Proceedings of CUChE Alumni Symposium 2022

On “Circular Economy on Sustainable Basis: The Role of Chemical Engineers”

CUChEAA ISBN: 978-81-954649-1-3

December 2022 P a g e | 75 Volume 2, Issue 1

Prospect of electrochemical process-induced separation techniques to redefine waste-water as

the resources – A journey towards circular economy

Pallab Kumar Bairagi

Ordnance Factory Nalanda, Department of Defence Production, Ministry of Defence, Rajgir, Bihar, India

Telephone: 06112-257-121 Extn. 4010/11

E-mail: pkbairagi@ord.gov.in, pallabchemengg2011@gmail.com

Abstract

Exponential population growth, rapid industrialization and urban expansion in 20

and 21

centuries have adverse effect

on natural resources and living beings because of industrial, municipal and agro-industrial waste generation in billion tons

per year. Efficiency of these resources can be enhanced by proper treatment of contaminated natural resources. Therefore,

to control the natural resources sacristy, to reduce anthropogenic activities on ecosystem and to minimize climate change,

efficient treatment and separation techniques need to be developed or chosen carefully. Water is one of those badly

affected natural resources, and therefore, treatment of waste-water is a major concern especially in India. However, waste-

water can be considered for mining the valuable precursors and bioactive substances present in it which needs highly

selective, fast, and efficient separation processes. The process must involve materials with high selectivity to capture target

compounds/molecules/species from complex systems or complex fluids. Herein, this review describes an outline of

different separation techniques used for the separation and treatment of precursors and bioactive substances present in

waste-water with a focus on electrochemical techniques. The review describes the recovery of nitrogen- and phosphorus-

nutrients as the case study for their important role in natural, semi-natural and artificial systems where nitrogen and

phosphorus present as several species, mainly, ammonia and nitrates. Different selective materials are also discussed for

their applications in selective separation. Moreover, this perspective provides an idea of the fast, efficient, and resource-

oriented separation techniques integrated with electrochemical processes, which will play a crucial role to make waste-

water as the useful resources for the nutrients-recovery and to enable the target molecule-specific circular economies in the

next few decades. This review may pave a way to develop different selective materials and separation techniques which

can integrate circular economy (CE), bio-economy and green-economy towards a total economy to redefine different waste

materials as the resources of different nutrients, bioactive substances, and microorganisms.

Keywords: natural resources, electrochemical processes, waste-water, bioactive substances, circular economy (CE).

1. Introduction

A special format of the periodic table was presented by

the European Chemical Society for celebrating 150

birthday of Mendeleev’s periodic table on 2019 to

describe and indicate the scarcity of elements and

subsequent potential threat [1, 2]. Increasing rate of

population growth in the urban areas and rapid

industrialization in 20

and 21

centuries have adverse

impact on natural resources and living beings by

generating billion tons of industrial, municipal, and agro-

industrial waste annually [3]. The European Chemical

Society emphasized that our precious resources must be

used carefully in the upcoming years with a special effort

on minimizing the waste generation and partial recycling;

failing which, a few natural elements which are highly

important and critical for our surrounding world may be

diminished because of their limited existence, area of

location, or our inability to recycle those elements

properly [4, 5]. Development of new techniques or

modification of existing methods and introduction of

those for taking remedial action through post-utilization

recycling of resources and recovery of precious elements

from the waste generated may enable the use of these

resources, elements and materials in a circular way which

is the key to conserve these precious natural elements [6,

7].

Proceedings of CUChE Alumni Symposium 2022

On “Circular Economy on Sustainable Basis: The Role of Chemical Engineers”

CUChEAA ISBN: 978-81-954649-1-3

December 2022 P a g e | 76 Volume 2, Issue 1

Steffen et al. and others [8, 9] classified the waste

problems into nine major planetary boundaries based on

their adverse effect on the living beings: climatic change,

ozone layer depletion, acidification of seawater, decrease

in biodiversity, deforestation, biogeochemical transfer,

increase in aerosol-content in the bio-atmosphere,

environmental pollution due to contamination of harmful

chemicals used in different sector, change in land

environment and excessive use of fresh-water [Fig. 1].

Unfortunately, important sustainability targets such as

rate of extinction, biogeochemical transfer of key

nutrients – phosphorus (P) and nitrogen (N), and carbon

dioxide-content in the atmosphere for some of those are

being pushed beyond the tolerable limit due to human

activities [1, 8]. Carbon (C), P and N are also the three

key biogenic-elements among the most important six

biogenic elements for the living organisms as the primary

constituents [10]. However, the waste materials generated

and accumulating in the environment are enriched with C,

P and N also; for example, carbon dioxide and methane

(greenhouse gases) as the carbon-waste, NO

, and

ammonia as the nitrogen-waste, and different phosphates

as the phosphorus-waste. Both the ammonia and

phosphates are highly important from the agricultural

point of view. But these waste materials are being

discharged into the waste-water stream, and thus, enter to

the aquatic system causing eutrophication and several

adverse effect into aquatic life. Therefore, in addition to

resource-management, advancing sustainable chemistry

and its implementation for the recovery and recycling of

various natural resources is highly needed to minimise

the environmental waste generation and relevant issues.

With the adaption of suitable techniques for the treatment

of contaminated natural resources, the efficiency of these

resources can be enhanced.

In view of the above, water is one of the most adversely

affected natural resources due to accumulation of waste

product in it. Moreover, consumption of fresh, useful, and

clean water in exponentially increasing rate due to rapid

industrialization and urban expansion is making its scarce

and will cause global water crisis in the upcoming years.

According to the latest CPCB annual report (2020-21)

rate of sewage generation in India is 72368 MLD, 5~50%

of which are being generated by five states: Maharashtra,

Uttar Pradesh, Tamil Nadu, West Bengal, and Gujarat

[11]. Increasing requirements of different natural

resources due to the exponential growth of population in

the urban areas, merging with global fresh water scarcity,

pointed out the necessity of water reuse and recycling of

used water [12]. Based on several scientific reports, the

world water consumption may increase by 20 to 40%

from the present water consumption in next three decades

[13, 14] which necessitates the reuse and recycling of

waste-water. Thus, it is critical to handle waste-water in

the water management cycle (UN Water, 2017) [12] and

consider water-water treatment for the resource’s

recovery as the solution for the water-shortage and

drought-based problems [15].

It is mentioned in several reports that maximum waste-

water treatment plants (WWTPs), which play a critical

role in waste-water recycling, are processing the waste-

water to bring the chemical parameters of waste-water

below the specified limits (as per environmental

regulatory or guidelines) so that the waste-water can be

disposed with a minimum conditioning cost [16].

However, waste-water may contain a number of various

sets of important resources: based on the waste-stream

mixed in it. The important resources which can be

recovered from the waste-water cellulose, phosphate,

biochar, bioplastics, biomass, biodegradable plastics, and

alginate-like exopolymers; and thus, the waste-water can

be redefined as the waste-water resources instead of

considering it as the wastage of natural resources.

Therefore, WWTPs can be crucial for the bioenergy

production and recovery of several important resources in

addition to the clean water generation by integrating

several suitable separation techniques and energy

producing system with the existing water purification

techniques. Advancing WWTPs with a focus on the

recovery of energy and resources can be useful for the

cost recovery in addition for improving the quality of

discharge water.

Figure 1. Framework representing planetary boundaries.

The image and relevant information are licenced under

CC BY-NC-ND 3.0, which is free to share, copy and

redistribute. Credit for preparing this framework to J.

Lokrantz/Azote who prepared this based on the

information shared by Steffen et al. 2015. The framework

can be downloaded from

https://stockholmresilience.org/research/planetary-

boundaries.html website.

Because of the several environmental and economic

challenges due to the adverse effect of some social

activities, circular economy (CE) is drawing continuous

attention as compared to the currently existing linear

economy from last two decades [17, 18]. The importance

of CE is continuously increasing to the governors,

scientists, stakeholders, policymakers, technology

Proceedings of CUChE Alumni Symposium 2022

On “Circular Economy on Sustainable Basis: The Role of Chemical Engineers”

CUChEAA ISBN: 978-81-954649-1-3

December 2022 P a g e | 77 Volume 2, Issue 1

developers and scholars because of the scarcity of various

resources and exponential growth in population. The

principles of the CE have been adopted: to decrease the

consumption of raw / input materials, to remove the

waste from the used materials/resources/substances as

much as possible so that the remaining substances can be

recovered for elemental balance and reutilization of

resources, and to contribute for achieving global

sustainability targets on water and sanitations

significantly [19, 20].

