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NaOH ALKALINE School of Chemical Engineering Unit of Environmental - - PowerPoint PPT Presentation

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National Technical University of Athens NaOH ALKALINE School of Chemical Engineering Unit of Environmental Science & Technology PRETREATMENT FOR IMPROVEMENT OF ENZYMATIC DIGESTIBILITY OF WHEAT STRAW AS AL TERNATIVE SUGAR J. Novakovic,

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7th International Conference on Sustainable Solid Waste Management, 26-29 June 2019, Heraklion, Crete Island, Greece

NaOH ALKALINE PRETREATMENT FOR IMPROVEMENT OF ENZYMATIC DIGESTIBILITY OF WHEAT STRAW AS AL TERNATIVE SUGAR SOURCE

  • J. Novakovic, N. Kontogianni, E.M. Barampouti, S. Mai, D.

Malamis, M. Loizidou

National Technical University of Athens School of Chemical Engineering Unit of Environmental Science & Technology

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7th International Conference on Sustainable Solid Waste Management, 26-29 June 2019, Heraklion, Crete Island, Greece

Agricultural Waste Biorefjnery

Forster-Carneiro, T., Berni, M. D., Dorileo, I. L., & Rostagno, M. A. (2013). Biorefjnery study of availability of agriculture residues and wastes for integrated biorefjneries in

  • brazil. Resources,

Conservation and Recycling, 77, 78-88.

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7th International Conference on Sustainable Solid Waste Management, 26-29 June 2019, Heraklion, Crete Island, Greece

  • Lignocellulosic material

corn stover on a fjeld credit: USDOE-NRE https://www.greenoptimistic.com

The major barrier to the enzymatic hydrolysis of carbohydrates towards the production of fermentable sugars

https://www.e- education.psu.edu/egee439/node/606

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7th International Conference on Sustainable Solid Waste Management, 26-29 June 2019, Heraklion, Crete Island, Greece

Pretreatments

Removal of lignin is favorable to reducing the recalcitrance

  • f lignocellulose for enzymatic attack.
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7th International Conference on Sustainable Solid Waste Management, 26-29 June 2019, Heraklion, Crete Island, Greece

A/A Reagent T Solid :Liquid (w/w) Time i H2O2 (5%) NaOH (pH=11,5) 50°C 1:20 1h ii H2O2 (10%) NaOH (pH=11,5) 50°C 1:20 1h iii NaOH 0.5M 50°C 1:10 96 h iv NaOH 0.5M 121°C 1:10 1h v CH5N 25 %w/w 50°C 1:10 96 h vi CH5N 25 %w/w 121°C 1:10 1h vii Na2CO3 0.5M 50°C 1:10 96 h viii Na2CO3 0.5M 121°C 1:10 1h ix NH3 25 %w/w 50°C 1:10 96 h x NH3 25 %w/w 121°C 1:10 1h

tested

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7th International Conference on Sustainable Solid Waste Management, 26-29 June 2019, Heraklion, Crete Island, Greece

Saccharifjcation of alkaline pretreated straw

1 2 3 4 5 6 7 8 9 10 11 10 20 30 40 50 60 70 80 90 100 50 100 150 200 250 300 %cellulose degradation Pretreatment methods % m g g l u c

  • s

e / g s t r a w

(i) alkaline peroxide 5%, (ii) alkaline peroxide 10%, (iii) NaOH 0.5M, (iv) NaOH 0.5M autoclaving, (v) methylamine 25 %w/w, (vi) methylamine 25 %w/w autoclaving, (vii) Na2CO3 0.5M, (viii) Na2CO3 0.5M autoclaving, (ix) ammonia 25 %w/w, (x) ammonia 25 %w/w autoclaving.

