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Environment, Development and Sustainability

https://doi.org/10.1007/s10668-020-01170-6

Treatment of digestate from swine sludge continuous stirred


tank reactor to reduce total carbon and total solids content

A. Chini1   · C. E. Hollas1   · A. C. Bolsan2   · F. G. Antes3   · H. Treichel4   ·


A. Kunz1,3,4 

Received: 3 September 2019 / Accepted: 16 December 2020


© The Author(s), under exclusive licence to Springer Nature B.V. part of Springer Nature 2021

Abstract
Anaerobic digestion is a biological process that can partially convert organic matter into
gases with potential to energy generation. However, in case of continuous stirred tank reac-
tor (CSTR) for the treatment of sludge from swine manure, a digestate with a high concen-
tration of solids, undigested carbon, nitrogen and phosphorus is usually obtained, which
can limit the  direct application to the soil or other direct uses or disposal. Therefore, an
additional treatment of digestate is still needed to meet environmental requirements for the
viability of an anaerobic digestion plant to enable the disposal of the  liquid effluent. In
this study, solid-liquid separation (SLS) strategies were studied for treatment of digestate
from swine sludge CSTR biodigester. The following processes were tested: settling, cen-
trifugation and chemical flocculation.The performance of each process was evaluated by
monitoring the concentrations of the following parameters in the raw digestate and after
treatment: total carbon (TC), phosphorus, total kjeldahl nitrogen, ammonia nitrogen, total
solids (TS), volatile solids and fixed solids. The factorial design was used for the optimiza-
tion of  centrifugation and chemical flocculation tests. Total carbon, solids and phospho-
rus were significantly reduced from digestate using the different SLS processes. How-
ever, higher removal efficiencies were obtained by centrifugation, being more expressive
to phosphorus, TC and TS (reduction of 95, 90 and 83%, respectively). Furthermore, the
sludge production by centrifugation was 3.8 and 7.3 times lower than by settling and chem-
ical flocculation, respectively. Thus, centrifugation could be considered the most appropri-
ate SLS process to enable digestate treatment and the liquid efluent is suitable to be treated
by deammonification process for nitrogen removal.

Keywords  Centrifugation · Chemical flocculation · Settling · Swine manure · Wastewater


treatment

* A. Kunz
airton.kunz@embrapa.br
Extended author information available on the last page of the article

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A. Chini et al.

1 Introduction

Anaerobic digestion (AD) gained prominence due to the possibility to convert organic
matter partially into gases which can be utilized for energy generation, reducing gaseous
emissions and replacing the use of fossil fuels. Additionally, the liquid fraction obtained
(digestate) is a plant nutrient-rich residue (Tápparo et al. 2020; Baranpouti et al. 2020).
This progress is justified due to the versatility of the feedstock for AD process. Many
different types of organic material are suitable such as livestock manure, lignocellulosic
biomass (crop residues), food waste, waste activated sludge, organic municipal waste,
fruit and vegetable waste and industrial waste (Gaspareto et al. 2020 ).
The digestate composition can change according to the substrates used for diges-
tion and the reactor type (Tápparo et al. 2018; Gaspareto et al. 2020; Baranpouti et al.
2020). The most usual reactor type for AD is a continuous stirred tank reactor (CSTR),
which is proper to digest a high-solid concentration substrate (Amaral et al. 2016 ). In
general, AD generates a digestate rich in nutrients such as ammonium and phosphorus
(Suzin et al. 2018), solids (Jørgensen and Jensen 2009; Gaspareto et al. 2020) and other
compounds (Tápparo et al. 2020). These characteristics confer to digestate a high agro-
nomic potential, making possible its use as fertilizer on arable land. However, despite
AD advantages, the increase in biogas production in some areas could generate a higher
digestate amount than the fertilization requirements due to nutrients overload in soil
(Magrí et al. 2017; Díaz-Vázquez et al. 2020). The digestate transport to other regions
with deficiency in nutrients is usually not attractive due to the inherent costs.
Transportation costs could be reduced by digestate separation into a solid and a liq-
uid fraction (Jørgensen and Jensen 2009), so it is a much smaller volume to be trans-
ported from one farm to another. To this end, there are different solid–liquid separation
(SLS) processes, for instance, mechanical screen separators, settling, centrifugation,
reverse osmosis, electrocoagulation and chemical flocculation (Mores et al. 2016; Akh-
iar et  al. 2017; Hollas et  al. 2019), flocculation aid (Kooijman et  al. 2017) and others
(Wang et al. 2020).
The total cost of SLS processes is crucial to define the kind of treatment to be
employed. Settling, chemical flocculation, mechanical screen separation and centrifuga-
tion are simple processes that are considered cost effective (Tambone et al. 2017), while
evaporation, ultrafiltration and reverse osmosis are complex and more expensive pro-
cesses (Kooijman et al. 2017). These devices present different efficiencies in separation
of solids from the liquid fraction (Jørgensen and Jensen 2009; Hollas et  al. 2019) and
there are several studies dealing about their use in wastewater treatments (Amaral et al.
2016; Hollas et al. 2019; Chini et al. 2020).
The solid fraction generated in the SLS processes has gained more interest in research
and development and there are different ways to give it a destination: composting or direct
application as organic fertilizer (Li et al. 2020b), biochar production (Li et al. 2020a), bio-
fuel production and other routes for solid fraction valorization (Tambone et al. 2017; Gas-
pareto et  al. 2020). The liquid fraction can be used to irrigate fields or also post-treated
according to its characteristics (Magrí et  al. 2017; Hollas et  al. 2019; Chini et  al. 2020)
that in general contain low biogas potential, but with high concentration of total nitrogen,
ammonia nitrogen (Chini et al. 2020) and phosphorus (Fernandes et al. 2012; Suzin et al.
2018). Thus, high nutrient concentration can limit the application straight to the soil, due
to soil and water contamination (Díaz-Vázquez et  al. 2020). Therefore, it is necessary to
implement a treatment system to reduce the pollutant potential of this waste.

