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Ram Thesis
Ram Thesis
The thesis work explores the utilization of raw wheat straw as a potential source for the
production of films and cups through phosphorylation. Initially, the delignification of raw wheat
straw was carried out, resulting in a 37.75% yield. The delignified wheat straw was then
phosphorylated for different curing times, and the yield of phosphorylation was found to be 63%.
The resulting gel was used to create films by casting them in plastic petri plates, which exhibited
flame retardancy, water absorbency, and good tensile strength. The water absorbency test
revealed that the films made from the gel could absorb a significant amount of water, with WSF-
45 absorbing 814% of its weight worth of water, WSF-60 absorbing 447%, and WSF-75
absorbing 387%. Flame retardancy studies indicated that the films had a reduced rate of burning,
with WSF-45, WSF-60, and WSF-75 showing a rate of burning of 0.9735cm/s, 0.5357cm/s, and
0.3571cm/s, respectively. Moreover, the mechanical strength of the films was measured, and the
results demonstrated good mechanical strength. The migration studies were also conducted,
which showed that the films were under the permissible limits of migration effects of isooctane
and 50% ethanol. Additionally, cups were made from the gel using molds, which were stable in
water at high temperatures. The water stability test showed that the cups were stable at 80, 100,
and 150°C. The charge content of the gel was determined using conductometric titration, with
results of 200mmol/kg, 266.66mmol/kg, and 350mmol/kg for WSF-45, WSF-60, and WSF-75,
respectively. The findings of this study suggest that phosphorylation of wheat straw could be a
potential approach for the development of eco-friendly and sustainable films and cups.
INTRODUCTION
Agricultural Biomass:
Agricultural biomass refers to organic materials derived from plants and animals used for energy
production, such as biofuels, electricity, and heat. This includes crops such as corn, wheat,
sugarcane, and soybeans, as well as residues like straw, husks, and stalks. Agricultural biomass
also includes animal manure and other organic waste from livestock and poultry farming. These
materials can be converted into usable forms of energy through various processes, such as
of energy because it is produced from living organisms that can be grown and replenished, unlike
Animal feed: Agricultural biomass such as hay, silage, and other crop residues can be used as
animal feed, providing a low-cost source of nutrition for livestock and poultry.
Soil amendment: Crop residues like straw, stalks, and husks can be incorporated into soil to
Food and beverages: Some agricultural biomasses such as corn and wheat can be processed into
food and beverages, such as corn syrup, cooking oil, and beer.
Overall, agricultural biomass is a versatile resource that can be used in many different
applications beyond fuel and energy production, contributing to sustainable agriculture and a
circular economy.
Advantages of Agricultural Biomass:
derived from plants and other organic matter that can be replenished over time. This makes it a
Reduces Greenhouse Gas Emissions: Agricultural biomass can help to reduce greenhouse gas
emissions, as it emits lower levels of carbon dioxide compared to fossil fuels. When crops are
grown for biomass, they absorb carbon dioxide from the atmosphere through photosynthesis.
When the biomass is burned, the carbon dioxide is released, but the net carbon dioxide emissions
are lower compared to burning fossil fuels, which release carbon dioxide that has been trapped
Provides Economic Opportunities: The production and use of agricultural biomass can provide
economic opportunities for farmers and rural communities. Farmers can earn additional income
by selling biomass crops, and biomass production can create jobs in rural areas.
Reduces Waste: Agricultural biomass can also help to reduce waste, as it can be derived from
agricultural residues such as crop stalks and husks that would otherwise be burned or left to
decompose.
Land Use: The production of biomass crops requires land, which can compete with food crops
and natural habitats. There are concerns that large-scale biomass production could lead to
Water Use: Biomass crops also require water for growth, and in regions where water resources
are limited, this could lead to water scarcity and competition with other uses, such as food
production.
Transport and Storage: Biomass crops need to be transported and stored, which requires
additional infrastructure and energy. This can increase the cost and environmental impact of
biomass production.
Pollution: Biomass combustion can release pollutants such as particulate matter, nitrogen oxides,
and sulfur dioxide, which can contribute to air pollution and have negative health impacts.
However, modern biomass combustion technologies have significantly reduced emissions
Overall, agricultural biomass has the potential to provide sustainable and renewable energy, but
its production and use must be carefully managed to minimize its environmental impacts and
Cellulose is the main component of agricultural biomass, and it can be extracted using a variety
of methods.
The following are some common methods for extracting cellulose from agricultural biomass:
Acid Hydrolysis: This method involves treating the agricultural biomass with an acid, such as
sulfuric acid or hydrochloric acid, which breaks down the cellulose into glucose. The glucose can
then be separated from the other components of the biomass using various separation techniques.