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7th International Conference on Sustainable Solid Waste Management, 26-29 June 2019, Heraklion, Crete Island, Greece

AIM

Optimisation of the NaOH pretreatment process along with the enzymatic hydrolysis in order to obtain more fermentable sugars and glucose recovery

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7th International Conference on Sustainable Solid Waste Management, 26-29 June 2019, Heraklion, Crete Island, Greece

Origin: From Aspropyrgos province, Greece

Raw material - Wheat straw

Parameter Value (% w/w) Cellulose 33.8 Hemicellulose 45.1 Lignin 16.4 Klason lignin 15.4 Acid-soluble lignin 1.0 Ash 4.7

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7th International Conference on Sustainable Solid Waste Management, 26-29 June 2019, Heraklion, Crete Island, Greece

Optimisation Parameters

Particle Size Enzyme Loading Recycling of alkaline solution Pretreatment Kinetics

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7th International Conference on Sustainable Solid Waste Management, 26-29 June 2019, Heraklion, Crete Island, Greece

PARTICLE SIZE

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7th International Conference on Sustainable Solid Waste Management, 26-29 June 2019, Heraklion, Crete Island, Greece

Particle Size- Experimental procedure

Comminution

  • FRITSCH Cutting

mill Pulverisette 15

  • Particle size

1mm

  • Particle size 10-

20mm

NaOH pretretment

  • NaOH 0.5M
  • S/L: 1/10 w/w
  • Autoclaved at

121°C for 1 h

Enzymatic Hydrolysis

  • 10% w/w dry

solid

  • 15μL g-1 dry

solid (CellicCT ec2)

  • 50°C and 300

rpm for 96 h

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7th International Conference on Sustainable Solid Waste Management, 26-29 June 2019, Heraklion, Crete Island, Greece

Particle Size

Efgect of particle size on enzymatic hydrolysis of pretreated straw

Conclusion The particle size in the range of 1 to 20mm didn’t afgect signifjcantly the performance of the pretreatment scheme

TOC Glucose 100 200 300 400 500 600 1mm mg/g pretreated straw

10 20 30 40 50 60 70 80 90 100 1mm %

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7th International Conference on Sustainable Solid Waste Management, 26-29 June 2019, Heraklion, Crete Island, Greece

ENZYME LOADING

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7th International Conference on Sustainable Solid Waste Management, 26-29 June 2019, Heraklion, Crete Island, Greece

Enzyme Loading- Experimental procedure

Comminution

  • Particle size 10-

20mm

NaOH pretretment

  • NaOH 0.5M
  • S/L: 1/10 w/w
  • Autoclaved at

121°C for 1 h

Enzymatic Hydrolysis

  • 10% w/w dry

solid

  • 50°C and 300

rpm for 96 h

  • Cellic CTec2 5,

10, 15 and 20 μL/g pretreated straw

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7th International Conference on Sustainable Solid Waste Management, 26-29 June 2019, Heraklion, Crete Island, Greece

Enzyme Loading

Efgect of enzyme loading on the straw solubilization and cellulose degradation during enzymatic hydrolysis

Conclusion

15 μL/g pretreated straw was selected as the

  • ptimum

cellulase dosage

% cellulose degradation TOC (mg/g pretreated straw) Glucose (mg/g pretreated straw) % c e llu lo s e d e g r a d a t io n 0 5 10 15 20
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7th International Conference on Sustainable Solid Waste Management, 26-29 June 2019, Heraklion, Crete Island, Greece

ALKALINE SOLUTION RECYCLING

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7th International Conference on Sustainable Solid Waste Management, 26-29 June 2019, Heraklion, Crete Island, Greece

Alkaline solution Recycling- Experimental procedure

Comminution

  • Particle size 10-

20mm

NaOH pretretment

  • NaOH solution

recycled

  • S/L: 1/10 w/w
  • Autoclaved at

121°C for 1 h

Enzymatic Hydrolysis

  • 10% w/w dry

solid

  • 50°C and 300

rpm for 96 h

  • Cellic 15 μL/g

pretreated straw

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7th International Conference on Sustainable Solid Waste Management, 26-29 June 2019, Heraklion, Crete Island, Greece