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The removal of nitrogen from digestate by the deammonification process is increasing


worldwide (Feng et al. 2017; Chini et al. 2019, 2020), and this process is being studied as
an alternative technology to other conventional options (Hollas et al. 2019). The application
of this treatment to the digestate seems to be a promising alternative due to the relatively
lower energy consumption and low sludge production compared to conventional nitrogen
removal processes (Miao et al. 2018). Nevertheless, the direct treatment of digestate rich
in solids and with high-organic carbon concentration can be deleterious to anammox pro-
cess (Feng et al. 2017; Chini et al. 2020). Chini et al. (Chini et al. 2019) investigated the
interference of total organic carbon (TOC) in the deammonification process (partial nitri-
tation and anammox) in a bioreactor fed with digestate from a CSTR biodigester treating
swine sludge. Samples were previously centrifuged for TOC and solids removal. Authors
observed that nitrogen removal efficiency decreased 22% when the TOC concentration
increased from 156 ± 8 to 255 ± 4 mg  L−1. These finding highlight the importance of using
an efficient pre-treatment technique previous to a deammonification process to digestate
treatment, especially in case of effluent from a CSTR biodigester.
To overcome this drawback, a pre-treatment step using SLS could be introduced to pro-
duce a wastewater suitable for treatment using deammonification. However, just few stud-
ies investigate the best SLS process employed to the digestate that came from a CSTR
(Akhiar et al. 2017; Hollas et al. 2019) in order to make possible the nitrogen removal from
the liquid fraction. Despite this, a comparison of SLS processes applied to a digestate with
similar characteristics was not systematically studied.
The reduction of total solids, total carbon, phosphorus and even nitrogen in digestate
from a swine sludge CSTR biodigester could improve the performance of nutrient removal
processes and also reduce treatment costs. Therefore, the aim of this study was to opti-
mize and compare the following SLS processes to a CSTR treating swine sludge digestate:
settling, centrifugation and chemical flocculation. The optimization of the conditions used
for each process were performed looking for a liquid fraction that could be treated by an
advanced nitrogen removal process like deammonification, i.e., with low concentration of
total solids, carbon and phosphorus. These SLS techniques were chosen because among
the options available, settling is the simplest process, while centrifugation and chemical
flocculation have higher cost.

2 Material and methods

2.1 Digestate collection

Raw digestate was sampled from a CSTR digester operating at mesophilic condition (37º
C), treating solid waste from a swine manure treatment system on a farm in Videira, Santa
Catarina, Brazil (27º02′38.8″S 51º05′35.7″W). The CSTR was fed at a flow rate of 21 ­m3
­d−1 and hydraulic retention time (HRT) of 32 days. A total volume of 200 L of digestate
was randomly sampled. Digestate was homogenized in a tank and then fractionated for
SLS experiments.

2.2 Experimental procedure

Three SLS processes were tested: settling, centrifugation and chemical flocculation. The
experiments were carried out at Embrapa Suínos e Aves laboratory, Santa Catarina, Brazil.

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A. Chini et al.

