Bioresource Technology 217 (2016) 233–238

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Phosphorus extraction and sludge dissolution by acid and alkali

treatments of polyaluminum chloride (PAC) treated wastewater sludge
Toor Umair Ali, Dong-Jin Kim ⇑
Department of Environmental Sciences and Biotechnology & Institute of Energy and Environment, Hallym University, Chuncheon, Gangwon 200-702, Republic of Korea

h i g h l i g h t s

P release characteristics of PAC treated wastewater sludge were studied.

Highest P release was found with 2 N HCl and 1 N NaOH concentrations at 2 h.

Kinetic studies of P release and sludge dissolution follow the first order reaction.

Sequential extraction with NaOH/HCl give maximum P release (91.7%).

a r t i c l e i n f o a b s t r a c t

Article history: Phosphorus (P) leaching characteristics of polyaluminium chlorides (PAC) treated wastewater sludge was
Received 30 December 2015 investigated by wet chemicals (acid and alkali). Sludge fractionation showed non-apatite inorganic P was
Received in revised form 3 February 2016 the dominant P (90.9% of TP) while apatite P only accounted for 3.7%. After 2 h extraction with 1 N NaOH or
Accepted 4 February 2016
2 N HCl, 80.5% and 77.9% of total P was leached, while sludge dissolution reached 72.7% and 75.6%, respec-
Available online 9 February 2016
tively. Kinetic study with HCl and NaOH showed that P release and sludge dissolution follow first order
reaction with rate constants of 0.50 and 0.35 min1 (P release) and 0.47  102 and 0.15  102 min1
Keywords:
(sludge dissolution), respectively. Sequential extraction by NaOH/HCl leached 91.7% of the total P. This
Phosphorus release
Sludge dissolution
study will help in understanding the P release behavior of the PAC treated wastewater sludge.
Polyaluminium chlorides Ó 2016 Published by Elsevier Ltd.
Wet chemical

1. Introduction back of P recovery. However, stringent P regulation in the wastew-

ater effluent induces chemical P treatment process. Therefore,
It is estimated that phosphate rock reserves may be exhausted chemical sludge production has been increased significantly and
in 60–80 years (Hong et al., 2005; Rittmann et al., 2011). Phospho- an appropriate P recovery technology needs to be developed.
rus (P) is an irreplaceable elemental resource and the phosphate In a conventional WWTP, Al3+ or Fe3+ based salts, such as
rock mines are regionally confined to only a few countries. There- Al2(SO4)3 (alum), polyaluminum chlorides (PAC), and FeCl3, are
fore, it is necessary to establish a permanent sustainable P recovery widely used for P removal. PAC have a polymeric structure
technology from wastewater to reduce the consumption of phos- ((Aln(OH)mCl(3nm))x) and it is a preferred coagulant over alum
phate rock. due to lower alkalinity consumption and less metal content in
Large quantity of P is spread on farmland for agricultural pro- the sludge (Gebbie, 2001). Moreover, PAC produces larger and
duction and it causes eutrophication and an environmental nui- stronger flocs than alum and provides more space for adsorption
sance in the receiving water body via domestic wastewater and (Gregory and Dupon, 2001). Kim et al. (2002) also proposed that
agricultural runoff. In order to solve the problem, biological and PAC can remove phosphates and particulate matters by the
chemical approaches have been widely used in wastewater treat- mechanism of precipitation and adsorption because of ionic state
ment plants to reduce P in the effluent. Biological sludge has a high of Al in PAC.
P bioavailability and it has been extensively studied for P recovery Since the disposal of P rich sludge is a P loss, the sludge needs to
(O’Connor et al., 2004; Usman et al., 2012). But, P in chemical be treated properly for P recovery. Hybrid processes of low pres-
sludge has a low bioavailability in many cases and it was the draw- sure wet oxidation/nanofiltration (Blocher et al., 2012) and wet
chemical extraction/thermochemical method have been tested to
recover P from sludge (Gorazda et al., 2013). Wet chemical extrac-
⇑ Corresponding author. Tel.: +82 332482154; fax: +82 332563420.
tion methods are based on acid and alkali leaching. The main char-
E-mail address: dongjin@[Link] (D.-J. Kim).