Enzymatic Hydrolysis: Enzymatic hydrolysis involves the use of enzymes to break down the
cellulose into glucose. This method is more environmentally friendly than acid hydrolysis, but it
steam, which causes the cellulose to break down and become more accessible for extraction.
Alkali Treatment: Alkali treatment involves treating the agricultural biomass with an alkaline
solution, such as sodium hydroxide or potassium hydroxide, which breaks down the lignin and
hemicellulose in the biomass and makes the cellulose more accessible for extraction.
Organosolv Treatment: Organosolv treatment involves treating the agricultural biomass with an
organic solvent, such as ethanol or methanol, which dissolves the lignin and hemicellulose and
Once the cellulose is extracted from the agricultural biomass, it can be further processed into
various products, such as paper, textiles, and bioplastics. The extracted cellulose can also be used
composites. Another approach is by using sodium chlorite, Sodium chlorite can also be used to
extract cellulose from agricultural biomass, particularly from non-wood sources such as straw,
corn stover, and bagasse. The process, known as the sodium chlorite method, involves treating
the biomass with a mixture of sodium chlorite, acetic acid, and sodium hydroxide.
During the process, the sodium chlorite breaks down the lignin in the biomass, which separates
the cellulose fibers. Acetic acid and sodium hydroxide act as buffers to control the pH and
prevent the breakdown of the cellulose. The resulting cellulose fibers can then be further
The sodium chlorite method has several advantages over other methods of cellulose extraction,
including:
High Yield: The sodium chlorite method has been shown to produce a high yield of cellulose,
Low Environmental Impact: The process does not use any hazardous chemicals, and the
Energy Efficient: The sodium chlorite method is energy-efficient compared to other methods,
However, the sodium chlorite method is not without its disadvantages. The process can be
expensive, and the resulting cellulose fibers can be less pure than those produced by other
methods. Also, using sodium chlorite raises concerns about the safety of workers who handle the
chemical. Overall, the sodium chlorite method is a promising approach to cellulose extraction,
but further research is needed to evaluate its commercial viability and environmental impact.
Introduction of cellulose:
Cellulose was found and coined by a French chemist named Anselme Payen in 1838. Cellulose is
found in plant cell walls which gives them structural strength along with lignin, hemicellulose,
etc. up to 50% of all tree trunks and other parts consist of cellulose. Cotton is the purest form of
cellulose; it is made up of 90% cellulose. Cellulose is the most abundant biopolymer on earth
Cellulose is very cheap and easy to obtain and can be derived from wastes like husk, straw, tree
parts, etc. Many hybrid materials can be derived from cellulose by functionalizing it with a
variety of different reagents. Some of them are celluloid, cellulose phosphate, cellophane, rayon,
cellulose acetate, ...etc. it has the potential to replace synthetic polymers which are harmful to
nature and provide us with a better alternative as it is biodegradable, cheap, easily available, and
non-toxic. Amounts exceeding 500 billion metric tons of cellulose are produced per year
worldwide.
cellulose has some unique features such as low density, biodegradability, high tensile strength,
and high Young's modulus. However, cellulose is lacking in some areas such as poor solubility
in aqueous and organic solvents, poor functionality, and poor dimensional stability. Derivatives
of cellulose by combining it with inorganics give rise to a promising class of materials that have
been widely applied as composite polymer films, sponges, hydrogels, membranes, dressing
shells, etc. these materials are also very attractive from a sustainability point of view since they
enable using of renewable sources and reduce the use of petroleum-based synthetic polymers
Structure of cellulose:
Cellulose is an unbranched molecule. Glucose is a polymer that has linearly organized polymeric
chains. Hydrogen atoms and hydroxyl groups securely keep the chains together by forming
hydrogen bonds between them. This causes the development of sturdy, rigid cellulose
microfibrils.
glycosidic bonds and every other monosaccharide is rotated 180 degrees to its neighbouring unit.
hydrogen bonding (intermolecular and intramolecular) not only provides cellulose with excellent
mechanical properties but also makes it insoluble in many solvents. The reactivity of the three
hydroxyl groups at carbons 2,3 and 6 offers possibilty for making many useful derivatives.
