How to synthesise a compound?

A + B = C Example:
A
B
1) Addition of
raw materials

2) Mixing &
Heating
A
B
C
D
3) Extraction
A
B
C
pure C
4) Purification
3) Extraction
A
B
A+B = C
B
+
C
=
D
A B

A
B
C
D
1) Addition of
raw materials
2) Mixing &
Heating
A
B
C
pure C
4) Purification 3) Extraction
A
B
A+B = C
B
+
C
=
D
A B

A
B
C
D
1) Addition of
raw materials
2) Mixing &
Heating
A
B
A+B = C
B
+
C
=
D
A B

A
B
C
D
1) Addition of
raw materials
2) Mixing &
Heating
A
B
C
pure C
4) Purification
A
B
C
pure C
4) Purification
Micro-Wave assisted
synthesis
Green Chemistry - Enabled Technologies
Supervisor: Dr. Phan Thanh Son Nam
Group 13:
ng Th Hng
Hunh Tin Phc
Nguyn Khnh
Nguyn Th o
Nguyn Th Giang
Content
1. Introduction
2. How to work
3. Microwave reactors
4. Advantages and disadvantages
5. Scale-out of Microwave reactors
6. Compare Microwave-assisted Chemistry to other methods
7. Applications of Microwave-assisted Chemistry
8. References
- Used the first time in organic chemistry in 1986.
- Nowaday, has used as new green and innovative machine in
synthesis of organic and inorganic compounds.
MICROWAVE ASSISTED SYNTHESIS
FAST AND HOMOGENEOUS HEATING OF
IRRADIATED MATERIAL
What is Microwaves?
Microwaves: electromagnetic waves 0.3 300 GHz
(frequency: 0.1 cm 100 cm)
Domestic Microwave Instrument
Magnetron
Waveguide
Feed
Oven
Cavity
Microwave Apparatus
Microwave Apparatus
How it work?
Microwave
Sample mix
Microwave irradiation
Laboratory Microwave Systems
Industrial Microwave Reactors
Microwave pilot plan
Industrial microwave reactor for large-scale production
Industrial Microwave Reactors
Energy can be applied
directly to sample, rather
than conductively via vessel.
Temperature gradients,
particularly near the
surfaces, can be minimized.
Vessel: no hotter than its
contents
Advantages:
Energy: too low to break chemical bonds.
Heating can be started or stopped instantly.

Advantages:
Numerous
successful
reactions with
dramatically
raised rates
have been
disclosed
Advantages:
Advantages:
Very high
yields and
clean
reactions
have been
achieved.
Advantages:
Offers possibility
of employing
milder & less
toxic reagents &
solvents
Advantages:
Advantages:
Offers possibility
of employing
milder & less
toxic reagents &
solvents
Disadvantages:
Microwave reactor is a potential BOMB!
Disadvantages:
Disadvantages:
Disadvantages:
Timing:
!
Explosion
Not reach
conditions
Disadvantages:
Pressure:
!
Gas and solvent
may increase
pressure
Disadvantages:
Hard to scale-up:
Hazard of explosion of
large scale
Disadvantages:
Unstable heat-supply
causes side-reactions.
Unwanted reactions:
Disadvantages:
Safety
Operation
Money
To increase products:
Scale-up:



Scale-out:
Scale-out Microwave Reactor:
Scale-out Microwave Reactor:
Batch Microwave Reactor Continuous Flow Microwave Reactor
Scale-out Microwave Reactor:
Continuous Flow Microwave Reactor
Fast heating and cooling
products.

Easy to control pressure
and temperature.

Avoid explosion occurs.
Compare Microwave-assisted
Chemistry to other methods

Compare Microwave-assisted
Chemistry to other methods

Microwave vs Conventional Heating
Convection currents
Sample mix
Sample mix
Microwave irradiation
Heat
conduction
flame oil bath heating mantle microwaves
Conventional Heating vs
Alternative Energy Source
Conventional Heating
Bunsen burner
Oil bath
Heating mantle


You heat what you dont want to heat (flask,
vessel, reactor).
Necessity of heated up and cool down
solvents for reaction and apparatus
Alternative Energy Sources
Microwave
Ultrasound
Sunlight / UV
Electrochemistry
Lower energy consumption
Three ways to get the reaction done, but different energy bills to pay
Energy Consumption
Energy consumption of the synthesis
oil bath heating mantle microwaves
Application of microwave- assisted
Synthesis of organic and inorganic compounds.
For example:
Synthesis benzoic acid from benzamide
Facile microwave-assisted hydrothermal synthesis
of TiO2 nanotubes
Microwave-Assisted Extraction(MAE)
Non-polar solvent Microwave-Assisted Extraction
( NPSMAE)
Improved Solvent-free Microwave Extraction (ISFME)
Called green technology because of solvent-free
APPLICATIONS
MICROWAVE -
ASSISTED
STEAM
DISTILLATION
SUPPORTED
MICROWAVE OVEN
Many ways to extract essential oil
PLANT
CELL
broken
WATER HEATS UP
P INCREASE SUDDENLY
broken
t(C)=103C
P = 540W
t = 1 hour


Microwave oven
Condenser
REFLUX??
THE ROUND BOTTOM FLASK
contained
Seeds, leaves and flowers
Dill Seed Oil
Color
Usage
Methods
SOLVENT
Air-dried leaves
Grinding
(blender- 1mm)
Fine powder
Water
SAMPLE
100g 1,7ml
100g (2,42,6)ml
Drill a
hole at
top
SYSTEM
TUBE
STIRRER
LID
LID
Extraction essential
oils

Clossed vessel
Powerful stirrer
Precise computer control
Cut the extraction time
=> Better than other extractions
References:
[1]. Madhvi A. Surati, Smita Jauhari, K. R. Desai, A brief review:
Microwave assisted organic reaction, 2012
[2]. Guo-Xiang Sun, Ming-Yan Yang, Yan-Xia Shi, Zhao-Hui Sun, Xing-Hai
Liu, Hong-Ke Wu, Bao-Ju Li, and Yong-Gang Zhang, Microwave
Assistant Synthesis, Antifungal Activity and DFT Theoretical Study of
Some Novel 1,2,4-Triazole Derivatives Containing Pyridine Moiety,
2014
[3]. M.S. Surendra Babu, K.Rajasekar, K.N.Jayaveera, Microwave
Assisted Synthesis, Characterization, DFT Studies and Antimicrobial
Activities of Novel Pyrazole Derivatives, 2012