[Link]
0960-8524/Ó 2016 Published by Elsevier Ltd.
234 T.U. Ali, D.-J. Kim / Bioresource Technology 217 (2016) 233–238

acteristics of the acidic leaching is the dissolution of heavy metals extracted for apatite phosphorus (AP) associated with Ca (Ca–P)
as well as Ca and Al combined P (Ca–P, Al–P) while it dissolves Fe– with 1 N HCl for 16 h. The extracted solution was measured for
P a little (Petzet et al., 2012). Heavy metals are undesirable in a TP analysis.
recovered P and strictly regulated when used as a fertilizer. On Crystallization pattern of the prepared PAC treated sludge was
the other hand, alkaline leaching dissolves amphoteric Al and Fe studied by X-ray diffraction (XRD) spectrometer (XRD, D/Max-
bound P but does not dissolve Ca–P and heavy metals (Levlin, 2500V, Rigaku, Japan). Elemental composition of the PAC treated
2005; Petzet et al., 2012). sludge was analyzed by ICP-OES spectrometer (iCAP 6300, Thermo,
Sludge leaching efficiency of P with acid and alkali depends USA) after digesting the sludge by HNO3 and aqua regia (Andersen
upon several factors such as the composition of sludge, type and and Kisser, 2004). For the HNO3 digestion 1 g PAC treated sludge
concentration of the extractant, pH and treatment time (Gorazda sample and 20 mL of 7 N HNO3 was mixed and autoclaved at
et al., 2013). Many different types of acid have been used for P 121 °C for 30 min. The sample was cooled at room temperature
leaching; H2SO4 (Franz, 2008), HCl (Schaum et al., 2007), HNO3 and filtered with 0.45 lm PTFE membrane filter (Cat No.
(Sano et al., 2012), citric acid and oxalic acid (Biswas et al., 2009) MTF045047H, Chm, Spain). The filtrate was analyzed by ICP-OES
while only NaOH was used for alkali treatment (Levlin, 2007; after dilution. In case of aqua regia, 3 g of the PAC treated sludge
Sano et al., 2012). sample was mixed with 1 mL of distilled water and treated with
P is bound with metals such as Ca, Al, and Fe. These metal 21 mL of HCl followed by 7 mL of HNO3. All the PAC treated sludge
bound P (Me-P) cannot be completely dissolved with a single leaching experiments were carried out in triplicate and the average
extractant (acid or alkali) because Me-Ps have different solubility values were used for the analysis.
depending on extractant (Wang et al., 2013). Ca–P and Fe–P easily
dissolve in acid while Al–P dissolves in both acid and alkali up to 2.3. Phosphorus release and dissolution of PAC treated sludge
some degree (Sano et al., 2012; Schaum et al., 2007). Therefore,
sequential extraction by acid and alkali is necessary to dissociate In this study, five different concentrations of the HCl and NaOH
most of the Me–Ps (Levlin, 2005; Petzet et al., 2011). Literature sur- were used for sludge treatment: 0.1 N, 0.2 N, 0.5 N, 1.0 N and 2.0 N.
vey showed that few studies have been carried out on P recovery For leaching, 10 g dried PAC treated sludge was mixed with 100 mL
from wastewater chemical sludge (Sano et al., 2012; Takiguchi of acid or alkali (L/S ratio 10) in 300 mL flask for P extraction. After
et al., 2007). Moreover, P recovery from PAC treated sludge has P extraction, the solution was immediately centrifuged at 10,000g
not been reported yet even though the PAC treated sludge occupies for 10 min and the supernatant was separated. The residual solid
a significant portion. In addition, most of the previous studies was washed by the respective extractant again in order to leach
focused on P release from sludge but did not pay any attention any remaining P and the TP in the supernatant was measured.
on dissolution of sludge. Sludge is usually disposed in landfill Sludge residue was weighed after drying at 105 °C for the calcula-
and it continuously reduces available landfill capacity (Adam tion of sludge dissolution after acid/alkali leaching. The pH was
et al., 2009). To cope with the issue sludge reduction is necessary also checked before and after the leaching. Sequential P extraction
before disposal. The objective of this study was to investigate the was carried out in order to measure the acid and alkali releasable
release characteristics of P with acid and alkali for P recovery from fraction of P. In a sequential extraction, dried PAC treated sludge
the PAC treated sludge. For the purpose, P release and dissolution residue after acid treatment was treated with alkali, and vice versa,
kinetics from the PAC treated sludge were studied. for extracting the remaining P in the sludge residue. The sludge
dissolution was measured by Eq. (1).
2. Methods Sf
Sludge dissolution ð%Þ ¼  100 ð1Þ
Si
2.1. Sludge collection and preparation
where Sf = sludge dry weight (g) after leaching, Si = sludge dry
PAC treated sludge was collected from a municipal wastewater weight (g) before leaching.
treatment plant in Chuncheon, Korea. The PAC treated sludge was The kinetics of P release (Eq. (2)) and sludge dissolution (Eq. (3))
first filtered with hardened ashless filter paper (Cat No. 1541-240, were analyzed with the first order kinetic model. The rate con-
Whatman, USA) in order to remove any dissolved P in the liquid. stants (k1, k2) were calculated by statistical data analysis and scien-
After filtration the sludge was dried in a convection oven at tific graphic software (SigmaPlot, V. 10).
105 °C for 48 h. After drying, the sludge was ground and pulverized C t ¼ C o ð1  ek1 t Þ ð2Þ
with mortar to a mesh size <500 lm before acid and alkali
leaching.
C 0t ¼ C 0o ek2 t ð3Þ

