Muryanto, S. 1,2,a,*, A.P. Bayuseno3,b, E. Supriyo4,b, and B. Hermanu5,a
1Office of Research, and 2Dept.Chemical Engineering
3Centre for Waste Management, Mechanical Engineering Graduate Program
4Chemical Engineering Diploma (Vocational) Program
5Faculty of Agricultural Technology
aUNTAG University in Semarang, Bendhan Dhuwur Campus, Semarang 50233, INDONESIA
bDIPONEGORO University, Tembalang Campus, Semarang 50275,INDONESIA E-mail: [email protected]
Phone:+62-24-8441771, fax: +62-24-8441772
Abstract
Intensified agriculture in response to the growing population has led to excessive nutrient discharges into waterbodies causing eutrophication, which affects biological diversity and water quality. One of such nutrients is phosphorus (P), an essential element for every living plant, and hence for food production. An attractive method to help minimise eutrophication is to remove P from wastewater by converting it from a soluble form into solid phase, i.e. a phosphate mineral commonly known as struvite (MgNH4PO4.6H2O), through a controlled crystallisation process. The method has increasingly gained particular interest since struvite can be utilised as fertilizer which simultaneously provides Mg, N, and P in proportional amounts to crops. Since struvite has low solubility in water, it may also act as slow-release fertilizer and may not cause burning of roots. P removal and recovery as struvite is also an effective method to address the problem of operating difficulties in wastewater treatment facilities, since under favourable conditions struvite can spontaneously form in wastewater, and the resulting struvite crystals agglomerate and excessively cover the piping systems, pumps, screens etc. This paper discusses the principles of P recovery from agroindustrial wastewater through struvite crystallisation. The findings of a preliminary experiment examining the onset of struvite crystallisation from synthetic liquors are presented.
Applicability of the struvite crystallisation method including its advantages and disadvantages, as well as typical operating conditions and the properties of the struvite crystals produced will be scrutinised.
Keywords: crystallisation, eutrophication, phosphorus, struvite, wastewater
Introduction
Intensified agriculture is an inevitable consequence of population growth. Such intensification demands extensive use of fertilizers, and over-application of phosphate fertilizers to soil has been frequently encountered [Harris et al., 2008; Nelson et al., 2003].
Accordingly, waste streams from agricultural activities contain considerable amount of soluble phosphate. Discharging such nutrient-rich streams to surface waters results in eutrophication which is unsightly, lethal to aquatic life, and negatively affects water quality [de-Bashan and Bashan 2004].
Phosphorus (P) is an essential element for living organisms, plants included, hence food production relies heavily on the availability of P. On the other hand, P is also regarded as the primary nutrient for eutrophication of surface waters. Efforts to prevent eutrophication by removing P from wastewater have been widely put forward.
A promising method to reduce eutrophication is to remove the excessive P from waterbodies by converting it into solid phase, i.e. a phosphate mineral known as struvite (MgNH4PO4.6H2O), through a controlled crystallisation process. Struvite can be used as fertilizer since it has low solubility in water, hence would not quickly leach in waterbodies.
Since the leaching potential is low, struvite can act as a slow release fertilizer, and can be applied at relatively high rates without damaging plant roots [Gaterrel et al 2000]. Struvite can be used individually or in combination with other agricultural fertilizers.
P crystallisation as struvite is also an effective method to address the problem frequently encountered in wastewater treatment facilities (WWTFs), since under favourable conditions struvite can spontaneously form in wastewater, and the resulting crystals agglomerate and excessively cover the piping systems, pumps, screens etc.
This paper discusses the principles of P removal and recovery from agroindustrial wastewater through struvite crystallisation. The findings of an experiment examining the effect of metal ions on the morphology of struvite are presented. Applicability of the struvite crystallisation method including its advantages and disadvantages, as well as typical operating conditions and the properties of the struvite crystals produced will be scrutinised.
Principles of P Recovery through Struvite Crystallisation
Agroindustrial waste is commonly land-applied or treated by anaerobic digestion. Land-application is not always desirable since it causes green house gas emissions, eutrophication, and groundwater pollution. Anaerobic digestion is preferred due to the possibility of alleviating enviromental concerns and generating biogas [Jin et al 2009].
However, anaerobic digestion of waste sludge gives rise to high concentrations of P and ammonia (N) in the sidestreams, and these high nutrient-rich loads have to be removed or preferably recovered. Moreover, anaerobic treatment increases the volume of the sludge.
In this respect, many researchers have found that struvite crystallisation is an attractive option for P removal and recovery.
After sludge separation, subsequent liquors contain high concentrations of soluble P and N, and lower concentrations of soluble Ca and Mg. Significant proportions of this soluble P can be recovered by a crystallisation process unit placed after sludge digestion [Pastor et al., 2010].
