4.chapter1 On 15.06.18

CHAPTER 1
INTRODUCTION, AIMS AND OBJECTIVES
In this chapter, a brief summary on the environmental pollution, various sources

of the water pollution, the properties of the natural organic components, namely, Humic
acids and treatment technologies of the Humic acids, different treatment methods of the
paper and tea factory wastes are presented. Most of the industries, like, paper and tea
industry use fresh water for a variety of purposes and produce wastewater. To avoid any
health hazards affected by discharging untreated effluents into the environment, the
effluents must be treated. The treatment of paper and tea industry waste effluent using
several separation processes is described and compared with advanced membrane
filtration technology. The detailed literature review on the treatment of paper industrial
effluent, tea factory solid and liquid waste is deliberated subsequently throughout this
chapter. The aims and objectives of this thesis work are also discussed in this chapter.
1. Introduction:
1.1. Environmental pollution:
Environmental pollution is the overview of impurities in a healthy and natural

environment which is the reason of uncertainty, syndrome, damage or discomfort to the
ecology for both the cases physical and living society (Margaritis and Kang, 2017,
Franklin and Fruin, 2017). Contamination of soil, air, ground and surface water with
various hazardous, toxic chemicals, and solid wastes due to the industrialization and
human activities are the major problem which is increasing rapidly (Khan et al., 2017;
Wang and Yang, 2016; Sarkar et al., 2017). Environmental Pollution became a prevalent
issue after the World War II, for the radioactive effect from atomic fighting and testing.
Not only that, a non-nuclear happening, The Great Smog of 1952 in London, killed a
massive number of people. However, The Great Smog of Delhi, 2017 is also a serious
environmental pollution event that affected the entire National Capital of India due to the
various sources of smoke such as production and manufacturing factories, vehicles, power
plants, garbage burning, road dust, etc. Serious action must be taken against
environmental pollution, as it has an adverse effect on the earth mainly, air and water.
Environmental pollution began to pull a major and serious public devotion, after passing
the Clean Air Act (Effective from 1963), the
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National Environmental Policy Act (Effective from 1970), the Clean Water Act (Effective
from 1972), and the Noise Control Act (Effective from 1972) (Raptis et al., 2017; Kirillin
et al., 2013; Titelboim et al., 2017).
1.1.2. Parameters of contamination:
For industrial stream estimation and study of wastewater treatment, the properties or
parameters of contaminants are enlisted here.
a) Color:
Natural organic components are the main responsible for the changing of color of natural
water. The industrial wastewater contains a huge amount of organic materials including
various dye reagents that are potentially harmful after leaching of this compounds into the
groundwater or surface water which can change the color of natural water. Not only that,
color of water is a vital index to measure dissolved humic substances in water body
(Hongve and Akesson, 1996; Turner and Renegar, 2017).
b) Odor:
The chlorination of water results in the formation of severe halogenated components

which are the reason for the change of quality of water. When the active chlorine
compounds react with organic matters present in the water the disinfected halogen
compounds formed. The musty odor is one of the major parameter to control the purity of
drinking water (Taha et al., 2017; Yuan et al., 2017). It is generated degradation of
organic components in soil by fungi, cyanobacteria, blue-green algae, actinomycete
bacteria. The determination of musty odor is a difficult task. The high selective and
sensitive technique is needed to analyze the musty-off aroma in water (Callejon et al.,
2016).
c) pH:
The pH level of soil and water is an important parameter to balance the environmental
ecosystem. Due to toxicity of chemicals and heavy metals the level of pH in the water and
soil is changing gradually which has an adverse effect in aquatic life. Acid rain due to the
nitrogen oxides, sulfur oxides present in the polluted air is the perfect examples of man-
made influence on the pH of water (Jie et al., 2017; Tran et al., 2017).
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Introduction, aims and
d) Suspended matters:
Suspended matters are some toxic pollutants which are larger than 2 µm in size and do
not dissolve in the water. The toxic suspended particles in water are dangerous for the
existence of marine life. It can cause severe problems in ground and surface water by
increasing the microbial activities (Wang and Yang, 2016).
e) Dissolved organic matters:
The remediation and control of dissolved organic materials from drink water and
industrial effluents are the high interest to protect the environment from pollution. Due to
the presence of dissolved materials the organoleptic properties, like, taste, color, odor of
drinking water is affected. The appearance of organic matters in fresh water is described
to rise the anthropogenic compounds in natural water. The solubility of the various
components may be increased in the presence of dissolved organic materials in the ground
water. Not only that, it causes fouling of membranes during treatment of wastewater. the
origin of dissolved organic matters in water is the microbial degradation of chemicals that
present in the soil and water due to the industrial activities (Levchuk et al., 2018; Jain et
al., 2011).
f) Dissolved oxygen:
One of the most important parameters in aqueous studies is measurement of dissolved

oxygen. For the good water quality adequate amount of dissolved oxygen is required. The
oxygen level in water is approximately 5 mg L -1. Due to the industrial activity the level of
dissolved oxygen changes currently which affects the aquatic culture (Mader et al., 2017).
g) Turbidity:
Turbidity is a significant and crucial characteristics of water. The increasing of turbidity

indicates the presence of excessive amount of inorganic and suspended materials,
dissolved organic materials, colored components, and microorganisms. The high turbidity
in drinking water can cause a health concern due to the growth of pathogens (Aboubaraka
et al., 2017).
h) Heavy metals:
Water pollution due to the high concentration of heavy metals is a universal anxiety and
required a worldwide care. Effluents coming from the mining, battery manufacturing
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factories, tanneries, and metallurgical industries are the responsible for the leaching of
different kind of heavy metals, like, cadmium, cerium, chromium, antimony, arsenic,
lead,
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mercury etc. (Fang et al., 2018). The determination of metallic concentration in water is a
major concern to protect the water pollution. Heavy metals containing wastewater should
be treated significant and properly. Untreated water can lead to severe injury to the
ecosystem resulting in a long-term effect on the environment (Tran et al., 2017).
i) Chloride content:
Petroleum, pulp and paper mills, pharmaceutical, and tannery industries generate high
saline effluents in a large quantity containing the huge concentration of chlorides. The
increase of chloride content in water would lead to major damage to groundwater, surface
water, soil etc. The presence of chlorides in drinking water is highly detrimental.
Regarding the sustainability of the freshwater, the determination and treatment of chloride
content in the industrial effluents have to become a vital concern to protect the
environment (Yan et al., 2016). In addition, various compounds such as humic substances
can react with chlorides present in natural water and form strong toxic and carcinogenic
complexes, like, aliphatic halogenated trihalomethanes. Thus, under such conditions, the
determination of color, taste, odor, pH, suspended and dissolved organic matters,
dissolved oxygen, turbidity heavy metals, and chlorides compounds is becoming a
dynamic task for the treatment of liquid effluents to get highly purified and efficient water
and protect the ecosystem from severe environmental pollution.
1.2. Water pollution - a threat to life:
Water contamination is a severe universal problem which needs ongoing estimation and
review of water resource policy at all stages (Sanchez et al., 2016). Water pollution has
been recommended as the leading international cause of deaths and diseases. Water is
stereotypically considered to as polluted when the anthropogenic contaminants impaired
into freshwater. Water pollution occurs from a number of different sources.
Direct disposal of waste materials from different industries, like, pulp and paper, textile
and dye industries into the natural waterways cause waste to build up within the
freshwater (Noorhosseini et al., 2017). Not only that the emission of hazardous fumes into
the fresh air causes acid rain. When the acid rain sprays, it pollutes the local natural water
lines including rivers, lakes, and streams. Not only that, the thermal pollution happens
when water is basically used to cool the hot instruments in the factories and is
released into
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waterbodies. As a result, the temperature of the freshwater is highly increased (Titelboim

