Periodic Reporting for period 2 - LIBERATE (Lignin Biorefinery Approach using Electrochemical Flow)
Berichtszeitraum: 2020-04-01 bis 2021-09-30
The overall concept of the LIBERATE project is to extract valuable chemical products from an existing waste stream: lignin. Lignin is one of the most abundant and renewable organic polymers on Earth, exceeded only by cellulose. Lignin constitutes 30% of non-fossil organic carbon and 20-35% of the dry mass of wood. Indeed, it is the largest renewable source of aromatic organic entities. As a by-product of the paper pulping process, around 40 million tonnes per year of lignin are produced, but the 95% of this is incinerated as a low value fuel. Then, lignin depolymerization into value-added aromatic products under mild conditions would greatly benefit both the value-added fine chemical industry and green/renewable chemistry sector. The LIBERATE project will divert lignin from incineration and use selective electrochemistry to depolymerise the lignin into value added products, delivering a fully characterized continuous electrochemistry-based biorefinery system for lignin valorisation. The system will use kraft and organosolv lignin as feedstocks and derive to vanillin, biogenic adipic acid analogues and bio-phenols which are high value and of high industrial interest. Due to the continuous process, lower heat and energy input requirements of these approaches they readily enable the integration of the process with renewable energy generators. The project will achieve the following benefits:
1) The obtention of vanillin from kraft lignin with a 7% yield;
2) To synthesize mixed phenolic derivatives from organosolv lignin with a yield higher than 35%;
3) The electrooxidation of biosustainable cyclohexanol to synthesise propyladipic acid with a yield of up to 70%;
4) A biorefinery process capable of: accommodating renewable energy fluctuations without loss in efficiency; exhibits a 95% improvement in the energy efficiency of the process and a 350% improvement in resource efficiency; and produce 29 times less CO2 than the conventional petrochemical alternatives.
1) The obtention of vanillin from kraft lignin with a 7% yield;
2) To synthesize mixed phenolic derivatives from organosolv lignin with a yield higher than 35%;
3) The electrooxidation of biosustainable cyclohexanol to synthesise propyladipic acid with a yield of up to 70%;
4) A biorefinery process capable of: accommodating renewable energy fluctuations without loss in efficiency; exhibits a 95% improvement in the energy efficiency of the process and a 350% improvement in resource efficiency; and produce 29 times less CO2 than the conventional petrochemical alternatives.
The definition of the initial system requirements was performed in WP1 during the first reporting period and the optimisation of the three processes is being performed in WP2. Various organosolv lignins were produced and evaluated together with various kraft lignins and the reactions of the different processes were optimized. Based on these results, reactors were designed, built and tested at lab-scale for all three processes. For the downstream process, separation concepts are being evaluated using membrane, ion exchange resins and other techniques. The influence of renewable energy sources (RES) fluctuation was examined, the effect of the RES fluctuation on yield was investigated. The implementation of the processes optimized in WP2 into a flow system is in progress in WP3. During this period, the activities have mainly been focused on: a) the development of simulation modules for the processes; b) optimization of several types of electrodes, focused on the materials, reactor for the implementation and chemical processes; c) evaluation of different separation techniques; and d) set up of a bench scale system for the vanillin-phenolic and propyl adipic processes. The techno economic validation (WP4) started in M27 with the definition of the battery limits for the economic and environmental evaluation. The “Test case definition” was successfully closed with an initial data set for the end-users where the coupling of the LIBERATE vanillin-phenolic process will be evaluated. The basics for the LCA, economic and process modelling were established and a comprehensive coupling between the project and in-situ renewable energy sources was developed. In WP5, the pilot plant for the demonstration of the vanillin-phenolic process has been designed and built and the reactor system is commissioned in full operation. The industrial demonstration of the concept of LIBERATE is being performed in WP6. The production of organosolv lignin and lignin fractionations for their applications as antioxidant and phenol formaldehyde resins is being performed as well as the transformation of products to market products is being evaluated by different end-users: CHIMAR, OXIRIS, MEGARA and EVONIK. In WP7, exploitation strategy and business plans of LIBERATE are under constant developing. The IP horizon scanning and network patent analyses (NPA) have been updated. Furthermore, two exploitation workshops have been organized, one on IPR strategy and focused on developing individual Value Proposition Canvases. The work on the second iteration of business plans is ongoing. It will include detailed descriptions of all value proposition canvases generated during this reporting period. In WP8 the Midpoint dissemination activities review, the 2nd report of completed and planned communication activities and the Research data management Plan were delivered. LIBERATE organized a joined webinar with PERFORM, about organic electrochemistry: “Towards a sustainable Chemical industry in 2030”.
LIBERATE achieved the production in batch of vanillin from commercial kraft lignin with up to 6 %wt of yield, at least, three times higher than the actual commercial process and 92% effectiveness. The best results about the propyl adipic acid production showed an obtention yield around a 35% of yield and the depolymerization of organosolv lignin in aqueous media is showing promising results with yields of around 70%. The transfer of the reactions to larger electrode surface and consequently a larger area was established without significant changes regarding yield or selectivity.
Various organosolv lignins were produced from softwood, hardwood and herbaceous biomass under various fractionation conditions and staged lignin precipitation and evaluated together with various kraft lignins. The different processes and reactions were optimized (reactions conditions, electrodes and corrosion studies). Based on these results, reactors were designed, built and tested at lab-scale for all three processes. For the downstream process, separation concepts are being evaluated using membrane, ion exchange resins and other techniques. The influence of renewable energy sources (RES) fluctuation was examined, simulations were created based on weather data and the effect of the RES fluctuation on yield was investigated.
The pilot plant for the demonstration of the vanillin-phenolic process has been designed and built and the reactor system is commissioned in full operation with current densities > 400 mA/cm2 without any observed damage or loss of performance and selectivity while parts of the downstream separation process are currently in the commissioning phase. This pilot plant will produce material that will be validated by the end users during the last period of the project. During the project, a total of 8 exploitable results have been identified and a more detailed business plan will be created for each of the results, as the project progress.
Various organosolv lignins were produced from softwood, hardwood and herbaceous biomass under various fractionation conditions and staged lignin precipitation and evaluated together with various kraft lignins. The different processes and reactions were optimized (reactions conditions, electrodes and corrosion studies). Based on these results, reactors were designed, built and tested at lab-scale for all three processes. For the downstream process, separation concepts are being evaluated using membrane, ion exchange resins and other techniques. The influence of renewable energy sources (RES) fluctuation was examined, simulations were created based on weather data and the effect of the RES fluctuation on yield was investigated.
The pilot plant for the demonstration of the vanillin-phenolic process has been designed and built and the reactor system is commissioned in full operation with current densities > 400 mA/cm2 without any observed damage or loss of performance and selectivity while parts of the downstream separation process are currently in the commissioning phase. This pilot plant will produce material that will be validated by the end users during the last period of the project. During the project, a total of 8 exploitable results have been identified and a more detailed business plan will be created for each of the results, as the project progress.