Upcycling of recycled agrifood materials and pilot scaling (public summary)

This project has received funding from the European Union’s Horizon 2020 research and innovation programme under grant agreement N° 101036838. D4.5 – Upcycling of recycled agrifood materials and upscaling August 2025 Authors: José M. de la Torre Ramírez (DMC); José M. García Madero (DMC) Ref. Ares(2025)6411325 - 06/08/2025 A2C – Deliverable D4.5v2.0 Page 2 І23 Technical references Project Acronym Agro2Circular Project Title TERRITORIAL CIRCULAR SYSTEMIC SOLUTION FOR THE UPCYCLING OF RESIDUES FROM THE AGRIFOOD SECTOR Project Coordinator Fuensanta Monzó CETEC [email protected] Project Duration October 2021 – March 2025 (42 months) Deliverable No. D4.5. Dissemination level* PU Work Package WP 4 – Upcycling of recycled agrifood materials and upscaling Task T4.1 – Formulation of the extracts at small scale T4.2 – Pilot scale up of the optimal extraction routes Lead beneficiary 17 (DMC) Contributing beneficiary/ies 13 (CTNC); 14 (MCT); 15 (ALM); 18 (CITRO); 19 (SAIREM); 20 (SSICA); 39 (LOL) Due date of deliverable 30 September 2024 Actual submission date 11 October 2024 * PU = Public PP = Restricted to other programme participants (including the Commission Services) RE = Restricted to a group specified by the consortium (including the Commission Services) CO = Confidential, only for members of the consortium (including the Commission Services) A2C – Deliverable D4.5v2.0 Page 3 І23 Document history V Date Comments v0.1 7/10/2024 First draft of document v0.2 10/10/2024 Revised version based on the comments of Jean David Peltier and Fuensanta Monzé from CETEC v1.0 11/10/2024 First final version, approved by the WP leader and the project coordinator, submitted to EC. v2.0 06/08/2025 New version including comments on cosmetics formulations submitted to EC Document Distribution Log Version Date Distributed to v0.1 07/10/2024 Jean David Peltier and Fuensanta Monzé from CETEC V0.2 10/10/2024 José Manuel de la Torre from DMC V1.0 11/10/2024 Project Coordinator V2.0 06/08/2025 Project Coordinator Verification and approval Name Date Verification Final Draft by WP leader José Manuel de la Torre Ramírez 06/08/2025 Approval Final Deliverable by coordinator Fuensanta Monzó 06/08/2025 A2C – Deliverable D4.5v2.0 Page 4 І23 Disclaimer and acknowledgement This project has received funding from the European Union’s Horizon 2020 research and innovation programme under grant agreement No 101036838 Disclaimer This document reflects only the views of the author(s) the European Research Executive Agency (REA) is not responsible for any use that may be made of the information it contains. Whilst efforts have been made to ensure the accuracy and completeness of this document, the A2C consortium shall not be liable for any errors or omissions, however caused. A2C – Deliverable D4.5v2.0 Page 5 І23 Table of contents List of abbreviations ……………………………………………………. 7 1 Introduction .................................................................................. 8 2 Formulations of the extracts at small scale.................................. 9 2.1 Key Outcomes ..................................................................................................... 9 2.2 Conclusion ......................................................................................................... 11 3 Pilot scale-up of route 1 including equipment adaptations ........ 12 3.1 Key Outcomes ................................................................................................... 13 3.2 Conclusion ......................................................................................................... 15 4 Pilot scale-up of route 2 including equipment adaptations. ....... 16 4.1 Development and assembly of the Microwave extractor. .............................. 16 4.2 Facilities conditioning. ...................................................................................... 17 4.3 Key Outcomes ................................................................................................... 18 4.4 Conclusion ......................................................................................................... 19 5 Validation of the extraction pilot scale up. ................................. 20 5.1 Conclusion ......................................................................................................... 21 6 WP4 General conclusions ......................................................... 22 A2C – Deliverable D4.5v2.0 Page 6 І23 List of Figures Figure 1. Juice enriched with flavonoids lemon extract (left). Jam formulation with apple fibre extract (right)....................................................................................................... 10 Figure 2. Nutraceutical samples prepared with different formulations............................... 10 Figure 3. Route 1 flowchart for obtaining bioactives from organic agri-food waste........... 12 Figure 4. Ultrasound-assisted extraction technology adapted for continuous flow operation..................................................................................................................... 13 Figure 5. Final extract of (a) phenolic compounds and (b) fibre........................................ 14 Figure 6. Route 2 flowchart for obtaining bioactives from organic agri-food waste........... 16 Figure 7. MW extractor and facilities for Demonstrator 4 after conditioning...................... 