The properties of derivatives depend on the type, distribution, and uniformity of the groups
substituting at carbons 2,3, and 6. Properties like solubility and plasticity depend on the degree of
substitution and molar substitution. They have beta orientation in which the -OH group of the
anomeric carbon or C-1 is directed above the plane of the glucose ring. The -OH groups of the
rest of the carbon atoms are directed below the plane of the ring. In cellulose, every alternate
glucose molecule is inverted to create beta 1-4 glycosidic linkages. In contrast to C-4, whose -
OH group is pointed down the plane, -OH group of C-1 is pointed upward. Now, one of these
molecules must be turned inside out so that both hydroxyl groups are in the same plane to form a
beta 1-4 glycosidic link. This is the reason for every alternate glucose molecule in cellulose
becoming inverted.
Cellulose phosphate is a type of biopolymer that has gained attention in recent years due to its
Cellulose phosphate is created by introducing phosphate groups onto the cellulose molecule,
This modification alters the properties of cellulose, making it more versatile and useful in a range
of applications.
One potential application of cellulose phosphate is as a biomaterial for medical and healthcare
has shown promise in applications such as drug delivery, tissue engineering, and wound healing.
Cellulose phosphate has also been studied for its potential use in water treatment applications. Its
negative charge and water solubility make it effective in absorbing heavy metals and other
pollutants from water, and it has been shown to have higher adsorption capacity compared to
Cellulose phosphate is a promising material that has potential applications in various fields,
including biomedicine, environmental science, and material science. Its unique properties and
biocompatibility make it an attractive candidate for a range of applications, and further research
Biomedical Applications: Cellulose phosphate has gained attention for its potential use as a
non-toxicity. Biocompatibility refers to the ability of a material to interact with living cells
without causing harmful effects, while biodegradability refers to the ability of a material to break
down into harmless components in the body. Cellulose phosphate has shown promise in drug
delivery applications, where it can be loaded with drugs and targeted to specific cells or tissues.
The negative charge of cellulose phosphate allows it to bind to positively charged drug
molecules, allowing for controlled release of the drug. Cellulose phosphate has also been studied
for use in tissue engineering, where it can be used to create scaffolds for cell growth and tissue
regeneration. Its biocompatibility and ability to support cell growth make it an attractive
candidate for this application. In addition, cellulose phosphate has been studied for use in wound
healing applications, where it can promote tissue regeneration and reduce inflammation. The
negative charge of cellulose phosphate can also attract positively charged molecules involved in
Water Treatment Applications: Cellulose phosphate's negative charge and water solubility make
it an effective adsorbent for heavy metals and other pollutants in water. It has been shown to
have higher adsorption capacity compared to other commonly used adsorbents, such as activated
carbon and chitosan. Cellulose phosphate can be used in various water treatment applications,
treatment, cellulose phosphate can be used to remove pollutants such as heavy metals, dyes, and
pollutants such as arsenic and lead. In desalination, cellulose phosphate can be used to remove
Food Applications: Cellulose phosphate has potential use in food applications, particularly as a
food additive. It has been shown to be an effective emulsifier and stabilizer in food products,
such as salad dressings and mayonnaise. Emulsifiers are substances that help to mix oil and
water, while stabilizers help to maintain the texture and consistency of food products. Cellulose
phosphate's negative charge allows it to interact with other food ingredients, such as proteins and
carbohydrates, to form stable emulsions and suspensions. In addition, cellulose phosphate has
potential use as a fat replacer in low-fat or reduced-fat food products. Its ability to form stable
emulsions can help to mimic the texture and mouthfeel of fats in these products.
Energy Applications: Cellulose phosphate can be used in energy applications, particularly in
biofuel production. This can make biofuel production more efficient and sustainable. Hydrolysis
is the process of breaking down a molecule using water, and in this case, cellulose phosphate can
help to accelerate the hydrolysis of cellulose. This can make biofuel production more efficient
and sustainable.
Overall, cellulose phosphate is a versatile material with potential applications in various fields.
While further research is needed to fully understand its potential and limitations, cellulose
phosphate holds promise as a sustainable and biocompatible material for a range of applications.
The delignification of wheat straw was carried out using a solution made up of 54g of sodium
acetate trihydrate, 30g of sodium chlorite, and 24ml of glacial acetic acid. In a conical flask, raw
wheat straw was taken and the delignifying solution was added to it. The flask was covered with
aluminium foil and kept in an oven set at 80°C overnight. The next day, the solution was
discarded and a new batch of delignifying solution was added to the wheat straw. The flask was
covered again with aluminium foil and kept in the oven overnight.
