LABORATORY

EXPERIMENTS
IN POLYMER
SCIENCE

Department of Materials
Science & Engineering
TABLE OF CONTENTS

S. No. Experiments Page

Safety in The Polymer Synthesis Laboratory 1

1. Identification of Polymers 3

2. Determination of Viscosity Average Molecular Weight 9

3. Interfacial Polymerization 12

4. Addition Polymerization 14

5. Preparation of Laminates 16

6. Blends and Composites 18

7. 3D Printing 22
 SAFETY IN THE POLYMER SYNTHESIS LABORATORY

We must insist on strict safety precautions in the laboratory, since we will be a relatively
large group of people working in a small area. Each person is, therefore, responsible not only
for his/her own safety, but for the safety of everyone in the laboratory.
Our safety policy consists of two distinct parts: A general philosophy of safety, as well as a
series of firm safety regulations upon which we will insist throughout the course. The sheet
briefly summarizes these two aspects of safety in the polymer synthesis laboratory:
Many different types of hazards are encountered in the laboratory:

• Chemical Toxicity (short and long range)

• Fire and Explosion (e.g. flammable solvents)
• Chemical Burns (e.g. strong acids and bases)
• Electrical Hazards (e.g. poorly wired equipment)
• Mechanical Hazards (e.g. motorized equipment)
• Compressed Gases (both mechanical and chemical hazards)
We will encounter hazards of each type. The most basic safety consideration in the face
of such potential hazards is this: BECOME WELL ACQUAINTED WITH THE PROPERTIES
AND DANGERS OF THE MATERIALS AND APPARATUS WITH WHICH YOU ARE
WORKING. There is no excuse for the improper handling of laboratory materials; the correct
methods for performing laboratory operations are readily available.
ADDITIONAL SAFETY CONSIDERATIONS
- Maintain “good housekeeping” habits in the lab. Neatness prevents many careless accidents
and prevents the catastrophic spreading of the often minor primary problems.
- Become acquainted with the available safety and first Aid facilities.
THINGS UPON WHICH WE WILL INSIST
1. Lab coats,
2. Proper cleaning of all equipment used in the experiment,
3. No readily flammable or loose floppy clothing,
4. No eating or smoking in the laboratory.
NOTEBOOK REQUIREMENTS FOR THE POLYMER SYNTHESIS LABORATORY
Each student will keep a bound notebook with numbered pages. Looseleaf books are not
admissible. The notebook should be always neat and up to date at all times. An original record
of performance is desired, including reports of troubles as well as successful synthesis. “write-
ups” done at home after experiments are completed, will be discounted. Do not tear out sheets
with unsatisfactory data. Make no erasures; correct errors by drawing a single line through
them.

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 Plan your written work as well as laboratory performance in advance. All sections except
data, observations and conclusions should be written prior to the experiment. Record of
weights, volumes or other numerical results should be written directly in the notebook. Do not
write number on scraps of paper then later transfer them to the notebook. Be sure all
experimental details and data are included in a neat manner. Use enlarged letters referring to
various sections for a given experiment.

Following is a format to be used in the laboratory report.

1. Table of Contents: The first page in the notebook should contain a list of experiments in the
order performed, the date performed and the page number on which they appear.
2. Statement of Purpose: This should be a statement of one’s overall objectives in the experiment.
3. Reactions: A list of all reactions taking place in the experiment is included here.
4. Materials: All materials used in the experiment should be clearly listed with appropriate physical
properties such as molecular weight, melting point etc.
5. Procedure: The procedure followed for the experiment should be included with actual amount of
materials used.
6. Data and Observations: This should include what you saw happen during the experiment such
as colour, consistency, or volume changes etc. This should also include any data gathered
during the experiment such as weights, volumes, and yields.
7. Discussion and Conclusion: Outline what was accomplished in the experiment. Include required
calculations. Include an analysis of errors and any deviations from the expected results. A
summary of results and critical comments concerning the experiment should also appear here.