Designing of WWTPs with a focus of integrating energy

recovery systems with waste-water treatment systems has

drawn significant interest to the engineers and scientific

community because of the increase in global energy

requirement (EIA, 2013) [21]. However, because of

conversion losses, maximization of energy recovery from

the waste-water resources may be irrational and

impractical [22]. Kehrin et al., 2020 illustrated in a

critical review that domestic waste-water resources

cannot meet the energy or elemental requirements [23]. In

spite of several technologies developed and tested for

their suitability in the recovery of energy, water, fertilizer

and other waste-water products in lab scale, a few have

been implemented in the large-scale production due to

technological limitations and non-technological

constraints. Development of a suitable energy recovery

system and the waste-water treatment unit in view of

resource recovery, and its integration with an existing

WWTP to consider waste-water as the natural resource

are the primary challenge. Focus should be given to the

recovery of different resources such as P- and N-based

nutrients, heavy metals, bioplastic, sulphur as S0, etc. by

integrating suitable as well as selective separation

techniques and maximum energy recovery, from the

waste-water and the suspended ingredients before

discharging the effluents. Legal requirements and

effective policy need to be established also for the

implementation of the processes. Minimization of the

environmental risks and human health issues during the

implementation of the technologies, and contaminants in

the recovered-product is also a challenging task.

Herein, this review gives an overview on the applicability

of the waste-water as the resources of different important

nutrients, water, and energy from CE point of view. This

review focuses on the recovery of different nutrients and

other waste-water based by-products considering the high

resources-content of waste-water generating from the

different sources. Firstly, we briefly demonstrated the

resources that can be mined from waste-water to reduce

the searching and exploration of new sources for those in

line of circular economy. The importance of these

resources in the water-energy-economy cycle and

productivity and subsequent challenges are briefly

discussed. Next, we elaborately mentioned different

separation techniques and their applicability in the

recovery of the waste-water resources-based products.

Then, we discussed about several electrochemical

techniques, with or without integrating with other suitable

and existing separation techniques, which are being used

for the resource recovery for the recovery of the nutrients

and other waste-water by-product from the waste-water

resources. Finally, prospects of the electrochemical

techniques for various resource recoveries by mining the

waste-water to minimise the scarcity of various resources

with a view of CE concept is briefly discussed. Therefore,

this review highlights the benefits and challenges for

mining waste-water showing the prospects of the same to

reduce and control element scarcity.

2. Waste-water as the resources for nutrients,

precursors, and other materials

Because of the exponential population growth and

varieties of industries formation, different kinds of

municipal and industrial waste are being generated and

the quantities of the waste generated per year (in billion

tons) are increasing rapidly. Most of these waste

materials, before or after its treatment, are mixed with the

water used for cleaning purposes. In some cases, waste-

water streams are generated after the use of fresh water in

industries, municipal areas, and agricultural lands. Due to

above mentioned diverse source of generation, waste-

water streams contain a variety of components as the

contaminants. Several biological bodies such as

microbes, bacteria, fungus etc. have been grown in the

waste-water streams and produce a few bioactive

substances in it some of which are precious which can be

used for different purposes after its successful recovery.

Due to its important roles as the fertilizers, nutrients

present in waste-water are becoming the point of interest

now. Different nutrients and high value-added products

such as N-nutrient as ammonia and nitrates; P-nutrient as

phosphates; sulfur as sulphate and sulfide, different heavy

metals both scarce and abundant; different biological

proteins, lipids, phenols and its derivatives, polyphenols,

pharmaceutical ingredients, and others can be recovered

from sewage-sludge, raw waste-water, and semi-treated

waste-water streams (Fig. 2) [24].

Egg processing waste-waters contain several essential

amino acids with high concentrations; dairy-based waste-

waters contain macro- and micronutrients type value-

added products, for example, different proteins and lipids

[25]; Soybean processing waste-waters contain Bowman–

Birk protease inhibitor which has promising anti-cancer

activity, soybean agglutinin, Kunitz trypsin inhibitor and

other value-added products [26]. Pharmaceutical waste-

waters have different recoverable resources of diverse

type based on the raw materials used in different

pharmaceutical industries, which is therefore difficult to

treat [27]. Nanofilters are commonly used for antibiotic-

containing aqueous solutions. It was observed that,

amoxicillin, a commonly used antibiotic to prevent

different kinds of bacterial infections, can be recovered

up to ~97% via nanofiltration [28]. Pharmaceutical

waste-waters may also contain different heavy metals

such as Ni, Cd, Zn, Pb, etc. [29]. Waste-water generating

during coal gasification contains phenol and its

derivatives [30].

Therefore, recovery techniques from nutrients and others

from the waste-water stream in WWTPs are gaining more

attention to the governing bodies, policy makers and

Proceedings of CUChE Alumni Symposium 2022

On “Circular Economy on Sustainable Basis: The Role of Chemical Engineers”

CUChEAA ISBN: 978-81-954649-1-3

December 2022 P a g e | 78 Volume 2, Issue 1

scientists. Recycling of ammonia or its recovery can

create renewable N-resources to using for agricultural

purposes. White phosphorus can be prepared from the

urine-based phosphate-waste. Recovery and/or recycling

of phosphorus from phosphate-waste can be used as the

resource for fertilizer production, manufacturing of

additives and other phosphorus-based chemicals. These

will reduce the fossil-based fertilizer and scarce

elements/material consumption in virtue of the principles

of circular economy. Recovery and capturing of

ammonium & phosphate ions can create the resources for

both N and P containing products. In some cases, the

recovery rates for N and P in urine are estimated about

70–80% and 50%, respectively. For example, struvite,

which is formed in the kidney as kidney stone, contains

both N & P (MgNH

.6H

O); and therefore, its

successful recovery from the N and P-based waste-water

can help to conserve phosphate rock mineral resources.

Recovery of different strategic elements such as gold,

silver, copper etc. from sewage-sludge ashes can also be

possible [31]. Also, several construction items, for

example, bricks, cement, and other light-weight materials

can also be recovered from the waste-water sludge.

Figure 2. Important resources available in waste-water.

Moreover, the adverse effect of continuous

industrialization, deforestation and uncontrolled

population growth is demanding the excessive energy

production which has obvious impact on the water

sources. However, the policies taken in this context to use

water sources more and more for the energy production is

increasing the stress on both water and energy. In this

context, waste-water resources have been acknowledged

as new resources for the recovery of energy based on the

increasing rate of waste production and its adverse effect

on environment. The greenhouse gases emitting from the

waste-water and other waste materials are mainly targeted

for the energy production via waste-water heat recovery

approach.

Post-treatment, the treated water can be used for meeting

industrial & agricultural water requirements, groundwater

replenishment, irrigation etc. Depending on the quality of

the effluent, this can be useful in domestic arena & fire

protection also. Therefore, recovery of the nutrients and

high-added value products is highly important in addition

to energy recovery during the treatment of waste-water

streams in view of circular economy principles.

3. Separation techniques for different components

Because of the diverse source of waste-water generation,

different waste-water stream contains different sets of

contaminants in it. This requires the treatment of waste-

water streams in a different manner for the recovery of

the nutrients, precursors, minerals, and other materials

present in these streams. For example, polyphenols

present in waste-water generated [5-25 g L

-1

] during the

extraction of olive oil can be separated by several ways

[32, 33]. Milk protein-coated activated carbon was also

tested and has been shown promising efficiency

(approximately 75.4% total phenol recovery) [34]. The

recovery was also performed after the pre-concentration

phenolic compounds in the waste-water generated due to

the processing of olive oil using Cloud Point Extraction

technique, which is a low-energy process [35]. Separation

techniques applicable for the different nutrients,

precursors, heavy metals and others can broadly be

divided into following categories: Physicochemical

techniques (for example, Ion exchange-and stripping

integrated with adsorption, use of gas permeable

membrane etc.), chemical methods (such as chemical

precipitation, struvite precipitation, reactive filtration

etc.), enzymatic treatment, microbiological treatment

(such as microalgae-based separation) and

electrochemical techniques (based on the mechanism

involved). The methods which are commonly used for

mining resources for different materials from waste-water

(except electrochemical techniques) have been discussed

below (Fig. 3). Electrochemical techniques-assisted

separation is discussed in next section (section 4).

3.1 Ion exchange/adsorption process

This separation technique is commonly used for the

removal of phosphate and ammonium form the waste-

water. The method is useful to recover these ions also as

the P- and N-nutrient. Zeolite, a porous adsorbent having

exchangeable cationic (Na

, Mg

, K

, Ca

, Ba

etc.)

[36, 37], is commonly used for the adsorption of

ammonium ions via cation exchange whereas P-selective

adsorbent is used for the exchange of phosphate ions with

a suitable anion [38]. Natural and modified zeolites and

clinoptilolite zeolites are mostly used [39, 40], which are

economically feasible, efficient ammonium adsorbent

with simple operational procedure [41]. The ammonia

adsorption-capacity is due to the NH

adsorption to -

COO

groups in the polymeric network [42, 43].

To enhance the ammonium adsorbing efficiency, zeolites

were synthesized from different sources such as from rice

husk ash (showed 46.56 mg g

-1

adsorption-capacity

which is higher as compared to that of natural mordenite

(15.13 mg g

-1

)) [44] and effect of pre-treatment was

studied such as with NaCl and by varying pH,

temperature, adsorbent dosage and initial NH4

concentration [45], as reported in the recent literatures.

