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Technological routes for production of new bio-products from the Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials. I JORNADAS VIRTUALES INTERNACIONALES Adaptación de Proyectos Agroalimentarios, Forestales y Enológicos a los principios del ODS

Technological routes for production of new bio-products from the Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials.

AUTHORS Rilton Gonçalo Bonfim Primo| Federal University of Bahia (UFBA), Brazil. Genyr Kappler | University of Vale do Rio dos Sinos (UNISINOS), Brazil.

TUTORS: Carlos Alberto Mendes Moraes | UNISINOS, Brazil. Luís António da Cruz Tarelho | University of Aveiro (UA), Portugal Jesús Martín-Gil | Valladolid University (UVA), Spain Fernando Cardoso Pedrão | Federal University of Bahia (UFBA), Brazil. Carlos Narciso Bouza | The Habana University (UH), Cuba Ricardo de Araújo Kalid | Federal University of Southern Bahia (UFSB), Brazil. 19, Marzo – 2021 – Palencia, España Technological routes for production of new bio-products from the Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials. COCOA POD HUSK PROBLEMS - Relative Quantity

COCOA POD HUSK – CPH

• Waste of chocolate industries

67 % to 76 % • Ten tons of wet CPH are generated for each ton of dry cocoa beans. 8,7 to 9,8 % • It constitutes 67 % to 76 % of 2,1 % to 2,3 % the weight of the cocoa fruit

21 % to 23 %

Source: Adapted of R. Campos-Vega et al. , 2018, with information of Babatope, 2005; Oddoye, Agyente-Badu & Gyedu-Akpto, 2013; Awarikabey et al., 2014; Sobowale el atl., 2015; Papalexandrator & Nielsen, 2016; *By difference. AdaptedTechnological from FAOSTAT, 2017. routes for production of new bio-products from the Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials. COCOA POD HUSK Cultivation and production of cocoa and CPH from top ten countries.

Dry Cocoa Beans Production CPH Country Tonnes % Tonnes % Cote D'Ivoire 1 472 313 35,46 14 723 130 35,46 Ghana 858 720 20,68 8 587 200 20,68 Indonesia 656 817 15,82 6 568 170 15,82 Cameroon 291 512 7,02 2 915 120 7,02 Nigeria 236 521 5,70 2 365 210 5,70 Brazil 213 843 5,15 2 138 430 5,15 Ecuador 177 551 4,28 1 775 510 4,28 Peru 107 922 2,60 1 079 220 2,60 Dominican Republic 81 246 1,96 812 460 1,96 Colombia 56 163 1,35 561 630 1,35

Source: Author’s elaboration with dates from FAOSTAT, 2017. Technological routes for production of new bio-products from the Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials. COCOA POD HUSK OBJECTIVES

 Identify, in the recent literature on CPH biorefinery (last 5 years):

• conceptual interrelations, • main research countries, • main areas, • bibliographic connections and publication chronology.

 Examine technological routes of extraction of bioproducts and subsequent pyrolysis of CPH and other agricultural waste.

 Describe and discuss experiments with controlled pyrolysis reactors and their applications in different agricultural waste. Technological routes for production of new bio-products from the Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials. COCOA POD HUSK

LITERATURE REVIEW: Portal Periódicos of CAPES: MATERIALS AND METHODS • Every year • Last five years Preliminary literature review step: Selection of approach lines and search terms required prospecting tests and previous Scopus database: studies. • Articles • Portal Periódicos of CAPES: 536 international reference bases • Peer reviewed https://www-periodicos-capes-gov-br.ezl.periodicos.capes.gov.br/index.php? • In the final state of • Central bibliographic database publication Web of Science • Posted in journals https://login.webofknowledge.com/error/Error?Error=IPError&PathInfo=%2F&RouterURL=https%3A%2F%2Fwww.webofk nowledge.com%2F&Domain=.webofknowledge.com&Src=IP&Alias=WOK5 Last update: Scopus https://www.elsevier.com/pt-br/solutions/scopus • Mar 14, 2021 • VOSViewer: for statistical analysis and graph generation. Technological routes for production of new bio-products from the DATABASE: Scopus Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials. SEARCH CODE: COCOA POD HUSK ALL (cocoa AND pod AND h RESULTS I usk AND biorefinery) DOCUMENTS: 141

