The project aims to study about the method of the production of bio-plastics using
the bio-plastics to added plasticizer (Additives) and fillers. The filler is cocos-
nucifera shell powder. The cocus-nucifra shell powder is reinforcing filler. The
plasticizer used is tri-hydric alcohol as glycerol. The bio-plastics are Poly lactic
acid. It is made as aid for sodium hydroxide and hydrochloric acid. The bio-plastics
are synthesized in the presence of micro wave irradiation. The radiation time
duration is based on the dielectric Constant of the substance. Then process layout of
bio-plastics production is discussed. And then hardness test is conducted as per the
ASTM standards of plastics and also comparision of the results of test analysis
ABSTRACT III
LIST OF TABLE X
LIST OF FIGURE XI
1 INTRODUCTION
1.1.1 POLYMER 1
1.1.2 PLASTICS 1
1.1.3 BIO-PLASTICS 2
1.1.4 PLASTICIZER 2
1.1.5 FILLER 2
1.1.6 HARDNESS 3
1.1.8 BIODEGRADATION 3
1.1.9 HYDROLYSIS 3
1.2.4 GLYCEROL 5
2 LITRERATURE REVIEW 6
5 METHODOLOGY 14
7.1 DESCRIPTION 23
TEST METHOD
METHOD
METHOD
METHOD 33
METHOD
METHOD
SPECTROSCOPY
PRODUCTS
10.5 CLOTHING 45
11 CONCULSION 48
REFERENCES 49
LIST OF TABLES
10.5 CLOTHING 46
3 K Kelvin 5
7 US United States 12
9 % Percentage 13
11 M Molarity 14
19 Mm Milli meter 28
20 N Newton 29
1.1.1 POLYMER
1.1.2 PLASTICS
Bio-Plastics, that are made from renewable resources (plants like corn,
tapioca, potatoes, sugar) and which are fully or partially bio-based, and/or
biodegradable or compostable are called bio-plastics.
1.1.4 PLASTICIZER
1.1.5 FILLER
Fillers are usually solid additives mixed with plastics to improve material
properties, to introduce specific characteristics, or to reduce the cost of the
compound. In the case of mass volume biodegradable polymers, cost reduction has
practical importance besides improvement in the mechanical properties. Fillers are
inorganic or organic materials, and each group consists of fibrous and non-fibrous
types. Individual fillers are available in a number of grades differing in average
particle size and size distribution, particle shape and porosity, chemical nature of the
surface, and impurities. As a result of the presence of filler, hardness and stiffness
are increased while impact and tensile strength are usually decreased. talc, which is
commonly added as a filler, also acts as a nucleating agent for poly(1actide) and
increases the number of spherulites in crystallization.
1.1.6 HARDNESS
1.1.8 BIODEGRADATION
1.1.9 HYDROLYSIS
1.2.1 STARCH
The Royal Society of Chemistry describes the generic process for the manufacture
of starch based bio plastics. This involves hydrolysis of the starch by using an acid.
Abdorreza et al (2011) have described in their paper the physiological, thermal and
rheological properties
of acid hydrolysed starch. This paper shows that the amylose content increases ini
tially but continuous hydrolysis causes a decrease in the amylose content.
This fact is also corroborated in the paper by Karntarat Wuttisela et al (2008). The
amylose content is responsible for the plastic formation in starch. Plasticizers are
used to impart flexibility and mould ability to the bio plastic samples.
The filler material coconut shell powder composition has been discussed in paper by
C.J. Ewansiha in (2012) Chemistry Department, College of Education, P.M.B 003,
Igueben, Nigeria, have described the chemical composition of coconut shell powder.
The proximate analysis and mineral compositions of coconut shell were carried out
in this paper.
And the shell powder added polymer matrix composite has been discussed in paper
by J.Olumuyiwa Agunsoye (2012) Department of Metallurgical and Materials
Engineering, University of Lagos, Lagos, Nigeria. Have described the filler volume
fraction of coconut shell powder and the effect of the particles on the mechanical
properties of the composite produced was investigated. Because we selected cocous
nucifra shell powder is as reinforcing filler material.
The testing of bio plastic formation has been discussed in paper by K. Kanimozhi
(2014) department of Chemistry in Periyar University, Salem , Tamilnadu, India.
She described the analysis of bio plastics formation and its structure using FTIR
spectroscopy in various phases.
3. HISTORY OF BIO PLASTICS
Over the next few decades, more and more plastics were introduced, including some
modified natural polymers like rayon, made from cellulose products. Shortly after
the turn of the century, Leo Hendrik Baekeland, a Belgian-American chemist,
developed the first completely synthetic plastic which he sold under the name
Bakelite.
