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Lignin Biorefinery Approach using Electrochemical Flow

Periodic Reporting for period 3 - LIBERATE (Lignin Biorefinery Approach using Electrochemical Flow)

Reporting period: 2021-10-01 to 2023-03-31

As one of the most abundant and renewable organic polymers found on Earth, lignin has the potential to be converted into a range of environmentally friendly, value-added products – including chemicals but nowadays the vast majority of this lignin is incinerated as a low-value, high-polluting fuel. LIBERATE’s main objective was the development of an electrochemical pilot plant to demonstrate the commercial opportunities of converting low-cost lignin feedstock into high value bio sustainable chemicals but other two processes were also evaluated and demonstrated at TRL 4 and 5. The commercial opportunities of the products were evaluated by 5 industrial end-users.

The vanillin-phenolic process was validated at TRL 6 with the construction and demonstration of an electrochemical pilot plant at SINTEF. This process produces vanillin and phenolic mixtures from kraft or organosolv lignin thanks to the oxidizer PODIC and a yield of 8 % of vanillin was achieved. The phenolic mixture was evaluated by Chimar for the production of phenol formaldehyde adhesives and by Oxiris as antioxidants. Vanillin was evaluated by Perstorp for the production of different vanillin derivatives.
The 3-propyl adipic acid (3PAA) process was validated at TRL 5 with demonstration of an electrochemical bench scale reactor at JGU for the production of 3PAA from propylcyclohexanol. A yield of 48 % of 3PAA was achieved and the produced material was evaluated by Megara for the production of unsaturated polyester resins and saturated polyester resins for powder coatings and by Evonik for the synthesis of lignin-derived dicarboxylic acids and polyamide.
The direct electrochemical degradation process of organosolv lignin was validated at TRL 4 with the process validation at the University of Alicante for the production of phenolic mixtures. Different separation techniques were evaluated and 80 % of yield was achieved.
The LIBERATE project finalized in March 2023 after 54 months of work and it was structured in 9 WPs and three reporting periods. The definition of the initial system requirements was performed in WP1 during the first reporting period and the system design, process optimization and chemistry development of the three LIBERATE processes was performed in WP2 and WP3. WP4 was dedicated to developing an initial techno-economic analysis and life cycle assessment based on a preliminary process model including information from the end-users and technology providers and the optimization of the integration of the LIBERATE system with renewable energy sources. WP5 was dedicated to the construction and commissioning of the pilot plant for the demonstration of the vanillin-phenolic process and the demonstration of the direct coupling of the two pre-pilot systems for vanillin-phenolic and propyl adipic acid processes to PV panels as renewable energy source. WP6 was focused on the optimization of the production and optimisation of end products for validation in end-user applications, including techno economical evaluations, life cycle analysis and validation of commercial upscaling. The vanillin phenolic process pilot was in operation for more than 1300 hours, first for the sample production for end-user testing (CHIMAR, OXIRIS and Perstorp) followed by process optimization to improve the technoeconomic evaluation of the process. The 3- propyl adipic acid bench scale system was used to produced samples for end-user testing (EVONIK and MEGARA). Techno-economical validation of the vanillin-phenolic process and updates of the life cycle assessments were carried out. In addition, production of organosolv lignin and lignin fractionations for phenol formaldehyde resins and antioxidant raw material was also performed in WP6. The exploitation of the project was carried out in WP7 with the creation of a viable business plan to maximize the chances of post-project commercial success of the nine identified key exploitable results and to assure that the project IP and results are adequately protected. Dissemination and communications activities were covered in WP8 with the preparation of the project video, the celebration of three webinars and the dissemination activities of project partners. The coordination of LIBERATE project was covered in WP9.

In terms of project objectives, the vanillin phenolic process was validated at TRL 6 with the construction and demonstration of an electrochemical pilot plant for the production of vanillin and phenolic mixtures from kraft or organosolv lignin thanks to the oxidizer PODIC and a yield of 8 % of vanillin was achieved. The phenolic mixture was evaluated by Chimar for the production of phenol formaldehyde adhesives and by Oxiris as antioxidants. Vanillin was evaluated by Perstorp for the production of different vanillin derivatives. Renewable energy fluctuations without loss in efficiency was achieved. The 3-propyl adipic acid (3PAA) process was validated at TRL 5 with demonstration of an electrochemical bench scale reactor for the production of 3PAA from propylcyclohexanol. A yield of 48 % of 3PAA was achieved and the produced material was evaluated by Megara for the production of unsaturated polyester resins and saturated polyester resins for powder coatings and by Evonik for the synthesis of lignin-derived dicarboxylic acids and polyamide. The direct electrochemical degradation process of organosolv lignin was validated at TRL 4 with the process validation for the production of phenolic mixtures. Different separation techniques were evaluated and 80 % of yield was achieved.

The biorefinery process showed a 37 % improvement in the energy efficiency of the process with a 97 % reduction in CO2 emissions but with an increased by at least 37 % in resource efficiency.
The vanillin phenolic process was validated at TRL 6 with the construction and demonstration of an electrochemical pilot plant for the production of vanillin and phenolic mixtures from kraft or organosolv lignin thanks to the oxidizer PODIC and a yield of 8 % of vanillin was achieved. The phenolic mixture was evaluated by Chimar for the production of phenol formaldehyde adhesives and by Oxiris as antioxidants. Vanillin was evaluated by Perstorp for the production of different vanillin derivatives. Renewable energy fluctuations without loss in efficiency was achieved. The 3-propyl adipic acid (3PAA) process was validated at TRL 5 with demonstration of an electrochemical bench scale reactor for the production of 3PAA from propylcyclohexanol. A yield of 48 % of 3PAA was achieved and the produced material was evaluated by Megara for the production of unsaturated polyester resins and saturated polyester resins for powder coatings and by Evonik for the synthesis of lignin-derived dicarboxylic acids and polyamide. The direct electrochemical degradation process of organosolv lignin was validated at TRL 4 with the process validation for the production of phenolic mixtures. Different separation techniques were evaluated and 80 % of yield was achieved.

The biorefinery process showed a 37 % improvement in the energy efficiency of the process with a 97 % reduction in CO2 emissions but with an increased by at least 37 % in resource efficiency.
Flow Electrochemical Cell LIBERATE
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