RESULTS II SEARCH CODE: all ( cocoa and pod and husk and biorefinery ) and ( limit- to ( pubstage , "final" ) ) and ( limit- to ( pubyear , 2021 ) or limit- to ( pubyear , 2020 ) or limit- to ( pubyear , 2019 ) or limit- to ( pubyear , 2018 ) or limit- to ( pubyear , 2017 ) ) and ( limit - to ( srctype , "j" ) ) and ( exclude ( subjarea , "phys" ) )

DOCUMENTS: 98

Source: Author's elaboration based on researched data through Scopus, Mar 14, 2021, Technological routes for production of new bio-products from the Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials. DATABASE: Scopus COCOA POD HUSK RESULTS III Articles by Area SEARCH CODE: all ( cocoa and pod and husk a Health Professions nd biorefinery ) and ( limit- Medicine to ( pubstage , "final" ) ) and ( Pharmacology, Toxicology and Pharmaceutics limit- Business, Management and Accounting to ( pubyear , 2021 ) or limit- Economics, Econometrics and Finance to ( pubyear , 2020 ) or limit- Social Sciences to ( pubyear , 2019 ) or limit- to ( pubyear , 2018 ) or limit- Immunology and Microbiology to ( pubyear , 2017 ) ) and ( li Materials Science mit- Engineering to ( srctype , "j" ) ) and ( exclu Agricultural and Biological Sciences de ( subjarea , "phys" ) ) Biochemistry, Genetics and Molecular Biology Chemistry DOCUMENTS: 98 Chemical Engineering Environmental Science Source: Author's elaboration based Energy on researched data through Scopus, 0 5 10 15 20 25 30 35 40 45 Mar 14, 2021, Technological routes for production of new bio-products from the Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials. Connections between the central concepts DATABASE: Scopus SEARCH CODE: all ( cocoa and pod and husk a nd biorefinery ) and ( limit- to ( pubstage , "final" ) ) and ( limit- to ( pubyear , 2021 ) or limit- to ( pubyear , 2020 ) or limit- to ( pubyear , 2019 ) or limit- to ( pubyear , 2018 ) or limit- to ( pubyear , 2017 ) ) and ( li mit- to ( srctype , "j" ) ) and ( exclu de ( subjarea , "phys" ) )

DOCUMENTS: 98

Source: Author's elaboration based on researched data through Scopus, Mar 14, 2021, with statistical treatment through the VOSviewer. Technological routes for production of new bio-products from the Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials. COCOA POD HUSK Connections between the central research countries

DATABASE: Scopus

SEARCH CODE: all ( cocoa and pod and husk a nd biorefinery ) and ( limit- to ( pubstage , "final" ) ) and ( limit- to ( pubyear , 2021 ) or limit- to ( pubyear , 2020 ) or limit- to ( pubyear , 2019 ) or limit- to ( pubyear , 2018 ) or limit- to ( pubyear , 2017 ) ) and ( li mit- to ( srctype , "j" ) ) and ( exclu Source: Author's elaboration based on researched data through Scopus, Mar 14, 2021, with statistical de ( subjarea , "phys" ) ) treatment through the VOSviewer. DOCUMENTS: 98 Technological routes for production of new bio-products from the Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials. COCOA POD HUSK Chronology between the central research countries

DATABASE: Scopus

Source: Author's elaboration based on researched data through Scopus, Mar 14, 2021, with DOCUMENTS: 98 statistical treatment through the VOSviewer. Technological routes for production of new bio-products from the Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials. COCOA POD HUSK DISCUSSION I: Extraction methods and properties

In biorefinery systems, several technological processes can be applied to convert biomass feedstock into marketable products.

