GROUP 13 - MICRO WAVE.pptx

8/10/2019 GROUP 13 - MICRO WAVE.pptx

http://slidepdf.com/reader/full/group-13-micro-wavepptx 1/61

How to synthesise a compound?

A + B = CExample:

AB

1) Addition ofraw materials

∞

2) Mixing &Heating

A

BC

D

3) Extraction

A

B

C

pure C

4) Purification



3) Extraction

A B

A+ B = C B + C

= D

AB

∞

A

BC

D


2) Mixing &Heating

A

B

C

pure C

4) Purification3) Extraction

A B

A+ B = C B + C

= D

AB

∞

A

BC

D


2) Mixing &Heating

A B

A+ B = C B + C

= D

AB

∞

∞

∞

A

BC

D


2) Mixing &Heating

A

B

C

pure C

4) Purification

A

B

C

pure C

4) Purification

Micro-Wave assisted

synthesis

Green Chemistry - Enabled Technolo



Supervisor: Dr. Phan Thanh Son Nam

Group 13:

Đặng Thị Hằng

Huỳnh Tiến Phúc

Nguyễn Khánh

Nguyễn Thị Đào

Nguyễn Thị Giang



Content1. 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

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 machin

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 GH

(frequency: 0.1 cm – 100 cm)



Domestic Microwave Inst

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 productio

Industrial Microwave Reactors



Energy can be applied

directly to sample, rather

than conductively via vessel.

Temperature gradients,

particularly near thesurfaces, 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:



Nu

suc

rea

dra

raihav

dis

Advantages:



Advantages:



Very high

yields and

clean

reactionshave been

achieved.

Advantages:



Offers possibility

of employing

milder & lesstoxic reagents &

solvents

Advantages:



Advantages:

Offers possibility

of employing

milder & lesstoxic reagents &

solvents



Disadvantages:

Microwave reactor is a potential BOMB!



Disadvantages:



Disadvantages:



Disadvantages:

Timing:

! Explosi

Not rea

conditio



Disadvantages:

Pressure:

!Gas an

may in pressu



Disadvantages:

Hard to scale-up:

Hazard of explosilarge scale



Disadvantages:

Unstable heat-supplycauses side-reactions.

Unwanted reactions:



Disadvantages:

Safet

Oper

Mone



To increase products:

Scale-up:

Scale-out:



Scale-out Microwave Reactor:




Batch Microwave Reactor Continuous Flow Microw




Continuous Flow Microwave Reactor

Fast heating and products.

Easy to control p

and temperature.

Avoid explosion

Compare Microwave assisted



Compare Microwave-assisted

Chemistry to other methods

Compare Microwave assisted



Compare Microwave-assisted

Chemistry to other methods

Micro a e Con entional Heating



Microwave vs Conventional Heating

Convection currents

Sample mixSample mix

Microwave irradiationHeat

conduction

Conventional Heating vs



flame oil bath heating mantle microwaves

Conventional Heating vs

Alternative Energy Source

Conventional Heating

• Bunsen burner• Oil bath• Heating mantle

• You heat what you don’t want to heat (

vessel, reactor).

• Necessity of heated up and cool

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 pa

Energy Consumption Energy consumption of the synthesis

oil bath heating mantlemicrowaves

A li ti f i i t d



Application of microwave- assisted

Synthesis of organic and inorganic compounds.

For example:

Synthesis benzoic acid from benzamide

F il i i t d h d th l th i



Facile microwave-assisted hydrothermal synthesis

of TiO2 nanotubes



Microwave-Assisted Extraction(MAE)

N l l t Mi A i t d E t ti



Non-polar solvent Microwave-Assisted Extraction( NPSMAE)



Improved Solvent-free Microwave Extraction (ISFME

Called ‘ green technology’ because of solvent-fre



APPLICATIONSMICROWAVE -

ASSISTED



STEAM

DISTILLATIONSUPPORTED

MICROWAVE OVEN

Many ways to extract essential oil

PLANT



CELL

broken

WATER HEATS U

P INCREASE SUD

broken



t(ᵒC)=103ᵒC P = 540W t = 1 hour

Microwave oven



Microwave oven

Condenser



Condenser

REFLUX??

THE ROUND BOTTOM FLASK



THE ROUND – BOTTOM FLASK

contai

S d l d fl



Seeds, leaves and flowers

Dill Seed Oil



Dill Seed Oil

SAMPLE 100g 1 7ml



SOLVENT

Air-dried leaves

Grinding (blender- 1mm)

Fine powder

Water

SAMPLE 100g – 1,7ml

100g – (2,4÷2,6)ml



Drill a

hole at

top



SYSTEM



SYSTEM

TUBE



TUBE

STIRRER



STIRRER

LID



LID

LID



LID

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, Xi

Liu, Hong-Ke Wu, Bao-Ju Li, and Yong-Gang Zhang, “Microwave

Assistant Synthesis, Antifungal Activity and DFT Theoretical Study

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 Antimicrob

Activities of Novel Pyrazole Derivatives”, 2012

Documents

GROUP 13 - MICRO WAVE.pptx