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General presentation of microwave equipment used by the chemical industry
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12 PORTE DU GRAND LYON01702 NEYRON CEDEX, FRANCE
tel. +33 (0)4 72018160 www.sairem.com
Any frequency, any power level ...
Confidentiality statement
This presentation has been prepared exclusively for the benefit and use of Sairem and does not carry any right of publication or disclosure, in whole or in part, to any other party. This presentation is the property of Sairem. Neither this presentation nor any of its contents may be used for any purpose without the prior written consent of Sairem.
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Agenda
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1. What are microwaves?- Transverse electromagnetic waves- Frequency and wavelength- Electromagnetic spectrum- ITU allocated bands for ISM applications
2. Electromagnetic energy interactions with matter
3. Microwave energy vs. Other electromagnetic energy. Ionizing or non-ionizing?
4. Microwaves and their interactions with matter- Main parameters- Heating mechanisms- Classification of materials- The effect of wavelength (frequency) on heating homogeneity- Rates of heating for liquids and solids- Thermal effect
5. Microwave heating vs. Conventional heating
6. Microwave equipment for heating applications- Basic equipment- Multimode applicators- Single mode resonant cavities & standing wave formation
7. SAIREM’s microwave assisted chemistry/extraction
What are microwaves? Transverse electromagnetic waves
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Electromagnetic waves propagated in free space have the electric and magnetic field perpendicular to each other and to the direction of propagation; they are known as transverse electromagnetic waves (TEM).
The plane of polarisation for a wave is, by convention, that of the electric field – vertical
WAVELENGTHλ= 12.2 cm for 2450 MHz
Direction of wave
E
E
E
H
H
H
What are microwaves? Frequency and Wavelength
Electromagnetic waves are characterized by three parameters:
frequency (f) = number of cycles/second
wavelength ()
photon energy (E)
Where:- c is the speed of light in vacuum, 3 x 108 m/s- is the dielectric constant of the propagating medium , for gases = 1- h is Planck’s constant, 6.62×10−34 J·s
For electromagnetic waves in free space, where f is in hertz:
Examples:- f = 2.45 GHz (2450 x 106 Hz) = 12.2 cm - f = 915 MHz (915 x 106 Hz) = 32.7 cm
fm
8103)(
fc
Hzf )(
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hc
JE )(
What are microwaves? Electromagnetic Spectrum
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What are microwaves? ITU allocated bands for ISM applications
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Fig. 2. Frequency band regions allocated by ITU
R1- Europe, Africa, Turkey, Russia (Siberia)
& Mongolia, Middle East (without Iran)
R2 – South & North America
R3 – Remaining countries
Radio-frequency and Microwave bands for Industrial, Scientific and Medical (ISM) applications allocated by the International Telecommunications Union (ITU)
Frequency band Central frequency
Wavelength World regions covered
6.765 – 6.795 MHz 6.78 MHz 44.2 m Under consideration
13.553 – 13.567 MHz 13.56 MHz 22.1 m R1, R2, R3
26.957 – 27.283 MHz 27.120 MHz 11.1 m R1, R2, R3
40.66 – 40.70 MHz 40.68 MHz 7.4 m R1, R2, R3
433.05 – 434.79 MHz 433.92 MHz 0.69 m R1
902 – 915 MHz 915 MHz 0.33 m R1, R2, R3
2400 – 2500 MHz 2450 MHz 0.12 m R1, R2, R3
5725 – 5875 MHz 5800 MHz 0.05 m R1, R2, R3
24 – 24.25 GHz 24.125 GHz 1.24 cm R1, R2, R3
61 – 61.5 GHz 61.25 GHz 0.49 cm Under consideration
122 – 123 GHz 122.5 GHz 0.24 cm Under consideration
244 – 246 GHz 245 GHz 0.12 cm Under consideration
Electromagnetic energy interactions with matter
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Region of the electromagnetic spectrum
Main interactions with matter
RadioCollective oscillation of charge carriers in bulk material (plasma oscillation). An example would be the oscillation of the electrons in an antenna.
Microwave through far infrared Plasma oscillation, molecular rotation
Near infrared Molecular vibration, plasma oscillation (in metals only)
VisibleMolecular electron excitation (including pigment molecules found in the human retina), plasma oscillations (in metals only)
UltravioletExcitation of molecular and atomic valence electrons, including ejection of the electrons (photoelectric effect)
X-rays Excitation and ejection of core atomic electrons
Gamma raysEnergetic ejection of core electrons in heavy elements, excitation of atomic nuclei, including dissociation of nuclei
High energy gamma raysCreation of particle-antiparticle pairs. At very high energies a single photon can create a shower of high energy particles and antiparticles upon interaction with matter.
