating salts showed that KHCO3 has the highest activity and that hydrogen carbonates are better than carbonates. The replacement of KHCO3 by reactive ionic liquids led to a substantial increase, both in yield (58 %) and STY (69,900 kg/(m3h)). The application of scCO2 did not significantly increase the yield despite an even more substantial change of the reaction medium. Using an electrically heated microstructured reactor resulted in a tenfold higher productivity (0.75 t/a) compared to the capillary reactor and does much better ensure scalability of the reaction.

Dana Kralisch - One of the best experts on this subject based on the ideXlab platform.

  • Agile green process design for the intensified Kolbe-Schmitt Synthesis by accompanying (simplified) life cycle assessment.
    Environmental science & technology, 2013
    Co-Authors: Sabine Kressirer, Annegret Stark, Dana Kralisch, Ulrich Krtschil, Volker Hessel
    Abstract:

    In order to investigate the potential for process intensification, various reaction conditions were applied to the Kolbe–Schmitt Synthesis starting from resorcinol. Different CO2 precursors such as aqueous potassium hydrogencarbonate, hydrogencarbonate-based ionic liquids, DIMCARB, or sc-CO2, the application of microwave irradiation for fast volumetric heating of the reaction mixture, and the effect of harsh reaction conditions were investigated. The experiments, carried out in conventional batch-wise as well as in continuously operated microstructured reactors, aimed at the development of an environmentally benign process for the preparation of 2,4-dihydroxybenzoic acid. To provide decision support toward a green process design, a research-accompanying simplified life cycle assessment (SLCA) was performed throughout the whole investigation. Following this approach, it was found that convective heating methods such as oil bath or electrical heating were more beneficial than the application of microwave ir...

  • Agile Green Process Design for the Intensified Kolbe–Schmitt Synthesis by Accompanying (Simplified) Life Cycle Assessment
    2013
    Co-Authors: Sabine Kressirer, Annegret Stark, Dana Kralisch, Ulrich Krtschil, Volker Hessel
    Abstract:

    In order to investigate the potential for process intensification, various reaction conditions were applied to the Kolbe–Schmitt Synthesis starting from resorcinol. Different CO2 precursors such as aqueous potassium hydrogencarbonate, hydrogencarbonate-based ionic liquids, DIMCARB, or sc-CO2, the application of microwave irradiation for fast volumetric heating of the reaction mixture, and the effect of harsh reaction conditions were investigated. The experiments, carried out in conventional batch-wise as well as in continuously operated microstructured reactors, aimed at the development of an environmentally benign process for the preparation of 2,4-dihydroxybenzoic acid. To provide decision support toward a green process design, a research-accompanying simplified life cycle assessment (SLCA) was performed throughout the whole investigation. Following this approach, it was found that convective heating methods such as oil bath or electrical heating were more beneficial than the application of microwave irradiation. Furthermore, the consideration of workup procedures was crucial for a holistic view on the environmental burdens

  • Tailor-made microdevices for maximizing process intensification and productivity through advanced heating
    Chemical Engineering Journal, 2010
    Co-Authors: Ulrich Krtschil, Volker Hessel, Patrick Löb, D Reinhard, S Hübschmann, Dana Kralisch
    Abstract:

    For the Kolbe–Schmitt Synthesis from resorcinol, large process intensification was achieved recently, using a simple continuous set-up comprising a capillary reactor. However, the productivity of such capillary is low and the design less convenient for scale-up to the pilot or even production scale. Consequently, a tailor-made electrically heated microdevice was developed and successfully tested for the pilot scale using the internal numbering-up approach and enabling external numbering-up. For the Kolbe–Schmitt Synthesis in aqueous potassium hydrogen carbonate solution, a productivity of 225 kg/h at 4 s residence time and 32% yield was achieved, corresponding to a space-time yield of 38,250 kg/(m3 h). As alternative heating approach, continuous microwave heating applying both multi-mode and single-mode devices and using capillary reactors of different dimensions and shapes was investigated and revealed the benefits of a compact design with respect to microwave absorption and of small dimensions for higher space-time yields up to 32,550 kg/(m3 h). The first attempt of developing a microstructured plate reactor made of PEEK for continuous microwave heating did not lead to the expected performance. The detected reasons are discussed.

  • Microwave‐Assisted Kolbe‐Schmitt Synthesis Using Ionic Liquids or Dimcarb as Reactive Solvents
    Chemical Engineering & Technology, 2009
    Co-Authors: Annegret Stark, Sabine Huebschmann, Martin Sellin, Dana Kralisch, Ronald Trotzki, Bernd Ondruschka
    Abstract:

    The activation of relatively inert carbon dioxide as a building block for organic products is of interest from both ecological and chemical points of view. One of the few industrially relevant processes using CO 2 is the Kolbe-Schmitt Synthesis. Two strategies to obtain the carboxylated product 2,4-dihydroxybenzoic acid from resorcinol are presented: both Dimcarb and hydrogencarbonate- or methyl-carbonate-based ionic liquids are employed as reactive solvents in a microwave-assisted reaction. Reaction optimization shows that the ionic liquids are more reactive than Dimcarb. However, Dimcarb offers advantages with regard to ecological aspects, such as the Global Warming and Human Toxicity Potential and the Cumulative Energy Demand, which were assessed as part of the process development.

  • Sustainability through green processing – novel process windows intensify micro and milli process technologies
    Energy & Environmental Science, 2008
    Co-Authors: Volker Hessel, Dana Kralisch, Ulrich Krtschil
    Abstract:

    Drawing on sustainability for chemical production processes demands the prior integration of sustainability aspects during process development, when further environmental impacts and production costs become predefined. Micro and milli process technologies provide novel ways for process improvement combined with ecological and economic advantages. This is demonstrated by current developments in this area. In this context, the idea of “Novel Process Windows” is discussed referring to examples of actual research. A short overview on how to assess sustainability using established tools of evaluation is given as well. This is rounded up with a recent case study of the Kolbe–Schmitt Synthesis, performed to disclose the key drivers of further green process development.