On the third day, the delignified wheat straw was washed thoroughly with distilled water 5-10
times to remove any remaining traces of the delignifying solution. The washed delignified wheat
straw was then kept for drying for 12 hours at room temperature. The drying process was carried
After the drying process, the delignified wheat straw was ready for further use. The
delignification process was carried out in triplicate to ensure the accuracy and reliability of the
results. The extent of delignification was determined by measuring the residual lignin content
using the standard analytical method. The results obtained from this study showed that the
delignification process was successful in removing a significant amount of lignin from the wheat
straw.
To study the effect of phosphorylation on wheat straw, delignified wheat straw was taken into a
glass bottle and phosphorylating solution was added to it. The phosphorylating solution was
prepared by dissolving 15g of di-ammonium hydrogen phosphate and 60g of urea in 1L of water
in the ratio of 4:1. The solution was stirred well until it was completely dissolved.
The mixture was initially incubated in an 80°C oven for 6 hours to ensure complete reaction
between the wheat straw and the phosphorylating solution. After 6 hours, the mixture was
transferred onto petriplates and dried at 105°C for 6 hours to obtain a dry powder.
To cure the cellulose, the powder was heated at 150°C for 45, 60, and 75 minutes. After heating,
the powder was allowed to cool to room temperature. For the preparation of the gel, the mixture
was washed thoroughly with distilled water for 5-10 times to remove any unreacted
phosphorylating solution.
The obtained gel was then grinded with a mixer to homogenize the mixture. The final gel was
used for further analysis. The extent of phosphorylation was determined by measuring the degree
The phosphorylation process was carried out in triplicate to ensure the accuracy and reliability of
the results. The results obtained from this study showed that the phosphorylation of wheat straw
led to an increase in the degree of substitution of the cellulose. The gel obtained from the
phosphorylation process can be further used for the preparation of various cellulose-based
materials. Overall, the phosphorylation process provides a promising route for the modification
To prepare the cellulose phosphate gel, 50g of the prepared gel was taken in a beaker. To form a
homogeneous solution, 100ml of distilled water was added to the beaker containing the gel. The
mixture was then stirred with a magnetic stirrer for 15 minutes to ensure complete dissolution of
the gel.
After stirring, the mixture was allowed to ultrasonicate for 45 minutes to remove any trapped air
bubbles and to improve the homogeneity of the solution. The ultrasonication process was carried
After ultrasonication, the mixture was casted on plastic petri plates. The plates were carefully
selected and cleaned beforehand to prevent any contamination. The mixture was evenly
distributed on the plates using a spatula to form a thin layer. The plates were then left to dry at
The results obtained from this study showed that the prepared cellulose phosphate gel had
excellent mechanical properties and can be used as a potential candidate for various applications
To make cups from cellulose phosphate gel, a beaker was taken as Mould. A little oil was
applied to the beaker to retrieve the gel easily when it forms. The gel was taken in generous
amounts and smeared on the beaker. Then the beaker was kept in an oven for 6 hours in an oven
set at 80°C
the water absorption behavior of the prepared cellulose phosphate gel, three strips of identical
weight were cut from each of the curing times, which were 45, 60, and 75 minutes. The strips
The weight of each strip was measured using a digital balance with an accuracy of 0.001g. The
strips were then soaked in water for 24 hours to ensure complete water absorption. The water
absorption process was carried out at room temperature to ensure uniform conditions.
After 24 hours of soaking, the strips were removed from the water and excess water was
removed using tissue paper. The strips were then re-weighed using the digital balance to measure
The water absorption experiment was carried out in triplicate for each curing time to ensure the
reliability and reproducibility of the results. The data obtained from the experiment was analyzed
using statistical methods to determine the significance of the differences between the water
The results obtained from this experiment showed that the water absorption of the cellulose
phosphate gel increased with increasing curing time. The highest water absorption was observed
for the strips cured for 75 minutes, while the lowest water absorption was observed for the strips
Overall, the water absorption experiment provided valuable insights into the water absorption
behavior of the prepared cellulose phosphate gel and its potential for various applications such as
Conductometric titration
To calculate the charge content of the gel, conductometric titration was performed by taking
enough gel containing 0.3 g dry wheat straw gel mass and adding 5 ml of 0.1M NaCl, and 80 ml
of distilled water. The pH of the fiber suspension was brought down to 3 by adding 0.1M HCl in
10µl increments. After the pH was brought down to 3 the solution was titrated with 0.05M
NaOH while monitoring the electrical conductivity of the suspension. NaOH was added at
increments of 100µl.
Graph was plotted between conductivity and vol. Of NaOH used in titration. The plot was used
To evaluate the flame retardancy properties of the films made with the prepared cellulose
phosphate gel, three strips of dimension 2cm*7.5cm were cut from the films cured for each time
period which were 45, 60, and 75 minutes. The strips were cut using a precision cutter to ensure
their uniformity.