In many places, the manure management for dairies consists of flushing the manure with water, followed by separating the coarse solids through screening or sedimentation. The liquid fraction is then sprayed to the fields as fertilizers. Such practice is favourable since the nutrients are recycled on-site. However, the liquid fraction generally contains high concentrations of both P and N in a ratio that is inappropriate for crop requirement [Harris et al 2008]. On the other hand, it has been reported [Suzuki et al 2007] that certain swine wastewater already contains Mg2+, NH4+ and PO43- in high concentrations. This condition is preferable since adjusting the pH of the wastewater to 8 – 9 would lead to spontaneous crystallisation of struvite. However, unless the crystallisation process is controlled, the struvite crystals can agglomerate and cause scaling of equipment, which complicates the
operation of WWTFs. Nutrient recovery from agroindustrial wastewater by struvite crystallisation is an advantageous method since the process prevents scaling problems [Doyle and Parsons 2002], removes soluble P [Battistoni et al 1997; Laridi et al 2005], as well as N [Çelen and Türker 2001; Altinbas et al 2002; Laridi et al 2005]. Integration of a struvite crystallisation unit into sidestream of WWTFs is becoming common practice [Caffaz et al 2008].
Availability of Struvite Ion Components
The three major components of struvite: magnesium (Mg2+), ammonium (NH4+
-N), and phosphorus (PO43--P) can come from a number of sources. As can be seen from its chemical formula: MgNH4PO4.6H2O, once these three ions are present in equimolar ratios, it is theoretically possible for the struvite to crystallise.
In most cases, agroindustrial wastewater is deficient in magnesium [Pastor et al 2010]. The amount of magnesium ions in swine lagoon liquid is usually only half of that required stoichiometrically for struvite crystallisation [Nelson et al 2003]. As reported by Marti and co-workers [Marti et al 2010], effluents from sludge digestion systems usually have high concentrations of P, Mg2+, NH4+
with Mg2+ being the least. Another group of researchers [Liu et al 2011] also stated that the magnesium content of agroindustrial wastewater is very low compared to the other two components: P and N. Hence, magnesium additions to wastewater is common practice to encourage struvite crystallisation. A number of different Mg-containing chemicals have been used as sources of magnesium ions. These sources are:
Mg(OH)2 [von Münch and Barr 2001], MgCl2 [Pastor et al 2010; Forrest et al 2008], MgO [Quintana et al 2008], magnesite [Gunay et al 2008], and bittern [Lee et al 2003]. Location of WWTFs may also influence the availability of magnesium ions. The ions can be plentiful in hard water area, certain industrial areas, as well as in places where seeping of sea water may take place [Doyle and Parsons 2002]. Yet another source of magnesium ions is the support materials placed inside anaerobic digesters, such as bentonite, dedicated to provide surface area for biomass attachment [Doyle and Parsons 2002]. In such cases the release of magnesium ions into the surrounding water can be significant if these materials were left in the digester for a long time.
Agroindustrial wastewater typically contains high concentrations of N due to the degradation of organic matter and nitrogeneous material such as proteins. Manure of domestic animals and poultry are also nutrient-rich wastes as sources of N [Ren et al 2010].
In general, wastewater contains relatively excess N compared to other components [Doyle and Parsons 2002].
Anaerobic digestion process releases polyphosphates into the liquid phase, which simultaneously increases the concentration of P, Mg2+ and K+ in the solution [Marti et al 2010]. Three soluble forms of P are usually present in wastewater: PO43-, HPO42-, and H2PO4- [Doyle and Parsons, 2002]. While sufficient P and Mg2+ contribute to the formation of struvite, the presence of K+ might encourage the crystallisation of another phosphate mineral: MgKPO4 [Huang et al 2011], reducing the yield of struvite crystals.
Effect of Component-Ion Molar Ratios
Although struvite crystallisation is theoretically possible when the ratio of Mg/N/P in a crystallising solution is 1:1:1, the crystallisation process is highly dependent on the pH of the solution (see chemical equation in the later section of this paper). It has been found
that depending on the stoichiometric condition alone, and neglecting the optimum pH level, the crystallisation of struvite might take a number of days [Battistoni et al 1997].
As guidance, for struvite to crystallise the ratio of Mg/N/P in the solution should be higher than equimolar. As an example, Mohan and co-workers [Mohan et al 2011] carried out experiments using three chemicals in a batch reactor (a 250-ml Erlenmeyer flask) to obtain a synthetic solution having an initial NH+/Mg2+/PO4
ratio of ~ 3.5/3/4. The pH of the solution was adjusted to 8.9 using 5.0 N NaOH and the crystallisation proceeded spontaneously. The experiment, which lasted about ten minutes, produced sufficient amount of struvite crystals.