Nylon was first prepared by Wallace H. Carothers of DuPont, but was set aside as
having no useful characteristics, because in its initial form, nylon was a sticky
material with little structural integrity. Later on, Julian Hill, a chemist at DuPont,
observed that, when drawn out, nylon threads were quite strong and had a silky
appearance and then realized that they could be useful as a fibre.
The World Wars also provided a big boost to plastic development and
commercialization. Many countries were struck by a shortage of natural raw
materials during World War II. Germany was cut off quite early on from sources of
natural latex and turned to the plastics industry for a replacement. A practical
synthetic rubber was developed as a suitable substitute. With Japan’s entry into the
war, the United States was no longer able to import natural rubber, silk and many
metals from most Far Eastern countries. Instead, the Americans relied on the plastics
industry. Nylon was used in many fabrics, polyesters were used in the
manufacturing of armor and other war materials and an increase in the production
synthetic rubbers occurred.
Advances in the plastics industry continued after the end of the war. Plastics were
being used in place of metal in such things as machinery and safety helmets, and
even in certain high temperature devices. Karl Ziegler, a German chemist developed
polyethylene in 1953,
And the following year Giulio Natta, an Italian chemist, developed polypropylene.
These are two of today’s most commonly used plastics. During the next decade, the
two scientists received the 1963 Nobel Prize in Chemistry for their research of
polymers.
In, 8th Sep, 1924 Henry Ford, in an attempt to find other non-food purposes for
Agricultural surpluses. Ford began making bio plastics for the manufacturing of
automobiles. The bio plastics were used for steering wheels, interior trim and
dashboards. Ford has been using them ever since.
In 13th Aug, 1941 Henry Ford unveiled the first bio plastic car in 1941. This car had
a bio plastic body and parts consisting of 14 different bio plastics. There was a lot of
Interest, but soon after, world war two was started and attentions were diverted.
In 9th Aug, 1990 A British Company, Imperial Chemical Industries, developed a bio
plastic, Bio polymer, which is biodegradable. This was the beginning of the bio
plastic Revolution.
4. ECONOMICS OF BIO PLASTICS
Over the next eight years, shares in demand of the individual world regions will
shift significantly. Ceresana forecasts two regions to considerably influence the bio
plastics market. Because of dynamic growth in consumption and production, Asia-
Pacific will expand its share of bio plastics demand. As a result, Asia-Pacific will
almost draw level with Europe and North America. In addition, South America will
see strong growth, mainly because of massive increases in production in Brazil.
The market research institute Ceresana expects the global bio plastics market to
reach revenues of more than US$2.8 billion in 2018 - reflecting average annual
growth rates of 17.8%. Bio plastics are supposed to contribute to protecting the
climate, provide a solution for the waste issue, reduce the dependence on fossil raw
materials, and improve the image of plastic products. With a roughly 35% share,
Europe was the largest outlet for bio plastics in 2010, followed by North America
and Asia-Pacific.
5. METHODOLOGY
Musa peels and Starch are boiling with water for 60 minutes over 373K.
The water is decanted from the beaker and the peels are now left to dry on
filter paper for about 45 minutes.
After the peels are dried. The peels are grinding by the mixer grinder over up
to 60 minutes and Starch solution was boiled 15 minutes. Now starch paste
was ready to use.
1 WATER 80.3
2 GLYCEROL 47 to 68
5 NaOH 57.5
6 STARCH 3.6
o The important thing is the DK value. If the DK value is low then, the rate of
heat is low and its takes more minutes.
o As the DK value is high the rate of heat is high its take less time.
o We consider only shell dust and hydro chloric acid. it have low DK value.
We put the paste in oven over 45 minutes.
5.6 SYNTHESIS OF BIO PLASTICS:
o 500gm of paste is placed in a beaker
o 60ml of (0.5 N) HCL is added to this mixture and stirred using glass
rod.
o 40ml Plasticizer is added and stirred.
o 0.5 N NaOH is added according to pH desired,
o And adding filler as per 0%, 5%, and 10% respectively.
o Then add gelatin for more adhesiveness for filler with PLA.
o The mixture is spread on a ceramic tile or petri dish and this is put in
the oven at 393K and is baked till dry.
o Than the specimen was out from oven, cool the specimen overnight.
o Now the specimen eligible for testing.
