Fraunhofer Institute for Environmental, Safety and Energy Technology UMSICHT
Fraunhofer Institute for Environmental, Safety and Energy Technology UMSICHT

Carbon2Chem® laboratory

Purifying gases as well as catalytically producing methanol and higher alcohols

Carbon2Chem®-Laboratory in Oberhausen, Grermany
© Fraunhofer UMSICHT
Carbon2Chem® laboratory in Oberhausen.

***Please note: Carbon2Chem® is entering its third phase. This page will be updated accordingly. It currently contains information from the second project phase.***

 

The Carbon2Chem® laboratory on the campus of Fraunhofer UMSICHT in Oberhausen measures 500 m2. Research and validations are conducted here concerning the catalytic production of methanol and higher alcohols from steel mill gases as well as gas purification.

In specific terms, components and processes are scaled up and optimum operating points, control strategies, and modes of operating are determined. To conduct preliminary experimental investigations, laboratory space, which can be used to test the technologies from all of the Carbon2Chem® subprojects, is also available.

The work focuses on the behavior of various catalysts when using steel mill gases and a dynamic operation of the processes. The results serve as the basis for work in the technical center.

Gas purification

The research focuses on developing and implementing gas purification and treatment technologies for steel mill gases.

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  • Thermal deoxygenation

    Investigation of different catalysts and process conditions in a complex gas matrix

    Aim

    Thermal deoxygenation

    • Heterogeneously catalyzed conversion of oxygen traces
    • Investigation of different catalysts and process conditions in a complex gas matrix

    Application

    • Gas purification and gas treatment

    Technical specification

    • High-temperature fixed-bed reactor
    • Quartz glass (Ø 25 mm; 1000 °C; max. 1 bar)
    • Stainless steel (Ø 25.4 mm; 550 °C; max. 60 bar)
    • Artificial steel mill gas
    • Metering system for minor components
    • MS analyzer
    • O2 sensor

  • Non-thermal plasma deoxygenation

    Investigation of different catalysts and process conditions in a non-thermal plasma

    Aim

    Deoxygenation of coke oven gas

    • Desorption of significantly adsorbed components
    • Utilization of electrical conductivity of active charcoal
    • Modification of non-conductive adsorbents
    • Variation of the adsorbent configuration

    Application

    • Separation of significantly adsorbed minor components from waste gases
    • Energy-efficient regeneration of adsorbents

    Technical specification

    • 2 adsorber/desorber containers (approx. 250 ml; max. 10 bar)
    • Measurement of the axial temperature distribution (max. 648 K)
    • Possibility of detecting the desorbed species

  • Thermal adsorption and desorption

    Testing of electric swing adsorption to separate minor components and recycling materials from various steel mill gases

    Aim

    Thermal regeneration of adsorbents via electricity

    • Desorption of significantly adsorbed components
    • Utilization of electrical conductivity of active charcoal
    • Modification of non-conductive adsorbents
    • Variation of the adsorbent configuration

    Application

    • Reversible separation of significantly adsorbed minor components
      from waste gases
    • Efficient regeneration of adsorbents
    • Protection for other adsorption technologies

    Technical specification

    • Adsorber containers each with a capacity of 60 L
    • Volume flow rate of up to 6 Nm3/h
    • Desorption up to 350 °C
    • Simultaneous adsorption and desorption in two containers

Methanol production

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  • Studies of the behavior of various catalysts in the tubular reactor with gas loop operation

    Aim

    Syngas experiments in near-real-life conditions

    • Long-term test with pellets or molded articles
    • Transfer of laboratory results on a technical scale
       

    Application

    • Production of alcohols and DME from alternative syngases
    • Testing of control strategies
       

    Technical specification

    • Reactor length with closed-circuit oil cooling
      • Length: 110 cm
      • Inside diameter: 19 mm
    • Up to 100 bar and 300°C
    • Gas compressor
    • Condensation of liquid products
    • At-Line-GC with FID and WLD
    • Online measurement of permanent gas concentrations

  • The rectification plant is used to purify the raw methanol, making it available for further applications in the project (e.g. methanol car or MtX). The downstream products are also processed.

    Aim

    • Sample production for further use in other plants and applications
    • Verification of simulation results for process optimization

    Application

    • Purification of raw methanol from the annexes to the pilot plant in Duisburg
    • Purification of the products from the MtX plant

    Technical specification

    • DN50 column
    • Packing column with 1.5 m active height (Sulzer DX™)
    • Vacuum to atmospheric pressure
    • Temperature up to 200 °C
    • Fully automated operation
    Rektifikationsanlage im Carbon2Chem®-Labor in Oberhausen
    Rectification unit in the Carbon2Chem® laboratory in Oberhausen

  • The Methanol-Production Plant in a flexible process design in a transportable container can be used to test the production of methanol with industrial catalysts using various industry-oriented process concepts.