2.2. Characterization and analysis of PAC treated sludge where Ct = concentration of solid (mM) at time t, Co = initial concen-
tration of P (mM), C0 t = concentration of sludge in TS solid (g/L) at
The PAC treated sludge was characterized after the sample time t, C0 t = initial concentration of sludge in TS solid (g/L), k1 = P
preparation. All the analytical methods were based on the Standard release rate constant at room temperature, k2 = sludge dissolution
Methods unless stated otherwise (APHA, 2005). Total phosphorus rate constant at room temperature.
(TP) was measured after calcination at 450 °C for 3 h and then
extracted with 3.5 N HCl for 16 h. Sludge fractionation was based 3. Results and discussion
on the Standard Measurement and Testing (SMT) method (Ruban
et al., 1999). Inorganic phosphorus (IP) was extracted with 1 N 3.1. Characteristics of PAC treated sludge
HCl for 16 h and residues of this extraction was calcined for 3 h
at 450 °C and then again extracted with 1 N HCl for organic phos- The dried PAC treated sludge (pH 6.4 ± 0.08) had a total sus-
phorus (OP). Non-apatite inorganic phosphorus (NAIP) associated pended solids (TSS) of 11.73 ± 0.74 g/L and volatile suspended
with oxides and hydroxides of Fe, Al or Mn (Fe/Al–P) was extracted solids (VSS) of 6.16 ± 0.23 g/L. Inorganic elemental composition of
with 1 N NaOH for 16 h and then some part of this extract was dried PAC treated sludge was obtained by ICP-OES spectrometry
treated with 3.5 N HCl. The residues of this extraction was and the fractions of major elements are shown in Table 1. The
 T.U. Ali, D.-J. Kim / Bioresource Technology 217 (2016) 233–238 235