Settling tests were conducted in a conic settler (1 L) (in triplicate), and data were col-
lected at intervals of 30 min for 3 h. Centrifugation tests were done in a centrifuge model
4–16 K (Sigma, Osterode am Harz, Germany) using 250 mL tubes. For chemical floccula-
tion, a 10% (v v­ −1) aqueous solution of polyphenolic organic polymer (Veta Organic®,
Brazilian Wattle Extracts, Brazil) commercially available in liquid form containing 30%
tannic acid (flavan 3.4-diol) was used as coagulant. The coagulant dilution was done in
water under vigorous shaking for 15  min. As a coagulation aid, 0.01% (w v­ −1) aqueous
solution of polyacrylamide (Activator Q®, Brazilian Wattle Extracts, Brazil), commer-
cially available in granular form was employed. These solutions were prepared prior to use,
thus avoiding their degradation and efficiency loss in the different tests. Experiments were
performed using a jar-test apparatus model JT102/3 (Milan, Colombo, Brazil). For each
individual test, 1 L of effluent was used and all tests were performed in triplicate.

2.3 Experimental design and statistical analysis

For the evaluation of solid–liquid separation processes, different experimental designs were
applied to establish the best condition of each one. Thus, to settling tests the volume of set-
tled sludge during three hours was evaluated. To centrifugation test, a central composite
rotatable design (CCRD) 2­ 2 was selected to evaluate the variables of centrifugation time
­(Ctime) (5.9, 10, 20, 30 and 34 min) and gravitational force (­ gforce) (80, 250, 1400, 2900 and
3800 g). The central point to centrifugation was based in previous data from Popovic et al.
(2017).
A factorial design 2­ 2 was selected to understand how the independent variables tan-
nin (TA) volumes (25, 50 and 75 mL L ­ −1) and polyacrylamide (PAM) volumes (5, 10 and
−1
15  mL ­L ) would influence the chemical flocculation of digestate. The initial polymer
amount was defined based on concentrations described by of Van Nieuwenhuijzen and Van
der Graaf (2012).
All the experimental data were statistically evaluated by StatSoft’s Statistica 5.0 soft-
ware, at a confidence level of 95%. The statistical significance of the models was justified
by variance analysis (ANOVA) for the polynomial model with a significance level of 95%
(p < 0.05) and the veracity of polynomial model was expressed by the determination of
coefficient ­R2 (Rodrigues and Lemma 2014). All analytical parameters were determined at
least in triplicate.

2.4 Analytical methods

The processes performance was assessed through the responses of the following physico-
chemical parameters: total carbon (TC), phosphorous (P), total kjeldahl nitrogen (TKN),
total ammonia nitrogen (TAN, expressed as N­ H3-N), total solids (TS), volatile solids (VS),
fixed solids (FS) and pH.
Total carbon was measured by CNHS elemental analyzer model Flash 2000 (Thermo
Fisher Scientific, Waltham, EUA) following the manufacturer recommendations. Briefly,
samples were previously dried at 105 °C and an among 10–20 mg were weighted for direct
analysis. Phosphorus was determined by the spectrophotometric molybdovanadate method
using a spectrophotometer Cary 50 (Agilent, Santa Clara USA). TKN was determined by
using the kjeldahl method on a digester and distillation unit model Kjeltec 8100 (Foss,
Hilleroed, Denmark), while TAN was measured by titration method after distillation on
the same unit than TKN. For TS, VS and FS determination samples were dried at 105

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Treatment of digestate from swine sludge continuous stirred…

ºC and after calcined at 550 ºC. pH was measured by a portable probe meter model HI
98,140 (Hanna Instruments, Woonsocket, USA). All these parameters were analyzed using
methods described on standard methods for analysis of water and wastewater (Rice et al.
2017), and all analyses were performed at least in triplicate following standardized proto-
cols based on good laboratory practices and quality assurance policy. Total organic carbon
(TOC) on digestate was determined using a TOC analyzer model TOC-LCPH/CPN (Shi-
madzu, Kyoto, Japan) equipped with an autosampler following the manufacturer recom-
mendations. Briefly, calibration curve in the range of 10 to 100 mg ­L−1 was constructed
using standards obtained by serial dilution of a 1000 mg L ­ −1 of TOC stock standard solu-
tion. Samples were diluted to fit the analytical range of calibration curve and the respective
dilution factor was included for results processing. The equipment used enable the intro-
duction of samples with suspended particles up to 800 µm. Therefore, it was possible to
analyze all samples without previous filtration.
The removal efficiency of chemical parameters was calculated by Eq. (1).
C0 − Ct
Efficiency (%) = × 100 (1)
C0

where ­C0 is the initial concentration, and ­Ct is the final concentration of the constituents.
A flowchart summarizing the experimental sequence adopted in this study is shown in
Fig. 1.