et al., 2017).
This temperature change can cause aquatic life to die. If the pollution arises from one
source, like, oil spill, it is named as point-source pollution. If the contamination comes
from a number of sources, then it is named as nonpoint-source water pollution. Figs. 1.1.
(a)-(b) describe the requirement of freshwater for the ecosystems on a worldwide scale in
2003 and 2015, respectively which indicates that the inadequacy of water is rapidly
increasing due to the consumption of fresh water. India is also considered as a water-
stressed country due to the rapid growth of civilization (World Resources Institute).
(a) (b)
Fig. 1.1. (a) The global scenario of the water scarcity in the environment in the 2003, (b)
the insufficiency of water on the universal scale in 2015 according to the World
Resources Institute
1.2.1. The different industries involved in water pollution:
Many causes are involved to pollute water bodies. The direct sources, like, effluents
discharge from various industries are one of the important contributors to freshwater
pollution. Industrial activities produce a huge variety of waste products. Paper and pulp,
textile, petrochemical refineries, food processing, metal working, tea, and dye factories
are the major industries which generate a wide range of waste effluents.
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Textile industry:
The effluents generated from textile industries have a high demand for chemical oxygen
demand due to the large number of suspended solids, acidity, and other soluble materials.
The contaminant features of textile wastes vary extensively among numerous organic
ingredients, like, chromium ions, pigments, starches, and detergents in waste undergo
biological and chemical variation which consume dissolved oxygen from the freshwater
bodies and abolish aquatic life (Jain et. al., 2014).
Tanning industry:
The tanning industry is generally considered as pollutants produced industries which

generate a huge amount of toxic chemicals. During the different unit operations, like,
soaking, liming, de-liming, tanning, etc. a huge amount of wastewater is generated which
consist of dissolved fats, bones, sodium chloride, sulfate, sulfide, chromium salts, keratin
etc. Due to the difference in raw materials, various organic and inorganic ingredients the
chemical and biological oxygen demand are changed to very high after discharging the
tannery effluents into the fresh water (Tran et al., 2017).
Food processing industry:
Food processing industries produce waste effluent, like, liquor from yeast culture system,
spent grain water, wastewater from a cooling tower, oil sludge etc. Food industry
wastewater contains a few amounts of hazardous materials which can be categorized as
nontoxic. In the dairy industry, a huge amount of freshwater is regularly used during
cheese making process and produced wastewater which contains inorganic and organic
materials (Frappart et al., 2008).
Petrochemicals and oil refining industries:
Petrochemicals and oil refining industries contain a high level of pollutants, like, oil
products, hydrocarbons, phenolic compounds, heavy metals which are tough to degrade
(Sarkar et al., 2017).
Metal industry:
Metal industries generally discharge wastewater containing heavy metals, like, chromium,
lead, cadmium, and other metals such as zinc, nickel, copper, aluminum etc. With the
rapid development of industries, heavy metal pollution is increasing now a day due
to the
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discharge of heavy metal-laden wastewater from these industries to the environment

without any proper treatment (Yuan et al., 2017).
Radioactive industry:
Radioactive waste components are also the important source of water pollution. The
radioactive wastes are mainly generated due to the various activities of Uranium mining
processing, Nuclear fuel production, and radioisotope production for the medicine
preparation and research purposes (Trznadel, 2017). The major wastes arising in a
radioactive industry are the active solids, like, stainless steel containing cobalt and nickel,
ion exchange resins, used uranium, radioactive liquids which can result in severe water
pollution (Trznadel, 2017).
Mining operation:
Mining operation can cause different kind of metal leaching into acidic effluents. These
effluents can increase the metal load in rivers, lakes, and groundwater (Ni et al., 2016).
Therefore, freshwater contamination due to the leaching of heavy metals during mining
operation has become a major environmental problem.
Agricultural industry:
The effluents generated agricultural industry are containing mainly farm and animal
wastes, fertilizers, suspended materials, insecticides, and pesticides etc. The highly toxic
chemicals can enter the groundwater by leaching and cause diarrhea, jaundice, dysentery,
and typhoid- like waterborne infections (Chen et al., 2015).
Tea processing industry:
Waste management is an abundant challenge towards tea processing industries in the

world. The raw materials, energy, water are the major inputs in tea factories which
produces solid and liquid wastes containing phenolic components. There is a lack of
inclusive review towards tea waste management systems. Highly colored wastewater
containing polyphenols from tea factories is released in to freshwater stream during the
cleaning purposes of production equipment. As a result, it changes the oxygen-containing
capacity of freshwater bodies (Uzun et al., 2010; Goswami et al., 2014).
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Paper and pulp industries:
With rising the use of papers in our daily life, the level of water pollution due to the paper
industries is a novel highlight. The paper and pulp industries consume a large quantity of
fresh water and generate highly contaminated wastewater. This effluent is renowned as a
severe ecological threat due to the highly toxic chemicals discharged including high
organic load, high salinity, suspended materials, inorganic components, and various
metals content. On the other side, solids and gaseous pollutants are also discharged into
the environment from paper and pulp industries. The effluents generated from paper and
pulp industries contain a huge number of lignin derivative organic components, like,
Humic substances. However, wood chips, bits of bark, cellulose, sulphur, and chlorine
compounds and dissolved lignin a complex mixture of various chemicals are also the
important impurities. All the contaminated materials produce a sludge which destroys
certain types of marine life and environment as well (Wong et al., 2006). With rising
consciousness of environmental protection, the significant and proper management of
pulp and paper industry wastewater has become an important public issue which should
be increased strictly (Guan et al., 2017).
Not only that, the paper industry wastewater contains a large number of natural organic
materials. Natural organic components many times replicate the action of an important
element in the living body, interfering with the metabolic system to cause severe sickness.
Many organic components, particularly colored components are toxic, but some are vital
for fertilization, like, Humic acids (HAs).
1.2.2. Generation, properties, benefits, and application of natural organic components,

like, Humic acids found from different sources:
Natural organic components are the elemental carbonaceous substances found in mainly
soil, sediment, and industrial effluents (pulp and paper industries). These materials mainly
known as environmental black carbon such as Humic acids have a significant affinity for
other organic and inorganic components (Radwan et al., 1997). Depending on their
limited abundance, it is an important issue to quantify and characterize the Humic acids,
like, natural substances which can play a major role as a natural pollutant in the
environmental system (Roipel et al., 2016).
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The properties of Humic acids:

Humic substances are recognized as one of the major essential component in the
environment (Ghabbour and Davies, 2001). Humic acids, natural heterogeneous
molecules comprise an extraordinarily complex, polyfunctional polymers, formed during
early diagenesis of bio matters and occur in soils, sediments, industrial effluents (pulp and
paper factory), and natural water (Radwan et al., 1997). The hypothetical structure of
Humic acids has been represented in the Fig. 1.2. The dominating functional groups of
the naturally occurring humic acids are amino acids, ester, amide, benzene rings, aliphatic
moieties, and carboxyl, ether groups, hydroxyl, amine groups, etc. (Ghabbour and Davies,
2001). These substances contain a huge number of organic compounds, higher hydrogen
to oxygen (H/O) molar ratio, higher surface activity, more nitrogen content, more lipids,
higher nitrogen to carbon ratio, a huge number of molecular weight distribution starting
from 2 kDa up to over 500 kDa than commercial Humic acids (Shao et al., 2011). These
substances are the most chemically active materials in the soil with the cation exchange
abilities. They can interact with different kind of toxic organic substances, like,
pesticides, herbicides, insecticides.
Fig. 1.2. Model hypothetical structure of Humic acids (Stevenson, 1994)
The hypothetical theory of the generation of Humic acids:
The formation of humic substances occurs during lignin decomposition. The generation
of humic substances may vary from one environment to another. Various techniques have
been recommended to explain the formation of humic materials during the deterioration
of
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plant cells such as lignin in the soil and the pulp and paper industrial wastewater. The
dead plant’s residue and lignin components are transformed into dark-colored compounds
by microbiological mechanisms. During the lignin decomposition, the carbon compounds
are utilized by microorganisms and the residual portion accumulates as humic substances
which can be fragmented into smaller materials, like, Humic acids during further
microbial decomposition (Ghabbour and Davies, 2001). However, the lignin and cellulose
are decomposed to phenolic acids during microbial degradation and then enzymatically
oxidized to quinones (amino compounds) and produced Humic acids, like, compounds. In
addition to the other possibilities, the pulp and paper industry is the major pathway to
generate a significant amount of Humic acids in their waste effluents as the major waste
materials of wood processing mechanism in the paper industry is lignin-derived
compounds, cellulose, sugar etc. (Mendez et al., 2005).
1.2.3. Benefits of Humic acids:
Current scientific researchers explore that the productiveness of soil depends on the
content of Humic acids. Humic substances are recognized to yield three types of benefits
which have been pointed out in the next paragraph (Mendez et al., 2005).
Physical effects:
 Improve the soil structure and fertility

