soluble phosphate concentration, while treatments at 350 ◦ C lead to greater phosphorus recovery in the solid

Overview

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Key numbers

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• sewage sludge hydrothermal treatment. Journal of Environmental Management, 2025, 381, pp.125239.
• ⟨10.1016/j.jenvman.2025.125239⟩. ⟨hal-05039217⟩
• HAL Id: hal-05039217
• https://hal.science/hal-05039217v1
• Distributed under a Creative Commons CC BY 4.0 - Attribution - International License
• Aix-Marseille Univ., CNRS, Centrale Med, M2P2 UMR 7340, Marseille, France
• wastewater treatment plant, was treated in a batch reactor at temperatures from 250 to 350 ◦ C for 5–45 min.
• phosphorus speciation. Treatments at 250–300 ◦ C promote organic phosphorus mineralization and increase
• soluble phosphate concentration, while treatments at 350 ◦ C lead to greater phosphorus recovery in the solid
• 1. Introduction 2022), but global reserves are expected to be depleted in the coming
• including in Europe (Bixio et al., 2006), and wastewater treatment is a develop a more sustainable anthropogenic P cycle and to avoid nutrients
• emphasize wastewater as a resource rather than waste (Kehrein et al., 2021b). Legislation has already moved in this direction by restricting
• 2020). Moreover, wastewater treatment plants (WWTPs) are increas­ sludge disposal and imposing P/N discharge limits (Directive
• ingly viewed as important hubs for the recovery of different resources 91/271/EEC).
• tile fatty acids, and CO2 (Kehrein et al., 2020). Most of these resources adsorption, ion exchange, ammonia stripping and the precipitation of N,
• by-product of SS anaerobic digestion for bio-gas production. (NH4MgPO4⋅6H2O), K-struvite (KMgPO4⋅6H2O), hydroxyapatite
• SS digestates contains important amounts of nitrogen(N), phos­ (Ca10(PO4)6(OH)2), and, more generally, calcium phosphate (Di Cos­
• phorus(P) and potassium(K), the three primary macronutrients central tanzo et al., 2021).
• and P fertilizers production is not sustainable (Cordell et al., 2009; gasification) have proven effective in converting various biomasses,
• Penuelas et al., 2023; Walling and Vaneeckhaute, 2022). P fertilizers including SS digestates, into valuable by-products such as hydrochar,
• production relies on extraction from natural apatite rocks (Zhu et al., biofuel, syngas, and other chemicals (Huang and Yuan, 2016). These
• (Biller and Ross, 2012). During HT treatments, the altered properties of environmental compatibility is assessed with a critical analysis of the
• ered in the solid by-products (hydrochars and ashes) (Zhu et al., 2022), 2. Materials and methods
• (Schnell et al., 2020). Hydrochars and ashes can be repurposed as fer­ 2.1. Sewage sludge digestate collection and preparation
• on the macronutrients relative content and pollutants such as heavy Fig. 1 shows a schematization of the experimental protocol. The SS
• recovery during wet biomass HT treatments (Aragón-Briceño et al., of France (175000 population equivalent). The collected SS digestate
• 2021; Huang et al., 2017; Liu et al., 2021b). Possible N reaction path­ contains a low total solids (TS) content (2.5 %). It was concentrated by
• ways have been identified and elucidate, suggesting that most of N is centrifugation at 4000 rpm for 20 min (Sigma 2-16P centrifuge), pro­
• recovered in the liquid by-product, but underlining the presence of ducing a thickened sludge with a higher TS content (6.7 %) that was
• incorporation in heterocycles (Aragón-Briceño et al., 2021). In the same products have been stored in sealed plastic containers and refrigerated
• way, there is a general understanding of P conversion mechanisms and at 4 ◦ C.
• schemes remain incomplete (Huang et al., 2017) and the interaction 2.2. Hydrothermal treatment experiments
• products involve gas stripping or struvite precipitation for the liquid 110 g of thickened SS digestate in a 0.2 L austenitic chromium-nickel-
• chars (Aragón-Briceño et al., 2021; Liu et al., 2021b). Less studies are wire system in the reactor jacket and cooled with the injection of cooled
• P-complexes speciation and thus to increase P fertilizer bio-availability The reactor is operated between 250 and 350 ◦ C for a time of 5–45 min.
• and efficiency (Huang et al., 2017). Moreover, the HT products need Pressurization and inerting of the reaction medium are managed with N2
• compatibility (heavy metals content and other contaminants). This a N2 pressure of 18 MPa. Mixing is provided with a Rushton turbine at
• would allow to integrate nutrients reclamation and energetic valoriza­ 700 rpm. At the end of treatment, the HT product is collected and cen­
• tion, leading to novel chains for digestate utilization. This is particularly trifugated at 4000 rpm for 20 min (Sigma 2-16P centrifuge), separating
• proper disposal, which has become a critical bottleneck in anaerobic containers and refrigerated at 4 ◦ C.
• digestion and biogas production (Brebbia and Itoh, 2016).
• mainly within the HTC range of 180–280 ◦ C (Tangredi et al., 2023). The TS contents of the thickened digestate feed and the solid pellet

Methods (brief)

• process parameters (temperature, time) on phosphorus behavior. A sewage sludge digestate, sampled from a
• by-product of SS anaerobic digestion for bio-gas production. (NH4MgPO4⋅6H2O), K-struvite (KMgPO4⋅6H2O), hydroxyapatite
• metals. digestate used in this study was collected from the Aix-La Pioline WWTP,
• recovery during wet biomass HT treatments (Aragón-Briceño et al., of France (175000 population equivalent). The collected SS digestate
• would allow to integrate nutrients reclamation and energetic valoriza­ 700 rpm. At the end of treatment, the HT product is collected and cen­
• digestion and biogas production (Brebbia and Itoh, 2016).
• More recent studies demonstrated that HTL of SS realized in a temper­ by-product were characterized by drying 3 g of wet samples at 105 ◦ C
• tions, allowing to observe the transition between these two processes tent. Ash content is determined by exposing the dried sample at 900 ◦ C
• reflect the short residence times typical of HTL(Tangredi et al., 2023). is calculated by difference. The dried solid digestate and pellet samples
• Unlike previous studies, which mainly used autogenic conditions (0.5 g of dried sample) have been mineralized with 8 mL of aqua regia
• This approach helps to clarify the individual impacts on P conversion (Zn) concentrations of the aqua regia digestion extracts were determined
• and HT product characteristics and allows investigation of P speciation by inductively coupled plasma atomic emission spectroscopy (ICP-AES)
• The by-products are comprehensively characterized through a novel measured by inductively coupled plasma mass spectrometry (ICP-MS)
• cess water were characterized by drying the samples at 105 ◦ C (EN evaluated with the ANOVA (ANalysis Of VAriance) test while the sta­
• measures were performed by a density meter (Anton Paar DMA 5000 M). the combination of propagated uncertainty and standard deviation, for
• The alkalinity of liquid samples was determined according to standard the measurements realized multiple times. For heavy metals content,
• Total P, Ca, Fe, Al, Mg and K concentrations in liquid samples were blanks. All chemicals used were of analytical grade.
• copy (ICP-AES) (Jobin Yvon Horiba Ultima-C).

Implications

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