Microwave energy versus other electromagnetic energyIonizing or non-ionizing?
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Radiation type
Typical frequency
(MHz)
Quantum (photon) energy Chemical bond
type
Chemical bond energy (eV)
eV kcal/mol eV kcal/mol
Gamma ray
X-Ray
UV
Visible
Infrared
Microwaves
Radio-waves
3.0 x 1014
3.0 x 1013
1.0 x 109
6.0 x 108
3.0 x 106
2450
1
1.24 x 106
1.24 x 105
4.1
2.5
0.012
1.6 x 10-5
4 x 10-9
2.86 x 107
2.86 x 106
95
58
0.28
0.037
9 x 10-8
H-OH
H-CH3
H-NHCH3
H3C-CH3
PhCH2-COOH
H-O-H ... O-H
H
5.2
4.5
4.0
3.8
2.4
0.21
120
104
92
88
55
4.8
Microwaves & their interactions with matter
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Pr
0
Material (’, ’’)
m
Air
d
Pa/e
Pa
Pi
Pf = forward power Pa = absorbed power
Pr = reflected power λm = wavelength in material
λ0 = wavelength in air ’ = permittivity (wavelength specific) = material capacity to stock energy
’’ = dielectric losses (absorption specific; absorption increases with ’’),
loss of energy by relaxation (important in microwaves) and conduction; in general, 10-2 < ’’
< 102
tg = loss tangent
λm < λ0
Dielectric constants ’ and ’’ are not constants; they depend on: - Wave frequency;- Material temperature;- Material phase, e.g. gas, liquid, solid, polymer etc.
Microwaves & their interactions with matterMain parameters
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VtgKfEKVfER
VPa '2''2
2
V''
Pa = absorbed power (watts)K = constant, 0.55 x 10-10 V = sample volume (m3)f = frequency (Hz)E = electric field inside the sample (V/m)’’ = dielectric loss (F/m)
1. Absorption
VKf
PE a
''2
2. Penetration depth, d
d = penetration depth in to material where the power is Pa/e or 36% of the Pa calculated at the point of entrance
Material Penetration depth, d27 MHz 2450 MHz
Air many km many kmWater 10 cm 1.5 cmBalsa wood 2 m 20 cmOak 30 cm 3 cmRubber 15 cm 2 cmAluminium 16 microns 1.7 microns
Microwaves & their Interactions with Matter Heating mechanisms
Conduction mechanisms (electrical conductor)
Heating via charge carriers (electrons, ions etc.) polarisation P (in approx. 10-8s)
Dipolar polarisation or Dielectric heating (polar liquids)
The electric field interacts with dipolar molecules
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Microwaves & their Interactions with Matter Classification of materials
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INSULATOR Total Transparent ΔT = 0
CONDUCTOR None Reflective
DIELECTRIC Partial to totalAbsorptive ΔT> 0
Examples: quartz, ice, non-polar solvents
Examples: metals
Examples: water, polar solvents, zeolites
Material type Penetration
~ 2cm /2 ~ 6 cm (2450 MHz)
Hot area
Cold areas
Ea/2
Ea
~ 2 m /2 ~ 5.6 m (27 MHz)
Microwaves & their Interactions with Matter The effect of wavelength (frequency) on heating homogeneity
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Video\progress wave MagnE face.aviVideo\progress wave MagnE.avi
Microwaves & their Interactions with Matter - Examples
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Material Depth of penetration Classification
Glass Quartz 150 m Insulator
Pyrex 2 m Insulator
Plastics PTFE 25 m Insulator
Polyethylene high density 25 m Insulator
Polypropelene 18 m Insulator
Foods Ice 12 m Insulator
Water 30 mm Dielectric
Meat 12 mm Dielectric
Metals Aluminium 2 μm Conductor
The transmitted electromagnetic energy penetrates into the interior of materials and attenuates to an extent depending on the dielectric constant.
The inverse of the attenuation constant is defined as the skin depth/depth of penetration.