 Prevent the high water content and nutrient losses in productive soils
 Soil cracking and erosion prevention
 The rise of water holding volume of the soil
 Darken the color of the soil and thus help absorption of the sun energy
 Increase the aeration of soil
Chemical benefits:
 Normalize the pH value of soils

 Increase the uptake of nutrients and water by plants
 Reduce the leaching of toxic inorganic materials in the root zone of plants.
 Enhance the metal ions chelating capacities of soil.
 Improve the transformation of essential nutrient elements, like, nitrogen, phosphate,
iron, zinc, potassium into forms available to plants.
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Biological effects:
 Improve the stimulation capacity of plant enzymes and increase their production
 Act as an organic catalyst in many biochemical processes.
 Stimulate the growth of desirable micro-organisms in soil.
 Increase the amount of amino acids, chlorophyll content, sugars in plant cells and help
in the photosynthesis process.
 The significant increment of vitamins and minerals content of plants.
 Improve the thickness of fruits cell walls.
1.2.4. Applications of Humic acids in different areas:
Humic substances, like, Humic acids are the natural plant growth promoter. Not only that,
in the modern years the interest for natural Humic acids in medicine and cosmetics
preparation purposes has been improved due to the high chemical activities such
antioxidant properties. They have numerous biologic activities, like, antibacterial,
antifungal, immunomodulatory and photo protecting functions (Mendez et al., 2005). The
applications of Humic substances have been listed here.
Agricultural application:
 Natural organic fertilizer for plants
 Nitrate leaking reduction into the groundwater
 Stimulator for the plant growth and increase the yield of crops production
 Reduce the harmful effects of inorganic fertilizer.
Environmental prospects:
 Environmental contamination reduction
 Anti-collapse agent for petroleum drilling fluid
 Reduce the leaching of toxic materials such as heavy metals, organic matters from the
soil
Industrial purposes:
 Natural dye production purposes
 As a natural additive to prevent seepage from large lagoons areas
 Use in the oil and gas drilling industry as additive materials to prevent collapse.
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Medicine purposes:
 Veterinary medicine purposes
 Anti-viral and anti-inflammatory, anti-allergic, estrogenic, hyperemic medicine
preparation
 Blood coagulation purposes
 Effective in contradiction of pathogenic bacteria
Cosmetic preparation purposes:
 Production of shower gels, creams, ointments due to the antioxidant properties
 Active against skin diseases, like, atopic dermatitis, psoriasis, and mild focal
hyperhidrosis.
 Active against chronic hand dermatitis
1.2.5. Separation of Humic acids substances from various processes:
The wastewater generated from food, paper and pulp industries contain a huge amount of
humic substances due to the decomposition of lignin, like, materials over years.
According to authors, the major groups were found in humic substances are, like,
carboxyl, aliphatic, amine, ester, phenols, amino acids etc. (Ghabbour and Davies, 2001).
Few studies have been found to separate and purify these highly polydispersed materials
towards fertilization.
1.2.5.1. Acid and alkaline extraction of Humic acids:

The alkaline extraction of Humic acids from peat sample using sodium hydroxide
(NaOH) and sodium carbonate (Na2CO3) has already been explored to prepare an organic
mineral based natural fertilizer. The efficiency of alkaline extraction of Humic acids was
found to be inversely associated with the amount of alkaline solution added during
extraction. The undesirable contamination of the extracted Humic acids was happened
due to the presence of unwanted fibers and inorganic materials, like, clay and sands which
were found to interfere during alkaline extraction process (Saito and Seckler, 2014).
Repetitive base extraction of peat sample was also carried out to obtain fractionated
Humic acids component. The extraction process was performed for the eight times with
the same peat sample until Humic acids was exhaustedly recovered. To identify the
differences in molecular and chemical properties among different humic substances
obtained from
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different extraction cycles and to explore the possible factors causing in single cycle
alkaline extraction were the two major objectives of this process. Due to the differences
in solubility humic substances materials with a lower affinity for solid surfaces and
having higher solubility were extracted during the earlier cycle and therefore, the large
molecular weight and low polarity substances having less solubility were obtained after
repetitive alkaline extraction (Li et al., 2003).
Humic and fulvic acid, like, materials were recovered from maize plant as the plant or
vegetable residues are the important sources of carbon, nitrogen for the fertilizer
purposes. The compost of maize plant residues was demonstrated to fractionate alkali
soluble and unhydrolyzed-alkali soluble humic acid materials using benzene and ethanol
mixture (2:1 v/v) and thereafter hot and cold sulfuric acid (H 2SO4) to obtain solubilized
lipids, waxes, hemicellulose, and cellulose, respectively to get more compact formation of
lingo humic complex matrix which was further extracted according to alkaline process
using NaOH and tetrasodium pyrophosphate (Na4P2O7). The high chemical cost and low
recovery were the major drawbacks during hot H2SO4 extraction of plant residue for the
recovery of Humic acids, like, substances (Adani and Ricca, 2004).
1.2.5.2. Supercritical fluid CO2 extraction of Humic acid from brown algae:
The supercritical fluid extraction of humic substances has a significant advantage over
conventional extraction with acetone, ether, dioxane, and ethanol that it extracts humic
materials within very short time period instead of the days needed for consecutive
extraction. Brown algae namely, Pilayella littoralis (Phaeophyta) was already used to
recover humic, like, substances efficiently using supercritical fluid CO2 extraction
process. However, it was reported that the extracted and isolated Humic acids sample had
lower carbon and nitrogen content than the samples extracted from conventional organic
solvent extraction due to the less removal of non-humic substances present in the
extractive solution. Though this process demands the shorter time of extraction, the high
operating cost and the less efficiency of removal of impurities are the major drawbacks
factor for the supercritical fluid extraction to obtain the essential quantities of purified
Humic acids (Radwan et al., 1997).
1.2.5.3. Application of ultrasonic vibration on the extraction of Humic acids:

Ultrasonic extraction of Humic acids from a brown soil was fruitfully reported earlier to
obtain a significant amount of yields and to avoid the contamination and modification of
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the components which were the main demerits of alkaline extraction of humic materials.
However, it was stated that the elemental composition of humic substances was different
from the classical extraction of Humic acids using acid-alkali titration. The high ash
content and low content of carboxyl (-COOH) and phenolic groups (-OH) were reported
while extraction of Humic acids using ultrasonication. It was stated that the application of
sonolysis on extraction of Humic acids using pyrophosphate as extractor can only be
reduced the time requirement from other rigorous processes though it can cause
differences in the chemical and physical properties of the substances (Humic acids) which
is not favorable towards use of Humic acids as a fertilizer (Ramunni and Palmieri, 1985).
1.2.5.4. Coacervate extraction method:

The coacervate extraction process was also applied for Humic acids extraction from
aqueous solution maintaining the micellar solubilization phenomenon and cloud point
polyethoxylated alcohols. Compare to the conventional extraction process of humic
substances this technique has delivered high extraction efficiency, however, this process
needs a huge amount of organic solvents, like, polyethoxylated alcohols for the
continuous process of extraction of Humic acids (Ghouas et al., 2012).
1.2.5.5. Electromagnetic and electrocoagulation process:

The electromagnetic and electrocoagulation separation was explored to treat Humic acids
content synthetic solution. The pH played an important role to enhance the removal
efficiency of Humic acids from aqueous solution. It was reported that the batch electro
coagulation process revealed the significant removal efficiency of more than 96% at pH 7
and 90 % at pH 3. Whereas, the reactivity of higher molecular weight parts of Humic
acids before removal was raised effectively after introducing the electromagnetic effect
during the separation process. However, the electromagnetic process in a continuous
mode revealed a lower effect on the removal of Humic acids from the synthetic aqueous
solution (Ghernaout et al., 2009).
1.2.5.6. Biological process to separate humic substances:

Aside from chemical processes, biological technology from food residue and green
wastes remain a major desirable method for the separation of humic substances.
Composting of vegetable residue for the separation of Humic acids has been reported
with significant results. Food and green residue were sent to the composting chamber to
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complete the two
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phase of composting process, like, active and curing phases. The composted materials
were subjected to treat with NaOH and thereafter acidified with sulfuric acid to
fractionate the composted materials into humic substances. It was reported that the
oxygen to carbon ratio and total acidity of Humic acids in this process were found higher
than other sources, like, peat and soil. Though the long duration of this biological process
was the major demerit towards the isolation of Humic acids from food and green wastes
(Adani et al., 2001; Quagliotto et al., 2006).
1.2.5.7. Microwave assisted soxhlet method:

The different sewage sludges collected from different wastewater were used to extract
Humic acids substances with a solvent mixture of methanol and dichloromethane (1:7) in
a microwave assisted soxhlet system. The main difference between the soil and sludge
extracted humic compounds has been reported about the distribution of elemental
components, like, hydrogen, carbon, nitrogen, and oxygen. High degree of aliphaticity
due to the high hydrogen and carbon ratio content has also been reported. Besides the
high organic compounds, it was stated that the enrichment of lipids in the humic acids
sample was difficult to determine during the methanol and dichloromethane solvents
extraction process. The extraction and isolation of lipid components from the humic
substances matrix was challenging which can be further improvised (Reveille et al.,
2003).
1.2.5.8. Fenton oxidation process:

The chemical oxidation processes, like, Fenton reaction and its modified version such as
ozone and hydrogen peroxide combination have been the matter of a substantial attention
for the recovery of natural organic components, like, humic substances from
contaminated water and soil materials. The treatment process of humic substances content
wastewater was carried out with the Fenton reagent, prepared by different ratios of
ferrous sulphate (FeSO4, 10%) and hydrogen peroxide (H2O2, 35%). However, the use of
H2O2 reagent was the major cost of this treatment and it was becoming an important
concern to design the process in a way where a significant recovery could be performed
using a minimum amount of H2O2. The need of many reactive chemicals, high operating
charge are also the important disadvantages during the oxidation process. Apart from this,
the oxidation process can bound the reuse of Humic materials as fertilizer in the
agricultural purposes due to the reduction of hydrogen/ carbon (H/C) ratio and nitrogen
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content (Kochany and Kochany, 2008).
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1.2.5.9. Nitric acid oxidation process:

The conventional biological and acid-alkaline processes are usually insufficient to recover
purified Humic acids substances for the agricultural purposes. It is well known that peat
coal samples have an effective amount of humic substances which can be further
chemically oxidized to achieve a huge yield of Humic acids. In view of that, the wet
oxidation process using a different concentration of the nitric acid solution (1 g coal
sample with 5 mL of 5%, 10%, and 15% nitric acid) has been developed to chemically
extract humic substances from coal samples. It was reported that the reuse of nitric acid
was also carried out during this oxidation process. The maximum purity was achieved
using a low concentration of the nitric acid solution (5%) whereas, the recovery efficiency
was not effective for the use of agricultural purposes. Nevertheless, the expensive
chemical cost and the generation of toxic gas (NO x) are not in favor of the use of wet
oxidation process industrially (Cho and Lwin, 2012).
1.2.5.10. Ferric chloride coagulation process:

Though the ferric chloride coagulation process was investigated earlier in the field of
effluent treatment and water supply, the recovery of humic materials from the dewatering
wastewater of thermally treated sludges towards organic fertilizer was introduced using
ferric coagulation technique. Approximately, 70% of humic substances were recovered
using hydrolyzed ferric ions at the pH level of 4.5 (Yang and Li, 2016).
1.2.5.11. Membrane electrolysis and electrocoagulation process:

When the biological process takes a long time interval for the recovery of humic
substances membrane electrolysis promises significant results to treat industrial
wastewater for the recovery of humic, like, substances. In the membrane electrolysis
process polyethersulfone microfiltration membrane, anion exchange, and cation exchange
membrane were chosen to perform the filtration process. Titanium oxide coated electrode
and a stainless steel electrode were applied as anode and cathode, respectively to perform
the membrane electrolysis process. Though the less generation of sludge materials, no
needed for extra chemical reagents and the easy operating system were the major
effective benefits for the use of membrane electrolysis, the recovery of humic, like,
colored components and the reduction of chemical oxygen demand were very less
efficient (up to 70%) after using high energy consumption of 3 kW h m-3 (Kliaugaite et
al., 2013).
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1.2.5.12. Application of membrane ultrafiltration for the treatment of humic