3 Results and discussion

3.1 Digestate characterization

Physico-chemical characteristics of digestate used in this study were (average ± stand-


­ −1, VS 13.5 ± 0.19 g L
ard deviation): TS 21.8 ± 0.33 g L ­ −1, TC 6.7 ± 0.11 g L
­ −1, TOC

Raw
digestate

Solid-Liquid
Separation

Settling: Centrifugation: Chemical flocculation:


1L conic settler Time: 5.9, 10, 20, 30 and 34 min; Tannin: 25, 50 and 75 mL L-1
(triplicate) per 3 h Gravitational force: 80, 250, 1400, Polyacrylamide: 5, 10 and 15 mL L-1
2900 and 3800 g

Solid fraction Liquid fraction Solid fraction Liquid fraction Solid fraction Liquid fraction

Characterization: TC, P, TKN,


TAN,TS, VS, FS and pH

Fig. 1  Flowchart of experimental sequence followed on this study

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A. Chini et al.

1.6 ± 0.1  g ­L−1 P 0.97 ± 0.04  g ­L−1, TAN 2.00 ± 0.03  g ­L−1, TKN 2.60 ± 0.01  g ­L−1,
alkalinity 9.57 ± 0.02  g ­CaCO3 ­L−1 and pH of 7.79 ± 0.01. The results highlight the
high concentration of nutrients which make the direct disposal of this waste impossible.
Additionally, the high TC, TOC and TS avoid the direct feeding of a deammonification
reactor for nitrogen removal (Chini et al. 2019). The digestate used in the present study
showed typical characteristics of waste from anaerobic digestion process in a CSTR
reactor (Amaral et al. 2016; Baranpouti et al. 2020). It is difficult to establish a compari-
son between digestate from different CSTR systems because of the high variability of
digestate characteristics. This happens due to different waste used in anaerobic digestion
and operational parameters, as hydraulic retention time, temperature and organic load-
ing rate (Amaral et  al. 2016; Akhiar et  al. 2017). Digestates usually contain abundant
TAN and TKN in ranges from 0.14 to 3.5 g ­L−1, phosphorous from 0.007 to 0.4 g ­L−1
and chemical oxygen demand (COD) from 0.2 to 6.9 g ­L−1 (Svehla et al. 2017; Lu et al.
2018; Baranpouti et al. 2020). Moreover, these wastewaters are usually slightly alkaline
or neutral, with a pH value in the range 6.7–9.2 (Adam et al. 2018).
According to the characteristics showed above it is possible to see the presence of
high concentration of nutrients in digestate. Considering situations where its use as fer-
tilizer is not environmentally allowed due to regulatory policy it is necessary to use an
appropriate treatment (Magrí et  al. 2017). Besides the several advantages of AD, the
lack of alternatives for digestate disposal is a big issue than can make a biogas produc-
tion plant unviable and, in this case, biological treatment strategies could be attractive.
However, some problems may be faced to submit the digestate with these characteris-
tics to biological processes for nitrogen removal due to its high total solids and carbon
content. Additionally, phosphorous removal by chemical processes would require high
amounts of chemical products, increasing treatment costs (Suzin et al. 2018). Therefore,
a digestate treatment to reduce interferences for subsequent nutrient removal processes
is suggested.

3.2 SLS by settling

The settling process is based on the density difference between particles and liquid.
Therefore, among the wastewater pre-treatments, settling is widely used due to its rela-
tively low cost and easy operation (Hjorth et al. 2010).
Settling as a digestate pre-treatment strategy showed low settling velocity of solid
particles, averaging 0.02  m  h−1, with a tendency to stabilize the sedimentation after
50–60 min of experiment. This is because the process presents a superior efficiency to
remove discrete particles (Hjorth et  al. 2010; Hollas et  al. 2019). For this separation
process, the removal efficiency of solids was of 46%, 50% and 41% to TS, FS and VS,
respectively (average). Moreover, to the parameters TC and P the average removal effi-
ciency was, respectively, 45% and 71%. In addition, TKN and TAN had a removal effi-
ciency of 13% and 8.5%, respectively. The volume of sludge generated by settling was
396 L ­m−3.
Considering the relatively low cost of settling, the applicability of this process to
digestate could be interesting. However, considering the high generation of sludge its
applicability is questionable because it is a considerable sludge volume to give destina-
tion. This becomes an issue, since it demands transport which is a challenge, consider-
ing that liquid and contaminants are still incorporated on it.

