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MICROWAVES FOR BIODIESEL PRODUCTION

Apr 03, 2018

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    introduction

    need to find clean, efficient ways to perform

    chemistry

    atom economy

    improved product yields

    renewable feedstocks

    energy efficiency

    new chemistry

    microwaves for biodiesel production:

    accelerating the biofuels revolutionUCONN Sustainable Energy Symposium, March 31, 2008

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    introduction

    as a tool for preparative chemistry, microwave

    heating has a number of advantages

    reactions complete in minutes instead of hours

    yields can be improved

    less by-product formation

    new chemistry

    microwaves for biodiesel production:

    accelerating the biofuels revolutionUCONN Sustainable Energy Symposium, March 31, 2008

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    physical chemistry concepts

    only four permitted frequencies for industrial,

    medical and scientific use of microwaves

    915 MHz

    2450 MHz (2.45 GHz)

    5800 MHz (5.80 GHz)

    27120 MHz (27.12 GHz)

    microwaves for biodiesel production:

    accelerating the biofuels revolutionUCONN Sustainable Energy Symposium, March 31, 2008

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    X-rays

    physical chemistry concepts

    ultraviolet infrared microwaves

    10-10 10-9 10-8 10-7 10-6 10-5 10-4 10-3 10-2 10-1 1

    3x1012 3x1010 3x108 3x106 3x104 3x102

    frequency (MHz)

    wavelength (m)

    molecular rotations

    molecular vibrations

    outer-shellelectrons

    inner-shell

    electrons

    radiowavesvisible

    microwaves for biodiesel production:

    accelerating the biofuels revolutionUCONN Sustainable Energy Symposium, March 31, 2008

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    .

    .

    .

    .

    .

    .

    physical chemistry concepts

    conventional heating by conduction

    convection currents

    temperature on the outside surface is greater than that of the contents

    microwaves for biodiesel production:

    accelerating the biofuels revolutionUCONN Sustainable Energy Symposium, March 31, 2008

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    physical chemistry concepts

    microwave irradiation results in direct heating of

    reagents and / or solvents

    microwave heating conventional heating

    microwaves for biodiesel production:

    accelerating the biofuels revolutionUCONN Sustainable Energy Symposium, March 31, 2008

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    new synthetic methods group

    expand microwave technologies and methodologies so thatmicrowave energy becomes the primary tool for scientists in

    any situation where heating and/or long reaction times are

    involved

    http://homepages.uconn.edu/~nil03002/index.html

    research group

    microwaves for biodiesel production:

    accelerating the biofuels revolutionUCONN Sustainable Energy Symposium, March 31, 2008

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    new synthetic methods group

    biologicalchemistry

    emergingareas

    inorganicsynthesis

    organicsynthesis

    microwaveirradiation

    microwaves for biodiesel production:

    accelerating the biofuels revolutionUCONN Sustainable Energy Symposium, March 31, 2008

    research group

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    alternatives to petroleum-based fuels have

    to be found

    biodiesel as an alternative to fossil fuel

    replacement of diesel fuel by biodiesel is something that is immediately

    applicable

    biofuels represent abundant carbon-neutral renewable resources for the

    production of bioenergy

    with little modification, diesel engine vehicles can use biodiesel

    can also be used as heating oil

    accelerating the biofuels revolution

    microwaves for biodiesel production:

    accelerating the biofuels revolutionUCONN Sustainable Energy Symposium, March 31, 2008

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    + MeOHcatalyst

    glycerin biodieselvegetable oil

    O

    ROO

    ROO

    RO

    OH

    OH

    OH

    +

    O

    OMeR

    stoichiometric ratio is 1 : 3 ratios of 1 : 9 1 : 30 usually used

    preparation of biodiesel

    biodiesels are the simple alkyl esters of fatty acids

    generally prepared by vegetable oil by transesterification with methanol

    microwaves for biodiesel production:

    accelerating the biofuels revolutionUCONN Sustainable Energy Symposium, March 31, 2008

    accelerating the biofuels revolution

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    preparation of biodiesel

    preparation of biodiesel

    most commonly used catalysts are NaOH, KOH and H2SO4starting oil and methanol are generally heated to near reflux and stirred with the catalyst

    in the case of the basic catalysts, the base is dissolved in the methanol prior to addition

    microwaves for biodiesel production:

    accelerating the biofuels revolutionUCONN Sustainable Energy Symposium, March 31, 2008

    accelerating the biofuels revolution

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    can biodiesel be made using microwave heating?