substances: In recent decades, the membrane ultrafiltration has become an innovative
separation technology to purify the effluents rather than conventional treatment process,
like, carbon adsorption, oxidation etc. Chemical and mechanical treatment processes was
used to treat natural organic matters which have already been discussed (Manttari et al.,
2008). Recent studies have shown that Humic substances are recognized as major foulant
during water treatment (Lowe and Hossain, 2008). Not a very significant removal rate of
Humic acids has been reported (Galambos et al., 2004; Shao et al., 2011; Lowe and
Hossain, 2008). The membrane separation techniques can deliver a huge number of
merits as compared to the conventional methods. This various filtration process is
becoming an important tool for the separation of a wide number of compounds ranging
from natural organic components separation to sludge purification. Membrane separation
techniques are potentially perfect techniques for the minimization of environmental
contamination since the membrane filtration requires the use of comparatively simple and
non-harmful materials. However, Humic acids substances can also be recovered using
membrane process.
The separation of humic substances in the presence of mineral salts ions (Ca +2) was
investigated using ultrafiltration membrane made of regenerated cellulose. Considering
the high amount of membrane permeability, the reduction of membrane fouling was tried
to adjust the pH conditions of the aqueous solution from 4.6 to 7.0. The filtration pressure
and the concentration of humic substances were maintained at 100 kPa and 20 mg L-3.
However, 90% retention of humic substances molecules was achieved when pH of the
solution was
7.0. Whereas, it was reported that with increasing mineral salts concentration from 50 to
100 mg L-1 the rejection of natural organic substances was decreased. The presence of
Ca+2 salts ions was not significant to improve the membrane fouling behavior of the
regenerated cellulose membrane. Due to the high ionic strength of the increased Ca +2
concentration humic substances particles displayed an affinity to shrinking which could
be increased the deposition of rejected materials on the active membrane surfaces. Thus,
the separation process and the transport properties of the membrane cellulose membrane
were deteriorated in the presence of Ca+2 ions (Korbutowicz et al., 1999).
The demand for the production and purification of the clean potable drinking water from
any natural or industrial sources is ignited to improve the research extensively towards
novel alternative processes. In this addition, the use of membrane ultrafiltration has
2
sparked significantly for the production of potable drinking water and the treatment of
industrial effluents as well. Regenerated cellulose membrane with the different molecular
weight cut
2
Chapter 1
off (3, 5, 10 kDa) and high surface area of 0.1 m 2 was applied to purify the tap water
containing Humic acids components. Although the removal efficiency of Humic
substances from the synthetic feed solution made of deionized water was approximately
90%, this process was affected due to the significant membrane surface fouling for the 3
and 5 kDa MWCO membranes. Whereas, with the help of high retentate flow rate and
transmembrane pressure drop of 210 kPa, 10 kDa MWCO membrane provided a
significantly high permeation of 140-180 L m-2 h-1 initially, within 10 min of operation it
reduced up to 100 L m-2 h-1 due to the severe irreversible pore clogging. On the other side,
the continuous decline of permeate flux from 100 to 60 L m-2 h-1 was observed within 20
min of ultrafiltration during the treatment of Humic acids from tap water due to the
presence of ions and other impurities (Lowe and Hossain, 2008).
The flat sheet membranes made of polyethersulfone and polyaryletherketone were used in
a cross-flow ultrafiltration module with the active surface area of 0.036 m 2 to treat Humic
acids model solution (concentration of 10 mg L-1) and high Humic acids content well
water. The result revealed that the 83% of recovery of Humic acids molecules was
achieved during ultrafiltration. Whereas, the performances of the above-said membranes
were not significant during the treatment of Humic acids content well water due to the
less rejection of the smaller molecular weight components present in the water. This
phenomenon was responsible for the less effective ultrafiltration of humic substances
containing well water (Galambos et al., 2004).
On the other side, one hollow-fiber module with nanofiltration membrane made of
polyamide (MWCO of 0.3 to 0.4 kDa) was also performed and compared with cross-flow
filtration with the same feed. It was reported that though the significant rejection was
achieved during hollow-fiber nanofiltration, the severe decline of permeate flux was
observed due to the irreversible membrane fouling and the operating cost was very high
during nanofiltration as the applied pressure drop was around 20 bar (Galambos et al.,
2004).
Humic substances, from the landfill leachate, was successfully recovered and utilized as a
natural fertilizer using continuous spiral wound membrane ultrafiltration (MWCO of
2500 Da) until the significant concentration of humic substances was achieved in the
retentate solution. it was reported that the efficiency of this process in terms of the purity
of humic substances compounds was about only 50% after applying transmembrane
pressure drop of 0.7 MPa. The fractional recovery of humic components was affected due
to the presence of salts ions, like, Na+, K+, Mg+, and Ca+ (Yue et al., 2011).
2
Several studies have revealed that membrane ultrafiltration process had a significant
rejection capacity of natural organic matters, however, fouling characteristic is the severe
factor that limits its widespread industrial applications. The low-pressure ultrafiltration
using polyvinyl chloride hollow-fiber membrane (MWCO of 50 kDa) was performed in a
full scale potable and drinking water treatment purposes. The process was performed in a
dead-end method. Before the membrane ultrafiltration, poly-ferric sulfate (PFS) was used
as a coagulant (dosage was 10-15 mg L-1) to remove the suspended materials from the
source water. However, the severe flux decline was found due to the membrane fouling as
humic substances, like, natural organic materials are already recognized as the major
foulant for membrane ultrafiltration especially ultra-low pressure filtration of potable
water. Enormous irreversible fouling may be occurred using hollow-fiber membrane
ultrafiltration due to the adsorption of humic substances during filtration. However, this
study focused on the investigation of organic foulant behavior on ultrafiltration using a
hollow-fiber membrane, the remediation of fouling layer using various advanced
processes were not addressed here (Xiao et al., 2012).
There are insufficient literatures have been found about the purification and recovery of
valuable materials, like, Humic acids from the waste effluents using membrane
ultrafiltration (Li et al., 2009). A hybrid method, like, alkaline treatment afterward
membrane ultrafiltration was investigated to extract Humic acids components from waste
activated sludge. After the centrifugation of the disintegrated sludge with NaOH, the
supernatant was subjected to send in an ultrafiltration membrane unit to extract and
concentrate Humic acids components. Based on the Humic acids molecular weight
distribution, a porous ceramic tubular membrane device (mesh size of 0.45 µm) was used
to perform the extraction of humic substances at a maximum pressure drop of 1.0 MPa. It
was informed that the concentration of Humic acids in the retentate was reached at 30 g L-
1
when the supernatant solution was concentrated about to 20 times during ultrafiltration.
The adsorption of protein and the other metal ions, like, Na +, and K+ on the membrane
active surface was the severe factor which made an impact over the permeation (Li et al.,
2009).
2
Chapter 1
1.3. Treatment of paper industrial wastewater and an approach to recycle the

produced water:
The precious resource in the environment is water. Recycling of water from the factories
and the industrial effluents can deliver considerable benefits towards living ecosystem.
Thus, treatment of industrial wastewater is very significant activity now a day, rather than
discharging untreated water to the surface water, rivers or oceans (Bhuiyan et al., 2016).
The purpose of the treatment of effluents is nothing but water conservation and
sustainability in our environment. Reuse of water is socially and environmentally feasible
and economically viable (Ruiz-Rosa. et al., 2016) The reason for the water recycling is
the reuse of treated wastewater for the favorable and valuable purposes, like, agricultural,
industrial, landscape irrigation, cooling water for power plants, construction purposes,
dust controlling, artificial lakes, processing water for various industries etc. Due to the
reckless civilization and industrialization, the scantiness of water is increased
continuously which will become scarce in our country and India can be considered as
water stress country in the coming periods (Tiwari et al., 2016).
Paper industry is one of the important economically advanced industry among all
industries present in the environment. The paper factory is categorized as a high water-
intensive industry for the large consumption of freshwater during the different stages of
papermaking purposes. According to the report, the pulp and paper industry consumes
approximately 60 m3 of water per ton of production of paper (Wong et al., 2006; Savant et
al., 2006). It is observed that pulp and paper industry discharges huge volume of highly
toxic and colored effluents regularly in the environment. It is found in literatures that
various pulp processing stages, like, wood casting, pulping and washing, bleaching,
screening, chemical pulping, papermaking and chemical recovery generate highly
polluted effluents containing soluble and non-soluble wood derivative products
(Chanworrawoot and Hunsom, 2012). This effluent contains high organic substances
causing high chemical oxygen demand (COD) as well as biological oxygen demand
(BOD) (Ghaly et al., 2011; Soloman et al., 2009). Apart from organic matters, suspended
solids, metals, fatty and resins acids, tannins lignin derivative compounds are responsible
for water pollution. Heavy metal ions, like, Pb, Cr, Hg, As can be present in this type of
effluent (Latorre et al., 2003; Ali and Sreekrishnan, 2001; Thompson et al., 2001). The
organic substances found in pulp and paper industry wastewater are mostly raw materials
dependent and vary with location, environmental situation, and process parametric
conditions. The discharge of inadequately treated
2
effluents into the river water can cause a severe problem for aquatic life, including air and
land pollution. Thus, the primary, secondary or tertiary treatment of paper and pulp
industrial waste effluent is needed regularly to minimize the environmental pollution
(Andrews et al., 2014; Pokhrel and Viraraghavan, 2004). Several studies were performed
to treat pulp and paper industrial waste effluents including conventional processes such as
aerated lagoons, activated sludge treatment, sedimentation or flotation, etc.
1.3.1. Anaerobic digestion process:
Anaerobic digestion plant is the most collective wastewater treatment process which is
used for the removal of dissolved organic materials in several countries (Meyer and
Edwards, 2014; Kumar et al., 2014). This process has reported maximum amount of
dechlorination of paper industrial wastewater (Savant et al., 2006). The coagulation
followed by anaerobic acidification and aeration package reactor was designed to treat
pulp and paper industrial effluents for the effective removal of adsorbable organic halides,
chemical and biological oxygen demand. The significant amount of toxic materials was
reduced through the coagulation process due to the acidification reaction in the anaerobic
digester. However, up to 88.1% and 81% removal of COD and BOD, respectively
indicated that the highly toxic organic halides were difficult to treat during the anaerobic
biological process (Chen et al., 2003).
1.3.2. Application of flocculation process using polymeric flocculants:
In the recent period, the application of synthetic polyelectrolytes, like, polyacrylamide