STATUS OF TRIAL:
STATUS OF TRIAL:
STATUS OF TRIAL:
7.1 DESCRIPTION:
Since this form of bio plastic product does not have a fixed, defined market,
the production has to be done in a batch process. The location of the plant should be
next to a banana processing facility which makes any value added product like
banana chips, flour, puree etc. The large amount of banana peel waste generated can
be used to make bioplastics in situ. The process for manufacturing the banana based
bioplastic is as shown in the flowchart. The banana peels are gathered in a
temporary storage vessel for processing. The peels are then moved via a screw
conveyor to the washing section where the samples are sprayed with water mixed
with mild surfactant to remove the dirt and grit. The samples are then rinsed again to
remove the residual surfactants. The peels are then transferred to an agitated vessel
with a jacket for heating where the banana peels are boiled. Peels are then filtered to
remove excess water and are transferred to stacks of trays to dry on for half an hour.
The drying is done at ambient temperature at atmospheric conditions. The dried,
boiled peels are then sent to an industrial grinder where they are ground to a
paste.This paste is then sent to a reaction chamber. In it the paste is mixed with
dilute 1 N HCl and a suitable plasticizer (here Glycerol) for a residence time of 15
minutes. The reaction taking place here involves acidic hydrolysis of starch. The
addition of the plasticizer aids in plastic formation. A tank with paddle type agitator
is selected. Paddle agitator will scrape from the sides and not allow for formation of
pockets. The reaction mixture is transferred into the neutralization tank to stop the
reaction. Here calculated amounts of 1 N NaOH are added to the reaction mixture to
neutralize the acid and stop the reaction. Finally the paste is spread into a thin film
and baked in an oven at about 393K. The thin film is peeled off the base and is now
ready to use. If thick plastic is needed it was made by using slow baking.
7.2 PROCESS LAY-OUT OF BIO PLASTICS PRODUCTION:
2. Tensile Test
4. Solubility Test
5. Flame Test
A tensile test, also known as tension test, is probably the most fundamental
type of mechanical test you can perform on material. Tensile tests are simple,
relatively inexpensive, and fully standardized. It was opposed to compressive test.
The test’s ASTM standard is D882.
A 2cm by 4cm rectangular slice is cut out of the sample for testing. The slice
dimensions are kept constant for all samples to ensure uniformity in the
testing procedure.
The slice of sample obtained is the clamped between 2 clips. One end of the
clip is attached to a support and the other end has a suspended pan for
placing weights in them.
The clamping positions are also kept constant. The figure below shows
the sample with the clamping locations. Applying the thumb rule for
tensile strength testing, the samples are clamped such that 60% of the
sample is between the clamps and is our testing region.
Once the sample has been clamped, weights are added in steps of 10
grams each. A gap of 20 seconds is provided between the addition of
weights to allow the sample to stretch and tear.
The final weight at which the sample tears is noted using an
electronic balance.
For tensile strength calculations, we use the following formula: The weight is
calculated from the electronic balance readings.
Now for the cross-sectional area we use a Vernier caliper, Least Count =
0.02 mm to measure the thickness. The product of the sample width and the
average thickness gives us the cross-sectional area of the sample. Thus using
the above equation we calculate the tensile strength for all samples.
Powder +Gelatin
Powder+ Gelatin
Acid and alkaline test was identifying the bio plastics durability in strong and
weak acid and alkaline.
The test was to identify the Time duration of the bio plastic is fully soluble in
acid.
The acid test solvent is sulphuric acid and acetic acid, the sulphuric acid was
strong acid, the acetic acid was weak acid. Now take 0.5 M of both acids of 400ml,
Than the bio plastic was placed in the beaker. The bio plastic is start soluble in acids
now check the time duration of bio plastics is fully soluble in strong and weak acid.
The test was to identify the Time duration of the bio plastic is fully soluble in
alkaline.
The alkaline test solvent is sodium hydroxide, the NaOH was strong alkaline,.
Now take 0.5 M of NaOH of 400ml,
Than the bio plastic was placed in the beaker. The bio plastic is start soluble in
alkaline now check the time duration of bio plastics is fully soluble in NaOH.
The test was to identify the Time duration of The bio plastic is fully soluble in
water.
The test was to identify the Time duration of the bio plastic is fully Fired &
Asher. This test was conduct only for check the bio degradability of bio plastics.
Bio plastics is become ashes it is bio degradable. It was easiest and quickest test to
find bio degradability of bio plastics.
The flame test is conduct in front of water. The bio plastics are fired use of
pun son burner. Now bio plastics was start burning, now note the time duration of
bio plastics fully burned.
FTIR spectra reveal the composition of solids, liquids, and gases. The most
common use is in the identification of unknown materials and confirmation of
production materials (incoming or outgoing). The information content is very
specific in most cases, permitting fine discrimination between like materials. The
speed of FTIR analysis makes it particularly useful in screening applications, while
the sensitivity empowers many advanced research applications.