Microwaves & their Interactions with Matter Rates of heating for liquids
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Solvent Dielectric constant ’
T 0C Bp 0C
Water 78.5 81 100
Methanol 32.6 65 65
Ethanol 24.3 78 78
1-Propanol 20.1 97 97
1-Butanol 17.8 109 117
1-Pentanol 13.9 106 137
1-Hexanol 13.3 92 158
Acetic acid 6.2 110 119
Acetone 20.7 56 56
Hexane 2.0 25 68
Heptane 2.0 26 98
CCl4 2.2 28 77
Temperature of 50 mL of several solvents after heating from room temperature 1 min at 560 W, 2.45 GHz
Polar solvents
Non-polar solvents
Rise of temperature depends on:- Dielectric constant- Specific heat capacity- Emissivity- Strength of applied field
Microwaves & their Interactions with Matter Rates of heating for solids (powder)
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Effect of microwave heating on temperature of solids 1 kW, 2.45 GHz Sample 25g (particle size 5-80 μm)
Chemical T, 0C Time, min
Al 577 6
C 1283 16
Co2O3 1290 3
CuCl2 619 13
FeCl3 41 4
NaCl 83 7
Ni 384 1
NiO 1305 6.25
CaO 83 30
CuO 701 0.5
Fe2O3 88 30
Fe3O4 510 2
TiO2 122 30
WO3 530 0.5
B4C (>400μm) 214 2
B4C (5 - 80μm) 665 2
Microwaves & their Interactions with Matter – Thermal effect
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The effect of microwave energy transfer in to a material results in its temperature increase
The relation between the absorbed power and temperature increase (without phase change)
where:Pa = absorbed power (W) m/t = sample weight per unit of time (gs-1)T = temperature gradient (K)Cp = specific heat capacity (J g-1 K-1)
! Pf > Pa
Efficiency of power (energy) transfer in to a material:- RF and microwaves 60 – 98 %- IR 20 – 60 %- Hot air 10 – 40 %
TCt
mP pa
Microwave heating vs. Conventional heating
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Microwave heating / Dielectric heating
Conventional heating / Heat conduction
Heating of polar molecules with an electric dipole moment; energy transferred directly from the electric field to molecules if walls of containment vessel are ‘microwave transparent’
Transfer of thermal energy from outside - energy transferred indirectly from containment vessel to reaction mixture. The time of heating depends on the thermal conductivity of the material to be heated and the distance from the heating source to the material.
Superheating of absorptive molecules due to rapid & selective energy transfer from the electric field temperature gradients in solution
Temperature of containment vessel walls is higher than the reaction temperature
p = power density, = field frequency’’
r = relative permittivity; 0 = permittivity of free spaceE = electric field strength
Fourier’s law2
0'' Ep r
Microwave heating vs. Conventional heatingMagic effect?
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RT
Ea
Aek
Arrhenius equation:
Temperature 0 C
Reaction rate increase
100 4.7 x 10-30 1
110 2.73 x 10-29 5.8
120 1.46 x 10-28 31
130 7.16 x 10-28 152
150 7.16 x 10-26 2914
RT
Ea
e
Ea = 50 kcal/mol
Microwave Equipment for Heating ApplicationsBasic equipment
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Microwave generator
Antenna for direct irradiation
Multimode cavity
Monomode cavity
MICROWAVE
APPLICATOR
POWER SUPPLY
AND PROTECTION
SYSTEMS
MAGNETRON
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Applicators are devices designed to ensure the transfer of electromagnetic energy from the transmission line to the material to be treated.
Waveguide launcherCirculator
Dummy load
MagnetronMode stirring
Sample
Waveguide
Antenna
Microwave Equipment for Heating Applications Multimodal Applicators
Microwave Equipment for Heating Applications Single Mode Resonant Cavities
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Metallic enclosure into which a launched microwave signal of the correct electromagnetic field polarization will suffer multiple reflections between preferred directions. These cavities represent volumes of large stored energy which is transformed into heat via displacement and conduction currents flowing through the dielectric material as soon as it is placed within the heating zone.
Operation must be within narrow frequency bands in order to maintain high coupling efficiencies.
In general, a single mode resonant heater will establish much higher electric field strengths than a traveling wave or multimode applicator; these structures are in general more compact with extremely high power densities (107 kW/m3).
Microwave Equipment for Heating Applications Single Mode Resonant Cavities
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a
b
E
Electric field distribution & intensity in TE10 mode waveguide, 2.45 GHz
Standard
waveguide
a mm
bmm
WR340 86.36 43.18
WR430 109.2 54.60
Microwave Equipment for Heating Applications Single Mode Resonant Cavities – Standing wave formation
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The superposition of the incident and reflected waves gives rise to a standing wave pattern which for some simple structures is very well defined in space
Video\standing wave MagnE3.aviVideo\standing wave MagnE.aviVideo\standing wave MagnE2.avi
E1
E2
λ0/2
In air = 61 mm
2
1
E
EWVSR
References
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1. Rochas, J.F., International Symposium on Microwave Science & its Applications to Related Fields, 28-30 July 2004, Takamatsu, Japan