This classification approach identifies four main subgroups of processes

1. Mechanical/physical (e.g., pressing, pre-treatment, milling, separation, distillation) 2. Biochemical (e.g., anaerobic digestion, aerobic and anaerobic fermentation, enzymatic conversion) 3. Chemical processes (e.g., hydrolysis, transesterification, hydrogenation, oxidation, pulping) 4. Thermochemical (e.g., pyrolysis, gasification, hydro-thermal upgrading, combustion) Technological routes for production of new bio-products from the Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials. COCOA POD HUSK CPH – Pectin and Extractants • Extraction optimization of pectin with ascorbic acid using response surface methodology The filtrate was mixed with 95 % ethanol (1:2, v/v) to precipitate the pectin. After 24 h at 4 °C, the pectin was removed by centrifugation at 10 rpm for 10 min. (F. Priyangini et al., 2018). • Optimized conditions employing aqueous nitric acid as an extractant Pectin gels (0.99 % galacturonic acid equivalent, w/w) were prepared at pH 2.5-3.0 in the presence of 60% sucrose (w/w). (Life Science Weekly, 2017). • Extraction and characterization of pectin with citric acid From the fitted model, extraction conditions with aqueous citric acid at pH 3.0 for 95 min at 95 C provided a predicted yield of approximately 9.0 g/100 g dry cacao pod husks (L.C. Vriesmann et al., 2012) Technological routes for production of new bio-products from the Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials. COCOA POD HUSK Operational parameters of pyrolysis to characterize the resulting CPH biochar

More important: Easily decomposed by thermochemical processing, • treatment excellent raw material for the temperature production of biochars. • residence time (%) / • pyrolysis onset temperature

between 200 °C and 450 °C with Weigh Important: 55 % weight loss • heating rate • peak temperature for maximum • feeding particle size weight loss at 320 °C. Temperature / (oC)

Source: Adapted of Chi-Hung Tsai, Wen-Tien Tsai & Sii- Chew Liu, Yu-Quan Lin, 2017. Technological routes for production of new bio-products from the Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials. COCOA POD HUSK CPH treated by pyrolysis to produce oil The pyrolysis oil from CPH contained : . Ketones . Carboxylic Acids . Aldehydes . Furans . Heterocyclic Aromatics . Alkyl Benzenes . Phenols Source: Mansur, et all., 2014 . Benzenediols Sources: Adi-Dako et al., 2016; Campos-Vega et al., 2018; Ghysels et al., 2020; Handojo et al., 2020; Kilama et al., 2019; Mansur et al., 2014; “New Findings on Biological Macromolecules from Federal University Summarized (Cacao Pod Husks as a Source of Low- Methoxyl , Highly Acetylated Pectins Able to Gel in Acidic Media ),” 2017; Ouattara et al., 2021; Priyangini et al., 2018; Putri et al., 2019; Rhein-Knudsen et al., 2018; C. H. C.-H. Tsai et al., 2018; W.-T. W. T. Tsai & Huang, 2018; Valadez-Carmona et al., 2017; Vriesmann et al., 2011, 2012; Yusof et al., 2016) Technological routes for production of new bio-products from the PROCESSING OF Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials. AGRICULTURAL WASTE

DISCUSSION II : before, during and after pyrolysis

Compared to the energy-driven biorefineries, the classification of material- driven biorefinery systems might need further specification as the subgroup ‘chemicals and building blocks’ is very large and with heterogenous composition. Technological routes for production of new bio-products from the PROCESSING OF Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials. AGRICULTURAL WASTE

Biorefinery combined system to produce material products

Source: Adapted from Cherubini et al., 2009. 17 Technological routes for production of new bio-products from the PROCESSING OF Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials. AGRICULTURAL WASTE

Technology readiness level for thermochemical processes

Thermochemical process Main product Process phase Product upgrading phase

Combustion Heat (flue gas) TRL 9 TRL 9

Gasification Syngas TRL 9 TRL 5-6

Fast pyrolysis Pyrolysis oil TRL 5-8 TRL 3-5

Slow pyrolysis Charcoal / Biochar TRL 9 TRL 9 / (TRL ?)*

Torrefaction Torrefied biomass TRL 7-8 TRL 9

* TRL for biochar is unknown because the applications of this material are still under development. Emphasis also added by source authors. Source: Adapted from charcoal KIC INNOENERGY, 2015; ORTWEIN; LENZ, 2015.