Several other adsorbents are also tested and found to be

promising such as Romanian volcanic tuff [46], carbon

nanotube (CNT) [47], wheat straw [48] and novel

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On “Circular Economy on Sustainable Basis: The Role of Chemical Engineers”

CUChEAA ISBN: 978-81-954649-1-3

December 2022 P a g e | 79 Volume 2, Issue 1

palygorskite nanocomposite [43] showing 19, 17.05,

148.7, 237.6 mg g

-1

ammonium adsorption-capacity,

respectively.

For the phosphate recovery P-selective media need to

have following characteristics: high surface area and

porous structure, high content of phosphate adsorbing

active sites [49]. Different Commercial media, for

example, hydrotacite-based compounds [50], amberlite

IRA-410, hybrid anion exchangers [51], purolite

composites [52] have been as the P-selective media.

Several synthesized media have also been developed and

tested for this purpose, for example, DOW-HFO, DOW-

NAB-Cu, DOW-FeCu and DOWCu [53, 54] successfully

for the P-removal and recovery from synthetic and real

waste-water. Studies were also carried out for the waste-

water having wide P-range [49] and low P-concentrations

[53, 55]. Kuzawa et al. (2006) reported a 47.3 mg-P per g

maximum adsorption-capacity in synthetic waste-water

with HTAL as adsorbent [50] and Johir et al. (2011)

performed the experiments successfully in MBR effluent

using A500P as the adsorbent [52]. Blanney et al. (2007)

tested HAIX as the adsorbent for the P-recovery in

synthetic waste-water and in secondary effluent

successfully (maximum adsorption efficiency 2 mg-P/g-

HAIX) [55], Awual et al. (2011) tested Zr-FPS as the

adsorbent for the P-recovery in synthetic waste-water

successfully (maximum adsorption efficiency 1.45 mg-P

-1

) [56], and Williams et al. (2015) reported a 0.5 g-P per

Lmedia, 1.5 g-P per Lmedia, 2.0 g-P per Lmedia

adsorption-capacity for the P-nutrient recovery when

tested with Dow-Cu, Dow-FeCu and Layne

as the

adsorbent, respectively [54]. The P-selective media

generation is easy and can be done by brine solution, by

an alkaline solution or by a combined brine and alkali

solution of fixed volume (one to twenty bed volume

based on the media used), for example, NaCl solution,

MgCl

solution and NaCl/NaOH mixture [51-54]. P-

nutrient recovery from the used brine solution is also

important (to reduce the cost also) which is commonly

done using calcium phosphates or struvite precipitation

by mixing a calcium salt or MgSO

.7H

O / NH

mixture [53]. Moreover, NaOH may be required to mix

into spent regenerated (post-PO4

precipitation) for

compensating the OH

losses during precipitation.

The method is easy to operate and found to be very useful

to discharge effluent with high quality by keeping P- and

N-based contaminants as low as possible. Effect of pH is

significantly lesser. However, the media regeneration

process requires a brine or NaOH solution and total

nutrients recovery cannot be achieved during media

regeneration. Moreover, the process facilitates N-removal

more than N-recovery and the adsorption/desorption

capacity is low. Additional stripping/ adsorption unit is

required for N-recovery from the regenerant. Leaching of

several other metal cations, for example, Al

, Ca

etc. is

also a concern.

Figure 3. Schematic showing methods for resources

mining from waste-water.

3.2 Stripping and absorption (especially for N-nutrients

recovery)

Studies have been reported the recovery of N-nutrient

using the air-stripping method for ammonia [57-60]

showing a high recovery efficiency (~94%). To improve

the efficiency for mass transfer efficiency, it is commonly

performed in a packed bed tower [40]. It is observed that

pH can influence the ammonia stripping kinetics more

[61] among the various ammonia stripping controlling

parameters such as gas flow-rate, time for desorption,

temperature, pH etc. [59, 61]. A very low recovery of

ammonia was observed in pH 8.3-8.6 [60] and an

optimum pH for ammonia stripping was reported as

greater than 9.5 [62]. Therefore, many studies used pH-

elevated concentrated NH

solutions for NH

stripping

and acid solutions for the recovery of NH

[57, 58, 60,

63]. In addition, several studies were conducted on waste-

water with high ammonia concentration [57, 64, 58, 65],

however, ammonia stripping was also found to be

promising for ammonia recovery at low ammonia

concentrations [66]. Cheung et al. (1997) reported a study

showed the applicability of ammonia stripping on the

landfill leached materials [67]. Although the ammonia

process is widely used for its low operational cost, high

recovery efficiency and easy installation of the units [61];

the high energy requirement [63], for example, 9 kWh kg

N energy requirement for ammonium sulphate

production from urine [68, 69], is a concern for operating

the process(es). However, jet loop reactor, aero cyclone

reactor or other much efficient stripping reactors can be

used to minimise the energy required for aeration [70,

71]. The stripping and acid absorption is also integrated

with the electrochemical and bioelectrochemical methods

as the final steps for the N-recovery as NH

[69, 72-74].

This kind of reactors is easy to install and has simple

operational procedure to recover N-nutrient directly as

the fertilizer. Energy requirement is also low or

comparable as compared to standard and available

ammonia production techniques. However, the process

requires the pH adjustment and control and is commonly

applicable in waste-water with high ammonia

concentrations. The process is not suitable in low

temperature region.

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3.3 Gas permeable membranes for the ammonium

recovery

In recent times, gas permeable membranes are drawing

significant attention to the researchers for their potential

suitability in ammonia separation and recovery. Several

studies have been reported showing a ~95% recovery of

ammonia from both liquid [75] and gaseous phases [76,

77]. Commonly, in the ammonia-rich waste-water, a

tubular membrane is submerged and sulphuric acid is

recirculated through it or the ammonia-rich waste-water

is circulated through a tubular membrane submerged in

sulphuric acid, to recover ammonia as ammonium

sulphate [78]. The optimum pH for these operations was

indicated as: above in several studies showing more than

90% ammonia recovery and removal [79, 80]. It was also

reported that the recovery and removal efficiency for

ammonia dropped to ~57% for small values of pH [78]

which also depends on the ammonia concentration [80].

Dube et al. (2016) reported that low-rate aeration in the

manure can help to eliminate the alkali addition step and

to reduce the optimum pH to 8.3. This also facilitates to

increase the rate of ammonia recovery as compared to

that achieved without aeration or alkali addition [81]. A

study was also reported showing a simultaneous N and P

recovery (~83% and >90%, respectively) using gas

permeable membrane [82].

Although this process facilitates a direct recovery of N-

nutrients as fertilizer and shifting of pH by low-rate

aeration in manure can be done, this requires the

adjustment and control of pH. Also, the process is

commonly applicable for the waste-water with high

ammonia concentration and is costly.

3.4 Magnetic microsorbents

These are the substances which have magnetic properties

as well as adsorbing capacity. The idea is to use the

suspended magnetic microsorbents in waste-water for the

recovery of the nutrients present in the waste-water via

adsorption. To do so, a high gradient magnetic separator

has been used to capture the suspended media from the

nutrients-adsorbed magnetic media followed by

regeneration and precipitation from regenerant steps [49].

Different kinds of magnetic microsorbents were tested for

the removal and recovery of trace P-nutrients from

synthetic and areal waste-water [83-85]. Among those

magnetic microsorbent materials, zirconium ferrite

(ZrFe

(OH)

, ferromagnetic) in treated waste-water [84],

carbonyl iron particles in synthetic waste-water [86],

magnetite and iron particles in synthetic waste-water

[87], and P selective MgFeZr LDH-, ZnFeZr-coated

nanoparticles-embedded SiO

-matrix in spike

treated and treated waste-water samples [85] were tested

successfully with high adsorption-capacity for P-

nutrients. The magnetic ion exchange resins can also be

used in secondary effluent [88]. With the increase in

adsorbent dosage and washing of adsorbent materials in

between cycles can help to achieve more than 90% P-

removal/ recovery [89]. As regeneration of the magnetic

microadsorbents and ion exchange resins is essential, it

was reported in a study that 88% adsorption and 95%

desorption can be achieved using MgFe-Zr when tested

by a pilot-scale experiment in a treated waste-water [90].

In another study, the authors reported 95.2% adsorption

and 86% desorption efficiencies for generating ZnFeZr

adsorbent using 1.0 M NaOH [85]. Ishiwata et al. (2010)

reported 83.8% desorption from ferromagnetic

ZrFe

(OH)

by treating with 7% NaOH [84].

Although magnetic microsorbents-based separation

techniques process is effective for reducing the

concentration of P-nutrient in the discharge based on the

quality of fed waste-water and the biological and

biochemical processes occurring in waste-water does not

affect the process much, NaOH is needed for the

regeneration. Also, adsorbent to P ratio controls the P-

removal efficiency; and therefore, the regeneration

solution contains low P-concentrations leading this to

become an uneconomical recovery process.