The strips were marked lengthwise in 1cm intervals using a permanent marker. The strips were
then subjected to a flame using a bunsen burner. The entire process was video-graphed for 40
seconds, and snaps were taken of each strip at regular intervals to monitor the burning behavior.
The experiment was carried out in a well-ventilated laboratory to ensure the safety of the
researchers. All necessary safety precautions, including wearing protective equipment, were
The video footage and snaps obtained from the experiment were analyzed to determine the flame
retardancy behavior of the films. The parameters analyzed include the time taken for the strip to
ignite, the time taken for the strip to extinguish, and the length of the strip burnt.
The results obtained from this experiment showed that the flame retardancy of the films
increased with increasing curing time. The films cured for 75 minutes exhibited the highest
flame retardancy properties, while the films cured for 45 minutes exhibited the lowest flame
retardancy properties.
Overall, the flame retardancy experiment provided valuable insights into the flame retardancy
behavior of the films made with the prepared cellulose phosphate gel and its potential for various
To evaluate the water stability of the cellulose phosphate cup, the cup was first placed in a
beaker and submerged in water. The beaker was then covered with aluminum foil to prevent
evaporation.
The beaker containing the cup was then subjected to different temperatures and time periods to
simulate various conditions. Specifically, the beaker was kept at 80°C for 5 hours, 100°C for 6
After each time period, the cup was removed from the beaker and checked for stability. Stability
was assessed based on whether or not the cup had maintained its shape and structure, and if it
The results obtained from this experiment showed that the cellulose phosphate cups were stable
at all temperatures and time periods tested. There were no signs of degradation or disintegration,
Overall, the water stability experiment provided valuable insights into the suitability of cellulose
phosphate cups for various applications such as food packaging and disposable tableware, where
WSF- 45 shows the best swelling property and the propert is decreasing with increase in curing
time
Conductometric titration
Figure no : plots of conductometric titration of WSF – 45, 60, and 90
(g)
FTIR
Figure no : FTIR spectrum of DWS, WSF-45, WSF-60, and WSF-75
In FTIR, peak at 898 shows the formation of P-O-C bonds, which confirms the phosphorylation
of cellulose
X-ray Diffraction
Figure no : intensity vs 2θ plot of DWS, WSF-45, WSF-60, and WSF-75
XRD plot of intensity against 2θ shows that there is not much structural change in cellulose upon
delignification and phosphorylation at different curing times, however chemical composition has
changed
Flame retardancy
As the charge content increases the flame retardancy of the film has increased
Water stability
Cups made were stable at 80°C, 100°C, and 150°C
Figure no :
All the films were under the permissible limits of migration for isooctane and 50% ethanol
Mechanical strength
Contact angle
The contact angle of WSF–45 is the lowest, which indicates it has the highest wettability.
The contact angle of all the films were 70° at the beginning of the experiment then later after 5
mins were reduced to 20°, 25°, and 33° for WSF-45, WSF-60, and WSF-75 respectively .
Conclusion
The production of eco-friendly and sustainable packaging materials has become increasingly
important in recent years due to the negative environmental impacts of conventional packaging
materials. This has led to a growing interest in exploring alternative sources for the production of
packaging materials. Raw wheat straw is one such alternative source that has gained significant
attention due to its abundance, low cost, and potential for sustainable production.
The thesis work presented here focuses on the utilization of raw wheat straw as a potential source
for the production of films and cups through phosphorylation. The process involved the
delignification of raw wheat straw, resulting in a high yield of 37.75%. The delignified wheat
straw was then phosphorylated, and the yield of phosphorylation was found to be 63%. The
resulting gel was used to create films and cups with desirable properties such as flame
retardancy, water absorbency, good tensile strength, and stability in high-temperature water.
The water absorbency test revealed that the films made from the gel could absorb a significant
amount of water, making them suitable for applications in which moisture absorption is required.
The flame retardancy studies indicated that the films had a reduced rate of burning, making them
safer for use in applications where fire hazards are a concern. The mechanical strength of the
films was also measured, and the results demonstrated good mechanical strength, indicating their
suitability for use in packaging applications that require strength and durability.
In addition to the properties of the films, the cups made from the gel were stable in high-
temperature water, making them suitable for use in applications such as hot beverages. The
migration studies also showed that the films were within the permissible limits, indicating that
approach for the development of eco-friendly and sustainable films and cups. This approach
packaging materials, and it could provide an alternative source of raw material for the packaging
industry. Further research in this area could lead to the commercialization of such materials and