Liquid fuels from sewage sludge through direct acid ethanolysis
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1 Liquid fuels from sewage sludge through direct acid ethanolysis Luigi di Bitonto, Vito Locaputo, Carlo Pastore Water Research Institute (IRSA), National Research Council (CNR), via F. de Blasio 5, Bari, Italy
2 Outlook Chemical characterization of sewage sludge Chemical exploitation of sewage sludge through ethanolysis Optimization of reactive conditions: fundamental study Valorization of sewage sludge through direct ethanolysis: feasibility study Conclusions
3 WWTPs PE PE PE Putignano PE
4 Primary Settlement Sewage scum Primary sludge Secondary sludge Mixed sludge Biological Oxidation
5 Sewage Scum Primary Sludge Secondary Sludge 20% 12% 4% 11% 24% 4% 11% 22% 25% 9% 0% 5% 9% 44% 22% 17% 23% 38% Mixed Sludge 20% 24% 4% 9% 23% 20% EHS Cellulose (Glucose, Xylose) Lipids (Glycerides, Soaps, FFAs) Proteins HA&L Ashes (Hemicellulose, Pectinic sugars, EPS) >50% Organic Fraction Average values derived by analysis conducted on two different sample per WWTPs in two different period of the year
6 Lipids Characterization 50 FAs S Scum PS SS MS % % % % Glycerides 16,8 0,4 42,9 1,4 Soaps 23,9 90,3 0,0 88,9 FFAs 59,3 9,3 57,1 9,7 % wt S Sc PS SS MS 10 0 C12:0 C14:0 C15:0 C16:1 C16:0 C18:2 C18:1 C18:0 C20:0 FAs Profile of FAs as «fingerprint» of different sewage sludge
7 Structural Sugars Characterization Cellulose EHS 350 Glucose 1 3 Sewage Scum IC HPAED nc Xylose Primary Sludge Secondary Sludge 1: Galactosamine 2: Arabinose 3: Glucosamine 4: Galactose 5: Glucose 6: Mannose + Xylose 50 0 Mixed Sludge Time / min time / min Profiles of EHS as «fingerprint» of different sewage sludge
8 Reactions to be involved in valorization of sewage sludge
9
10 Main objective: To find out reactive conditions capable to convert sewage sludge components in a single step in to the defined target molecules.
11 Lipid Valorization Soaps FFAs FAEEs Direct Trans Esterification Esterification Glycerides Acid Catalysis Base or Acid Catalysis C C to C 2 4 h 2 4 h to h
12 Sugar Valorization : Brønsted acid Catalysed : Lewis acid Catalysed
13 A direct homogeneous Brønsted Lewis acid catalysis was optimised Brønsted Acid: H 2 SO 4 High pressure Reactor Lewis Acid: Aluminium and Iron salts were tested Operative Temperature: 180 C Reaction Time
14 Ethanolysis of glucose E Catalysts Res. G (%mol) Conv. EG (%mol) EF (%mol) EMF +HMF (%mol) EL (%mol) Total (%mol) 1 No catalyst ± ± ± H 2 SO ± ± ± ± AlCl 3. 6H 2 O ± ± ± ± FeCl 3. 6H 2 O ± ± ± ± H 2 SO 4 + AlCl 3. 6H 2 O (0.8 mmol mmol) ± ± ± ± H 2 SO 4 + Al₂(SO₄)₃. 18H₂O ± ± ± ± H 2 SO 4 + Al(NO 3 ) 3. 9H 2 O ± ± ± ± H 2 SO 4 + Al 2 O ± ± ± ± H 2 SO 4 + FeCl 3. 6H 2 O ± ± ± ± H 2 SO 4 + Fe(NO 3 )₃. 9H₂O ± ± ± ± H 2 SO 4 + Fe 2 (SO 4 ) 3. 12H 2 O ± ± ± ± H 2 SO 4 + AlCl 3. 6H 2 O (0.8 mmol mmol) H 2 SO 4 + AlCl 3. 6H 2 O (0.8 mmol mmol) H 2 SO 4 + AlCl 3. 6H 2 O* (0.8 mmol mmol) ± ± ± ± ± ± ± ± ± ± ± ± Al salts were found more active than respective Fe salts In the case of AlCl 3 6H 2 O (30%mol respect to G) a synergic effect with H 2 SO 4 was obtained After only 2 h, about 60% of starting glucose was converted into EL+HMF+EMF Reactive conditions: 180 C, 2h