3.5 Chemical precipitation

This process, which is considered as a stable process [91],

is used very often for the removal of metal ions to release

the discharge or effluent as per the environmental

standards fixed by the government or the local/ national

regulatory bodies [92-93] by maintaining chemical

consumption low [94]. Using this process, 0.1 mg L

-1

P in

the effluent can be achieved with high chemical doses.

By integrating with an advanced filtration technology

applicable for the removal of P, the cost for the chemicals

can be lowered [95]. Ca

, Fe

, Al

are the commonly

used metal ions in the chemical precipitation processes

[40, 93, 96-100] to remove P by removing the precipitates

with sludge from waste-water, however, handling and

disposal of the sludge is a challenging task [101] due to

increase in sludge volume by ~35%. The other

disadvantages of chemical precipitation are: reagent cost

(e.g., coagulants), adjustment of pH is difficult, inhibition

due to different biological processes [102] and heavy

metal leaching etc. Post-processing (extraction or

leaching of wet-chemical) of the sludge is needed for

increasing the metal phosphate compound’s solubility

[93]. Different cost-effective methods can be helpful to

dissolve hydroxyapatite, for example, phosphate-

solubilizing fungi- or bacteria-assisted methods [103-

105]. Sludge releases P-nutrients because of anaerobic

conditions of the stripper which further precipitated out

as hydroxyapatite in a reactor (pH 9). Recovery of

phosphates from the supernatant solutions, which can be

collected from the sludge settler, can be done by Phostrip

method [106], however, the process requires additional

sludge digestion and increase the operational costs [99].

Chemical precipitation is easy to operate, can withstand

shock-loading and can maintain low P concentration in

the effluent. However, the process is primarily used for P

removal, requires dosing of external chemical(s) and can

be affected by different biological processes (which can

be occurred in waste-water). In addition, chances of

heavy metal contamination and cost may be enhanced for

the sludge generation in excess and its handling.

3.6 Struvite precipitation

Struvite (NH₄MgPO₄·6H₂O) is a yellowish or brownish

white phosphate mineral with orthorhombic crystal

structure; and has pyroelectric and piezoelectric

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characteristics. This is a slow-release fertilizer and can be

mixed with other complex fertilizers to increase its

agronomical properties [107-109]. Several studies for P-

recovery via struvite crystallization with EBPR have also

been reported [110-112]. It was also showed that during

the struvite precipitation in an anaerobic digester, P-

concentrations in the EBPR discharge can be low. Study

also showed that more than 80% P removal is because of

the struvite precipitation [113-114]. The first continuous

pilot struvite plant operation was carried out by feeding

source-separated urine and the achieved struvite has more

than 90% purity [115]. Several studies have been reported

on the P-removal via struvite precipitation from urine and

the factors which are affecting the process [116-119].

Study of mixing excess Mg

as MgCl

[115], RO

concentrate [120], or seawater and brine [121] was also

performed. Struvite precipitation has been occurred when

the concentration of phosphate, ammonium and

magnesium ions in the solution exceeds the solubility

index and its minimum solubility is at pH 9. According to

Mavinic et al. (2007), to achieve 80% P removal and

recovery, a super saturation ratio of 20 is required at least

[122]. In this context, Mg

is found as the limiting

reagent for the precipitation process [112]. Basxakc-

ilardan-Kabakci et al. (2007) reported a 95% P recovery

as ammonium or potassium struvite [64]; however,

ammonium struvite has a higher tendency to precipitate

because of its low solubility compared to others [117].

The struvite precipitation reaction is as follows -

+ PO

3−

+ Mg

+ 6H

O → MgNH

⋅6H

Struvite precipitation also facilitates the ammonium

recovery from the waste-water. However, the waste-water

under treatment must content phosphate; otherwise, both

and PO

need to mix to initiate precipitation.

Moreover, a low phosphate content can cause partial N

recovery [123-126].

Crystallization of struvite helps to maintain low

impurities in the recovered product and the process

outcomes can be used as a slow-release fertilizer and

contain magnesium as an additional nutrient. However,

the process requires the adjustment of pH and needs

addition of various chemicals leading to cost increase

during the P-recovery.

3.7 Biological P recovery

Enhanced biological phosphorus removal (EBPR) can be

applied for the P-removal and recovery as a biological

process. In this process, phosphateaccumulating

organisms accumulate P which produces P-rich sludge

[127] resulting 80–90% of P removal [110]. Moreover,

integration of an anoxic tank can facilitate the N-recovery

and removal also [128]. The denitrifying

phosphateaccumulating organisms can accumulate a part

of their dry biomass in P (up to 20% by weight) [129].

Sometimes, this process is favourable as compared to

chemical precipitation based on the P-limits in the

solution [112, 126]. Recovery of P-nutrients using EPBR

are commonly done by the collection of digestion

supernatant of nutrient-rich anaerobic sludge [130].

Temperature, pH, fatty acid content (volatile), ratio

between food and microorganism, hydraulic and solid

retention time, concentration of dissolved oxygen and

cations and several other factors need to be controlled to

operate EPBR. EBPR is also a complex process and is

expensive to operate [131].

Although the process is applicable for the recovery of P-

and N-nutrient simultaneously, economical as compared

to standard chemical precipitation processes and a low P-

content in the discharge water can be maintained using

this separation techniques; the complexly operated

process is sensitive to the characteristics and inherent

properties of influent such as concentration of cations and

dissolved oxygen, pH, temperature, etc.

3.8 Algae harvesting

In view to move towards circular economy considering

the environmental crisis and present status of elemental

scarcity, nutrient recovery using algal-biomass is drawing

significant interest. Algal ponds and macrophytes can be

helpful to recover nutrients for which only 1/10

or less

land is required as compared to land required to do the

same by terrestrial crops/ pastures [132]. P-content in dry

algal-biomass can be achieved up to 3.4% [131, 133].

Moreover, algae can be grown in algal-turf scrubbers and

immobilized-beads [134-135], and the process was used

for the treatment of various type waste-water such as

dairy waste-water [136] and swine manure [137].

However, as algal-biomass requires large time for

releasing nutrients, additional processing unit for algal-

biomass, for example, hydrothermal liquefaction [138],

can be introduced to produce fertilizer. Also dried algal-

biomass, with heavy metal loading by maintaining

environmental regulatory, has been successfully used as

commercial fertilizer [97]. Presently, government as well

as environmental regulatory and public acceptance are the

main barriers for algal-biomass to use as fertilizer [139];

and the adverse effect of algal biomass-based fertilizer on

the environment and human beings, nutrient-availability

for the crops, [140], and micropollutants and pathogens-

content [97] must be thoroughly investigated. Several

studies reported promising outcomes by using algae for

livestock production and as food crops, however,

techniques involving the algae-cultivation must be cost-

effective [141]. Algal-biofuel production cost is the main

constraints for its large-scale implementations [142].

The process can facilitate to recover the P-nutrients up to

3.4% of the weight of the dry biomass, can be

implemented offshore and heavy metal loading is well

below the permitted limits as per provided guidelines the

different regulatory bodies. However, post-processing

may be needed to improve the rate of nutrient release.

More importantly, the presence of different pathogens,

micropollutants, allelochemicals and/or cyanotoxins is

the main concern, and therefore a systematic and

thorough investigation is needed before its exploration for

the nutrient recovery.

3.9 Direct conversion to the useful resources

Similar to algae harvesting, heterotrophic

microorganisms can be used to convert the nitrogen-

based waste materials present in waste-water to protein-

rich food sources [143]. The technology is gaining

interest to the researchers, industrialist, national

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governing bodies, and the policy-makers as this method

can help to synthesize food-products directly from the

waste-water resources and can meet various

requirements. For example, using the Biofloc technology

N-based and other waste materials can be converted to

biomass which can be used for fish and aquatic creatures

as the feed [144]. In the Marine aquaponics conversion

techniques, N waste can be directly converted to plant

proteins by growing edible plants [145]. Several studies

indicated that the single cell proteins can be an alternative

for human which can reduce the present food scarcity

[143, 146]. However, the production cost in respect to

that of conventional sources is high [143, 147].

Moreover, contamination due to the presence and

improper separation of toxins, and heavy metal in SCP

during its growth on hydrocarbon-based media is the

main concern which necessitates a thorough study before

its practical applications as an alternate protein source

[146].

3.10 Reactive filtration for the P recovery

Several studies have been reported for the P-removal and

recovery as the both particulate P and orthophosphates

using reactive filtration method. Mechanisms such as co-

precipitation, filtration, adsorption etc. are being used in

these methods. Moving-bed iron-oxide-sand filters were

used in a study showing a 90.3% removal of P [148].

FeCl

was used for the continuous regeneration.

Backwash from the filtration process may be helpful for

the slow fertilized release [149]. Polonite [150-152],

activated zeolites [153-155] etc. are the commonly used

filter materials. Zeolites are also helpful to recover

phosphates and ammonia simultaneously via brushite and

struvite formation and precipitation and also promising

materials to form slow-release fertilizer [153-155]. P-

removal and recovery capacity of steel slag [149, 150,

156-158], fly ash [159] and oil shale ash [160] is also

tested and reported as promising materials as these can

precipitate hydroxiapatite and calcium phosphates.