2. Metaxas, A.C., Meredith, R.J., industrial Microwave Heating, IEE Power Engineering Series 4, 1993.
3. Kingston, H.M., Haswell, S.J., Microwave-Enhanced Chemistry, American Chemucal Society, Washington, DC.,1997.
More information:- CEM Corporation cem.com- General Microwave Corp. generalmicrowave.com- Holaday Industries Inc. holadayinc.com
SAIREM’s Microwave assisted SAIREM’s Microwave assisted Chemistry/ExtractionChemistry/Extraction
Process-specific combined high-frequency generators and reactors
Enhanced safety Process compatibility Minimum footprint Reduced cost of ownership
Innovative method for energy transmission directly into the reaction media via an Internal Transmission Line INTLI & U-waveguide (Sairem patents WO 2009/122101 and WO 2009/122102) combined with the latest generation of high-frequency generators and intelligent controllers.
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HIGH FREQUENCY GENERATOR
REACTOR(APPLICATOR)
Energy transmission line
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HIGH FREQUENCY GENERATORS
MICROWAVE GENERATORS915 MHz & 2450 MHz
RADIO-FREQUENCY GENERATORS13.56 MHz & 27.12 MHz
GENERATORS > 2450 MHz
Radio-frequency generators Radio-frequency generators 13.56 MHz & 27.12 MHz up to 90 kW13.56 MHz & 27.12 MHz up to 90 kW
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13.56 MHz, 12 kW
Microwave generatorsMicrowave generators 915 MHz, 600 W – 100 kW 915 MHz, 600 W – 100 kW
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600 W 5 kW 30 kW
Microwave generators 2450 MHzMicrowave generators 2450 MHz
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Solid state 25 W – 120 W 300 W – 15 kW
2oo W generator 2 kW 6 kW
2oo W integral module 15 kW
Generators frequency > 2450 MHzGenerators frequency > 2450 MHz
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2 kW @14 GHz & 18 GHz
Power supply 10 kV x 1A for klystron
10 kW @ 28 GHz
Power supply 30 kV x 1.5 A for gyrotron
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ENERGY TRANSMISSION LINE
COAXIAL CABLE
WAVEGUIDE
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REACTORS (APPLICATORS)
BATCH
CONTINUOUS FLOW
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Industrial microwave chemistryTreatment of residual acids from nitrocellulose fabrication
Residual acid treatmentNitroglycerin destructionMicrowave: 8 kW (2 kW + 6 kW) 2.45 GHzCapacity: 300 kg/hProcess temperature: 150 °C
Preheated residual acid
PROCESS DIAGRAM
Residual acid mixture
Regenerated acids
Heat exchanger
MWHead
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Industrial microwave chemistry Laurydone synthesis
6 kW 2.45 GHz Laurydone synthesis
MW reactor
Pyroglutamic acid + Lauryl alcohol NO NEED FOR CATALYST (p-toluene sulphonic acid) and solvent (toluene) Microwave powerMicrowave power : 6 kW 2.45 GHzBatch production : 150 kg in 4 hoursReaction time reduced 5 times
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NEW!!!!
LABOTRON X & LABOTRON S
Minilabotron 2000
MICROWAVE ASSISTED MICROWAVE ASSISTED CHEMISTRY/EXTRACTIONCHEMISTRY/EXTRACTION
LABOTRONExtraction/Synthesis = Integrated microwave generator and reactor
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+=
LABOTRON X and S
MW Generator ≤ 6 kW
2.45 GHz
INTLI + U-waveguide+
Batch ~ 0.5-17 L
REACTOR
Continuous flow CF
LABOTRON X and S, Microwave-assisted LABOTRON X and S, Microwave-assisted extraction and synthesis extraction and synthesis
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LABOTRON 6 kW with batch reactor LABOTRON 2 kW with CF reactor
LABOTRON X and SLABOTRON X and S - Batch reactors- Batch reactors
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Batch reactor 1.7 L Batch reactor 17 L
LABOTRONLABOTRON X and S - Continuous flow X and S - Continuous flow reactorsreactors
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SPIN S SPIN M
LABOTRON X and SLABOTRON X and S - Batch Reactor- Batch Reactor
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Minilabotron 2000 with batch reactorMinilabotron 2000 with batch reactor
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Minilabotron 2000 with CF reactorsMinilabotron 2000 with CF reactors
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Minilabotron 2000 with horizontal SPINreactor
Minilabotron 2000 with horizontal column reactor
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PILOT-scale up to 30 kW, 915 PILOT-scale up to 30 kW, 915 MHzMHz
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PILOT up to 30 kW, 915 MHz – ReactorsPILOT up to 30 kW, 915 MHz – Reactors
Batch reactor 100 L Continuous flow reactor