The total scope of FTIR applications is extensive.
FTIR analyses were made to determine the functional groups of the products
obtained in order to understand more deeply what happens in the polymerization of
Poly (lactic acid). A qualitative analysis of absorption bands with reaction time
shows a decrease in the intensity of some bands and, the formation of new ones,
indicating the end groups which decrease and those formed due to the
polymerization reaction progress. Analysis of FTIR spectrum of the sample from
step obtaining lactide allows us to confirm that there was formation of the product,
verifying the characteristic bands of the material. Figure shows the spectrum
obtained compared to lactide of lactic acid. It can be seen the band around 3667 cm-
1
, which decreases the ring lactic acid, as well as the characteristic bands of the ring
indicating that there was formation of lactide, a dime of structure cyclic.
Figure shows the FTIR spectrums of the monomer and the poly (lactic acid) which
was obtained from 2 of reaction. The PLA spectrum shows the bands at 3046.98 cm-
1 and 2,821.35 cm-1 from symmetric and asymmetric valence vibrations of C-H
from CH3, respectively. It is possible to observe a band shift related to the C=O
stretch in the monomer in 1,644.02 cm-1 to 1,412.60 cm-1 in the polymer.
These bands that show shifts of monomer to polymer also show a difference in the
peak intensity which suggests the arrangement of molecules in the polymer chain.
Bands corresponding to bending vibrations of CH3 (asymmetric and symmetric)
were found in 1,412.60 cm-1 and 1,005,70 cm-1 in the polymer spectrum as greater
intensity peaks compared with those from monomer found in 1,412.60 cm -1 and
1,644.02 cm-1. C-O-C asymmetrical and symmetrical valence vibrations were found
at 1,250.73 cm-1 and 1,200.59 cm-1 respectively; at 1,333.68 cm-1 is detected the C-
O-C stretching vibration. The band around 3046.98 cm -1 is related to the stretching
of OH group and this decreases from the monomer to the polymer due to reaction
poly esterification that consumes the OH groups when they react with the acid
groups to form the ester bond.
The analyses of FTIR spectrum of the sample of PLA were confirmed checking the
characteristic bands of the material. The spectrum compared lactic acid and this
material indicated that was formation of PLA, a cyclic dimer structure.
9. ANALYSIS OF BIO PLASTICS
10.5 CLOTHING:
As said above bio plastics are used for interior of cars, but bio plastics are
present also in other automotive applications. Those applications have very specific
requirements (as a fuel line made from renewable resources - nylon).
This project work shows synthesis of bio plastics (PLA) from musaceae family
plants and increases the hardness of the bio plastics with use of coconut shell
powder. The filler volume is increased 5% and 10% the hardness value is increased
but same time tensile strength was decreased due to porosity. Coconut shell powder
increase the hardness of the bio plastics. Than the acid and alkaline test results
shows bio plastics durability and solubility test results shows osmosis nature of bio
plastics. A flame test result shows bio degradability nature of bio plastics. The FTIR
spectroscopy results shows poly lactic acid‟s functional group the FTIR result
shows formation of PLA from starch and Hydrochloric acid with glycerol . Finally
the filler material is increase the hardness. This property is an added requirement for
automobile interior, packaging, agriculture and sports goods
REFERENCES
.
1. J. O. Agunsoye , Talabi S. Isaac, Sanni O. Samuel (2012) “Study of
Mechanical Behaviour of Coconut Shell Reinforced Polymer Matrix
Composite”. Journal of Minerals and Materials Characterization and
Engineering, 2012, 11, 774-779.
2. C.J. Ewansiha1, J.E. Ebhoaye, I.O. Asia, L.O. Ekebafe and C. Ehigie(2012)
“Proximate and Mineral Composition of Coconut (Cocos-Nucifera) Shell”
International Journal of Pure and Applied Sciences and Technology ISSN 2229
– 6107.
5. Veeran Gowda Kadajji and Guru V. Betageri (2011) “Water Soluble Polymers
for Pharmaceutical Applications”. Polymers 2011, 3, 1972-2009;
doi:10.3390/polym3041972. ISSN 2073-4360
6. www.plastice.org
7. www.youtube.com/user/plasticeproject
10. http://en.european-bioplastics.org
11.Guido Giachi, Marco Frediani, Luca Rosi and Piero Frediani, “Polymers by
Microwave Irradiation”, University of Florence, Italy.
.
12. Seong-Kyun Lee. Principles of Microwave Oven, 0240126.
14. Nanou Peelman et “Application of bio plastics for food packaging Trends” in
Food Science & Technology 32 (2013) 128 to 141.