17 A2C – Deliverable D4.5v2.0 Page 7 І23 List of abbreviations WP → Work package EAE → Enzymatic assisted extraction MEA → Microwave assisted extraction UAE → Ultrasound assisted extraction MW → Microwaves LCA → Life Cycle Assessment LCC → Life Cycle Costing F&V → Fruits and Vegetables US → Ultrasound A2C – Deliverable D4.5v2.0 Page 8 І23 1 Introduction This document provides a public summary of the work carried out under Work Package 4 (WP4) of the Agro2Circular (A2C) project, which focuses on the upcycling of recycled agrifood materials and their scale-up. The deliverable compiles and summarises the main outcomes and advancements achieved throughout WP4, describing the processes and results obtained in Deliverables 4.1, 4.2, 4.3, and 4.4. The activities in WP4 primarily revolved around the development, formulation, and pilotscale upscaling of extraction techniques to recover valuable bioactive compounds from agrifood residues, including fibres and phenolic compounds. These efforts aim to transform agricultural waste into high-value products that can be used in food, nutraceutical, and cosmetic applications, aligning with the project's circular economy principles. This public summary outlines the scope of the work covered, highlighting the technological innovations developed and the successful upscaling of extraction routes. It serves as a bridge to the detailed results discussed in each deliverable, including the small-scale formulation of bioactive extracts (D4.1), the scaling up of enzymatic and ultrasound-assisted extractions (D4.2), the implementation of microwave-assisted extraction (D4.3), and the validation of these methods at the pilot scale (D4.4). By summarising these achievements, this public report aims to present the key findings in a manner accessible to both technical and non-technical audiences, emphasizing the project's contribution to enhancing the sustainability and circularity of the agrifood sector. A2C – Deliverable D4.5v2.0 Page 9 І23 2 Formulations of the extracts at small scale The Agro2Circular (A2C) project aims to demonstrate the potential of upcycling agricultural residues, particularly from the food industry, into high-value formulations for food, nutraceutical, and cosmetic applications. The goal is to develop sustainable products by incorporating bioactive extracts from agrifood waste, aligning with circular economy principles. D4.1 – “New formulations based on the extracts" provides technical information on the smallscale formulation of food and nutraceutical products. The formulations incorporate bioactive compounds, such as antioxidants and fibres, extracted from waste products such as fruits, vegetables, and other agricultural by-products. The final products are designed to meet both consumer demands and technical specifications, paving the way for potential large-scale production (to be conducted in future work packages). 2.1 Key Outcomes 1. Food Formulations: Several partners in the project developed new food formulations, including: o Vegetable Desserts: Extracts of apple and lemon were tested to enrich desserts with fibre. While apple extract performed well in terms of taste, challenges with texture arose. Lemon extract's bitterness limited its use in sweet products. o Veggie Burgers: Artichoke fibre extract was identified as the most promising for enhancing the nutritional value of veggie burgers, providing both fibre content and acceptable taste and texture. o Juices and Jams: Lemon peel extracts were incorporated into juices and jams to enrich them with fibre and flavonoids. Adjustments in formulation improved consumer acceptance, though higher concentrations of extracts resulted in changes to taste and appearance. A2C – Deliverable D4.5v2.0 Page 16 І23 4 Pilot scale-up of route 2 including equipment adaptations. This section relates also to Task 4.2 and is fully detailed in Deliverable D4.3, which describes the scale-up of extraction and purification methodologies for recycling organic agri-food waste, but now implementing route 2. This route focuses on the microwave-assisted extraction (MAE) of bioactive compounds like polyphenols and soluble fibres from agri-food waste, specifically artichoke and lemon Figure 6. Route 2 flowchart for obtaining bioactives from organic agri-food waste 4.1 Development and assembly of the Microwave extractor. The microwave system used for extraction in Route 2 was designed and assembled by SAIREM for pilot-scale operations. This system combines microwave and ultrasound technologies to enhance extraction efficiency through their synergistic effects. • Equipment Specifications: The reactor has a maximum capacity of 120 Liters, with adjustable microwave power ranging from 600 W to 6,000 W, and ultrasound power from 200 W to 1,400 W. It is made of stainless steel, easy to clean, and equipped with a variable-speed mechanical stirrer and a temperature control system. • Prototype Development: Initially, a 20-liter tank was developed to validate the concept, before scaling up to the 120-liter version. The final design included A2C – Deliverable D4.5v2.0 Page 17 І23 additional features such as an automated opening system for the lid and adjustable tank height to accommodate various containers for unloading. This equipment was critical for scaling up the microwave-assisted extraction (MAE) process to handle larger volumes of agri-food waste efficiently. 