However, the effluents released from these slug filters

have high pH value [156-158] which necessitates the

thorough study on the applicability of these materials as

fertilizers [161]. However, the process requires the

addition of various external chemicals (like FeCl

) and

further treatments may be required for the resource

recovery from backwash.

Considering the drawbacks of the different separation

techniques discussed above such as external chemical

addition, heavy metal leaching, presence of toxins, high

energy requirements, adjustment of pH and others;

electrochemical techniques and electrochemical

techniques integrated with different nutrient selective

suitable techniques are gaining significant interest from

last few decades. These methods are briefly discussed in

the next section of this review with suitable examples and

case studies.

4. Electrochemical techniques used for waste-water

mining for the resources

It is observed from the market survey that the scarce and

precious waste-water resources have increasing demand

and therefore, have remarkable market prices although

these are harmful to the environment and human beings.

Several electrochemical techniques have been observed

to be effective as compared to other separation

techniques, when applied for the treatment and mining of

waste-water resources. For example, electrochemical

decomposition has been found to be suitable for

recovering heavy metals and/or treatment of heavy metal-

rich waste-water based on the redox phenomena; organic

pollutants are separated via electro catalytic oxidation at

the electrode surface from the phenolic derivatives-rich

industrial effluent and pharmaceutical waste-based waste-

water; recovery of various elements using

electrochemical techniques- supported hydrometallurgy

etc. Several electrochemical techniques successfully used

in different studies for the recovery of various nutrients,

precursors, heavy metals and other important materials

from waste-water. Among those capacitive deionization

(CDI), electrochemical oxidation and reduction

processes, electrochemically-induced precipitation,

electrocoagulation, microbial electrolysis cell,

electrochemical-stripping, electro-fenton, photo-

electrochemical methods (based on UV irradiation) etc.

have been used in several studies and are found to be

promising. Along with suitable examples the above

techniques are discussed below, with a focus on their

applicability for mining nutrients and resources from

waste-water.

4.1 Capacitive deionization for mining waste-water

This method, for the desalination and softening of water,

is gaining importance in the waste-water treatment sector

(more efficient when TDS is lesser than 5000 mg L

-1

) by

removing charged materials (charged particles/ metals/

organometallics/ nutrients etc.). Ions and charged

particles present in waste-water stream can be separated

by generating an electric field between two closely

assembled electrodes. Because of that positively charged

particles and negatively charged particles move towards

the oppositely biased electrodes. To avoid co-ion

expulsion, sometimes ion exchange membranes are used

in the CDI cells. In this process, voltage bias is applied to

polarise the non-Faradic electrodes. It is observed in few

studies that integrating with ion exchange method,

membrane-based capacitive deionization (MCDI) can

mine more than 65% ammonium as the N nutrient and

more than 40% phosphates as P nutrient. Therefore, this

method, on integrating with suitable separation

technique(s), can efficiently separate charged nutrients

and help to recover maximum nutrient in addition to

reducing salinity in view of CE. Carbon-based electro-

conductive porous electrodes are commonly used into the

CDI cell to increase the electro-active surface area.

Although high voltage facilitates the thicker electrical

double layer formation as well as movement of charged

particles/ ions towards counter electrode with a faster

rate; in CDI, low potential window (less than 1.5 V) is

generally applied for restricting the generation of faradic

current. This requires low energy also, as compared to

other desalination methods. A schematic drawing

showing flow CDI (FCDI) and MCDI is presented in Fig.

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Figure 4. Schematic for Flow and membrane CDI.

Similar to the other techniques, ammonia (N-based

nutrient) is the most common nutrients which can be

recovered from waste-water using CDI. Conventional

ammonia recovery techniques consist of an ammonia

separation/ enrichment technique followed by acid

adsorption which requires excessive chemicals and are

high energy process. In this context, CDI method, both

flow electrode and membrane-based, has been

implemented in different studies [162-165]. In these

processes, ammonium along with other positively

charged ions first transport through the ion exchange

membrane and absorbed in the activated carbon-based

cathode where ammonium ion deprotonates and converts

to aq. Ammonia (NH

). It is then expected to be trapped

in or within the cathode, resulting ammonia-rich solution

due to the de-protonation of ammonium ions via Faradic

reaction. The constantly-charged positive ions (mainly

, Na

, and Ca

) are largely released back into the

waste stream because of polarity reversal. Recovery of

ammonia has also been studied from coal gasification

gray-water [166] which confirmed that the recovery can

be done along with TOC removal and from real digestate

waste-water with a recovery percentage greater than 65%

[167]. In a study performed by Pastushok et al. (2019), a

recovery of 21% of nitrate ions with 5.5 mg g

−1

electrosorption capacity and 48% removal efficiency was

achieved [168]. A K

-activated carbon mixture

electrode has also been tested for increasing the ammonia

recovery percentage which showed that the recovery can

be done up to ~80% [169].

As discussed earlier, because of its environmental and

economic benefits, recovery of P-nutrient and high-purity

phosphate from waste-water is significantly gaining

interest. In a FCDI cell, both P and Cl

–

will be moved

across the ion exchange membrane and absorbed in the

anode during the charging process. Absorbing the H

, the

P ions converts into uncharged H

and spontaneously

desorbs into the electrolyte. On polarity reversal, most

–

ions would be moved into the spacer chamber and

neutral H

is expected to be trapped in the anode

chamber resulting P-rich solution. Xu et al. [2021]

showed that the P-recovery can efficiently be done in

FCDI cell [170]. Based on the suitability of the

separation of P-rich nutrient and phosphates in FCDI,

several electrodes have been developed and tested for

their efficiency in the P-nutrient recovery. Zhang et al.

developed and tested ZnZr-COOH/CNT composite

electrode which showed excellent recovery with an

equilibrium concentration of 0.3 mg L

-1

and low energy

consumption [171]. Gao et al. [2022] introduced a

guanidinium-functionalized electrode which showed

adsorption of 23 to 30 mg phosphate ions per g of

phosphate solution [172]. In their study Epshtein et al.

[2020] showed that ~90% phosphorus can be recovered

from industrial waste-water using FCDI [173]. Magnetic

iron oxide-based carbon flow-electrode was also tested

successfully [174]. Bian et al. (2019) reported a study for

determining the potential suitability of selective recovery

of P- and N-nutrients simultaneously [175]. In their

study, a simultaneous recovery of 49–91% phosphates as

P-nutrient, 89–99% ammonium and 83–99% nitrate as

the N-nutrient from the waste-water with salinity ~70-

98.5% using FCDI. A simultaneous recovery of ~89% of

P and ~77% of ammonia was also reported when the

electrochemical separation was carried out in an

integrated system developed by coupling bipolar

membrane electrodialysis and MCDI [176].

Studies were also performed for the carbon recovery as

oxalate and acetate. In their study Yu et al. (2021)

successfully recovered acetate and oxalate (greater than

80%) from waste-water. Moreover, the energy

consumption is low (0.45 kW h m

-3

) [177]. Xu et al.

(2021) studied the recovery of formic acid from EDTA-

based waste-water using FCDI method coupled with

ozonation which confirmed the effective recovery of

formic acid via complete degradation of EDTA [178].

Iodine, which is a non-renewable and scarce element, has

been recovered as shown in few studies by flow-electrode

capacitive deionization (FCDI) [179]. Cohen et al. (2018)

also reported a CDI system integrated with a physical

adsorption unit. Activated carbon-based electrode was

used in this study considering the activated carbon-

bromine interaction, which also facilitates bromine

adsorption [180].

CDI has been found to be suitable for recovering different

toxic metals, both commonly found and abundant, such

as arsenic, mercury, cadmium, copper, zinc, nickel etc.

which has a tendency to accumulate into the living cells.

Based on the working mechanism involved, CDI can be

useful to remove the hazardous metals from the waste-

water followed by regeneration of those metals. As, along

with heavy metals, alkali metals and other non-toxic

metals are also present into waste-water streams,

separation setup should comprise of selective metal ion

trapping/ adsorbing materials which is a challenging issue

for recovering different heavy metals from the waste-

water. In this context, a study carried out in a CDI cell for

determining the preference of different heavy metal ions:

chromium, cadmium and lead showed that the rate of

adsorption is ~ 13% which is more than 45% for the

remaining two metal ions [181]. Study has also been

performed for the Cd

ions recovery in a FCDI

confirming the applicability of the process for the same

[182]. In a study, nickel foam plate electrode dispersed

with CAs/MO hybrids was used to recover copper using

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electrochemical reduction-assisted CDI [183]. It was

observed that the copper removal efficiency is ~96%.