As described earlier (see previous sub-section), the Mg content of the wastewater is usually in deficit, i.e. the Mg/P molar ratio is less than one, which theoretically would not encourage the formation of struvite. In such cases, addition of Mg-containing chemicals are needed and this addition may involve significant cost.
Song and co-workers [Song et al 2011] have used CO2 stripping method and were successful in crystallising struvite without chemical additions. The main reason being the molar ratio of Mg/P was kept constant between 1.31 and 2.42. This condition is in agreement with similar experiments on struvite crystallisation from swine waste [Burns et al 2003; Jordaan et al 2010] where for an effective struvite crystallisation, the Mg/P ratio was maintained at 1.6.
Effect of pH
Struvite crystallises as white orthorhombic crystals according to the following reaction:
Mg2+ + NH+ + HnPO4n-3
+ 6 H2O MgNH4PO4.6H2O + nH+
Depending on the pH of the solution, the values of n can be 0, 1, or 2. Obviously, the crystallisation process is highly dependent on pH. The range of pH suitable for struvite crystallisation can be sufficiently wide, namely from 7.00 to 11.00 [Ali 2005]. However, individual investigations have shown that the precise and optimum pH where struvite has the maximum potential to crystallise is narrower in range as can be seen in Table 1. It can be inferred from the table that in most cases, the optimum pH for struvite crystallisation is about 9.0. pH level plays an important role in struvite crystallisation process since increasing the pH from 7.0 to 9.0 would result in a 250 fold increase in the amounts of PO4
3-ions, while NH4+ reduces slightly [Stumm and Morgan 1970]. As described previously (see Availability of struvite ion components) pH adjustment is a crucial factor for the completion of struvite crystallisation.
Table 1. pH values for struvite crystallisation used by different researchers.
Crystallisation Time mg:p Agitation pH References
120 minutes 1:1 to 1.6:1 120 rpm 7.5-9.5 Nelson et al., 2003
24 hours 1:1 200 rpm 7.0-11.0 Ali, 2005
25 minutes 1:2 None 9.0(fixed) Le Corre, 2006
10.5 to 12.5 hours 0.8:1 to 1.7:1 unknown 8.7 (adjusted) Pastor et al., 2010
4 hours 1:1 air bubbling 8.09-8.43 Rahman et al., 2011
4 hours 0.5:1 to 1.2:1 air bubbling 7.82 to 8.92 Liu et al., 2011 Effect of Impurities
Although impurities are usually present in trace (or ppm) amounts, their effects on crystallisation can be significant [Hoang et al 2009], since these impurities may block the
“active sites”, thus hindering the growth of crystals. Depending on the type of wastewater, there is a wide range of impurities which can affect the crystallisation of struvite.
Wastewater originating from agroindustrial sector typically contains high concentrations of Ca2+ as impurities [Parsons et al 2001], which can interfere with struvite [MgNH4PO4.6H2O]
formation due to the tendency of Ca2+ to react with the phosphate ions forming calcium phosphate: Ca3(PO4)2 [Pastor et al 2008; Song et al 2011]. According to Yi and co-workers [Yi et al 2005), however, such competition for phosphate ions could start taking place only when the Ca2+ concentrations are significantly high, i.e. above 300 ppm. A recent investigation by Pastor and his colleagues [Pastor et al., 2010] showed that the presence of Ca2+ could also give rise to the formation of both calcite: CaCO3 and dolomite: CaMg(CO3)2, if the solution also contains sufficiently high concentrations of Mg2+.
Swine wastewater usually contains high concentrations of Cu2+ and Zn2+ which originate from the food supplement given in the piggery. These two ions are regarded as not environmental friendly, so their presence in wastewater has been actively investigated [Lake et al 1985]. It has been found [Lisitsin et al 2005] that trace amounts of Zn2+ (about 2 ppm) was capable of retarding the growth of CaCO3 crystals either in the bulk of the solution or as scale in the RO membranes of a desalination facility.
An Experiment on Struvite Crystallisation from Synthetic Liquors
We carried out a bench-scale experiment using synthetic liquors to investigate the effect of metal ions, namely Cu2+, and Zn2+ on the morphological change of struvite.
Materials and Methods
All reagents used were of analytical grade (Merck®) or equivalent. MgCl2.6H2O and NH4H2PO4 were separately dissolved in doubly-distilled water, which was previously boiled to purge CO2, to provide Mg2+, NH4+
-N, and PO4
3--P with varying concentrations. For pH adjustment, up to 9.00, NaOH solution was used. Effect of ppm amounts of metal ions (Cu2+, and Zn2+) on struvite crystallisation was investigated in this study, and for this purpose, crystals of CuCl2.2H2O, and ZnCl2 were separately dissolved in MgCl2 solution.