The notebook should be signed and dated immediately after the conclusion of the experiment.

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 EXPERIMENT – 1

IDENTIFICATION OF POLYMERS

Identification of polymers is carried out by -

(a) Preliminary tests such as hot rod penetration, floatation, burning, appearance,
bending, drop test and tear test.
(b) Melting point, MFI and density measurements,
(c) Instrumental methods of analysis like TGA, DSC, FTIR.

Softening or melting occurs only with linear polymers. In some cases, the polymers degree
before melting and in crosslinked polymers, there is no softening till crystalline low molecular
weight organic compounds.
Softening range of a plastic can be determined with the usual methods of organic
chemistry using melting point apparatus /or by using differential scanning calorimetry / or
differential thermal analysis. A hot stage microscopy can also be used to determine the melting
point with an accuracy of 2 – 3°K.
The melting range of some important plastic materials are given below:

Thermoplastics Softening/melting range °C

PS 70 – 115

PVC 75 – 90 (soften)

PE d = 0.92 g/cm 3 ~ 110

d = 0.94 g/cm 3 ~ 120

d = 0.96 g/cm 3 ~ 130

PP 160 – 170

Nylon 6 215 – 225

Nylon66 250 – 260

Nylon 610 210 – 220

Nylon 11 180 – 190

Nylon 12 170 – 180

PET 250 – 260

PBT 220

PC 220 – 230

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 1. Scratch test
PE and PP can be differentiated by this test. Scratch the samples with your finger nail and
observe.
PE will show scratch marks whereas PP is scratch resistant. PE and PP can also be
distinguished by their melting point.

2. Bending Test
Plastics show bending behavior when applied certain amount of force to some extent.

Polyethylene (PE) Bend tends to remain

Polypropylene (PP) Unbend most of the way

Polystyrene (PS) Cracks but remains bent

Acrylonitrile Butadiene Styrene (ABS) Bend tends to remain

Poly(vinyl chloride) – Rigid (RPVC) Bends easily and springs back quickly
(Plasticized PVC is more flexible)
Cellulose Acetate (CA) Bend tends to remain

Poly(methyl methacrylate) (PMMA) Cracks and splinters

Polyamides Difficult to bend, springs back

3. Drop/Sound Test
When a molded component is dropped on hard surface, they give either metallic sound or dull
sound.
Metallic sound – PS, HIPS, SAN, ABS, PC, PPS, PPO, Polysulfones.
Dull sound – Polyamides, PTFE, PMMA, Polyacetal, PVC, Polyolefins, Cellulosics.

4. Float Test
Simplest test is density. Contrary to the behavior of other plastics, polyolefins float on water.
The only other polymer that float on water are foamed plastics or those containing foaming
agents.
Some materials are listed below with their specific gravity.

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 Float /Sink Materials Specific Density

PP 0.89 – 0.90

LDPE 0.91 – 0.92

Floats on water
HDPE 0.94 – 0.96

PS 1.05 – 1.06

SAN 1.1
Sink in water but floats in
hypo ABS 1.05 – 1.1

Nylon 1.1

CAB 1.3

CA 1.4

Polyacetal 1.4
Sink in hypo
UF 1.5

PTFE 2.15

5. Tear Test
Tear testing provides information on the energy or force required to propagate a tear through
a material. Tearing tests are commonly performed on foils, plastics, paper, and textiles.

Polyethylene (PE) Tough, stretches before tearing

Polypropylene (PP) Tough, stretches a lot before tearing

Polystyrene (PS) (Biaxially oriented) Tears straight

Poly(vinyl chloride) (PVC) Stretches then tears rapidly

Cellulose Acetate (CA) Tears easily and straight

Cellophane Tears easily and straight

Poly(vinyl alcohol) Stretches then pulls apart

6. Burning Test
The sample is held in flame for few seconds till it catches fire and then withdrawn from the
flame.

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Observed whether material burns continuously or self-extinguishes.

