Newcastle University Process Intensification Group Adam Harvey Process Intensification Group Chemical Engineering & Advanced Materials Newcastle University

“P.I.” Process Intensification “The strategy of making dramatic* reductions in the size of process plant items by re-examining the fundamentals of their heat and mass transfer” *at least anorder of magnitude

Process Intensification Group [PIG] 5 academic staff: Adam Harvey (OBRs, biofuels) Kamelia Boodhoo (SDRs, polymerisation) Jonathan Lee (RPBs, carbon capture) David Reay (heat pipes, all HT) Sharon Orta (algae, fuel cells) 5 research associates & visitors 18 PhDs http://pig.ncl.ac.uk

PI @ Newcastle: Technologies/Expertise Oscillatory Baffled Reactors Spinning Disc Reactors Rotating Packed Beds Heat Pipes Reactive Extraction Microreactors Heterogeneous catalysis Application Areas High throughput screening Heterogeneous Catalysis Crystallization Biofuels & biorefining Polymerisation Thermal management: use of waste heat Bioprocessing

Case Study 1: A Saponification reaction in an Oscillatory Baffled Reactor

OBR characteristics Long residence times in a compact reactor, whilst maintaining plug flow and good two phase mixing. Niche: BATCH  CONTINUOUS For “long” processes

The Reaction Hydrolysis of a naturally occurring mixture of alkyl and steryl stearates, using concentrated sodium hydroxide in an ethanol and water solvent. 75 m3 Batch Reactor [50 m3 fill] 115 oC 2h "reaction time” in a 24h batch cycle Molar ratio ~ 0.9

Incentives for Change SAFETY Product quality Energy savings

Experiments Conducted Temperature fixed at 115 oC Molar ratios in the range 0.6 - 1.05 Residence times in the range 8 - 25 minutes TARGET PRODUCT Desired product, sterol A > 23 % Undesired product, sterol B < 10 %

Can it be done ?

Effect of Temperature

SUMMARY: OBR Saponification The OBR could be used to perform the reaction: ..at lower temperature ..with improved product quality ..more consistently ..in a reactor 1/100th the volume The product can be monitored Operation is flexible

Biofuel Research Projects Reactive Extraction (Biodiesel) Rapeseed [PhD] Malaysian Govt Jatropha + other inedible [PhD] UKIERI Reactor engineering [PhD] Malaysian Govt Algae [RA] Carbon Trust Oscillatory Baffled Reactors: Bioethanol production [PhD] Nigerian Govt Biobutanol production [PhD] Malaysian Govt/TSB Biodiesel screening [PDRA] EPSRC Catalysis: Heterogeneous, Biodiesel [PhD] EPSRC Vegetable oil cracking [PhD] Nigerian Govt Catalytic cracking of algae [PDRA] Carbon Trust + various other biofuel/biorefining projects

Case Study2 : Direct Production of Biodiesel from Oilseeds (“Reactive Extraction”) Whole seeds Drying Crushing & Solvent Extraction: capital and running cost intensive. usually performed in very large, centralised plants (to achieve economies of scale) Also: solvent extraction uses Hexane Maceration Hexane CRUSHING Solvent Extraction Meal Refining Transesterification can actually be carried out from the plant seeds without prior extraction of the oil. In this scheme, the seeds are crushed And fed directly into the reactor where both extraction and transesterification simulatneosly take place. In this case, your methanol or ethanol behaves as Both the reactant and the solvents. Transesterification Glycerol Purification Waste water Methanol + NaOH Biodiesel

Biodiesel Production: Reactive Extraction Whole seeds Whole seeds Drying Grinding Grinding Hexane CRUSHING Solvent Extraction Meal Refining Transesterification can actually be carried out from the plant seeds without prior extraction of the oil. In this scheme, the seeds are crushed And fed directly into the reactor where both extraction and transesterification simulatneosly take place. In this case, your methanol or ethanol behaves as Both the reactant and the solvents. Transesterification Reactive Extraction Meal Glycerol Purification Waste water Purification Glycerol Methanol + NaOH Methanol + NaOH Waste water Biodiesel Biodiesel

Biodiesel Production: Reactive Extraction Whole seeds Whole seeds 1. Farm Drying Maceration 2. Oil plant Maceration Hexane CRUSHING Solvent Extraction Meal Refining Transesterification can actually be carried out from the plant seeds without prior extraction of the oil. In this scheme, the seeds are crushed And fed directly into the reactor where both extraction and transesterification simulatneosly take place. In this case, your methanol or ethanol behaves as Both the reactant and the solvents. 3. Biodiesel Plant Reactive Extraction Meal Transesterification Glycerol Purification Glycerol Purification Waste water Methanol + NaOH Waste water Methanol + NaOH Biodiesel Biodiesel Reactive Extraction / In situ transesterification

Biodiesel Production: Reactive Extraction Whole seeds Whole seeds Drying Farm? Maceration Maceration Hexane CRUSHING Solvent Extraction Meal Refining Transesterification can actually be carried out from the plant seeds without prior extraction of the oil. In this scheme, the seeds are crushed And fed directly into the reactor where both extraction and transesterification simulatneosly take place. In this case, your methanol or ethanol behaves as Both the reactant and the solvents. Reactive Extraction Meal Transesterification Glycerol Purification Glycerol Purification Waste water Methanol + NaOH Waste water Methanol + NaOH Biodiesel Biodiesel Reactive Extraction / In situ transesterification

Biodiesel Production: From Oilseed to Final Product Whole seeds Reactive Extraction Benefits Reduced number of unit operations ( reduced CapEx) Eliminate use of hexane Reduction in production cost? Potential for small-scale and local operation Maceration Transesterification can actually be carried out from the plant seeds without prior extraction of the oil. In this scheme, the seeds are crushed And fed directly into the reactor where both extraction and transesterification simulatneosly take place. In this case, your methanol or ethanol behaves as Both the reactant and the solvents. Reactive Extraction Meal Purification Glycerol Methanol + NaOH Waste water Biodiesel Reactive Extraction / In situ transesterification

Biodiesel Direct from Seed: “Reactive Extraction” Alcohols + Catalyst Biodiesel Reactive Extraction Oilseeds Glycerol Meal Demonstrated for rapeseed and jatropha Reactor development underway More water-tolerant than conventional process Jatropha meal may be more edible May facilitate distributed production? Basis of biorefinery?

Ongoing Project: Algal Biofuels WEAB: Water-tolerant Extraction of Algal Biofuels () Aims: Remove or reduce drying duty Integrate reaction with other steps Technologies: Reactive Extraction Catalytic Cracking Supercritical Extraction

Algae harvesting by foam fractionation Algal Biofuels Algae harvesting by foam fractionation Foam column concentrates algae Macroalgae gasification NB: Newcastle University unique in having Marine Science and Chemical Engineering. Various collaborations underway and in development

PIG: Summary Wide range of technologies Wide range of application areas Particular focus on biofuels currently

Before

After

Acknowledgments Dr Jon Lee Dr Rabitah Zakaria Dr Anh Phan Dr Sharon Velasquez Orta Hafizuddin Wan Yusof Farizul Kasim Elizabeth Eterigho Nasratun Masngut Joseph Ikwebe