    Aim

    • Catalyst testing in industry-standard tablet form
    • Performance evaluation using the temperature profile
    • Methanol sample production

    Application

    • Comparison of industrial catalysts
    • Flexible use at different locations made possible by the annex's self-sufficiency

    Technical specifications

    • Simulation of any fresh gas by mixing pure cylinder gases H2, CO and CO2 over a wide section, including dilution with inert components
    • Two reactors, each 1.8 m long, with parallel or serial flow
    • Reactors equipped with boiling water cooling
    • Measurement of the temperature profile in both reactors with 30 measuring points each
    • Operating pressure up to 100 bar and 270 °C cooling jacket temperature
    • 2-stage makeup gas compressor up to 6 Nm³/h
    • 1-stage cycle gas compressor up to 90 Nm³/h
    • Condensation of liquid products with pseudo-differential sampling
    • Online main component analysis and detailed analysis using gas chromatography at the reactor outlet
    • Automation with PCS7 and integration of data into the UMSICHT cloud

Catalyst testing

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  • Heterogeneous catalytic synthesis of methanol from syngas with different CO/CO2 concentrations. Possibility of adding low concentrations of liquids even at increased pressure in the gas phase to test the influence on productivity and stability. 
     

    Aim

    Determination of activity as part of methanol synthesis under the influence of certain reaction parameters 

    • Optimization of the parameters in methanol synthesis including dynamic operation
    • Influence of various concentrations on methanol productivity
    • Multiple usage of unreacted educts and their influence on conversion and selectivity 


    Application

    • Examination of catalysts in methanol synthesis under industry-related process conditions
    • Parameter optimization (reaction temperature, pressure, gas composition, etc.)


    Technical specification

    • Use of 2 fixed-bed reactors with catalyst quantities of up to 1g
    • Volume flows of various compositions within the range of 100 to 1500Nml min-1 possible
    • Temperatures of up to 400°C in a stainless steel reactor and pressures of up to 50 bar
    • Online analysis: 4 sampling points for gas chromatography

  • Transient and stationary examination of various catalysts. Examination of various gas compositions with a range of pressures and temperatures to obtain information about the structural response relationship in the examined reaction.


    Aim

    Catalyst and activity screening of the individual reactions

    • Temperature-programmed methods of characterization
    • Influence of impurities in the educt gas via pulses and in continuous operation
    • Activity measurements in methanol synthesis and ammonia synthesis to assess deactivation due to impurities, especially O2 and the like.
    • Variation of different disturbance variables in the process sequence


    Application

    • Dimensioning of the necessary purification of the educt gases for catalysis
    • Parameter optimization (reaction temperature, pressure, gas composition, etc.)


    Technical specification

    • Temperature range from -200°C to 600°C in a stainless steel U reactor up to 60 bar
    • Online analysis via quadrupole mass spectrometry and GC analysis

  • The "Spider" test system is designed to test eight catalysts in parallel. It represents an intermediate stage between classic individual examination and high-throughput screening.

    Aim

    Catalyst screening as part of catalyst development

    • Consideration of the influence of important reaction parameters
    • Comparison of different catalysts under identical conditions


    Application

    • Rapid screening of different catalysts
    • Residence time variations
    • Parameter optimization (reaction temperature, pressure, gas composition, etc.)
       

    Technical specification

    • Eight parallel reactors
      • Øad ¼ inch
      • isothermal length 40 mm
    • Up to 60 bar and 450 °C
    • Gas supply: H2, CO, N2
    • Online gas chromatography (TCD, FID)
    • Separate flow control

  • The pilot plant “ReCat” is used to test powder and shaped body catalysts under industry-related conditions. The annex is designed for the production of methanol, higher alcohols and olefins from synthesis gas and is used to test, optimize and further develop catalysts. Particularly noteworthy is the reactor heating with thermal oil, which enables isothermal reaction control in exothermic reactions. In addition, a compressor has been integrated that allows part of the product gas to be recirculated into the reactor and the process efficiency to be increased.