PLASTCS COMBUSTIBILITY EFFECT FLAME

PE Continuous burning, Melts and decompose Blue base with yellow tip
easy to ignite
PP Continuous burning, Melts and Blue base with yellow tip
easy to ignite decompose, dripping
nature
PS, ABS, Continuous burning, Soften only Golden yellow with soot
HIPS easy to ignite
PVC Flame extinguishes on Softens first, Yellow – orange soot with
removal, difficult to decomposes with green edges
ignite black residue
PC Flame extinguishes on Melts, decompose, Bright soot
removal, difficult to charred
ignite
PA Flame extinguishes on Melts, drips and Yellow – orange soot with
removal, difficult to decompose, bubble blue edges
ignite around edges
PET, PBT Continuous burning on Softens, melts and Yellow – orange soot
removal, difficult to drips
ignite

7. Hot Rod Penetration Test

A red-hot electric soldering iron is pressed against the unknown sample. If the material softens
and the rod penetrates in to sample, it’s thermoplastic.
If it does not soften and the rod does not penetrate the sample, it’s thermoset.
If sample is in the form of granules or powder, it is taken in a nickel spatula and heated directly
on the flame and observed, whether the material melts or not.
8. Melt Flow Index (MFI) Test
The melt flow index (MFI) is a measure for the ease of flow of
melted plastics. It is often used in the plastic industry for quality
control of thermoplastics.
According to ASTMD 1238, Rate of extrusion of a resin in molten
condition under specified temperature and pressure through a
specified size of die in 10 min is defined as melt flow index. The
unit of MFI is g/10min.
In general, a higher MFI indicates a lower material viscosity, and
when comparing polymers of the same class, a lower melt flow
rate corresponds to a higher molecular weight and/or less
branching. It can also be useful to study the relative thermal
effect with respect to barrel residence time of plastics.

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 MATERIALS TEMPERATURE (°C) LOAD (kg)

PP 230 2.16

125 0.325/2.16
PE
310 12.5

PC 300 1.2

PS, HIPS 190 5.0

PET 210 2.16

9. Differential Scanning Calorimetry (DSC)

o Two samples, each heated independently.
o Temperature difference is monitored.
o Control heat flow into analysis sample (adjusting heater power) to keep the
temperature difference ∆T = 0.

Typical DSC transitions

10. Thermogravimetric Analysis (TGA)

It is a method of thermal analysis in which a mass of a sample is examined over time as a

function of temperature. It also provides information about –

➢ Thermal stability of materials,

➢ Oxidative stability of materials,
➢ Composition of multi – component system,

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 ➢ Estimated lifetime of a product,
➢ Decomposition kinetics of materials,
➢ Effect of corrosive or reactive environment on product,
➢ Moisture and volatile content in materials.

11. Fourier-transform Infra-red Spectroscopy (FTIR)

FTIR spectroscopy is used to quickly identify compounds such as plastics, blends, fillers,
paints, rubbers, coatings, resins, and adhesives.

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 EXPERIMENT – 2

DETERMINATION OF VISCOSITY AVERAGE

MOLECULAR WEIGHT OF POLYMERS

INTRODUCTION
The viscosity of a very dilute solution of a polymer of high molecular weight is
considerably greater than that of the pure solvent. The possibility of correlating dilute solution
viscosity with polymer molecular weight was first suggested by Staudinger in 1930’s.
Considerable developments in theory and experiments have taken place since then but even
to-date the viscometric determination of molecular weights has not achieved the status of an
absolute method and the correlation is only empirical. This is primarily due to the fact that the
solution viscosity measures the molecular size (which may be different in different solvents)
and not the mass. For each polymer-solvent system the viscometric method has to be
calibrated by samples having narrow molecular weight distributions and characterised by one
of the accepted absolute methods such as osmometry or light scattering. In such systems,
where molecular weight viscosity relationship have been established, viscometry is the easiest
and most rapid method for obtaining molecular weights. In a given linear polymer-solvent
system, viscometry alone may be used for assessment of the molecular weights.
THEORY
The semi-empirical relationship given by Mark Houwink and Sakurada has been
widely used for correlating limiting viscosity number (intrinsic viscosity) and molecular
weight.