Alkaline solution Recycling

Cycle No %TS hydrolysis %cellulose degradation %AIL degradation %ASL degradation %hemicellulose degradation 1 36.6 1 ± 0.1 2 2.74 ± 0.26 86.36 ± 2.1 6 99.5 4 ± 2.84 51.7 1 ± 2.59 2 30.1 6 ± 0.2 1 4.12 ± 1.47 79.51 ± 3.5 8 99.4 8 ± 2.93 26.3 4 ± 2.31 3 26.8 ± 0.3 2 7.34 ± 1.61 72.21 ± 5.2 3 99.4 1 ± 3.65 15.6 7 ± 3.26 4 30.0 8 ± 0.7 8 8.50 ± 2.44 76.47 ± 2.4 5 99.4 1 ± 5.62 44.0 2 ± 6.19 5 14.0 3 ± 0.1 3 5.05 ± 2.63 65.96 ± 1.3 6 99.3 8 ± 3.18 23.6 5 ± 4.36

Solid fractions’ degradation after the difgerent cycles of pretreatment of wheat straw.

Conclusion

The alkaline solution could be recirculated at least 4 times before being “saturated” although after each experiment it needed to be supplemented with some fresh solution.

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7th International Conference on Sustainable Solid Waste Management, 26-29 June 2019, Heraklion, Crete Island, Greece

PRETREATMENT KINETICS

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7th International Conference on Sustainable Solid Waste Management, 26-29 June 2019, Heraklion, Crete Island, Greece

Pretreatment Kinetics - Experimental procedure

Comminution

  • Particle size 10-

20mm

NaOH pretretment

  • NaOH 0.5M
  • S/L: 1/10 w/w
  • 50°C for 0-96 h

Enzymatic Hydrolysis

  • 10% w/w dry

solid

  • 50°C and 300

rpm for 96 h

  • Cellic 15 μL/g

pretreated straw

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7th International Conference on Sustainable Solid Waste Management, 26-29 June 2019, Heraklion, Crete Island, Greece

Pretreatment Kinetics

Conclusion

In the time interval of 3-5h of pretreatment, the delignifjcation effjciency reached its maximum and remained statistically constant the rest 90h. Timeline of total organic carbon (g/L) and delignifjcation effjciency (%) during NaOH 0.5M pretreatment at 50°C

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7th International Conference on Sustainable Solid Waste Management, 26-29 June 2019, Heraklion, Crete Island, Greece

SCALE-UP

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7th International Conference on Sustainable Solid Waste Management, 26-29 June 2019, Heraklion, Crete Island, Greece

Scaling-up - Experimental procedure

5g/batch Vreactor= 250mL 200g/batch Vreactor= 4L 3000g/batch Vreactor= 200L

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7th International Conference on Sustainable Solid Waste Management, 26-29 June 2019, Heraklion, Crete Island, Greece

Scaling-up

5 200 3000 20 40 60 80 100 120 %Delignifjcation VFA (mg/gstraw) Phenols (mg/gstraw) Capacity (g/batch)

NaOH pretreatment step

5 200 3000 50 100 150 200 250 300 Capacity (g straw/batch) Glucose (mg/g straw)

Saccharifjcation step

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7th International Conference on Sustainable Solid Waste Management, 26-29 June 2019, Heraklion, Crete Island, Greece

CONCLUSIONS

NaOH pretreatment 50oC, 5h Enzymatic Hydrolysis 50oC CelliCT ec 10.5μL/g straw Straw 1kg NaOH 0.5M 6.25kg Hydrolysate 7kg mg/L TSS 23000 VSS 21390 TOC 30507 VFA 6387 Phenols 127 Glucose 37444 mg/L TSS 3000 VSS 2700 TOC 29256 VFA 976 Phenols 125 Exhausted Alkaline Solution 1,25kg

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7th International Conference on Sustainable Solid Waste Management, 26-29 June 2019, Heraklion, Crete Island, Greece

The authors acknowledge funding through European Horizon 2020 NoAW (No Agro Waste, Grant no. 688338) project for supporting this work.

Acknowledgements