during flocculation has ignited the effective removal of suspended materials from the
paper industrial waste effluents. The jar test experiments with different dosages of
polyacrylamide (0.5 to 15 mg L -1) were achieved 93% and 98% removal of chemical
oxygen demand (COD) and total suspended solids (TDS), respectively, from the paper
and pulp mill wastewater. Though the several merits of the polymeric flocculation are the
no residual metal ions, and good settling characteristics with dense and strong flocks, the
extensive industrial application of polymeric flocculation is still challenging due to the
complex behavior of this process (Wong et al., 2006).
2
Chapter 1
1.3.3. Consortium bacterial treatment of paper industry effluent:
The conventional processes have been carried out worldwide, it produces an adequate
amount of untreated sludge which itself requires further treatment. Being low shock
loading, low capacity to remove biodegradable toxic substances and the high cost of the
common treatment processes, the biological approach was obtained as an environmentally
friendly technology for the treatment of waste effluents. Researchers studied sequential
batch reactor using Klebsiella sp., Alcaligens sp. and Cronobacter sp. bacterial
consortium for the potential degradation of lingo-cellulosic compounds from the effluents
of paper and pulp industry. It was reported that the consortium bacteria were capable to
remove the lingo-cellulosic components after 16 to 18 h of incubation and up to 91%
removal of BOD was achieved. Whereas, this process was less effective to remove
colored components and chemical oxygen demand. 55% and 72.3% removal capacity of
coloring compounds and COD were reported, respectively during bacterial treatment of
paper industry effluents. Therefore, more advanced eco-friendly alternative techniques
should be required to treat the pulp and paper mill wastewater appropriately and set the
strict discharge limits for this type of industry (Kumar et al., 2014).
1.3.4. Electrocoagulation process:
Currently, the most studies on purification of waste effluents have been made with the
electrochemical process. Previous reports demonstrated that the electrochemical method
is more capable to remove chemical and biological oxygen demand from any industrial
effluents. The pulp and paper industrial effluents cause a severe pollution to the fresh
water after discharging untreated wastewater with a high level of COD, BOD, suspended
solids, adsorbable chlorinated compounds, resins, lignin derivative humic substances,
sulphur compounds, fatty acids compounds etc. Recently, electrochemical process,
including electrocoagulation for the removal of organic components in the pulp and paper
industry wastewater has been performed extensively. Two different electrodes made by
aluminum (Al) and iron (Fe) were studied to degrade lignin and phenolic component and
to reduce COD and BOD from the paper mill wastewater at the various current density
and different electrolysis time. The removal efficiency of lignin and phenolic component
was increased with increasing current density by creating metallic hydroxide flocks
within the wastewater. There was a high probability of coagulation of smallest charged
particles due
2
to the formation of the electric field by which small colloidal materials were removed.
However, the removal capacities of this method using two different electrodes, like, Fe
and Al in terms of COD (55% and 75%, respectively) and BOD (80% and 70%,
respectively) removal were not significant due to the formation of the complex chemical
structure of lignin during electrochemical treatment. The operating cost consumption is
high for the hybrid continuous electrochemical process (Ugurlu et al., 2008).
1.3.5. Photocatalytic treatment of paper mill wastewater:
In the current years, the advanced oxidation process is developed for the effective
treatment of industrial wastewater. Heterogeneous photocatalytic degradation of organic
and toxic pollutants is a challenging technology from industrial wastewater. The
photodegradation activates and surface properties of titanium dioxide (TiO 2) loaded
activated carbon fibers (ACF) were investigated during the treatment of paper mill
wastewater. It was observed that the maximum COD removal of 72% was occurred
within 40 min of photocatalytic reaction and reached its equilibrium condition gradually.
The untreated lignin-derived materials were the main responsible for the low removal of
COD from the wastewater (Yuan et al., 2007).
The activity of nano titanium dioxide particle as a superior photo catalyst was evaluated
to treat the paper industrial waste effluents under solar irradiation. The result showed that
the removal efficiency of COD increased from 46.3 to 70.5% with increasing photo
catalyst dosage from 0.25 to 0.75 g L-1, and pH 6.5 to 10. The maximum percentage
removal of COD at high TiO2 loading was happened due to the significant photocatalytic
degradation of organic pollutant present in wastewater. This process reduced the total
suspended solid materials up to 80.4% from the effluent which was not effective. The
recovery of TiO2 materials is an essential issue during industrial application of this
photocatalytic degradation process (Ghaly et al., 2011).
1.3.6. Membrane technology for the treatment of wastewater:
More experiments are going on to focus on environmental pleasant processes for the
treatment of wastewater. To minimize the cost-effectiveness, membrane filtration
suggests an attractive alternative process for the purification of waste effluents
2
Chapter 1
(Manttari et al.,
2
2006). For an illustration, ultrafiltration has been used effectively for the recovery of
natural organic materials and also for the reuse of process waters from various industries
(Galambos et al., 2004).
Ultrafiltration, nanofiltration, hybrid membrane filtration, and advanced membrane

module are now applying apparently to purify and reuse the effluents from the pulp and
paper industries. Few studies have been performed with advanced type membrane devices
for wastewater treatment purposes. Membrane filtration delivers an effective alternative
to purify paper industry effluent for reuse. The treatment of wastewater using membrane
separation has a reputable influence on environmental science due to the huge advantages
of membrane technology. The low operating cost of membrane filtration gives numerous
opportunities to apply this technology to a wide range. However, an enormous decline of
permeate flux is the critical restriction to remove organic substances using membrane
ultrafiltration. Recent studies have shown that organic substances are recognized as major
foulant during water treatment (Lowe and Hossain, 2008). The advanced separation of
natural pollutants from wastewater are facing a vital problem due to the building up of gel
or cake layer formation of rejected particles on the membrane surfaces during filtration
(Mousa, 2007). To restrict the formation of concentration polarization at the time of
cross- flow filtration, researchers had stated the enrichment of very high feed velocity. It
has been delivered that the increase in feed flow-rate leads to boost the turbulence at
membrane area, which tends to minimize the concentration polarization layer thickness
(Deon et al., 2010; Deon et al., 2013). Researchers have pointed out about the shear-
induced or dynamically enhanced membrane filtration processes to enhance permeate
flux. As because, vibratory shear enhanced (VSEP) and rotating disk membrane (RDM)
modules can be the alternatives to decrease the cake layer formation on the membrane
active areas during separation (Jaffrin, 2012). Development of advanced membrane
module to decrease the concentration polarization is a big encounter now a day. For the
reduction of fouling, comprehensive studies have already been started over last two
decades (Sarkar et al., 2012).
Few results are reported about the treatment of waste effluents from effluents using shear-
induced separation. High shear rate and transmembrane pressure drop were performed to
achieve high rejection of solutes to treat dairy wastewater using nanofiltration rotating
disk membrane. According to the total power input, a high specific energy ingestion was
found under extreme hydraulic conditions during the nanofiltration of dairy industry
2
Chapter 1
effluent using rotating disk module (Luo et al., 2010). Except rotating disk module,
nearly 18.15
3
kW power consumption was stated during shear-induced reverse osmosis treatment of