[η] = K.[M]a − − − − − − − − − − (1)

where K and a are the constants depending on polymer, solvent and temperature. For a
̅ v is obtained by using above
polydisperse system, the viscosity average molecular weight M
relationship.
1+a 1/a
̅̅̅̅v = { ∑ N1 M1
M } − − − − − − − − − − (2)
∑Ni Mi

The magnitude of exponent ‘a’ for flexible polymers lies in the range of 0.5 - 0.8. For
extremely rigid polymers such as aromatic polyamides, it is larger on than unity.
The viscosity of a liquid (η)can be determined by a capillary viscometer and is given by -
η = Aρt + Bρ/t − − − − − − − − − − (3)

where ρ is density of liquid, t is the flow time, A and B are characteristics of a given viscometer
incorporating kinetic energy and end-effect corrections.

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A is defined as

hgπr2
A= − − − − − − − − − − (4)
8vl

where ‘h’ is the mean hydrostatic head of the liquid, ‘g’ is the gravitational constant, v = volume
of liquid flowing through a capillary of radius ‘r’ and length ‘l’.
The term B is due to kinetic energy corrections and arises from the fact that energy is
dissipated as a result of convergence and divergence of flow lines of different velocities at the
capillary ends.
In a dilute polymer solution, the density of solvent and solution is similar, and if flow
time is reasonably long (>100 seconds) one may neglect the Bρ/t term and in such cases
viscosity will be proportional to the flow time.
Relative viscosity of dilute solutions, therefore, may be determined from a knowledge
of efflux time of solution (t) and solvent (to),
η t
ηr = = − − − − − − − − − − (5)
ηo to

Specific viscosity ηsp indicating relative increment in viscosity of the solution over that
of solvent is given by
η - ηo t - to
ηsp = ηr - 1 = = − − − − − − − − − − (6)
ηo to

ηr and ηr are dimensionless ratios.

Specific viscosity per unit concentration ηsp ⁄c is designated as reduced viscosity (ηred )
and is dependent on concentration (g/ml). Extrapolation of reduced viscosity to zero
concentration gives intrinsic viscosity [η]. (written always in square brackets). The units of ηred
and [η] are reciprocal concentrations. The IUPAC nomenclature of various viscometric terms
is given in table 1.

TABLE 1: IUPAC NOMENCLATURE OF VISCOMETRIC TERMS

Symbol IUPAC nomenclature Defining equation

ηr Viscosity ratio η⁄ηo

ηred Viscosity number ηsp ⁄c

ηinh Logarithmic viscosity number lnηr ⁄c

[η] Limiting viscosity number (ηsp ⁄c)
c→0

The straight lines obtained by plotting ηred or ηinh vs. concentration are described by
number of empirical equations. Two of such equations given by Huggins in 1942 and
Kraemer in 1938 (eq. 8) are described as follows:

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 ηsp ⁄c = [η] + K' [η]2 c − − − − − − − − − − (7)

lnηr ⁄c = [η] + K'' [η]2 c − − − − − − − − − − (8)

where K’ is Huggins’ constant having a value of 0.35 in strongly solvating solvents and K”
Kraemer’s constant which is usually negative. K” is generally smaller in magnitude then K’
indicating thereby a smaller change in ηinh with concentration compared to the value ηred .
The value of ηinh at a fixed concentration (0.002 – 0.005 g/ml) may therefore be approximated
to [η].