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3.3 SLS by centrifugation

Centrifugation is a technology that employs equipment with relatively high cost (Popovic
et al. 2017). However, the separation efficiencies are usually high and it is expected that the
sludge volume generated would be lower than other techniques due to solids compaction.
The CCRD planning matrix ­22 of centrifugation tests performed in this study is presented
on Table  1 with the experimental responses of dependent variables: TC, P, TKN, TAN,
TS, VS, FS and pH. It is possible to observe that the nitrogen chemical species (TAN and
TKN) showed different removal efficiencies, which were 11 to 26% for TAN and 18–36%
for TKN. The best TAN removal condition (26% of efficiency) was at the axial point where
the strength variable ­gforce reached 3800  g and the best TKN removal condition (36% of
efficiency) was when a ­gforce of 1400 g was applied.
Total solids removal efficiencies were in the range of 60–83%. The maximum efficiency
was obtained at 20  min with a gravitational force of 3800  g. The solid fraction removal
before a biological treatment as deammonification is an important issue, since it can dam-
age the process that could not be able to remove nitrogen (Chini et al. 2019). Additionally,
solids discharge into the reactor can cause failure in the nitrogen removal process due to
shortage of solids retention time (SRT) (Feng et al. 2017).
The carbon removal efficiency for all tests was above 56%, reaching 90% efficiency
with a gravitational force of 3800 g at 20 min. At this condition, TOC in liquid fraction
was 250 ± 5 mg ­L−1, corresponding to a removal efficiency of 84.4%. The organic carbon
removal is important for wastewater treatment by deammonification, since heterotrophic
denitrifying bacteria that uses organic carbon as electron acceptor, can suppress anammox
bacteria leading to process failure (Feng et al. 2017; Zhou et al. 2018; Chini et al. 2019). It
has been reported that the anammox activity was severely inhibited and even deteriorated
at chemical oxygen demand higher than 500 mg L ­ −1 or C/N > 2.0 (Zhou et al. 2018). Shan
et al. (Shan et al. 2018) also reported similar inhibitory effects on potential rates of anam-
mox, in which the anammox activity was significantly decreased. At this point, the solids
and carbon reduction in liquid fraction obtained by centrifugation in this study is a promis-
ing result that allows suggesting the treatment by deammonification for nitrogen removal
(Chini et al. 2019, 2020).

Table 1  Matrix of CCRD design (coded and real values) and the responses related to gravitational force and
time. Results in % correspond to the removal efficiency
gForce (g) Ctime (minutes) TAN (%) TKN (%) TS (%) FS (%) VS (%) TC (%) P (%) pH

− 1(250) − 1 (10) 12.56 18.22 60.93 59.03 62.08 56.57 83.01 7.80
1 (2900) − 1 (10) 11.56 25.19 74.52 69.33 77.68 76.57 91.81 7.80
− 1(250) 1 (30) 13.07 22.48 65.89 63.39 67.33 62.84 86.53 7.80
1 (2900) 1 (30) 13.07 28.68 80.49 72.48 85.37 84.93 94.61 7.80
0 (1400) 0 (20) 14.07 25.97 74.24 69.82 76.94 78.36 95.54 7.80
0 (1400) 0 (20) 14.57 26.74 74.79 69.94 77.83 79.40 95.54 7.80
0 (1400) 0 (20) 14.57 27.13 75.62 70.30 78.79 75.97 95.75 7.80
− 1.41 (80) 0 (20) 23.55 27.52 68.82 64.00 71.77 68.94 89.38 8.02
1.41 (3800) 0 (20) 26.16 31.78 83.29 74.06 88.91 90.13 95.24 8.05
0 (1400) − 1.41 (5.9) 20.34 35.66 76.12 68.85 80.56 78.20 95.37 8.07
0(1400) 1.41 (34) 19.32 34.50 81.96 74.18 86.70 88.09 95.24 8.09

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A. Chini et al.