    Aim

    • Testing of heterogeneous catalysts for the production of methanol, higher alcohols and olefins from synthesis gas
    • Determination of reaction-related key figures such as conversion and selectivity
    • Optimization of the reaction control
    • Development of processes for the economic production of methanol, higher alcohols and olefins

    Application

    • Testing of catalysts for methanol, alcohol and olefin synthesis under industry-related conditions
    • Identification and optimization of operating conditions

    Technical specifications

    • Reaction temperature up to 300 °C, operating pressure up to 80 bar
    • Isothermal reaction control through heating with thermal oil
    • Fully automated test control
    • Compressor for returning part of the product for recycling
    • Flexible testing options with powder and molded body catalysts
    • Online gas chromatography for the analysis of gaseous educts and products
    Frontansicht des Teststands »ReCat«
    Front view of the ReCat test rig

  • The catalyst test stand “Spider II” is used for the rapid screening of newly developed catalysts. One field of application is the investigation of catalysts for the conversion of synthesis gas into chemical products, such as olefins or longer-chained alcohols. The test stand can be used to operate up to eight reactors simultaneously in order to test different catalyst samples under uniform conditions. The test stand enables high process temperatures and pressures, so that catalysts can be examined under industry-related conditions and a far-reaching optimization of process parameters can be carried out. It is also possible to separate high-boiling products downstream of the respective reactor of the test stand and thereby precisely determine a wide range of product spectra, such as those that occur with Fischer-Tropsch catalysts.

    Aim

    • Rapid screening of new, promising catalysts
    • Increasing efficiency and further developing catalysts with regard to the parameters of activity, selectivity and stability
    • Optimizing reaction control
    • Identifying and testing industry-related and economical catalysts and process conditions

    Application

    • Screening of catalysts under industry-related conditions in eight reactors operated in parallel, e.g. for the conversion of synthesis gas into chemical products such as olefins or longer-chain alcohols
    • Investigation of process-relevant parameters such as pressure and temperature
    • Determination of reaction-relevant parameters such as conversion and selectivity
    • Identification and analysis of a wide range of products, e.g. by online gas chromatography

    Technical specifications

    • Reaction temperature up to 500 °C, operating pressure up to 90 bar
    • Separation of high- and low-boiling substances
    • Fully automated test procedure
    • Sulfine-resistant piping for use with sulfurous gases and catalysts
    • Online gas chromatography for the analysis of gaseous educts and products
    Frontansicht des Katalysatorteststands »Spider II«
    Front view of the catalyst test stand “Spider II”

Analytics

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  • The PTR-TOF1000/10K spectrometers were generated for what are known as “volatile organic compounds” (VOC), among other things, and can analyze trace components as well as the fragmentation patterns of these compounds using mass spectrometry. In addition, these spectrometers are connected to a HovaCAL gas generator system, which should make it possible to simulate gas mixtures and analyze them online.


    Aim

    Simulation of various simulated gas mixtures (e.g., metallurgical gases) and immediate subsequent online measurement, identification, and analysis.

    • Identification of potential impurities (catalyst poisons, etc.) in the ppb to ppt range
    • Quantification and analysis (e.g., fragmentation patterns) of critical components


    Application

    • Characterization of the trace components is enabled with three different primary ions (H3O+, NO+, and O2+)
    • Calibration and simulation of relevant substances using a HovaCAL calibration gas generator
    • Long-term measurement campaigns
    • Parameter optimization (dilution factor, collision energy, pressure, temperature, etc.)
    • Analysis of components in liquid and gas phases.


    Technical specification

    • Online trace analysis (PTR-TOF-1000 and PTR-10K)
    • Calibration gas generator (HovaCAL), (possibility of liquid and gaseous sample injection and additional option of humidifying gases in a targeted manner.)
    • Gas supply: H2, O2, N2, He, Ar, compressed air, and as required
    • ppb/ppt sensitivity

  • TD-GC-TofMS (Thermal desorption-gas-chromatography-time-of-flight mass spectrometer) was developed to identify and quantify compounds within the gas phase at a trace level.


    Aim

    Identification of trace compounds in untreated and treated metallurgical gases and in liquid samples.

    • Identification of unknown compounds at a trace level
    • Quantification of selected trace compounds


    Application

    • Analysis of gaseous, liquid, and solid samples
    • Differentiation of isomers possible
    • Fast screening of complex compounds


    Technical specification

    • Automated introduction of samples, GC separation, and detection via a TofMS
      • TD tube for sampling (selection based on the matrix and analyte)
      • Limited to thermally stable compounds (C3-C44)
    • Tandem ionization possible (conventionally 70 eV and soft EI ionization)
    • High sensitivity down to ppt level