EXPERIMENTAL
APPARATUS - glass capillary viscometer (Ubbelohde suspended level viscometer), constant
temperature bath, timer, 25 ml volumetric flask, pipette, stopwatch.
In Ubbelohde suspended level viscometer, for determination of [η], the effluent from
the capillary flows into a bulb separated from the main liquid reservoir. This allows the dilution
of polymer solution in the viscometer itself without transferring it. The solvent flow time should
be at least 100 sec. The viscometer should be cleaned with a chromic acid cleaning solution
(prepared by adding conc. H2SO4 to saturated sodium dichromate solution 1:1). The polymer
solution should be filtered through a fine sintered glass filter. A constant temperature bath with
an accuracy of ±0.1OC is essential for viscosity measurements because viscosity of a liquid
and hence efflux time is dependent on temperature.
In the volumetric flask dissolve 0.3 g (accurately weighed to 0.1 mg) of polymer in
appropriate solvent at room temperature.
Pipette exactly 10 ml of filtered solvent and introduce it into the bulb of Ubbelohde
viscometer. Place the whole assembly in a constant temperature bath. The solvent is then
brought into the bulb A and B attached above capillary of viscometer by closing tube C with
one finger and applying suction with a rubber bulb. When bulb B is partially filled then suction
is stopped, and finger is removed from C. The bulb B will start draining, creating a suspended
level at the bottom of the capillary. The stopwatch is started when the liquid meniscus passes
the upper mark on bulb A and stopped when it reaches the lower mark. These readings are
repeated at least three times and should agree to within 0.1% of average flow time.
Add 5 ml of filtered polymer solution and agitate the contents for thorough mixing. After
temperature equilibrium determine the flow time of this solution in similar manner as described
for solvent. Add another 5 ml of polymer solution and repeat the same steps as described till
readings for four polymer solutions have been taken.

RESULTS
Prepare a table listing concentration (g/ml), flow time of solvent and solution,
ηr , ηsp , ηred , ηinh . A plot of ηred (ηinh ) vs. concentration will yield the value [η] as intercept.
Calculate K and K’ and from the slope of these lines and [η]. From the value of ‘K’ and ‘a’
̅ v of polymer.
reported in literature, calculate M

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 EXPERIMENT – 3

INTERFACIAL POLYMERIZATION
(PREPARATION OF NYLON 6,10)

OBJECTIVES
Preparation of Nylon 6,10 by interfacial polymerisation

PRINCIPLE
Many of the polymers that are produced by the usual high temperature reactions could
be produced at low temperature by using the faster Schotten-Baumann reaction of acid
chlorides. Thus polyesters and polyamides could be produced by replacing the diacid or
diester by corresponding diacyl chloride.
Temperature used for interfacial polymers in the range of 0-50OC. Polymerization of
the two reactants take place at the liquid phases, each containing one of the reactants.
Polyamidation is carried out at room temperature by placing an aqueous solution of diamine
on top of the organic phase containing acid chloride. The reactants diffuse and undergo
polymerisation at the interface, the polymer product precipitated and is continuously withdrawn
in the form of filament and film if it has sufficient mechanical strength. The polymerisation rate
is usually diffusion controlled.
Interfacial polymerisation is mechanistically different from the usual step
polymerisation in that the monomer diffusing to the interface will react only with the polymer
chain ends.
By interfacial polymerisation, high molecular weight of polymer can be easily obtained
compared to the usual process. Polymerisation does not require overall bulk stoichiometry of
the reactants in the two phases.
There is always a supply of both reactants at the interface due to diffusion from the
organic and aqueous phase. Furthermore high molecular weight polymer is formed at the
interface regardless of the overall percent conversion based on the bulk amount of the two
reactants. An organic base must be present in aqueous phase to neutralise the by product
HCL. In controlling the molecular weight, the choice of solvent is very important (organic) as
polymerisation is usually taking place in organic solvent side of the interface in most systems.
The reason for this is the greater tendency of the diamine to diffuse into the organic solvent
compared to the diffusion of diacid chloride into the aqueous side of the interface. The organic
solvent can also affect the polymerisation by affecting the diffusion characteristics of the
reaction system.
It has been found that optimum molar ratio of two reactants in terms of producing
higher yield and or highest molecular weight is not always 1:1 but varies with solvent. The
optimum ratio of concentration of two reactants is that which approx the diffuse ratio of the two
reactants to the interface.