Table 1 ICP-OES results showed 53.6 mg P/g sludge by aqua regia extrac-
Elemental composition of the PAC treated sludge (ICP-OES analysis). tion and Al was the major element in the PAC treated sludge. Since
mg/g of sludge Digesting with 7 N HNO3 Digesting with aqua regia Al has an amphoteric nature, both acid and alkali can oxidize Al
Al 154.24 158.38 and release P (Petzet et al., 2012). XRD analysis of the PAC treated
P 52.7 53.6 sludge indicated that the sludge did not have a crystalline structure
Ca 5.19 5.16 since no distinctive diffraction peaks could be found (data not
Cu 0.14 0.15 shown). Alum treated sludge also showed an amorphous structure
Fe 10.79 10.67
Mg 1.43 1.45
(Yang et al., 2006).
Mn 0.55 0.57 For the fractionation of PAC treated sludge, SMT protocol was
Ni 0.00 0.01 used (Ruban et al., 1999; Xu et al., 2015). The fractionation of the
Si 2.90 1.49 PAC treated sludge showed that inorganic P (IP) and organic P
Ti 0.06 0.05
(OP) accounted for 97.2% and 2.8% of TP, respectively (Table 2).
Zn 0.79 0.41
K 2.56 2.43 IP of the PAC treated sludge was further classified into apatite P
(AP) and non-apatite inorganic P (NAIP). AP is a P combined with
Ca while NAIP is a P combined with metals other than Ca (i.e. Al,
Fe, and Mg). NAIP in the PAC treated sludge accounted for 90.9%
Table 2 of TP while AP only accounted for 3.7% of TP. High portion of NAIP
Phosphorus fractions of dry sludge, according with SMT protocol. in the PAC treated sludge was due to the precipitation of P in the
P fraction mg P/g of sludge Fraction (%)
wastewater by PAC for P removal.
TP 52.1 –
P 50.6 97.2
3.2. Phosphorus release and sludge dissolution by HCl and NaOH
OP 1.4 2.8
NAIP 47.3 90.9 treatment
AP 1.9 3.7
In this study different concentrations of HCl and NaOH solu-
tions (0.1 N, 0.2 N, 0.5 N, 1 N and 2 N HCl) were used to find out
the effect of extractant concentration on P leaching from the

Fig. 1. Phosphorus leaching profiles of the PAC treated sludge with different Fig. 2. Sludge dissolution profiles of the PAC treated sludge with different
concentrations of HCl (A) and NaOH (B). concentrations of HCl (A) and NaOH (B).
236 T.U. Ali, D.-J. Kim / Bioresource Technology 217 (2016) 233–238