    literature survey

    one report of the use of a domestic microwave for reaction between methanol

    and seed oils (J. MW Power Elecromag. Energy 1999, 34, 3)

    scientific microwave apparatus has been used for transesterification of

    triglycerides to fatty acid methyl esters and involves a zeolite catalyst,

    heating to 170 C for 2 h in a sealed vessel and only moderate conversions

    are obtained (C. R. Chemie, 2004, 7, 601)

    three patent applications have been filed - involve use of specially designedapparatus (WO 03/014272 A2, US 0274065 A1, US 0162245 A1)

    accelerating the biofuels revolution

    microwaves for biodiesel production:

    accelerating the biofuels revolutionUCONN Sustainable Energy Symposium, March 31, 2008

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    can biodiesel be made using microwave heating?

    towards a simpler, faster, more efficient modular design

    starting on a small scale in a 125 mL open vessel

    accelerating the biofuels revolution

    + MeOH10 g oil quantitative conversion to biodiesel5 wt % KOH

    MW

    oil to methanol ratio of 1 : 6 heat to 50 C and hold for 1 min

    microwaves for biodiesel production:

    accelerating the biofuels revolutionUCONN Sustainable Energy Symposium, March 31, 2008

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    can biodiesel be made using microwave heating?

    towards a simpler, faster, more efficient modular design

    scaling up the reaction

    using a 1 : 6 oil to methanol ratio and 1 wt% KOH the reaction mixture is heated to 50 C

    and held at this temperature for 1 min

    quantitative conversion to biodiesel

    can be performed on scales up to 3 kg (~3.5 L) of oil

    Fast easy preparation of biodiesel using microwave heating

    Leadbeater N. E.; Stencel, L. M.Energy Fuels, 2006, 20, 2281-2283

    accelerating the biofuels revolution

    microwaves for biodiesel production:

    accelerating the biofuels revolutionUCONN Sustainable Energy Symposium, March 31, 2008

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    can biodiesel be made using microwave heating?

    towards a simpler, faster, more efficient modular design

    scaling up the reaction

    used vegetable oil can be processed

    accelerating the biofuels revolution

    microwaves for biodiesel production:

    accelerating the biofuels revolutionUCONN Sustainable Energy Symposium, March 31, 2008

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    can biodiesel be made using microwave heating?

    towards a simpler, faster, more efficient modular design

    modification for continuous-flow processing at atmospheric pressure

    use a 2 L reaction vessel

    stirbar

    product removal line

    raw materials input line

    accelerating the biofuels revolution

    microwaves for biodiesel production:

    accelerating the biofuels revolutionUCONN Sustainable Energy Symposium, March 31, 2008

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    can biodiesel be made using microwave heating?

    towards a simpler, faster, more efficient modular design

    modification for continuous-flow processing in a 2 L vessel

    feedstock is pumped through the vessel at a flow rates of 1 -2 L / min

    microwave unit is working at ~80 % of power output

    at this rate, material is in the microwave cavity for 1-2 min

    still maintain very high levels of product conversion

    Continuous-Flow Preparation of Biodiesel Using Microwave Heating Barnard, T. M.; Leadbeater, N. E.;

    Boucher, M. B.; Stencel, L. M.; Wilhite, B. A.Energy Fuels, 2007, 21, 1777-1783

    accelerating the biofuels revolution

    microwaves for biodiesel production:

    accelerating the biofuels revolutionUCONN Sustainable Energy Symposium, March 31, 2008

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    can biodiesel be made using microwave heating?

    towards a simpler, faster, more efficient modular design

    modification for continuous-flow processing at atmospheric pressure

    a 4 L vessel is about the largest possible before issues arise with penetration depth

    accelerating the biofuels revolution

    microwaves for biodiesel production:

    accelerating the biofuels revolutionUCONN Sustainable Energy Symposium, March 31, 2008

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    can biodiesel be made using microwave heating?

    towards a simpler, faster, more efficient modular design

    modification for continuous-flow processing in a 4 L vessel

    feedstock is pumped through the vessel at a flow rates of ~ 7 L / min (~110 gallons / hr)

    microwave unit is working continuously at 100 % of power output

    at this rate, material is in the microwave cavity for less than 1 min

    still maintain very high levels of product conversion

    Continuous-Flow Preparation of Biodiesel Using Microwave Heating Barnard, T. M.; Leadbeater, N. E.;