Phosphorous removal had a variation from 83 to 95% independent of the evaluated con-
dition. This high efficiency probably occurs through the P adsorption on the solid particles
(Kunz et al. 2009), a physico-chemical process through phosphorus precipitation. Calcium
can precipitate as calcium phosphate or hydroxyapatite, due to the high concentration of
calcium ions in the sludge and alkaline pH (Fernandes et al. 2012). In addition, crystalliza-
tion of phosphorus in struvite structure could also happen due to the presence of M ­ g2+ and
+
­NH4 anions in wastewater (Capdevielle et al. 2013).
The results of P removal are extremely important, because in areas with high swine
manure production, phosphorus has to be removed before disposal to avoid negative envi-
ronmental impacts. As discussed for nitrogen, land absorption capacity could be lower than
its concentration on effluents (Kunz et al. 2009). The concentration of P in liquid fraction
after centrifugation was lower than 50  mg ­L−1. In this case, a subsequent treatment for
P removal using chemical precipitation could be performed with significant reduction in
chemical products demand (Fernandes et al. 2012; Suzin et al. 2018).
To better understand the effect of the studied variables on SLS, the Pareto diagrams
(Fig. 2) graphically illustrate the effects of time and gravitational force and their interac-
tions during the AD centrifugation tests, to the removal responses of TAN, TKN, TS, FS,
VS, P and TC. The magnitude of each effect corresponds to p < 0.05.
The increase on gravitational force and time had effect on removal efficiencies
(p < 0.05). The ­gforce presented positive effect for all variables (TAN, TKN, TS, FS VS,
P and TC) thus increasing the force exerted from 80 to 3800 g in a centrifuge separation
favors the increase in removal efficiency. The same was observed for the time, where the
increase in centrifugation time favors the removal of all parameters Only for the dependent
variable P the time had a negative effect, that could be attributed to the relatively low phos-
phorous concentration in digestate compared to the other evaluated parameters.
The interaction lack between the variables ­Ctime and ­gforce, related to the parameter TAN,
are justified because ammonia nitrogen is a high soluble specie (Feng et  al. 2017). This
data are consistent with the low efficiency in TAN removal regardless of C ­ time and g­ force
applied.
The sludge volume generated was 100 L ­m−3, which is 3.8 times lower than the volume
generated on settling process.

3.4 SLS by chemical flocculation

Chemical flocculation consists of adding a coagulant resulting in particles destabiliza-


tion by reducing the forces that tend to keep them apart. This process has been chosen
as the primary treatment in wastewater treatment systems (Kooijman et  al. 2017). The
factorial design 2­ 2 planning matrix to the chemical flocculation tests with the experimen-
tal responses of dependent variables TC, P, TKN, TAN, TS, VS, FS and pH is shown
on Table  2. It can be observed that the nitrogen forms (TAN and TKN) showed similar
removal efficiencies, which varied from 9.5 to 15% for TAN and 16 to 22% for TKN. The
best TAN (15.08% of efficiency) and TKN (22.87% of efficiency) removal conditions
were in the same experimental test, with concentrations of TA and PAM of 75  mL ­L−1
and 15 mL L ­ −1. This condition also allowed the maximum efficiency of removal of solids
(60%), carbon (62%) and phosphorus (83%).
Through factorial design ­22 it was possible to investigate the effects of independent
variables (TA and PAM) and their interactions on the dependent variables (TC, TAN,
TKN, TS, FS, VS, P). The results were submitted to variance analysis (ANOVA), and

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Fig. 2  Pareto chart for TAN a, TKN b, TS c, FS d, VS e, P f and TC g removal on centrifugation tests

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A. Chini et al.

Table 2  Factorial design matrix (coded and real values) and the responses in relation to chemical floccula-
tion tests. Values in parenthesis are tannin (TA) and polyacrylamide (PAM) volumes added, respectively.
Results in (%) correspond to the removal efficiency

­ −1) PAM (mL L


TA (mL L ­ −1) TAN (%) TKN (%) TS (%) FS (%) VS (%) TC (%) P (%) pH

− 1 (25) − 1 (5) 9.55 16.28 51.70 53.45 50.70 50.45 77.82 7.98
1 (75) − 1 (5) 10.05 16.67 46.97 56.12 41.39 43.88 67.88 7.73
− 1 (25) 1 (15) 12.56 19.38 54.87 52.00 56.39 54.93 81.45 7.86
1 (75) 1 (15) 15.08 22.87 60.88 60.85 60.90 61.79 83.42 7.76
0 (50) 0 (10) 12.56 19.38 52.48 57.21 52.33 52.09 76.58 7.75
0 (50) 0 (10) 11.56 19.38 56.15 57.82 55.14 56.87 78.24 7.78
0 (50) 0 (10) 11.06 18.60 57.53 57.58 49.37 57.91 78.86 7.79

Table 3  Mathematical model to TAN, TKN, VS and P in the chemical flocculation


Parameter Model Fcal/Ftab R2

TAN Efc. % = 11.81 + 1.51*TA + 4.02* PAM + 1.01* PAM * TA 1.76 0.94231


TKN Efc. % = 18.80 + 1.94*TA + 4.65* PAM + 1.55* PAM * TA 5.16 0.97958
VS Efc. % = 52.35–2.40*TA + 12.60* PAM + 6.91* PAM * TA 1.37 0.92737
P Efc. % = 77.64–3.99*TA + 9.58* PAM + 5.96* PAM * TA 5.35 0.98026