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REACTION SCHEME

H2N (CH2)6 NH2 ClOC (CH2)8 COCl

HMDA Sebacoyl Chloride

NaOH

* HN (CH2)6 NHCO (CH2)8 CO * NaCl H2O

Nylon 6,10

PROCEDURE
1. 1 g of hexamethylene diamine (HMDA) was weighed and dissolved in 25 ml of distilled
water.
2. One NaOH pellet was added to this aqueous solution.
3. 1 ml of sebacoyl chloride was mixed in 10 ml of CCl4 solvent.
4. Now into the organic solution, aqueous mixture was added slowly and with the help of
a glass rod the film formed was withdrawn from the interface.

OBSERVATION
A fine film of nylon 6,10 was obtained in the form of fiber.

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 EXPERIMENT – 4

ADDITION POLYMERIZATION
(BULK POLYMERISATION OF MMA)

INTRODUCTION
Free radical polymerisation of liquid monomer in bulk or with only small amounts of diluents
is a simple technique. The reaction can be carried out in the presence/absence of chain transfer
agent. The polymerization reaction can be investigated in terms of percent conversion as a function
of time. The effect of the concentration (chain transfer agent) and reaction time can be investigated
on the molecular weight of polymer (Molecular weight can be obtained by dilute solution viscosity
measurement).

PRINCIPLE
The free radical polymerisation of MMA is initiated by Azobisiso-butyronitrile (AIBN). The
degree of conversion is determined by refractometry/gravimetrically or by dilatometry.

APPARATUS AND MATERIALS

1. Constant temp. Bath,
2. Methyl methacrylate monomer,
3. Methanol,
4. Azobisisobutyronitrile (AIBN)

PURIFICATION OF METHYL METHACRYLATE

Wash the monomer with 10% NaOH to remove the inhibitor, usually an aromatic such as
hydroquinone or t-butylpyrocatechol. Shake the monomer with equal amounts of 10% sodium
hydroxide in a separating funnel. The heavier aqueous phase (brown in colour) is drained off. Repeat
the washing till you get brown colour in the aqueous layer. When the lower layer becomes colourless
then after draining, the monomer is washed repeatedly with distilled water till the washings are
neutral. Check with litmus paper.
The monomer is then placed over anhydrous sodium sulfate (100 g/L of monomer) overnight.
The monomer is then distilled under vacuum and stored in refrigerator.
AIBN is purified by recrystallisation. Recrystallisation of AIBN is done by preparing a
saturated solution in methanol and cooling in refrigerator. Collect the crystals after filtration and dry
under vacuum.

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PROCEDURE
Place 11 mg of recrystallised AIBN in a dry Erlenmeyer flask which is capped with a serum
stopper.
11 ml of freshly distilled MMA are introduced with the help of a syringe maintaining the
nitrogen flow. The mixture is swirled occasionally until the AIBN is dissolved.
Three dry test tubes are prepared by capping with serum stoppers and flushing with dry
nitrogen. Place 1 ml of the AIBN/MMA solution in each test tube and then add 5 ml of MMA. Tubes
are then placed in a water bath maintained at 60oC.
The tubes are removed after about 30, 60 and 90 min. and cooled quickly. The polymer was
precipitated by pouring into 200-300 ml of methanol. The percent yield - (P) of polymer after filtration
and drying in vacuum to constant weight, was then determined.

Yield of polymer (g)

P =
Monomer taken in feed (g) × 100

REPORT
Calculate the extent of polymerisation (P), gravimetrically and plot it as a function of time.
Report the rate of polymerisation.