4.2 Facilities conditioning. To accommodate the microwave extraction system, DMC had to modify its facilities significantly. The lab space, initially an empty storage area, was conditioned with thermal and acoustic insulation to meet the equipment's requirements. Thermal control was essential to maintain temperatures between 5°C and 40°C, especially for the machine's electrical components, while acoustic insulation was necessary to reduce noise from the ultrasound probes, which could reach levels of up to 150 dB. Additionally, power supply, air conditioning, and water connections were installed to ensure the optimal functioning of the equipment. Figure 7. MW extractor and facilities for Demonstrator 4 after conditioning A2C – Deliverable D4.5v2.0 Page 18 І23 4.3 Key Outcomes • Raw Materials: The main raw materials used are lemon and artichoke waste, with plans to extend the extraction process to grape waste in future, pending availability due to seasonality. • Microwave-Assisted Extraction (MAE): The primary goal is to scale up the MAE process, which has proven effective at the laboratory level, for semi-industrial use. The methodology uses a combination of microwaves and enzymatic treatment to optimize the extraction of bioactive compounds from waste materials. During the initial treatment it was used pectinase to hydrolyse the cell walls of fruit and vegetable residues, enhancing the release of fibres and polyphenols. Following EAE, microwave extraction further breaks down cellular structures to recover more polyphenols in a short amount of time. • Green Solvents: The extraction process employs eco-friendly hydroalcoholic solutions (water and ethanol) to align with the project’s sustainability goals, minimizing chemical waste. • Purification: Polyphenols and fibres are purified using ultrafiltration and resin purification (Diaion HP20 resin). These processes concentrate the bioactive compounds to achieve polyphenol content above 70%, meeting project specifications. The extracted compounds are stabilized by drying or freeze-drying, depending on their final use in food, nutraceutical, or cosmetic products The MAE process significantly increased the polyphenol content in lemon and artichoke extracts when it is compared with the enzymatic treatment alone. The antioxidant capacity of the lemon extract was particularly notable, even exceeding that of the artichoke extract, likely due to the presence of other bioactive compounds such as organic acids. Soluble fibres extraction also achieved high yields, with the highest concentrations found in artichoke waste. As it was previously mentioned, the absence of grape waste due to seasonal availability delayed the processing of this material, but future work will include its extraction. A2C – Deliverable D4.5v2.0 Page 19 І23 The optimization of the purification and stabilization stages, particularly the removal of solvents, demands considerable time and energy, potentially affecting industrial scalability. Further improvements will be investigated through the Life Cycle Assessment (LCA) and Life Cycle Costing (LCC) studies to enhance efficiency and ensure viability at scale. The MAE process will be further tested in Demonstrator 4 (WP6) to validate its scalability and effectiveness in industrial settings. Additionally, the leftover waste from the extraction process will be used as a carbon and nitrogen source in yeast fermentation for bio-based product development (WP5). 4.4 Conclusion The pilot-scale implementation of MAE for the extraction of polyphenols and fibres from agrifood waste demonstrates a viable and sustainable solution for upscaling. While some adjustments are needed to optimize fibres purification and reduce energy consumption, the project has successfully met key milestones in achieving extract purity and scalability targets. The results will be disseminated at various scientific events and published in openaccess journals to support further research and industrial adoption. A2C – Deliverable D4.5v2.0 Page 20 І23 5 Validation of the extraction pilot scale up. This section relates also to Task 4.2 and is fully detailed in Deliverable D4.4, which describes the results of the characterization analysis performed during the scale-up of two extraction routes developed within the Agro2Circular (A2C) project. The objective of this analysis was to validate the scalability of the extraction processes initially optimized at the laboratory scale and to assess their effectiveness when applied at a pilot scale. This section involved a comprehensive evaluation of extracts derived from residues of lemon, artichoke, broccoli, apple, and grape. Two primary types of extracts were assessed: fibre extracts and phenolic extracts. For each type, the characterization included an in-depth analysis of their composition, microbiological quality, and the presence of specific contaminants, following standard methodologies. The evaluation aimed to ensure that the extracts met the required quality standards for their potential applications in food, nutraceutical, and cosmetic industries. The results confirmed that the fibre extracts achieved a purity milestone of ≥ 70%, with artichoke and lemon residues showing the highest extraction yields and purity levels. Improvements in the extraction processes, such as optimized purification techniques and reduced water consumption, led to higher-quality extracts compared to the laboratory scale. Phenolic extracts also demonstrated