dairy process water (Frappart et al., 2008). Though the vibratory shear enhanced module
is capable to produce a high amount of permeation, the increase of high energy ingesting
due to module vibration is the important limitations for this module. To reduce
concentration polarization and cleaning cost, shear enhanced spinning basket membrane
module has already been designed and developed to recover polyethylene glycol (PEG)
with fixed retentate flow of 10-4 m3 s-1. Inbuilt back rotation system of this novel module
can save the operating cost. They have stated that higher permeate flux was found at a
power consumption of 0.94 kW which was very marginal compared to the all existing
membrane modules they have enlisted (Sarkar et al., 2012).
1.4. Application of advanced separation technology towards tea factory generated

wastewater:
Tea production is an important component in the global food and beverage industry. In
terms of global production, India is the second largest producer of tea processing in the
world following China (Pasrija and Anandharamakrishnan, 2015). The geographic
conditions favor the growth of tea in the north-eastern part of India. However, processing
of fresh tea leaves from the garden to readymade market requires various industrial
processes (Gadhkari et al., 2015). Wastes generated by tea industries are of both solid and
liquid in nature. The liquid waste is produced in a tea factory during cleaning of
equipment and factory sites. The amount of effluent generated during cleaning of
equipment needs an immediate attention and proper waste management procedure. The
tea factory effluent contains high levels of organic matter, high chemical oxygen demand
(COD) and suspended materials as well as dissolved solids. The reddish color of the
effluent indicates the presence of polyphenolic and other organic components, which need
to be treated to reuse the water prior its discharge in the environment (Uzun et al., 2010;
Goswami et al., 2014). Due to industrial reluctance to maintain the profit margins,
sometimes such effluents are directly disposed into the river. In the recent decades, many
of the research attempts were directed towards the effective abatement and minimization
of water pollution (Bhuiyan et al., 2016). A number of methodologies have been
incorporated to treat industrial wastewater, including chemical, biological processes
(Andrews et al., 2014; Ali and Sreekrishnan, 2001; Meyer and Edwards, 2014). A few
results are reported to remove
3
Chapter 1
the organic and inorganic compounds from tea industry wastewater. To prevent quick
fouling in membrane-based processes, a pre-treatment stage is often necessary to be
integrated during the treatment of wastewater.
Previous studies have reported about the feasibility of cement kiln dust containing
calcium oxide (CaO) and silicon dioxide (SiO2) as a low-cost coagulant in the treatment
of wastewater from tea industry. However, at the optimum dose of 2.5 g L-1 coagulant, it
failed to reduce COD concentration in the treated effluent (only by 9.09%) because of the
low removal efficiency of proteins, theaflavins, and thearubigins. It was suggested that
the treatment of tea factory wastewater can be performed using membrane filtration
specifically reverse osmosis for the potable water (Yadav and Kalaiyarasi, 2015).
For the treatment of instant tea powder factory effluent, a combination of the coagulation-
membrane system was adopted. To reduce the reversible or irreversible fouling on the
active membrane surfaces the coagulation-flocculation was performed as a new
pretreatment technique. However, employing polyaluminum ferric chloride (PAFC) as
the coagulating agent, at optimum conditions of pH at 5, the temperature at 20°C and
coagulant dose of 800 mg L-1, coagulation as pre-treatment removed only 44.1, 32.6, 72.5,
and 57% of turbidity, COD, TSS and TOC, respectively. It was suggested that when
polyaluminum ferric chloride and the organic components react with each other, a part of
the complex materials undergoes a charge reversal mechanism that causes the adverse
repulsion between PAFC and organic components resulting weaker removal efficiency
during treatment of tea factory wastewater (Chen et al., 2015).
The approach of combined advanced oxidation process with other technique, like,
adsorption has expanded substantial attention in the treatment of wastewater. The
application of a combined adsorption and advanced oxidation to purify tea factory
effluent is possibly more operative than the conventional processes such as activated
sludge methods, single adsorption process. Natural zeolite with a range of 50 to 200 mg
L-1 was used as an adsorbent. The dose of oxidant reagent such as hydrogen peroxide
(H2O2) was
0.1 to 0.4 mL. This process was successful in reducing color intensity by 88% when the
adsorbent dose was 200 mg L-1. In case of H 2O2, only 68% color removal was observed
with 0.4 mL oxidant dose due to the generation of intermediate products during oxidation
(Otieno et al., 2014). This is where the membrane filtration steps in being a promising
technology which is eco-friendly, modular designed and flexible process with reduced
consumption of energy and materials (Manttari et al., 2006).
3
Being the most popular pre-treatment method for membrane separation processes, alum
coagulation has proved to be a simple and efficient method for reducing membrane
fouling and hence aids in improving flux. The efficiency of coagulation process is found
to be dependent on factors, like, type of coagulant and its dosage, pH, mixing speed,
mixing time (Konieczny et al., 2009). This research is directed towards integration of
coagulation process followed by membrane-based processes, where it is absolutely
necessary to optimize the parameters of coagulation to improve process efficiency. This
study is focused on the development of a new green process that permits continuous
treatment of tea industry wastewater by generating clean and reusable effluent in a small,
compact, energy- saving, and environment-friendly system. Researchers are really scanty
using such coagulation-spinning basket membrane ultrafiltration integrated technology
exploiting alum for coagulation (pre-treatment) and a spinning basket module for
membrane filtration (final treatment).
1.5. Utilization of tea factory solid wastes towards environmental management:
Waste management is a global concern that mainly brings emerging countries into the
limelight. It requires suitable strategies, essential resources and healthy infrastructures for
an organized and sustainable waste management system (Uzun et al., 2010). Though it is
reported that tea industry does not pose any huge threat to the environment, a significant
portion of solid waste is being treated and reused in some scientific ways (Malkoc and
Nuhoglu, 2007). Tea solid waste is mainly the part of unwanted woody shoots. During
harvesting, these unwanted parts are mixed with tea leaves. The lignin-based woody
slices are not treated by the tea industry during the production and made into tea industry
solid waste (Malkoc and Nuhoglu, 2006). Furthermore, solid wastes are again generated
from the packaging, sorting area and the weighing section in the factories. The highest
amount of solid waste is also generated from the withering stage due to spillage
(Amarasinghe andWilliams, 2007). The solid tea waste is about 2.5% of the total
production. Generally, these wastes are mainly returned to the field to deposit into the
store area (Malkoc and Nuhoglu, 2005). In the matter of solid waste management, the
products which can be produced from tea solid waste using extraction methods are mainly
polyphenols, caffeine, pigments, foaming reagents (Yuan et al., 2008) or tea seed bio-oil
(Uzun et al., 2010; Lin et al., 2015). Among those products, polyphenols mainly represent
the most plentiful constituents in tea leaves as well as tea processing solid wastes
3
Chapter 1
(Todisco et al., 2002). Tea
3
polyphenols have antioxidant activities. The phenolic compound has a deep impact on
pharmaceutical purposes, like, anti-carcinogenic, anti-ulcer, anti-mutagenic activities etc.
(Nawaz et al., 2006; Halake and Lee, 2017). The natural phenolic compounds have also
good effects in the field of corrosion inhibition (Prabakaran et al., 2016). These
compounds can be used as a natural dye reagent also. It can be used to replace some of
the phenol in phenol-formaldehyde resins to manufacture polymers as well. A numerous
number of experiments have been performed towards the removal of heavy metals, like,
Cu, Cd, Pb, Cr, Ni from various wastewater using low-cost tea solid waste as it contains a
huge amount of cellulose, lignin, hemicellulose components with a large number of
surface area (Malkoc and Nuhoglu, 2006; Amarasinghe and Williams, 2007; Malkoc and
Nuhoglu, 2005; Yuan et al., 2008; Cay et al., 2004; Weng et al., 2014). According to
literature, the efficiency of the adsorption of metals significantly depended on phenolic
compounds which are present in the tea solid wastes (Malkoc and Nuhoglu, 2007; Malkoc
and Nuhoglu, 2006). The usage of tea factory solid waste to extract the total polyphenols
towards solid waste management is a novel and innovative approach. The present work
uses the existing science to explore the different solvent leaching and diffusion of total
polyphenols from the tea industry solid waste materials. The eco-friendly management of
solid waste materials after fruitful leaching of polyphenols, like, value-added products has
been performed successfully in the current study. No such result has been reported on the
recovery of valuable phenolic compounds from tea industry solid waste previously. Most
of the cases solid waste was used for metal removal purposes. In the literature, it is
mentioned that before going to adsorption, de-colorization of solid waste is the important
process of metals removal (Cay et al., 2004; Weng et al., 2014). No such results have
been found about the recovery of polyphenols from the tea factory generated solid waste
during the de-colorization process.
1.6. Knowledge gap and objectives of the project work:
The specific utilization of the spinning basket module membrane (SBMM) for the Humic
acids ultrafiltration, treatment of paper and tea industry effluents is novel, compact,
energy- saving, and environment-friendly. For the identification of the pattern of fluid
flow in the membrane basket at various flow rates and basket rotational speeds to purify
the synthetic wastewater at a fixed molecular weight cutoff (MWCO) membrane (50
kDa), spinning basket membrane module was used previously (Sarkar et al., 2012).
3
Chapter 1
Concerning the
3
cleaning process, the membrane turbulence was not enough to eliminate small particles
from the active membrane pore walls (Sarkar et al., 2012). Thus, the only back rotation
was not efficient to recover hydraulic flux after cleaning. Therefore, the application of
ultrasonication for the fouled membrane cleaning purposes has been presented in this
study as a way to handle the cleaning process. The mechanism of preliminary permeate
flux decline due to the membrane irreversible pore blocking has found no evidence in the
literature previously. The process parameters, such as transmembrane pressure drop
(TMP), rotational speeds, and retentate flow rate are optimized using response surface
methodology (RSM) during the treatment of industrial effluents to achieve the maximum
level of removal of organic or inorganic compounds. An overview of rotational diffusion
model is reported in the present study to evaluate the module performance. In addition,
the current study proves that the shear-enhanced spinning basket membrane ultrafiltration
can be used with low power consumption than other processes for continuous operation
process during the industrial effluents treatment with be fruitful results. However, the use
of tea factory solid waste for the recovery of the total polyphenols using solid-liquid
extraction or leaching towards solid waste management is also an innovative approach.
Research endeavors are really scanty using such leaching- membrane ultrafiltration
integrated technology to explore the effects of various solvents during the leaching of
total polyphenols and a spinning basket module to concentrate the phenolic compounds
towards the eco-friendly management of solid waste materials. The present work uses the
existing science to explore the different solvent leaching and diffusion of total
polyphenols from the tea industry solid waste materials. No such result has been reported
on the recovery of valuable phenolic compounds from tea industry solid waste previously.
Most of the cases solid waste was used for metal removal purposes. In the literature, it is
mentioned that before going to adsorption, de-colorization of solid waste is the important
process of metals removal (Cay et al., 2004; Weng et al., 2014). Nobody has reported
about the recovery of polyphenols from the tea factory generated solid waste during the
de-colorization process. Thus, a significant recovery of polyphenols using batch leaching
followed by spinning basket membrane ultrafiltration has been demonstrated in the
present study.
3
Chapter 1
The specific objectives are designed to carry out this project work.
Performance characterization study of spinning basket membrane module during