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 EXPERIMENT – 5

PREPARATION OF LAMINATES

OBJECTIVES
1. Preparation of a one stage phenolic resin (resole),
2. Application of the resin preparation to the formation of laminates and carrying out the
curing process,
3. Synthesis of urea formaldehyde resin and fabrication of filled mouldings,
4. Preparation of a cold set adhesive, application of formulation to wood joining and
testing of the joint,
5. Synthesis of a melamine formaldehyde resin and carrying out its cross linking.

EXPERIMENTAL

1. PREPARATION OF A ONE-STAGE PHENOLIC RESIN

PROCEDURE
a) Mix together 25 g of phenol and 25 ml of formaldehyde solution. Add slowly with
swirling 2.5 ml of ammonia solution and heat the mixture carefully under reflux until
bubbles appear.
b) As soon as the reaction subsides continue heating until the liquid becomes cloudy.
Heat for a further 10 minutes after the cloud point and then allow to cool, when two
layers should separate.
c) Remove as much of the upper aqueous layer as possible with a small bulb pipette then
vacuum distil at approximately 80 rpm (Rotary evaporator) to complete the removal of
water. Continue the distillation until a sample of the hot resin withdrawn on the end of
a glass rod becomes brittle on cooling.
d) Stir in small amounts of ethanol until a mobile syrup is produced. It is advisable to stir
in the ethanol before resin cools and hardens. A minimum volume of ethanol should
be used, 10-15 ml should suffice.
e) Pour the resin into an aluminium foil tray and allow to cool.
f) Gently heat some of the resin syrup in a foil tray until it becomes hard and brittle. Grind
up some of this material and test its solubility in ethanol. Discuss reasons for the
change in solubility.
g) Discuss the applications of phenolic resins and the methods used to mould such
resins.

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 2. PREPARATION OF A PHENOLIC RESIN LAMINATE

REQUIREMENTS
Sheet of filter paper cotton cloth; Heated press; polyester film, slat dish.

PROCEDURE
a) Pour the resin syrup from 1 above into a flat dish and dilute with some ethanol. The
total volume of ethanol in the resin (including 1.4) should be about 20-25 ml. if the
syrup is too dilute then there will not be sufficient resin impregnated in the laminate to
give good adhesion. If the syrup is too thick it does not readily penetrate the paper and
is difficult to work with.
b) Impregnate sheets of papers and cloth by dipping into the syrup and then holding up
to drain. Surplus syrup is removed by presuming the sheets on a piece of glass and of
glass rod over them.
c) Dry the impregnated sheets in an oven for an hour keeping the temperature below
30OC.
d) Stack separately about 5 sheets of resin impregnated paper and about three sheets of
resin impregnated cloth. Separate the two stacks by a sheet of polyester film to allow
subsequent separation. Placed polyester film at the top and bottom of the stack.
e) Place the laminate stack between stainless steel sheets and place between the hot
plates of the press. The press should be at 180OC for adequate curing of the laminates.
f) Apply pressure and leave for 20 minutes. Open the press and remove the laminated
paper and cotton. Describe the appearance and physical properties of the laminates.
g) What is the advocate of laminated structure? Comment on this applies to your
samples.
h) Write equations for the reactions taking place. When the phenolic resin is cured.

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 EXPERIMENT – 6

BLENDS AND COMPOSITE

OBJECTIVE

a) To study the Extrusion process for making polymer blend and composite specimens.
b) To prepare polypropylene/Polystyrene blend and Polypropylene/Glass composite by
using Extruder.

INTRODUCTION

Extrusion is a high-volume manufacturing process in which polymer is melted, mixed

and formed into a continuous profile. The raw material used as powder or granules is fed

through a hopper into a heated barrel containing a rotating screw. As the material is conveyed

along the barrel, it is heated by conduction from the barrel heater and shear due to its

movement along the screw flights. The depth of the screw channel is reduced along the length

of the screw so as compact the material. At the end of the extruder, the material passes

through a die to produce an extrudate of the desired shape

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DIFFERENT ZONES OF EXTRUDER SCREW

(1) FEED ZONE

➢ The function of this zone is to preheat the material and convey it to the subsequent

zones

➢ The design of this section is important since the constant screw depth must supply

sufficient material to the metering zone so as not to starve it but must not supply so

much material that the metering zone is overrun.

