FREE RADICAL

POLYMERIZATION OF
POLYANILINE
Submitted to: Dr. Yasir Qayyum Gill

Polymer Structures and Synthesis Lab

OCTOBER 19, 2021

SUBMITTED BY
2020-PE-19
PAN Lab Report 2020-PE-19

Contents
Objective:....................................................................................................................................................2
Abstract:......................................................................................................................................................2
Introduction:...............................................................................................................................................2
Reaction:.....................................................................................................................................................3
Chemicals:...................................................................................................................................................3
Apparatus:...................................................................................................................................................3
Procedure:...................................................................................................................................................3
Yield:............................................................................................................................................................4
Confirmation Tests:.....................................................................................................................................4
Ftir:..............................................................................................................................................................5
Degradation Table:......................................................................................................................................6
Discussion and Calculation:.........................................................................................................................6
References...................................................................................................................................................6

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PAN Lab Report 2020-PE-19

Objective:

To study the preparation of polyaniline by free radical polymerization. Report the nature yield
and conformation test of the polymer obtained.

Abstract:

Polyaniline can be polymerized with the help of free radical chain mechanism. The oxidation of
aniline with ammonium peroxydisulfate in various aqueous settings yielded polyaniline (PANI),
a conducting polymer. A granular morphology of PANI was formed when the polymerization
was carried out in a solution of strong (sulfuric) acid. It is prepared in the beaker. All the
chemicals are allowed to mix for 15 minutes and with continuous stirring and then leave. When
the blue black precipitates of polyaniline are formed they were dried and their yield is calculated.
Then different confirmation tests are performed on them such as solubility and FTIR which
confirms that polymer is polyaniline.

Introduction:

Polyaniline (PANI) is a well-known conductive polymer that has gotten a lot of attention from
nanotechnology researchers for improving sensors, optoelectronic devices, and photonic devices.
Polyaniline (PANI) was originally known as black aniline and comes in a variety of forms
depending on the degree of oxidation. PANI is also recognized for its ease of use, environmental
stability, and ability to dope with protonic acids. [1]The oxidation of aniline with ammonium
peroxydisulfate in various aqueous settings yielded polyaniline (PANI), a conducting polymer. A
granular morphology of PANI was formed when the polymerization was carried out in a solution
of strong (sulfuric) acid. Polyaniline-based compositions can be used to create electrically
conductive, colored, and transparent thin films and coatings that would otherwise be difficult to
obtain with traditional filled materials. Due to its unique characteristics, polyaniline (PANI) is
utilized in a variety of applications, including medication delivery, photovoltaic cells, plastic
batteries, display devices, microelectronics, chemically modified electrodes, corrosion
prevention, and polymer light-emitting diode (PLED) displays.
The repeating unit of polyaniline is

Some of the properties of polyaniline are

 Wide and controllable range of conductivity

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 In addition to providing conductivity, they serve as processing aids.

 Electrically conductive items that are colored and clear
 Conductive blends with many commodity polymers

Reaction:

Chemicals:

Aniline, Ammonium persulphate or benzoyl peroxide, 1 M HCL or any other acid

Apparatus:

 250 ml beaker
 hot plate cum magnetic stirrer
 Thermometer

Procedure:

 Take a 250 ml beaker, put 4.6 ml of aniline and 100 ml of aqueous hydrochloric acid.
 Place it over the apparatus and press the start button.
 Through a separating funnel add 100 ml of 0.1 M ammonium persulphate solution over a
period of 15 minutes of vigorous stirring.
 After the addition the reaction mixture is continuously stirred after which the mixture is
transferred to another beaker containing 50 to 100 ml of acetone with constant stirring.

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 A blue black powder of polyaniline is precipitated out.

 It is then washed with water and ethanol
 The powder was filtered and then put into oven for dry at 50 oC

Yield:

Mass of paper = 2.04 g.

Mass of paper + polymer obtained = 4.78g.
Mass of monomer = 10 g = input.
Mass obtained of polymer = 4.78-2.04 = 2.74g = output.
Yield can be easily calculated as:
Yield = Output/input*100
= 2.74g/10 g*100
= 27.4%.

Confirmation Tests:

Sr.
No. Test Name Test Procedure Observation Inference
Put a small amount of The specimen readily Polyaniline
1 Solvent Test
polymer specimen in dissolved in DMF confirmed
DMF
Put a small amount of The specimen does Polyaniline
2 Solubility Test
polymer specimen in not dissolve in water confirmed
water
Flame Retardancy Over time, the specimen
Place the polymer fire became red hot but Polyaniline
3 Test
specimen over direct did not catch. confirmed
flame
Put a small amount of The specimen sank in Polyaniline
4 Density Test
polymer specimen in water confirmed
water

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Ftir:

Graph 1: FTIR result obtained from the specimen

Graph 2: FTIR result obtained through literature. (1)

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Degradation Table:

Discussion and Calculation:

During polymerization, the monomer undergoes a chain reaction that results in the development
of regular macromolecules, and the expanding chains are ordered into the structure at the same
time. In this regard, developing methods of controlled synthesis that produce polymers with
predefined characteristics and supramolecular structure is critical. The hue of the precipitates
evolved from light blue to blue-green, copper tinge, and green as the usual polymerization
reaction progressed. In these tests, aniline is oxidized because its oxidation potential in acidic
solution is around 1.0 eV. The low value of yield can be attributed to incomplete reactions,
inconsistent/insufficient/ or incorrect temperature. The green color at the end confirms that
product obtained is emerladine.

References

[1] S. A. Rashid, "Preparations, Properties, and Applications of Polyaniline and," MDPI.

[2] "ACME PLASTICS.com," ACME PLASTICS, [Online]. Available: https://www.acmeplastics.com/what-is-

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pmma. [Accessed 15 10 2021].

[3] "Resinx.com," RESINX, [Online]. Available: https://www.resinex.co.uk/polymer-types/pmma.html.

[Accessed 15 10 2021].

[4] Research Gate. [Online] jan 2012. [Cited: oct 17, 2021.]
https://www.researchgate.net/figure/FT-IR-spectrum-of-polyaniline-sample-IP_fig1_270603092.