Study was performed to recover chromium in Cr(III) and

Cr(VI) states (Recovery percentage: 95.5% to 98.5% for

Cr(III), and 90.0% to 99.0% for Cr(VI); recovery time:

60 min), simultaneously [184]. A combination of

electrolysis, electrodialysis and CDI was also tested

successfully in a study presented for nickel recovery by

Peng et al. (2014) [185].

These studies confirm the potential recovery of P- and N-

nutrients recovery using CDI technique, with or w/o

integration of conventional separation method. These also

indicate that with suitable integration of separation

techniques and energy recovery units, total recovery of

these nutrients can be possible separately and/or

simultaneously which will facilitate to recover the

maximum amount of energy which will be critical step

towards CE. This process can be useful for recovering

various nutrients and charged particles from the waste-

water streams.

4.2 Electrochemical redox processes for mining waste-

water

Redox reaction-driven conversion of the central elements

of the target ions into a separate oxidation state may leads

to effective and selective separation of the target ions.

The electrochemical oxidation techniques generally

employed for treating organic compounds by

decomposition and mineralization [186-190]. The

oxidation reactions occur on anode either by facilitating

the electron transfer directly between reductants and

anode (direct electrochemical oxidation) [191] or by

generating the in situ oxidation species (indirect

electrochemical oxidation) [192-194]. The

electrochemical reduction employed for the waste-water

treatment purposes, where the electron generated in

anodic reaction or supplied by externally are being

consumed at the cathodic reduction reactions. This

method is also employed in several other electrochemical

process such as electrochemical denitrification,

electrodeposition etc. [195-198]. By employing

electrochemical reduction in waste-water - metals are

recovered from free metal ions [199, 200], nitrate and

nitrite are converted to ammonium [201, 202] etc. In case

of the requirement for maximizing the redox potential,

introduction of electrochemical system to carry out

electrochemical redox reaction can be helpful. Moreover,

several resources may be present in normal stage, i.e.,

zero-valent condition instead of ionic form such as metals

for which electrochemical redox reaction can be more

helpful for its recovery. The method also provides more

selectivity in several cases. Because of the governing

mechanism involved in electrochemical redox-based

processes, the primary focus for using electrochemical

redox-based separation techniques (with or w/o

integration of other suitable separation methods based on

the target components to be recovered) to recover scarce

and abundant heavy metals with high market values.

However, in few studies some of these techniques were

successfully tested for P- and N-nutrients recovery as

ammonia-rich solution, and phosphates or phosphoric

acid-rich solution.

Reusable scarce and abundant heavy metals, for example,

copper, gold, silver, zinc and cadmium may be present in

the waste-water generated from electroplating. CDI

systems, assembled with modified electrodes

(functionalized for enhancing the selectivity towards the

target ions/ resources can be effective, and therefore,

several studies have been performed recently for

reviewing the efficacy of capacitive deionisation systems

for recovering heavy metals via electrochemical redox

process [203]. In electroplating industries, the recovery of

these metals is being carried out via electrowinning

method. In this method, the ion transport mechanism is

similar to the CDI; however, after their adsorption on the

cathode, the metal ions are reduced and deposited as the

solid metal at the cathode surface and the remaining

dissolved species or water is oxidized at anode. For

example, in case of zinc recovery,

cathodic reaction is: Zn

+ ne

–

→ Zn(s)

and reaction at anode is: 2H

O →O

+ 4H

+ 4e

–

In case of a waste-water polluted with multiple metal

ions, metal ions with more positive electrode potential

will absorb and reduce first, and will separate first from

the solution than other metal ions.

Among different metals, recovery of copper using

electrochemical reduction and electrodeposition is very

common. Direct electrochemical reduction has been used

in several studies using different synthetic electrodes with

similar or separate electrode assembly and electrode

design confirming its high efficiency towards copper

removal and recover; for example, electrochemical

assembly with Pb/PbO

electrodes at both anode and

cathode showed copper deposition with 52–98% current

density [204], with RuO

/TiO

DSA plate anode and

stainless-steel 316-based electrode as cathode showed up

to 85% and 60% recovery in potentiostatic and

galvanostatic experiments, respectively [205], with

IrO

−Ta

/Ti electrode as anode and stainless-steel as

cathode showed copper deposition with 90.3% current

density [206], with IrO

−Ta

/Ti electrode as anode and

stainless-steel cathode showed 98.3% copper recovery

and 93.2% tellurium recovery with ~85% current

efficiency [207]. In few studies, recovery of other metals

such as silver (more than 99%) [208], uranium (more

than 98%) [209]. Among different electrochemical

reduction-based method, modified-electrodeposition

methods are widely used to recover different metals from

waste-water streams. For example, electrooxidation-

integrated electrodeposition for nickel recovery [210];

integrated electrodeposition for copper recovery [211];

BES assisted electrodeposition for copper recovery [212,

213], zinc recovery [214], silver recovery [215], and

simultaneous recovery of zinc copper and cadmium

[216]; electrochemical-osmotic system assisted

electrodeposition to recover copper and other metals

[217] have been successfully used in different studies.

Unlike electroplating-based waste-water and industrial

waste-water streams rich with heavy metal ions, other

industrial waste-water streams contain a number of

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pollutants as and impurities. So, in industrial waste-water,

heavy metal ions commonly co-exist with different

impurities some of which are also chelating agents (for

example, EDTA, oxalate, citrate, etc.). Because of the

formation of chelating complex between the heavy metal

ions and these ligands, recovery of heavy metal ions from

industrial waste-water is difficult via electro-deposition

discussed above. However, integrated with suitable

separation technique(s) such as advanced oxidation

processes, thermal decomposition, photo-electrocatalysis

etc. the heavy metal ions can be released for its separation

via electrowinning [218]. Sometimes the presence of

other metal ions as the impurity helps to reduce the

energy consumption of the separation as well as recovery

process. For example, presence of iron ions in the waste-

water streams lowers the specific energy required for

recovering copper [219]. However, recovery of Cr(VI)

using electrowinning is a very challenging task because

of its high negative reduction potential (-1.586 vs SCE).

Similar problem has also been observed for other metals

with similar characteristics.

Sulfur and its derivatives, which generally enter and exist

in the environment in the form of sulfate and sulfide are

corrosive in nature, produce unpleasant odour and toxic

to aquatic lives [220, 221]. These also cause several

harmful effects to human beings. However, there is a

huge demand of sulfur and sulfur-based compounds in

fertilizer market and in different industries. Also, S(0) is a

crucial components of Li-batteries because of its potential

suitability as cathode materials [222, 223] which

increased the market value and demand of sulfur world

wise (additional demand of ~70 million tons per annum

zero-valent sulfur as cathode material) [224]. Therefore, a

maximum recovery of the sulfur element is necessary to

minimise the searching and exploration of new resources

in view of circular economy. Direct electrochemical

oxidation or electrochemical reduction-coupled EO of

sufide (-SH) or sulphate (SO

) to convert to S(0) (based

on the electrochemical activity) is commonly used for the

recovery and removal of sulphide from waste-water [225-

227]. Dutta et al. (2010) reported a decrease in sulfide-S

concentration from 44±7 mg L

−1

to 8±2 mg L

−1

and more

than 60% sulfur recovery [228] via direct oxidation

carried out in a double-chamber electrochemical cell. It is

also observed that the recovery process of sulfur as S(0)

can cause S(0) deposit at the anode surface leading to

anode passiveness [229, 230]. This can be avoided by

forming a biofilm at the anode surface or by switching

the anode and cathode during the operation on periodical

basis [231]. Liquid redox sulfur recover process is also

found to be promising one involving the following two

steps: (i) sulfide and an intermediate (in the oxidized

form) reacted with each other to S0 (solid), and (ii) re-

oxidation of the reduced intermediate [232, 233].

Considering the above points, Zhai et al. (2012) reported

a fuel cell-assisted iron redox apparatus for sulfur

recovery where fuel cell was used to regenerate Fe(III).

The recovery efficiency observed is 78.6±8.3% [234].

Selvaraj et al. (2016) reported an electrochemical

membrane-based separation process using flattened or

standard titanium mesh coated with Ti/TiO

–RuO

–IrO

as anode material and Ti as cathode which can recover

~78% of sulfur [235]. Using a MEC integrated with an

electrochemical deposition reactor and a novel boost

circuit, 46.5±1.5% of elemental S-recovery was reported

without any net energy intake [236]. Ntagia et al. (2019)

carried out the sulfur recovery experiments with different

anode: Ir-MMO, Ru-MMO, TiO

/IrTaO

, Pt, Pt/IrOx and

PbOx; and reported that Ru MMO is the most active

(coulombic efficiency: 63.2± 0.5%) for sulphide

oxidation whereas Ir MMO is the maximum stable among

the six tested anodes [225]. Integrated bio-

electrochemical reactors also tested for the elemental S-

recovery [235, 237]. With the Ti/TiO

–RuO

–IrO

-coated

titanium mesh anode and titanium mesh cathode, 70% of

elemental sulfur (purity of 100%) was recovered in an

anaerobic biological reactor [235]. A resource recovery

microbial fuel cell (RRMFC) is also reported showing a

59% sulphate recovery as the concentrated solution

starting from fresh synthetic urine [238].