Humic acids ultrafiltration
 To study permeate quality with variation of TMP drops and rotational speeds.
 To analyze the fouling characteristics using modified Hermia’s pore blocking
mechanism.
 To identify the effects of ultrasonication on irreversible fouling.
 To study energetic consideration
Treatment of paper industry and tea factory generated effluents using shear induced
membrane ultrafiltration
 To evaluate the performance of spinning basket membrane for the treatment of paper
industry wastewater.
 To study permeate quality with variation of TMP drops, rotational speeds and MWCO
of membranes.
 To analyze the fouling characteristics using modified Hermia’s pore blocking
mechanism
 To optimize the process parameters using Response Surface Methodology (RSM).
Recovery of polyphenols from tea factory solid waste materials using a hybrid
process of leaching-membrane filtration
 To extract the total polyphenols from tea factory solid waste by varying different
parameters, like, various solvents (ethanol, methanol, acetone, ethyl acetate), Solid
content, temperature, time
 To optimize the parametric conditions using RSM
 To study kinetics of leaching using different kinetics models
 To study spinning basket membrane filtration for polyphenols concentration
3
References:
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CHAPTER 1

INTRODUCTION, AIMS AND OBJECTIVES

In this chapter, a brief summary on the environmental pollution, various sources

1.1. Environmental pollution:

Environmental pollution is the overview of impurities in a healthy and natural

1.1.2. Parameters of contamination:

The chlorination of water results in the formation of severe halogenated components

e) Dissolved organic matters:

One of the most important parameters in aqueous studies is measurement of dissolved

Turbidity is a significant and crucial characteristics of water. The increasing of turbidity

1.2. Water pollution - a threat to life:

waterbodies. As a result, the temperature of the freshwater is highly increased (Titelboim

1.2.1. The different industries involved in water pollution:

The tanning industry is generally considered as pollutants produced industries which

Food processing industry:

Petrochemicals and oil refining industries:

discharge of heavy metal-laden wastewater from these industries to the environment

Tea processing industry:

Waste management is an abundant challenge towards tea processing industries in the

Paper and pulp industries:

1.2.2. Generation, properties, benefits, and application of natural organic components,

The properties of Humic acids:

Fig. 1.2. Model hypothetical structure of Humic acids (Stevenson, 1994)

The hypothetical theory of the generation of Humic acids:

1.2.3. Benefits of Humic acids:

 Improve the soil structure and fertility

 Normalize the pH value of soils

1.2.4. Applications of Humic acids in different areas:

1.2.5. Separation of Humic acids substances from various processes:

1.2.5.1. Acid and alkaline extraction of Humic acids:

1.2.5.3. Application of ultrasonic vibration on the extraction of Humic acids:

1.2.5.4. Coacervate extraction method:

1.2.5.5. Electromagnetic and electrocoagulation process:

1.2.5.6. Biological process to separate humic substances:

complete the two

1.2.5.7. Microwave assisted soxhlet method:

1.2.5.8. Fenton oxidation process:

content (Kochany and Kochany, 2008).

1.2.5.9. Nitric acid oxidation process:

1.2.5.10. Ferric chloride coagulation process:

1.2.5.11. Membrane electrolysis and electrocoagulation process:

1.2.5.12. Application of membrane ultrafiltration for the treatment of humic

1.3. Treatment of paper industrial wastewater and an approach to recycle the

1.3.1. Anaerobic digestion process:

1.3.2. Application of flocculation process using polymeric flocculants:

In the recent period, the application of synthetic polyelectrolytes, like, polyacrylamide

1.3.3. Consortium bacterial treatment of paper industry effluent:

1.3.4. Electrocoagulation process:

1.3.5. Photocatalytic treatment of paper mill wastewater:

1.3.6. Membrane technology for the treatment of wastewater:

Ultrafiltration, nanofiltration, hybrid membrane filtration, and advanced membrane

kW power consumption was stated during shear-induced reverse osmosis treatment of

1.4. Application of advanced separation technology towards tea factory generated

1.5. Utilization of tea factory solid wastes towards environmental management:

(Todisco et al., 2002). Tea

1.6. Knowledge gap and objectives of the project work:

Performance characterization study of spinning basket membrane module during

A. U. Ramunni, F. Palmieri, Use of ultrasonic treatment for extraction of humic

D. O. Otieno, A. Kumar, M. S. Onyango, O. Aoyi, Treatment of Tea Industry