A series of batch crystallisation experiments were conducted using a one-litre clean (“scratchless”) glass beaker. The beaker was agitated using a variable speed pitched blade impeller (in-house made), and was placed in a thermostatically controlled water bath.
Stirring rate was fixed at 125 rpm as it was found that this speed was sufficient to make the solution visibly well stirred. The two solutions of MgCl2 and NH4H2PO4 were placed in the crystalliser, the timer was started (= which corresponded to t = 0 or zero time), and the impeller was activated vigorously for five seconds and then reduced to 125 rpm until the crystallisation completed. During the experimental run, pH values of the solution were measured (using combined pH meter: Martini-Mi 805-Romania) at 0, 1, 2, 3, 4, 5, 10, 15, 20, 25, 30, 35, and 40 minutes, respectively. As crystallisation proceeded, the pH of the solution decreased gradually and levelled off after about 30 minutes, and therefore extension to 40 minutes was considered to be the end of the crystallisation reaction. Next, the whole solution was filtered (0.20 μm Whatman filter paper) and the crystals were air dried overnight at room temperature. The morphology of these crystals were then
examined using a light microscope (Yenaco XS2-107 BN-Japan). After completion of one experiment, the beaker and its accessories were cleaned and prepared for the next run.
Results and Discussion
The typical morphology of the struvite crystals obtained is shown in Figure 1. Fig. 1.a depicts struvite crystallised in pure solution without impurities addition. As can be seen the elongated needle-like crystals confirm the typical struvite morphology [Stratful et al 2001;
Kabdasli et al 2006]. On the other hand, Figs.1.b and 1.c. exhibit the crystals obtained when 20 ppm of Cu2+ and Zn2+ were added, respectively. The two images show that the crystals were no longer needle-like but agglomerated. This morphological change could be the result of Cu2+ and Zn2+ blocking the active sites of the crystal surface. Hence the growth of the crystals was stopped and the crystals failed to form the extended needle shape [Muryanto 2002]. Considering the agglomerated struvite crystals as shown in Figs.1b and 1.c., it is still difficult to distinguish the specific influence of either Cu2+ and Zn2+ on morphological change of crystals.
Figure 1. Struvite crystallised at 40 min. (a) pure solution; (b) 20 ppm Cu2+ added; (c) 20 ppm Zn2+ added. (solution concentration: 4.0 mM; image magnification: 40x).
a
c
b
Typical Full-Scale Struvite Crystallisation
The method of struvite crystallisation falls into three categories [Le Corre, 2006], namely, (1) selective ion exchange, (2) air-agitated reaction, and (3) stirred reaction. The third method comprises a fluidised bed reactor (FBR) and is by far the most promising. A number of industrial scale FBR for struvite crystallisation have been operational, such as the one shown in Fig. 2. As depicted in the figure, P- and N-rich filtrate from an anaerobic unit is pumped upward from the base of the inverted cone-shaped column (see Fig.3 for details of the FBR column). Near the base of the inverted cone (see Fig. 3), two separate inlets were made to supply NaOH and MgCl2 solutions, for pH adjustment and Mg2+ additions, respectively. Once the pH level of the solution has been adjusted and reached the alkaline conditions of ≥ 8.0, struvite spontaneously crystallises, and subsequently carried to the upper section of the FBR by the continuous upflow stream. During this period, the struvite crystals collide among themselves and start agglomerating with each other to form pellets.
The pellets fall to the base of the column due to their high density, while smaller struvite crystals are suspended inside the column and continue to grow or agglomerate. The struvite pellets with sizes from 1 to 2 mm in diameter, are periodically harvested from the bottom of the FBR. For easier handling, a straightforward additional process is usually required, such as air drying.
Figure 2. Schematic diagram of an enhanced biological phosphorus removal (EBPR) unit coupled with an FBR to recover P as struvite fertiliser (Courtesy of Multiform Harvest Inc. Seatle, Washington, USA, www.multiformharvest.com - personal communication with first author).
Figure 3. Detailed description of the FBR (Courtesy of Multiform Harvest Inc. Seatle, Washington, USA, www.multiformharvest.com - personal communication with first author).
Conclusions
Agroindustrial wastewater is a highly potential source for struvite crystals. Struvite crystallisation from agroindustrial wastewater needs addition of chemicals especially as sources of magnesium ions. Trace amounts of metal ions: Cu2+ and Zn2+ can change the morphology of struvite crystals from typically needle-like to become agglomerated crystals.
A number of full-scale struvite crystallisation projects using agroindustrial wastewater are already in operation.
Acknowledgement
The authors gratefully acknowledge the financial support (2011 Fundamental Grant - Hibah Fundamental) given by the DGHE, the Indonesian Ministry of National Education, for the experiment reported in this paper. The skillful lab work mostly carried out by N. Kartikasari is also appreciated.
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