During the production of oil and gas, brine solution

including produced and flow-back water is produced

which contains a very high bromide ion concentration (~1

g L

-1

) along with chloride (up to 200 g L

-1

) [239].

Bromine- and its derivative-based chemicals have high

importance also in pharmaceutical and agricultural

chemical producing industries [240]. These bromine and

brominated by-products have adverse effect on human

health, and therefore the recovery of such substances is

important. This also helps to reuse and recycling the

bromine element which is a key step towards the

implementation of circular economy. The reduction

potential difference between bromine and chlorine (Cl

(aq)/Cl

‒

: +1.36 V, Br

(aq)/Br

‒

: +1.09 V (vs. SHE)) [241]

can be exploited for the recovery of bromine. Sun et al.

(2013) designed and reported an electrolyzer which was

successfully used for bromine recovery by oxidizing

bromide to bromine. A stripping unit was used to recover

the produced bromine with air [239].

4.3 Electrochemical-stripping for mining waste-water

Electrochemical-stripping techniques, with or without

integrating other suitable units has been extensively used

the recovery of different resources from the waste-water

generating from diverse sources. Electrochemical-

stripping has several advantages such as multi-analyte

capability, low instrumentation cost, consumables

required in small quantity, low input energy process,

potential for on-site analysis, speciation capability high

sensitivity and low detection limit, and scope for indirect

bio-sensing [242]. The method is a combination of

electrodialysis modified with stripping (either membrane

or acid stripping). In this process, a pre-concentration

step of the target molecules/substances is coupled with a

stripping technique. The pre-concentration step is

operated and controlled by a suitable electrode (working).

The concentrated solution is then used for stripping

purposes electrochemically [242]. Tarpeh et al. (2018)

and Liu et al. (2020) reported a 93% and greater than

63% N-recovery efficiency, respectively in their studies

[243, 244]. The experiments were carried out in a three-

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chamber parallel plate reactor. CEM was used to separate

anode and cathode. However, different membranes were

used to separate the cathode and the trap chamber:

microporus polypropylene membrane [73] and gas

permeable membrane [244].

Based on the mechanism involved, this method is found

to be useful for the N-nutrient recovery as the

ammonium, and thus used in few studies. Coupling with

acid adsorption, electrochemical-stripping has been

successfully used to recover N-nutrient as reported in

different studies. Desloover et al. (2012) and Luther et al.

(2015) used a double-chamber electrochemical cell (with

a Ir-coated Ti anode and stainless-steel cathode)

separated by a CEM for N-nutrient recovery, and reported

the 96% charge transfer efficiency for ammonium with

120 g N m

−2

−1

flux [69] and 57±0.5% N-nutrient

recovery as ammonium sulphate from urine [73]. A

similar study, performed with hydrophilic nickel in the

upmost layer and gas-stripping membrane, showed a 40%

increase in ammonia recovery rate and 20% decrease in

energy consumption [245]. Arredondo et al. (2017)

carried out similar experiments in a double-chamber

electrochemical cell (with a set of Pt-coated Ti as both

anode and cathode) coupling electrochemical-stripping,

TMCS module and acid adsorption, and reported ~100%

ammonium recovery with 433 g N m

−2

−1

flux [246].

Kuntke et al. (2016) reported a MEC composed with four

pairs of anode and cathode which was followed by

assembling degassing vessel, TMCS module and acid

absorption system. The study showed 95% N-nutrient

recovery as ammonium [247].

4.4 Electrochemically induced precipitation

Similar to the applicability of electrochemical redox

processes (with or w/o integration with other techniques)

for scarce and abundant heavy metals recovery,

electrochemically induced precipitation is found to be

promising for P-nutrient recovery in the form of

phosphate and simultaneous P- and N-nutrients recovery

as struvite. Therefore, this technique modified with some

other methods has been widely used for P-nutrient as well

as struvite recovery. In this process, suitable dissolved

substances present in waste-water can undergo chemical

reaction and form some insoluble precipitates when an

external potential bias is applied. Because of the applied

bias, water splitting can be occurred generating hydroxide

ions which are essential for the precipitation. The thus

formed precipitates can be separated out from the waste-

water.

Recovery of P-nutrient has been extensively carried out

from the waste-water generated from different streams

using the electrochemically induced precipitation method

as reported in different literature. Mostly double

chambered electrochemical cells where the compartments

are separated by a CEM are used in this purpose. Either

platinum (Pt) or modified-Pt electrode has been used as

anode. Electrodes prepared from different electrode

materials have been used as cathode to ensure the

selectivity and performance of the recovery process. For

example, reported 70-95% phosphate recovery from

municipal waste-water using steel plate as cathode [248],

Lei et al. (2018) reported a maximum of 58.5±1.2% P

recovery in the presence of 1.0 mg L

-1

natural organic

matter using a Ru-Ir/Ti as anode and a Ti plate as cathode

[249], Lei et al. (2019c) reported a maximum of 92% P

recovery using a Pt- coated titanium (Ti) as anode and a

Ti plate as cathode [249] and Perera et al. (2020) showed

more than 94% P recovery from septic tank effluent in a

3-compartment reactor using isomolded graphite plates as

both cathode and anode [250] as the calcium phosphate.

The effect of different parameters such as distance

between the electrodes, pH, electrolyte etc. on P-recovery

as calcium phosphate via electrochemically induced

precipitation was also studied [249, 250, 252-254].

Recovery of P-nutrient along with N-nutrient as struvite

was also reported in several studies. Wang et al. (2019a,

2019b) reported a study showing successful recovery of

P-nutrient as struvite in different studies: 99.51 % [255]

and 97.69% after dosing plant ash and magnesium metal

[256] from actual swine waste-water and Cid et al. (2018)

reported ~80% P-nutrient recovery as hydroxyapatite

[257]. MEC assisted precipitation was also reported in

few studies and the methods are found to be promising

showing a P-recovery: 20.1±1.5% to 73.9±3.7% as

calcium phosphate [258] and 70-85% as struvite [259]. A

MAP precipitation process using an electrochemical

precipitation process integrated with recycling technology

was also reported for the simultaneous recovery of

ammonium and phosphate as struvite [260]. Recovery

and removal efficiency was reported as ~99% for P-

nutrient with 2 mA cm

−2

current density and >90% of

ammonia. Precipitation-based P-nutrient recovery using

other electrochemical set-up has also been reported with

promising outcomes, for example, more than 99% P-

recovery as struvite with recovery rate 321.18 mg-P L

−1

using a single-chamber Mg-air fuel cell [261], 59.6%

hypophosphite recovery as ferric phosphate using a

electrofenton catalysed ferric phosphate precipitation

[262] and 8-56% P-dissolution efficiency using a MEC or

MFC-based electro-fermentation [263].

In addition to this, Perera and Engleherdt (2020) reported

an electrohydromodulation reactor by coupling the

electrochemically-induced precipitation of calcium

phosphate with NH

-stripping for the simultaneous

recovery of P- and N-nutrients. An

electrohydromodulation unit is assembled with a calcium

phosphate precipitation tank followed by an ammonia

stripping unit. The authors reported ~ 89% N-nutrient and

~97% P-nutrient recovery, and an energy consumption of

1.21 kWh m

−3

[264].

Rare earth metals are mixed into the waste-water streams

from the industrial waste coming with waste generated

during the mining of rare earth elements, coal mine

discharge, acid mine drainage water, industrial waste etc.

and has adverse effect on the environment. These have

several uses in electronics materials, permanent magnets,

and catalysis [265], and therefore, their recovery from the

waste materials, waste-water streams, used electronics

and other consumer products is important to reduce the

searching and exploration of new mineral resources.

However, these metals are present in low concentrations

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(less than 80 nmol L

-1

) [266] as compared to other heavy

metallic species such as copper-, nickel-, arsenic- and

chromium-based pollutants. These metal species can be

captured by the hydroxide ions as metal hydroxides

which can undergo dehydration to form their stable metal

oxides. Considering the above mechanisms, water

splitting and oxygen reduction reaction, O’Connor et al.

(2018) reported a study where CNT-based filters were

used to capture Eu, Ga, Nd, and Sc as their oxides via

electrochemically induced precipitation method [267].

CNT has been chosen for its high electrical conductivity,

high porous surface area and capability to capture rare

earth metallic species even at low concentration.

Selective separation of heavy metals also shown in this

study for Eu and Cu using a two-stage filter system with

variable voltages based on the reduction potentials.