Efc. Efficiency

it was verified that the models presented a good fit to TAN, TKN, VS and P responses
(Table 3). ­Ftest showed that ­Fcalculated was larger than ­Ftabulated, with a confidence level
of 95%. The correlation coefficient was 0.94231, 0.97958, 0.92737 and 0.98026 for
TAN, TKN, VS and P, respectively.
From these models (Table 3), the surfaces to TAN, TKN, VS and P were generated
(Fig. 3). It is possible to observe that the behaviors of TAN, TKN, VS and P were simi-
lar. As the tannin concentration raised, there was an increase in the removal efficiency
of these parameters, with the optimal region with 75 mL L ­ −1 of TA and 15 mL L ­ −1 of
PAM.
The response surfaces allowed to consider an optimal region between the tannin and
polyacrylamide quantity. In addition, it was possible to note that the gradual increase
in these variables favors the removal efficiency.
Furthermore, it can be concluded that TS and TC removal had better result when the
tannin increased. This is an important result given that TS and TC are as important as
TAN to subsequent effluent treatment for example on deammonification process.
The sludge volume generated by using the best condition of SLS by chemical floc-
culation (75 mL L ­ −1 of TA and 15 mL L ­ −1 of PAM) was 730 L m ­ −3, meaning that just
27% of the initial volume was able to go to a post treatment. Moreover, the manage-
ment of this sludge makes impracticable to use chemical flocculation as a digestate
pre-treatment, meaning that chemical flocculation is unfeasible as a digestate pre-treat-
ment due to the difficulties in handle this sludge.

13
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Treatment of digestate from swine sludge continuous stirred…

(a) (b)

15
14
13 24
12 22
11 20
10 18

(c) (d)

60
85
55
80
50 75
45 70

Fig. 3  Surfaces of TAN a, TKN b, VS c and P d for chemical flocculation tests. The increase in color inten-
sity in graphs corresponds to the removal efficiency increase. TA = tannin and PAM = polyacrylamide

Fig. 4  Comparison of SLS processes. Removal efficiencies were calculated considering the best conditions
obtained in each process as discussed previously

13
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A. Chini et al.

3.5 Comparison of SLS processes

In order to compare, the SLS processes evaluated in this work the conditions where the higher
removal efficiencies were obtained for each process are shown in Fig. 4 (settling, 3 h; cen-
trifugation, 20 min and g­ force of 3800 g; chemical flocculation, TA of 75 mL L­ −1 and PAM of
15 mL ­L−1).
Regarding to TAN and TKN removal, the behavior was similar in the three SLS processes
evaluated. As expected, settling, chemical flocculation and centrifugation exerts low influence
of removal (removal efficiencies were 7%, 15%, and 26%, respectively) because TAN is a sol-
uble specie and remains mostly on liquid fraction. However, the reduction obtained by centrif-
ugation is not negligible and considering the relatively high concentration found in digestate,
subsequent treatment to reduce this parameter in digestate would be favored.
The TS removal efficiencies resulting from the best results of settling, chemical floccula-
tion and centrifugation were, respectively, 46%, 61% and 83% that, respectively, represents
1.86, 2.55 and 5.98 times less solids than the initial digestate concentration, which was 21.8 g
­L−1.
Centrifugation showed an efficiency of 90% for TC removal from the liquid fraction, it
means that the digestate had 6.7 g ­L−1 of carbon and just 0.66 g L ­ −1 remained in the liquid
after this pre-treatment. Meanwhile the chemical flocculation showed 62% of efficiency result-
ing in 2.56 g ­L−1 of carbon in the liquid fraction. Moreover, the settling process presented TC
concentration of 3.67 g L­ −1 corresponding to a removal efficiency of 45%.
The P concentration was significantly reduced from the digestate by centrifugation, with
a residual concentration of 0.05 g ­L−1, thus presenting an efficiency of 95% of removal. The
other pre-treatments had lower removal efficiencies that were around 83% (0.16 g ­L−1) to the
chemical flocculation and 74% (0.25  g ­L−1) to settling. This high efficiency in removing P
probably is due to the ability of being incorporated into crystallized solid particles and thus
removed along with the sludge (Kunz et al. 2009; Suzin et al. 2018).
As expected, no significant changes in the pH values were observed after application of
pre-treatments, probably because of buffer capability of TAN and also alkalinity, which was
9.57 ­gCaCO3 ­L−1 in the digestate and it probably had not been removed from the liquid (Fer-
nandes et al. 2012). The pH, TAN and TKN of digestate were, respectively 7.79, 2 and 2.6 g
­L−1, and the average values after the three pre-treatments were 7.8 to pH, 2.07 g ­L−1 to TKN
and 1.76 g ­L−1 to TAN. So, when digestate fractions were separate (solid from liquid), the
inorganic nitrogen was not transferred to the solid fraction, just the organic form of it was
fixed on the solids (Jørgensen and Jensen 2009), which justifies the absence of these param-
eters variation comparing the digestate to the liquid fractions.
The sludge generated on different SLS processes was also analyzed for mass balance evalu-
ation. It was observed that the amount of all parameters in the sludge was equivalent to the
amount removed from liquid fraction. The sludge volume generated in the processes of set-
tling, centrifugation and chemical flocculation was 377, 100 and 730 L ­m−3, respectively.
Considering all aspects presented in this work, centrifugation could be considered the most
suitable process for digestate pre-treatment besides this remark did not consider economical
aspects.