significant concentrations of polyphenols, with compounds like hesperidin, eriocitrin, and chlorogenic acid present in substantial amounts. These findings highlight the viability of these extracts for use as active ingredients in various formulations, supporting their potential commercial value. Microbiological tests confirmed the safety of the extracts, with no detection of harmful microorganisms such as Salmonella or Listeria monocytogenes, and minimal levels of mould, yeast, and E. coli. These results underline the reliability and safety of the extraction processes, crucial for industries that require high standards of product purity and consistency. A2C – Deliverable D4.5v2.0 Page 21 І23 Furthermore, the validation of the pilot-scale extraction confirms the scalability of the technologies employed, ensuring that the quality and composition of the extracts can be consistently replicated on a larger scale. This reproducibility is essential for meeting regulatory requirements in the food and nutraceutical sectors, where product consistency is critical to market approval and consumer acceptance. 5.1 Conclusion WP4 emphasizes the importance of valorising agrifood residues by transforming them into high-value resources, thereby promoting a circular economy approach. By demonstrating that waste from the agrifood sector can be upcycled into valuable compounds, the Agro2Circular project contributes to reducing environmental impact and enhancing sustainability within the industry. This aligns with the European Union’s Horizon 2020 research and innovation framework, which supports innovative solutions to environmental challenges and resource efficiency. The successful scale-up of the extraction routes not only validates the technical feasibility of these processes but also positions the A2C project as a pivotal initiative in advancing circular economy practices in the agrifood sector. The insights gained from this study will guide further development and optimization of upcycling strategies, paving the way for a more sustainable and resilient agrifood value chain. A2C – Deliverable D4.5v2.0 Page 22 І23 6 WP4 General conclusions The Agro2Circular (A2C) project has successfully demonstrated the viability of upcycling agrifood waste into valuable bioactive compounds through innovative extraction and formulation techniques. The pilot-scale implementations of both enzymatic and microwaveassisted extraction processes confirmed that these methods can effectively recover highpurity fibre and phenolic extracts from agricultural residues, such as lemon, artichoke, and grape. Key findings indicate that the optimized extraction techniques not only achieve significant yields but also maintain the quality and bioactive properties of the compounds, making them suitable for applications in food, nutraceutical, and cosmetic products. The project's emphasis on using sustainable and green technologies, such as eco-friendly solvents and energy-efficient methods, aligns with the goals of enhancing resource efficiency and promoting circular economy principles within the agrifood sector. The use of environmentally friendly methodologies, combined with equipment like the microwave extractor designed for the project, which has enabled these processes to be scaled up beyond the laboratory, represents significant progress in the valorisation of agrifood residues, with a focus on the industrialization of the products obtained. Despite some challenges encountered in the stabilization processes and water consumption, the progress made in the upscaling efforts has set a strong foundation for future large-scale industrial applications. The project’s achievements in improving the scalability and reproducibility of these techniques highlight its potential to transform agrifood residues into valuable ingredients, thereby reducing waste and supporting a more sustainable production cycle. The insights gained from this work will guide further optimization of the extraction routes and the development of new bio-based products, positioning the A2C project as a key contributor to advancing circular economy practices and valorisation of agrifood waste. A2C – Deliverable D4.5v2.0 Page 23 І23 The results obtained in this Work Package 4 will enable the successful implementation of Demonstrators 3 and 4 included in WP6, ensuring a solid foundation for these large-scale validations. Furthermore, these findings will support the precise execution of the Life Cycle Assessment (LCA) and Life Cycle Costing (LCC) analyses to be developed in WP7. These analyses are critical for evaluating the environmental and economic impact of the upscaled extraction processes, guiding the project toward sustainable and cost-effective solutions that align with the overarching goals of the Agro2Circular initiative. By integrating these assessments, the project aims to enhance its contribution to a circular economy in the agrifood sector, ensuring that resource efficiency and sustainability remain at the core of its innovations. Finally, the methodologies developed here are likely to be replicated in different regions and with various agrifood residues. During WP7, the replicability of the work carried out in this WP4 will be described in the regions of Lombardy and Lithuania. The analysis will focus on identifying which vegetable and fruit residues are most abundant in these regions, and their polyphenol and fibre content will be described.