18 Technological routes for production of new bio-products from the PYROLYSIS OF Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials. AGRICULTURAL WASTE Pyrolysis process Reactor types:

Bosnic kiln (semi-continuous) Earth pits for charcoal making Brazilian beehive kiln

Source: FAO, 1987.

Source: Emrich, 1985; FAO, 1987. Source: Authors, 2020.

19 Technological routes for production of new bio-products from the PYROLYSIS OF Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials. AGRICULTURAL WASTE Pyrolysis process Reactor types: Rotary drum (continuous) Auger reactor (continuous)

Heating systems: Pyrolysis kiln Pyrolysis reactor

Source: Ronsse; Nachenius; Prins, 2015. 20 Technological routes for production of new bio-products from the PYROLYSIS OF Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials. AGRICULTURAL WASTE

Pyrolysis process

Important operating parameters:

. Particle Size . Heating Rate . Residence Time (Particle) . Residence Time (Gas) . Pyrolysis Temperature . Type of Biomass

21 Technological routes for production of new bio-products from the PYROLYSIS OF Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials. AGRICULTURAL WASTE Pyrolysis feedstock: General scope and objectives

MAIN OBJECTIVE: . Convert biomass waste into biochar SPECIFIC OBJECTIVES: . Access biomass properties; . Produce bio-oil, gas and char; . Characterize products and understand the effect of operating conditions over the yield and properties of biochar; . Obtain mass and energy balance;

. Simulation of continuous biochar rector. 22 Technological routes for production of new bio-products from the PYROLYSIS OF Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials. AGRICULTURAL WASTE Pyrolysis products

The goal of the research:

Source: Basu, 2013; Neves, Thunman, Matos et al, 2019. Technological routes for production of new bio-products from the PYROLYSIS OF Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials. AGRICULTURAL WASTE Biochar production (Pyrolysis reactions inside the reactor) I

Source: Adapted from Neves, 2013. 24 Technological routes for production of new bio-products from the PYROLYSIS OF Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials. AGRICULTURAL WASTE

Biochar production (Pyrolysis reactions inside the reactor) II TG / (%) / TG

Temperature / (oC)

TG (%) / TG DTG (%/min) / DTG

Temperature / (oC) Temperature / (oC) Source: Adapted of ÇEPELIOĞULLAR et al., 2018 Technological routes for production of new bio-products from the Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials. MAIN CONCLUSIONS • CPH is an abundant waste raw rich in useful and marketable nutrients. • The processes of extracting bioproducts by bio-refining methods and subsequent obtaining of pyrolysis derivatives optimize the potentials of CPH. • The available technologies can be applied to cacao, but also to other agro-forest residues, in a sustainable and accessible way for small and medium-sized enterprises. Technological routes for production of new bio-products from the Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials.

PROSPECTS TO RESEARCHES • To determine the chemical index of efficiency of pyrolysis and biorefines. • To determine logistical boundaries for the viability of CPH biorefineries according to volume, prices, characteristics and distances. • To project and operate a pilot plant for micro-biorefinery combined with pyrolysis for CPH for small and medium producers. Technological routes for production of new bio-products from the Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials. REFERENCES I