15 Ethanolysis of simple sugars Glucose (no catalyst) Glucose (H 2 SO 4 ) Glucose (AlCl 3 6H 2 O) Glucose (H 2 SO 4 /AlCl 3 6H 2 O) Galactose (H 2 SO 4 /AlCl 3 6H 2 O) Mannose (H 2 SO 4 /AlCl 3 6H 2 O) Glucosamine (H 2 SO 4 /AlCl 3 6H 2 O) Xylose (H 2 SO 4 /AlCl 3 6H 2 O) Arabinose (H 2 SO 4 /AlCl 3 6H 2 O) F EL EMF+HMF EF EG S Besides EL, HMF and EMF, EG were mostly obtained Ethanolysis occurred efficiently on all sugars and amino sugars Reactive conditions: 180 C, 2h %
16 Ethanolysis of simple sugars: effect of water Glucose (H 2 SO 4 /AlCl 3 6H 2 O) Galactose (H 2 SO 4 /AlCl 3 6H 2 O) Mannose (H 2 SO 4 /AlCl 3 6H 2 O) Glucosamine (H 2 SO 4 /AlCl 3 6H 2 O) Xylose (H 2 SO 4 /AlCl 3 6H 2 O) Arabinose (H 2 SO 4 /AlCl 3 6H 2 O) F EL EMF+HMF EF EG S Solubilization of starting sugars was obtained EGs represent the main products Reactive conditions: 180 C, 2h %
17 Ethanolysis of complex sugars Glucose D W Cellulose EL EG HMF+EMF %mol D 5 Starch D WReaction time: 6 h EL EG 25 HMF+EMF %mol W time / h time / h
18 Ethanolysis of Sewage Sludge (1) Ethanol 6h, 180 C GC FID GC MS IC HPAED Derivatization Sludge Evaluation of RS Characterization
19 Ethanolysis of Sewage Sludge (2) Sludge Lipid Conversion Carbohydrates Conversion Yield of EL Yield of HMF+EMF Yield of F %wt %wt %m* %m* %m** Sewage scum > Primary > Secondary > Mixed > % 100 Results were congruent with RS analysis: EHS, proteins and lipids were completely absent. Cellulose was present in traces and with a different profile: no xylose was found.
20 Ethanolysis of Sewage Sludge (3) Mixed Sludge EL, HMF and EMF Dry conditions 24% 4% 9% 20% FAEEs (Biodiesel) 20% 23% EHS Cellulose Lipids Proteins HA&L Ashes RS
21 Fine chemicals and new materials
22 Ethanolysis of Sewage Sludge (4) Mixed Sludge EGs In presence of water 24% 4% 9% 20% FAEEs (Biodiesel) 20% 23% EHS Cellulose Lipids Proteins HA&L Ashes RS (partial content of cellulose)
23 Ethanolysis of Sewage Sludge (5) EGs Ethanol 6h, 180 C HMF EMF Aminoacids Sludge FAEEs 1 Tonn (as dewatered sludge) MJ/Kg ST RS (45% of starting sludge) 70 Kg of Dry Residual Solids MJ/Kg ST HA&L (25%)
24 Conclusions Direct ethanolysis of sewage sludge was investigated. Through a combined Brønsted Lewis acid ethanolysis, the following main points were achieved: 1. Structural carbohydrates were mainly converted into EL, HMF and EMF under dry conditions, in EGs in presence of water 2. Lipids were always efficiently converted in FAEEs (namely biodiesel): potentially such a process could satisfy about the 20% of the present European Demand of Biodiesel 3. Proteins were also hydrolised and aminoacids were ethyl esterified and preserved in solution by thermal degradation 4. Residual Solids resulted significantly reduced
25 Aknowledgements This study was financially supported by MIUR (ERANETMED Project WE MET) Insert contact picture Luigi di Bitonto PhD/Researcher Insert contact picture Vito Locaputo Collaborator/Technician Insert contact picture Sandro Menegatti Collaborator/Technician
26
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