sludge. Fig. 1(A) represents the time profiles of P release with var- may be due to the dissolution of other metals. It can also be
ious HCl solutions. P release reached maximum at 78% (39.7 mg P) inferred that the new compounds formed by re-precipitation were
of TP with 2 N HCl in 2 h. After that P release decreased next 4 h to non-acidic leachable P compound which also caused no further
74%. Ottosen et al. (2013) also reported that 2 h treatment gave increase in P concentration in the leachate (Ottosen et al., 2013;
maximum P leaching with sludge ash. Petzet et al., 2011).
P release profile with NaOH is shown in Fig. 1(B). The maximum Interestingly, higher P release was found with 1 N NaOH while
P release reached 80.5% (41.7 mg P) at 1 N NaOH in 2 h which is higher dissolution of the PAC treated sludge was found with 2 N
similar to HCl treatment. From the above results, NaOH showed NaOH in alkali treatment. On the other hand, both higher P release
slightly higher P release than HCl. The reason seems to the higher and sludge dissolution were found with 2 N HCl (Figs. 1 and 2). The
Al and Fe content than Ca in the PAC treated sludge. It is well rec- reason of NaOH behavior upon the PAC treated sludge dissolution
ognized that alkaline condition favors the dissolution of Al–P and is not fully understood yet, but it is expected that some metals
Fe–P rather than Ca–P. The result coincides with the previous study reacts with OH to form metal hydroxides which are hardly solu-
that reported high P recovery with NaOH using Fe containing ble. The result also indicates that P release does not always depend
sludge (Sano et al., 2012). upon the sludge dissolution and the presence of high Al content in
Dissolution of PAC treated sludge increased with the extractant the sludge also contributed to some extent.
concentration and the profiles were similar to those of P leaching. Effect of HCl and NaOH concentrations on Al and Ca leaching
Dissolution of PAC treated sludge reached 75.6 and 72.7% with HCl from the PAC treated sludge were compared. Fig. 3(A) shows the
and NaOH, respectively, at the maximum P release condition leaching behavior of Al, Ca and P at various concentration of NaOH.
(Fig. 2). However, the dissolution of PAC treated sludge by HCl The result showed that Al and P leaching increased with NaOH con-
slowly increased after 2 h. It is obvious that dissolution of the centration, but the highest P release was found at 1 N NaOH and
PAC treated sludge increases with the reaction time to reach equi- almost no increase in Ca concentration with the increase in NaOH
librium while P release was not increased as in Fig. 1. The reason is concentration. At this condition the final pH was 13. Previous study
that P re-precipitate or combines with Al to form Al–P after the dis- also reported that P release was high at pH 13–14 (Stark et al.,
solution of Ca–P (Petzet et al., 2011, 2012). On the other hand, acid 2006).
dissolves not only P but also most of the metals (Petzet et al., 2011) Fig. 3(B) represents the leaching of P, Al and Ca leaching with
and the increase of the PAC treated sludge dissolution with time various concentration of HCl. Al, Ca and P leaching increased with

Fig. 3. Leaching profiles of P, Al, and Ca from the PAC treated sludge at optimized leaching time of 2 h. (A) NaOH; (B) HCl.
 T.U. Ali, D.-J. Kim / Bioresource Technology 217 (2016) 233–238 237

Table 3 4. Conclusion
Rate constants of phosphorus release and sludge dissolution based on first order
reaction rate kinetics.
The PAC treated sludge contained high Al and P (mostly inor-
Extractant P release Sludge dissolution ganic), but low Ca. Alkali treatment of the PAC treated sludge
k1 (min1) r2 k2 (min1)  102 r2 released more P than acid, which is different to sludge ash, due
HCl 0.50 0.99 0.47 0.98 to high Al–P and low Ca–P contents. Sequential treatment with
NaOH 0.35 0.99 0.15 0.99 NaOH/HCl was effective to release 91.7% of TP from the PAC treated
sludge. Further study is needed to fully understand the interaction
of P and PAC in the sludge.
the concentration of HCl. The highest Ca leaching was found at
0.5 N HCl and the pH was 3.5. The result is close to the previous
Acknowledgements
result that 0.4 N HCl was the optimum concentration for Ca leach-
ing from sewage sludge ash (Petzet et al., 2011, 2012).
This research was supported by Basic Science Research Program
P release from sludge or sludge ash is a function of pH (Petzet
through the National Research Foundation of Korea (NRF) funded
et al., 2012; Schaum et al., 2007; Xu et al., 2015). HCl treatment
by the Ministry of Education (2015R 1D 1A 1A01060589). This
clearly showed that pH became in steady state after 2 h at all the
research was also supported by Hallym University Research Fund
HCl concentrations (SFig. 1). In case of higher NaOH concentrations
(HRF-201511-009).
(0.5 N, 1.0 N and 2.0 N NaOH) the pH became steady state after 2 h,
while at lower NaOH concentrations (0.1 N and 0.2 N) remained
steady state after 6 h (SFig. 2). The longer pH stabilization time Appendix A. Supplementary data
means longer sludge dissociation at low alkaline condition.
In order to get more insights about the behaviors of P leaching Supplementary data associated with this article can be found, in
and dissolution of PAC treated sludge, kinetic study was conducted the online version, at [Link]
for the optimized condition of P release. It was found that P leached 017.
out at the initial leaching stage mostly and attained steady state in
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