    Boucher, M. B.; Stencel, L. M.; Wilhite, B. A.Energy Fuels, 2007, 21, 1777-1783

    accelerating the biofuels revolution

    microwaves for biodiesel production:accelerating the biofuels revolution

    UCONN Sustainable Energy Symposium, March 31, 2008

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    can biodiesel be made using microwave heating?

    energy efficiency of the process: conventional heating

    data for conventional routes reported in the 1998 joint USDA / DOE study

    accelerating the biofuels revolution

    microwaves for biodiesel production:accelerating the biofuels revolution

    UCONN Sustainable Energy Symposium, March 31, 2008

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    can biodiesel be made using microwave heating?

    energy efficiency of the process: microwave heating

    the microwave is working at 100 % of the maximum power output

    the magnetron is not 100 % efficient

    accelerating the biofuels revolution

    microwaves for biodiesel production:accelerating the biofuels revolution

    UCONN Sustainable Energy Symposium, March 31, 2008

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    can biodiesel be made using microwave heating?

    energy efficiency of the process: comparison

    accelerating the biofuels revolution

    conventional heating 94.3 kJ / L

    microwave, continuous-flow at 7.2 L / min feedstock flow 26.0 kJ / L

    microwave, continuous-flow at 2 L / min feedstock flow 60.3 kJ / L

    microwave heating, 4.6 L batch reaction 90.1 kJ / L

    microwaves for biodiesel production:accelerating the biofuels revolution

    UCONN Sustainable Energy Symposium, March 31, 2008

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    can biodiesel be made using microwave heating?

    single unit applications

    small biodiesel manufacturer

    accelerating the biofuels revolution

    microwaves for biodiesel production:accelerating the biofuels revolution

    UCONN Sustainable Energy Symposium, March 31, 2008

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    can biodiesel be made using microwave heating?

    single unit applications

    small biodiesel manufacturer

    cooperative of biodiesel manufacturers

    accelerating the biofuels revolution

    microwaves for biodiesel production:accelerating the biofuels revolution

    UCONN Sustainable Energy Symposium, March 31, 2008

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    can biodiesel be made using microwave heating?

    single unit applications

    small biodiesel manufacturer

    cooperative of biodiesel manufacturers

    biodiesel for heating oil

    accelerating the biofuels revolution

    microwaves for biodiesel production:accelerating the biofuels revolution

    UCONN Sustainable Energy Symposium, March 31, 2008

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    can biodiesel be made using microwave heating?

    multiple units in parallel

    offers high throughput still with a small footprint

    accelerating the biofuels revolution

    microwaves for biodiesel production:accelerating the biofuels revolution

    UCONN Sustainable Energy Symposium, March 31, 2008

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    can biodiesel be made using microwave heating?

    multiple units in parallel

    offers high throughput still with a small footprint

    offers redundancy

    accelerating the biofuels revolution

    microwaves for biodiesel production:accelerating the biofuels revolution

    UCONN Sustainable Energy Symposium, March 31, 2008

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    can biodiesel be made using microwave heating?

    latest results

    acid catalyzed methodology has been developed

    butanol can be used as a feedstock

    accelerating the biofuels revolution

    Batch and continuous-flow preparation of biodiesel derived from butanol and facilitated by microwave heating

    Barnard, T. M.; Leadbeater, N. E.; Stencel, L. M.;Energy Fuels, 2008,in press

    microwaves for biodiesel production:accelerating the biofuels revolution

    UCONN Sustainable Energy Symposium, March 31, 2008

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    microwave heating offers a viable approach to

    biodiesel production

    the methodology is fast and easy

    acid- and base-catalyzed routes are possible

    microwave unit has a small footprint but high throughput

    calculations show that the microwave methodology is efficient

    future is exciting and will bring many new opportunities

    summary

    microwaves for biodiesel production:accelerating the biofuels revolution

    UCONN Sustainable Energy Symposium, March 31, 2008

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    acknowledgements

    T. Michael Barnard

    Lauren Stencel

    Matthew Boucher

    Benjamin Wilhite

    University of Connecticut Research Fund

    NSF-REU program

    CEM Microwave Technology

    acknowledgements

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    acknowledgementsWEBSITE http://chemistry.uconn.edu/leadbeater.html

    finding out more