1. Adi-Dako, O., Ofori-Kwakye, K., Frimpong Manso, S., Boakye-Gyasi, M. EL, Sasu, C., & Pobee, M. (2016). Physicochemical and Antimicrobial Properties of Cocoa Pod Husk Pectin Intended as a Versatile Pharmaceutical Excipient and Nutraceutical. Journal of Pharmaceutics, 2016, 1–12. https://doi.org/10.1155/2016/7608693 2. BASU, P. Biomass gasification, pyrolysis, and torrefaction: Practical design and theory. second ed. [S. l.]: Elsevier Inc., 2013. E-book. 3. Campos-Vega, R., Nieto-Figueroa, K. H., & Oomah, B. D. (2018). Cocoa (Theobroma cacao L.) pod husk: Renewable source of bioactive compounds. Trends in Food Science and Technology, 81(September), 172–184. https://doi.org/10.1016/j.tifs.2018.09.022 4. CHERUBINI, F. et al. Toward a common classifi cation approach for biorefi nery systems. [S. l.], 2009. Disponível em: https://doi.org/10.1002/bbb.172. Acesso em: 17 abr. 2020. 5. ÇEPELIOĞULLAR, Ö. et al. 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Cocoa bean skin waste as potential raw material for liquid smoke production. Environmental Technology (United Kingdom), 41(8), 1044– 1053. https://doi.org/10.1080/09593330.2018.1520306 11. KIC INNOENERGY. Energy from Chemical Fuels. Strategy and Roadmap 2015-2019. [S. l.: s. n.]. Disponível em: www.kic-innoenergy.com. Acesso em: 2 mar. 2020. 12. Kilama, G., Lating, P. O. P. O., Byaruhanga, J., & Biira, S. (2019). Quantification and characterization of cocoa pod husks for electricity generation in Uganda. Energy, Sustainability and Society, 9(1). https://doi.org/10.1186/s13705-019-0205-4 13. Mansur, D., Tago, T., Masuda, T., & Abimanyu, H. (2014). Conversion of cacao pod husks by pyrolysis and catalytic reaction to produce useful chemicals. Biomass and Bioenergy, 66, 275–285. https://doi.org/10.1016/j.biombioe.2014.03.065 Technological routes for production of new bio-products from the Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials. REFERENCES II 15. 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F., & Petkowicz, C. L. D. O. (2011). Optimization of nitric acid-mediated extraction of pectin from cacao pod husks (Theobroma cacao L.) using response surface methodology. Carbohydrate Polymers, 84(4), 1230–1236. https://doi.org/10.1016/j.carbpol.2011.01.009 25. Yusof, F., Khanahmadi, S., Amid, A., & Mahmod, S. S. (2016). Cocoa pod husk, a new source of hydrolase enzymes for preparation of cross-linked enzyme aggregate. SpringerPlus, 5(1), 1–18. https://doi.org/10.1186/s40064-015-1621-3 Technological routes for production of new bio-products from the Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials.

Este trabajo se realizó con el apoyo de la Coordinación de Perfeccionamiento del Personal de Educación Superior - Brasil (CAPES) - Código de Financiamiento 001, y por el CAPES PRINT - Programa de Internacionalización Institucional (Proceso 88887.468908 / 2019-00) y por el Programa de Doctorado Sandwich en el Extranjero (PDSE - 88881.189947 / 2018-01.

Gracias al CNPq - Brasil, por el apoyo financiero otorgado a la subvención Desarrollo Tecnológico y Extensión Innovadora - DT2 de uno de los autores.

_____

This study was financed in part by the Coordenação de Aperfeiçoamento de Pessoal de Nível Superior – Brasil (CAPES) – Finance Code 001, and by CAPES PRINT - Institutional Internationalization Program (Process 88887.468908 / 2019-00) and by the Sandwich Doctorate Program Abroad - 88881.189947 / 2018-01.

Thanks to CNPq – Brazil, for the financial support given the grant Technological Development and Innovative Extension – DT2 of one of the authors. Technological routes for production of new bio-products from the Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials.

ACKNOWLEDGMENTS

The University of Valladolid (UVA), Spain, in the person of Prof. Dr. Jesús Martín-Gil, for receiving and guiding our investigations.

The University of Aveiro (UA), Portugal, in the person of Professor Dr. Luís António da Cruz Tarelho in guiding the doctorate internship of Genyr Kappler in the (DAO) Department of Environment and Planning. Technological routes for production of new bio-products from the Cocoa Pod Husk – CPH (Theobroma cacao) and other agricultural wasted materials.

¡Thanks for the attention!

CONTACTS: Rilton Gonçalo B. Primo Research Program in Industrial Engineering | PEI-UFBA Amalia Soler Street, 171, ground floor, door 2, Vilafranca del Penedès, Barcelona, PC 08720, Spain. +34 6203-2971 | +55 71 99705-0564 | [email protected]

Genyr Kappler Graduate Program in Civil Engineering at the University of Vale do Rio dos Sinos – UNISINOS +5551985313071 | [email protected] | [email protected]