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Treatment of digestate from swine sludge continuous stirred…

4 Feasibility of SLS processes: practical applications and future


research perspectives

The results obtained at this study showed that centrifugation is the most appropriate SLS
process to be used to digestate treatment. In practice, the conditions established in centrifu-
gation tests could be performed using commercially available centrifuge decanter equip-
ment. This equipment could be installed after the CSTR biodigester and the liquid fraction
submitted to a nitrogen removal process. This arrangement was already evaluated at lab
scale as demonstrated by Chini et  al. (Chini et  al. 2019, 2020). In these works, a deam-
monification reactor was operated and fed with digestate pre-treated by centrifugation. The
reactor showed very good performance for TAN concentration up to 800 mg L ­ −1 in influ-
ent (Chini et  al. 2020). Deammonification process, after suitable digestate pre-treatment,
seems to be a promising alternative for nitrogen removal from high strength wastewater,
as swine sludge digestate. This approach could favor installation of biodigestion units for
energy production in farms where digestate disposal into the soil for fertilization purposes
is impossible.
Centrifugation has a small footprint in terms of area requirement, have less odor and
low operational costs. Settling also has relatively low investments and operational costs.
Otherwise, the operational costs related to chemical flocculation are higher, mainly due
to chemical products requirement. The sludge management is also an important issue that
cannot be neglected, since process to handle this residue can highly affect treatment cost
in a wastewater treatment system. Likewise, considering the sludge volumes generated by
each process, centrifugation seems to be the more viable treatment process because signifi-
cantly less sludge volume is generated.
To have more detailed conclusions, it would be necessary to evaluate the different pro-
cesses at field scale conditions since more data are necessary to evaluate the economic
viability of each process and its efficiency in full scale could be not the same as obtained
in laboratory. Additionally, implementation cost would be different according to specific
countries conditions, and therefore, economic viability was not evaluated in this work
although this issue remains open for future research.
Finally, the choice of the most suitable SLS process is associated to the purpose of
wastewater treatment: the level of treatment that is required and if removal of nutrients is
necessary (eg., nitrogen or phosphorous). Considering nitrogen removal using a biological
process the limitations of each technology should be taken into account for decision on
previous SLS technology.

5 Conclusions

The present study reveals the possibility to apply different solid–liquid separation pro-
cesses to digestate to enable the reduction of solids, TC and P concentrations. Centrifuga-
tion at the optimized condition was able to reduce these parameters to satisfactory levels,
with a relatively low sludge generation (3.77 times lower than the sludge volume generated
by settling and 7.3 times lower than chemical flocculation). Digestate pre-treatment by cen-
trifugation would facilitate the implementation of subsequent biological nitrogen removal
by deammonification. Additionally, it would reduce the treatment cost of chemical phos-
phorus removal.

13
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A. Chini et al.

Acknowledgments This study had financial support from CAPES, CNPq and SISTRATES FUNTEC-
BNDES (grant number 15.2.0837.1).

Compliance with ethical standards 


Conflict of interest  The authors declare no conflict of interest.

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Affiliations

A. Chini1   · C. E. Hollas1   · A. C. Bolsan2   · F. G. Antes3   · H. Treichel4   ·


A. Kunz1,3,4 
1
Agricultural Engineering Graduate Program, Western Paraná State University, Cascavel,
PR 85819‑110, Brazil
2
Universidade do Oeste de Santa Catarina, Joaçaba, SC 89600‑000, Brazil
3
Embrapa Suínos e Aves, Rodovia BR‑153, Km 110, Distrito de Tamanduá, Caixa Postal 321,
Concórdia, SC 89715‑899, Brazil
4
Departamento de Ciência e Tecnologia Ambiental, Universidade Federal da Fronteira Sul,
Erechim, RS 99700‑000, Brazil

13
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