➢ The optimum design is related to:

• The nature and shape of the feedstock.

• The geometry of the screw.

• The frictional properties of the screw and barrel in relation to the polymer.

(2) COMPRESSION ZONE

➢ In this zone the screw depth gradually decreases so as to compact the plastic.

➢ This compaction has the dual role squeezing any trapped air pocket back into the feed

zone and improving heat transfer through the thickness of material.

(3) METERING ZONE

➢ In this section the screw depth is again constant, but much less than the feed zone

➢ The melt is homogenised to supply at a constant rate, material of uniform temperature

and pressure to the die.

➢ This zone is the easiest to analyse since it involves a viscous melt-flowing along a

uniform channel.

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 Systematic representation of Extrusion process

PROCEDURE FOR THE PREPARATION OF PP/PS BLEND AND PP/GLASS FIBER

COMPOSITE
1. BLEND/COMPOSITE PREPARATION
➢ First prepare a pre-mixture of two different polymers/additives by adding some
wetting agent. A wetting agent helps the filler to stick to the granules so that
the final compositions may not vary. When a reinforcing agent is required for a
particular formulation then accordingly it may be added either along-with the
premix or at a later stage.
➢ Set the extruder temperature to the processing temperature of the major
polymer phase.
➢ When the temperature of each zone reaches to the set temperature, start the
screw rotation at a predetermined rpm so that the torque does not exceed the
permissible limit of the extruder. Add the premix to the extruder and make the
wire out of the extrudate followed by cooling and winding.

2. MATERIALS AND MACHINE SPECIFICATION

Materials Required: Propylene granules, polystyrene, Glass fibre.

OPERATING CONDITION

Extrusion process for making composites

Zone-1 Zone-2 Zone-3 Zone-4 Zone-5 Zone-6

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PRODUCT DEFECT AND TROUBLESHOOTING

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 EXPERIMENT – 7

3D PRINTING

OBJECTIVE

To study the material extrusion 3D printing technique of PLA material.

INTRODUCTION

Material extrusion 3D printing is a technique that utilizes layer-by-layer deposition

technology. Material extrusion 3D printing based on FDM technique is highly versatile for

polymeric materials due to convenient production of complex geometrical parts, production

speed, variety of build styles, variety of engineering polymers, ease of support removal and

cost- effectiveness. In the FDM method, a filament of thermoplastic polymeric material made

in the extruder is passed through a spool into a heated nozzle where it gets converted into a

molten state as it is heated upto the melting temperature of polymer and then deposited layer

by layer on the print bed according to CAD. The layers deposited fuses with each other to form

bond.

Feedstock feeding mechanism in FDM 3D printing process

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PARTS OF 3D PRINTER

FEEDER – Through feeder filament is inserted to the liquefier.

LIQUEFIER – Liquefier is attached with heating element, where filament gets melted and
passed to the nozzle.

NOZZLE – Melted material is passed through heated nozzle of a definite diameter.

BED PLATE – After leaving from nozzle material gets deposited on print bed layer-by-layer to
get a desired geometry.

CONTROLLING SCREEN – Process parameters appear on controlling screen, from where

we can change the parameters according to the material.

PROCEDURE FOR THE 3D PRINTING OF PLA MATERIAL

MATERIAL REQUIRED – Polylactic acid (PLA)

OPERATING CONDITIONS

PROCESS PARAMETERS
Material :
Print temperature :
Layer thickness :
Bed temperature :
Infill density :
Raster angle :
Print speed :

PRINTER SPECIFICATIONS
Equipment model :
Filament diameter :
Nozzle diameter :
Max. bed temperature :
Max. extrusion temperature:

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OBSERVATION AND RESULTS

PRODUCT DEFECTS AND TROUBLESHOOTING

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