4.5 Electrocoagulation

Electrocoagulation is widely used for the treatment of

inorganic, organic, and pathogenic contaminants. The

method is applicable to treat urban, domestic and

municipal waste-waters, sea-water, surface water and

others [268]. In this process, a metal is added to the

waste-water under treatment to form in situ metal oxides

electrochemically [268]. To do so, direct current is

applied on the electrodes dipped into the electrolytes. The

thus formed metal oxides are destabilized and aggregate

precipitates and particles. These also adsorb the

contaminants present in the solution in dissolved state

(Fig. 5). Earlier, phosphorus was recovered via

electrocoagulation (EC) using Mg, Al ,and Fe electrodes

[269-272]. Reilly et al. (2021) showed a recovery of 22.4

mg-P g-Fe

−1

by metal dosing (Fe) for the

electrocoagulation of P- and N-nutrient in food waste,

however, ammonium ion concentration was not affected

during EC treatment [273]. Xu et al. (2002) reported a

recovery of by-products from simulated egg processing

waste-water, egg processing plant waste-water (EPW),

EPW with carboxymethylcellulose (50 mg L

-1

added) and

EPW with bentonite (200 mg L

-1

added) using

electrocoagulation. The authors also showed that different

amino acids: such as threonine, valine, leucine,

isoleucine, phenylalanine, and lysine can be recovered

with similar concentrations in which these are present in

liquid whole egg [274].

Recovery of various heavy metals from the

electrocoagulation sludge can be done by integrating

chemical leaching, thermal process, or other suitable

process [268]. García-Carrillo et al. (2019) used Al

electrode in their study to recover gold and silver via

electrocoagulation method [275]. With the polarity

reversal in every minute, a recovery of 99.73% for silver

(383 mg L

−1

, as initial concentration) and 98.59% for

gold (49.48 mg L

−1

, as initial concentration) was

observed [276]. Uranium removal and recovery

(~89.71%) using an algerin S and a Fe anode by

electrocoagulation method was also reported [277].

Gajda et al. (2017) showed a high percentage of heavy

metals (Fe, Cu, Zn) recovery in a microbial fuel cell

(MFC) via electrocoagulation in their study (performed

with synthetic fresh urine and hydrolysed urine) [278].

Metal can also be recovered in its hydroxide form.

Hydrogen recovery using the electrocoagulation method

has also been reported from a dye containing waste-water

[279].

Figure 5. Schematic representation of electrocoagulation.

4.6 Electrolysis / Microbial Electrolysis

Bioelectrochemical systems (BES) is the one of the

newest and promising bioenergy technology for the

simultaneous waste-water recovery and energy

production which can also facilitate recovery of various

resources from the waste-water [280-286]. Among the

two type BES, microbial electrolysis cell (MES) deals

with hydrogen energy production via an external electric

supply [283, 287]. According to the present status, MFC

(the most popular BES) is uncompetitive in comparison

with other energy sources (based on the economic and

environmental values for electricity). Therefore, the

scope of MFCs is broadened for different value-added

applications, such as hydrogen production by MECs [Fig.

6]. MECs have several advantages: such as production of

hydrogen from various organic substances [288-291], the

dark fermentation by-products [288, 290], and a relatively

low energy input (0.2 - 0.8 eV) as compared to other

biological hydrogen production processes [292].

Bioelectrochemical reactors were designed and reported

for recovery of different nutrients recovery [293] and

ammonia recovery [74] successfully.

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Figure 6. Schematic representation of microbial

electrolysis cell.

Using a stainless-steel plate cathode and Ti/RuO

–IrO

–

TiO

–SnO

anode in an electrolysis cell, the study

showed a 53% potassium recovery and ~99% phosphate

recovery [294]. In their study, Li et al. (2019) reported a

cation-exchange electrolysis process integrated with

crystallization process for magnesium potassium

phosphate (MgKPO

) to recover P-nutrient as MgKPO

A study designed and performed with four parallel frame-

based BES-ECC reactor with an abiotic anode, a

biocathode (to reduce autotrophic sulfate), an anode for

ECC (to oxidize sulfide to S0, partially), and an abiotic

cathode for ECC reported a 92.9±1.9% of sulfate was

removal with low specific energy consumption

(9.18±0.80 kWh kg S

−1

) [295]. Wan et al. (2020),

coupling bioelectrochemical reduction with microbial

electrolysis for dissimilaratory nitrate reduction to

ammonia (DNRA), reported ~44% DNRA efficiency and

a stable ammonia recovery in their study [296]. Microbial

electrolysis, integrated with anaerobic membrane

bioreactors showed a ~56% enhanced methane yield as

compared to anaerobic membrane reactors [297]. Lei et

al. (2018) carried out a study to investigate the sequence

of precipitation during electrolysis of municipal waste-

water with a focus on phosphate recovery [298]. The

study reported that low Ca/P molar ratio, amorphous

calcium phosphate precipitation is preferred over calcite

and at high Ca/P molar ratio, reverse phenomena was

observed. The study also reported that current density and

surface area of the electrode are the two important

parameters. Current density was observed to affect the Ca

and Mg removal more as compared to cathodic surface

area; whereas for P, reverse phenomena was observed.

The study also revealed that although there is no

sequence in the amorphous calcium phosphate, calcite

and brucite, precipitation can be influenced by targeting

P-rich waste-water, low current density, and high

cathodic surface area.

4.7 Microbial desalination cells

Among the several other electrochemical processes used

in different waste-water treatment plants for different

purposes, microbial desalination unit has been

extensively used. Therefore, microbial desalination unit

has been used in some studies for investigating its

suitability in recovering nutrients from waste-water. Chen

et al. (2017) reported a stacked microbial nutrient

recovery cell consisting three chambers: one for cathode,

one for anode, and a staked chamber for nutrients

recovery (insulated by three pairs of IEMs). Synthetic

urine was used as the electrolyte and 76–87% N-nutrient

and 72–93% P-nutrients recovery was reported [299].

Gao et al. (2018) reported a microbial desalination cell of

seven chambers: one for anode, one for cathode chamber,

two chambers for dilution and three chambers to recover

P-and N-based concentrated nutrient solutions

simultaneously. All chambers were separated from others

by IEM. The study reported ~73.1% N-nutrient and

86.2% P-nutrient recovery when used for source-

separated synthetic fresh urine [300]. Lu et al. (2019)

reported a resource recovery RRMFC for recovering total

nitrogen and phosphates. The study showed ~42% of total

N and ~37% of PO

recovery when tested with synthetic

fresh urine [301]. Li et al. (2020) reported a microbial

electrolysis desalination cell as an energy efficient

technology which can simultaneously recover P- and N-

nutrient with 66±5.3%c and 66.7±4.7% recovery

efficiency, respectively [302].

5. Conclusions and future outlook

The aim of this review is to demonstrate different

resources management techniques, their advantages,

operational constraints, and functional challenges in view

of implementing circular economy. Achieving the

environmental sustainability goals is one of the key steps

among the major steps which can facilitate the

implementation of circular economy. Therefore, the idea

of this perspective is to investigate about the applicability

of circular economy over linear economy due to the

exponentially growing deficiency of useful nutrients and

important natural resources, and elemental scarcity

considering the presence resources consumption rates,

elemental abundance, and low reusability and recovery.

Similar to other natural resources, a circular economy has

been tried to apply for water which is an essential natural

resource from last three decades by reclaiming and

reusing the waste-water. To do so, waste-water treatments

facilities has been applied all around the globe including

the regions where no water scarcity is projected to make

positive impacts on environmental reclamation.

Reclamation of the different nutrient, natural and

synthetic resources, heavy metals, scarce elements and

others has been performed for their recovery and

reusability from waste-waters generating from diverse

sources in addition to energy recovery, to reduce their

deficiency due to increased demand and high

consumption rate. This also facilitates the maximum

energy recovery from the waste-water by reclaiming the

energy present in the resource-composites present in

waste-water. These integrated nutrients/ resources

recovery techniques with the energy recovery processes

have been widely implemented in current-generation

waste-water treatment plants although the focus is to

recover various nutrients, value-added products, heavy

metals, and other resources along with maximum energy

generation. The sewage sludge can be used as the

platform for new products such as bioplastic, construction

materials and different types of adsorbents. Therefore,

this review will help the society, policy-makers, scientific

community, industrialists, and national resource

regulatory bodies to rethink about the waste-water

streams and the quality of the effluents to be released;

and to redefine waste-water streams as the “Waste-water

resources for nutrients and value-added products” with

remarkable economic and environment impacts.

Moreover, in this review, several existing separation

techniques were discussed based on SWOT analysis

(Strength, Weakness, Opportunity, and Threat) for

achieving for moving towards the circular economy from

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the existing linear economy and mixed economy.

Advantages of these methods with operational constraints

and inevitable challenges for their application in nutrients

and resources recovery are highlighted. New generation

separation techniques and electrochemical techniques,

with or without integration with existing and potentially

suitable separation techniques, applicable for the nutrients

and resources recovery are demonstrated with suitable

examples and case studies. Most of these techniques are

helpful to move towards green economy also. Therefore,

an improved mind-set with appropriate government

policies and commitments of private and government

companies/ agencies can be helpful to achieve the goals

related to environmental sustainability and to implement

circular economy.

Acknowledgement

The author with to acknowledge Munition India Limited,

Directorate of Ordnance (C&S), Ministry of Defence for

their support to carry out this study.

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