Phosphorus Adsorbent Derived from Concrete Sludge (PAdeCS) and

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Phosphorus Adsorbent Derived from Concrete Sludge (PAdeCS) and its Phosphorus Recovery Performance Atsushi Iizuka,*,† Takeshi Sasaki,‡ Teruhisa Hongo,‡ Masato Honma,§ Yasuyuki Hayakawa,§ Akihiro Yamasaki,‡ and Yukio Yanagisawa∥ †

Research Center for Sustainable Science and Engineering, Institute of Multidisciplinary Research for Advanced Materials, Tohoku University, 2-1-1 Katahira, Sendai, Miyagi 980-8577, Japan ‡ Department of Materials and Life Science, Seikei University, 3-3-1 Kichijoji-kitamachi, Musashino, Tokyo 180-8633, Japan § Nippon Concrete Industry Co. Ltd., 1-8-27 Kounan, Minato-ku, Tokyo 108-0075, Japan ∥ Department of Environment Systems, Graduate School of Frontier Sciences, The University of Tokyo, 5-1-5 Kashiwanoha, Kashiwa, Chiba 277-8563, Japan ABSTRACT: Solid adsorbents for phosphorus recovery (PAdeCS) were prepared from real concrete sludge sampled from an industrial site that produces concrete poles and piles. The concrete sludge was diluted with water at dilution ratios from 1 to 15 to prevent hardening of the cement components. The diluted concrete sludge was then filtered, dried, and used as a solid adsorbent. Two drying methods were examined: natural drying under atmospheric conditions and forced drying in an oven at 105 °C. The phosphorus recovery performances of prepared adsorbents were examined using a potassium dihydrogen phosphate (KH2PO4) solution containing 100 mg-P/L (close to the effluent produced by the sewage sludge dewatering process) as a synthetic for wastewater. All the prepared adsorbents were able to recover phosphorus. Using the forced drying treatment during adsorbent preparation greatly improved the rate of phosphorus recovery from solution. The adsorbent prepared with dilution ratio 10 and forced drying exhibited the highest phosphorus recovery performance. The final phosphorus concentration in solution was 0.83 mg/L, 4 h after addition of the optimized adsorbent, which is extremely promising for application in inexpensive phosphorus recovery processes. phosphorus capture.11 Wastes such as acid mine drainage sludge,12 iron and steel slags,13−17 aluminum and iron drinking water treatment residuals,18−20 fly ash,21 limestone,13,15 biologically produced iron oxides,22 palygorskite clay,23 manganese ore tailings,24 wood ash,25 and flue gas desulfurization gypsum26 have been tested so far. In our previous study, to develop a more economical and feasible phosphorus recovery process, we utilized waste concrete, fine particles mainly composed of hydrated cement components obtained by crushing waste concrete, as an inexpensive substitute for these chemicals.27,28 The results indicated that phosphorus ions in wastewater could be removed in the form of HAP with low crystallinity by addition of fine waste concrete particles. HAP was precipitated on the surface of the waste concrete particles. In the process, waste concrete can act as the calcium source, alkali substance, and seed material. In this paper, the phosphorus recovery performance of concrete sludge, another form of waste concrete, was examined based on laboratory scale experiments. Concrete sludge is a waste slurry generated on construction sites. It includes excess fresh concrete, wastewater contaminated with fresh concrete, and fresh concrete where the specification did not pass a particular standard for construction. The generation of concrete

1. INTRODUCTION The demand for phosphorus fertilizers is expected to increase as the global population increases. There is an urgent need to develop a process that facilitates the recovery of phosphorus from waste streams. Various methods for removing and recovering phosphorus from wastewater streams have been developed, such as precipitation, biological phosphorus removal, crystallization, ion exchange, tertiary filtration, and sludge treatment.1 Among these phosphorus recovering methods, the crystallization method to produce magnesium ammonium phosphate (MAP: MgNH4PO4) or hydroxyapatite [HAP: Ca10(PO4)6(OH)2] by addition of chemicals is a useful method as it yields materials of high purity.2 Several full-scale plants employing these crystallization methods have already been constructed and operated.3−8 However, the cost of recovering phosphorus is still high compared with the market price of phosphorus. For the crystallization processes, magnesium or calcium sources, alkali substances, and seed materials are generally added to the wastewater. The largest portion of the operational cost is the cost of these chemicals, which accounts for approximately 50% of the total cost of operation.3,4 Approximately 90% of the material cost can be attributed to the cost of the alkali substances such as sodium hydroxide (NaOH).9 Most of phosphorus recovering methods are more expensive than the phosphate recovery cost from phosphate ore, which results in scarce economic incentive for implementing phosphorus recovery technologies.10 The key issue for cost reduction is the use of low-cost materials for © 2012 American Chemical Society

Received: Revised: Accepted: Published: 11266

May 11, 2012 July 23, 2012 August 2, 2012 August 2, 2012 dx.doi.org/10.1021/ie301225g | Ind. Eng. Chem. Res. 2012, 51, 11266−11273

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2. MATERIALS AND METHODS 2.1. Materials. Real concrete sludge generated at the Kawashima-Daini Plant of the East Nippon Concrete Company Ltd., Chikusei, Japan, was used for the preparation of the phosphorus adsorbents. In this plant, concrete poles and piles are produced by a centrifugal molding method. The concrete sludge was from excess fresh concrete used in the molding process. The excess concrete was diluted with water to form concrete sludge, and transferred to the waste treatment site in the plant. There, the aggregate components were recovered by sieving. This study used samples of the sludge after sieving. The density of the concrete sludge was 1.3 × 103 kg/m3. Table 1

sludge is inevitable, and several percent of fresh concrete prepared is typically disposed of as concrete sludge. Concrete sludge has been disposed of as an industrial waste after neutralization because it is strongly alkaline. The main solid component of concrete sludge is calcium, originating from the cement component of the concrete. Various methods for concrete sludge recycling have been investigated so far, such as reuse as raw material for cement, as road bed materials, soil neutralizers, neutralizers for incinerator waste, and fine aggregate for concrete production. Reuse as a recycled soil by mixing with construction sludge,29 a raw material for highfluidity concrete,30,31 sludge water recycling for concrete production,32 in alkaline stabilized biosolids,33 a concrete sludge-based geopolymer,34 in glass-ceramics,35 water clarification materials,36−38 as a calcium source for the mineral carbonation process for global warming mitigation,39,40 and as a desulfurization agent41 have also all been investigated. However, at present this waste is sent to a landfill after solid/ liquid separation and neutralization with acid, at a cost of around 60 USD per metric ton of concrete sludge. The cost of disposal of waste concrete increases the construction cost of concrete buildings and products. From the material point of view, concrete sludge is strongly alkaline, and rich in calcium. In addition, the concrete sludge is generated as a slurry of solid powder in water. Thus, concrete sludge can act as the calcium source, hydroxide source, and seed crystal for HAP crystallization from wastewater streams containing phosphorus. Thus, concrete sludge can be regarded as a candidate raw material for a phosphorus recovery method based on crystallization of HAP. In this study, we developed a new type of solid material for phosphorus recovery derived from concrete sludge, namely, PAdeCS (Phosphorus Adsorbent Derived from Concrete Sludge), and examined its performance in phosphorus recovery from synthetic wastewater. The expected phosphorus recovery reaction for the present system is as follows: 10Ca 2 + + 6PO4 3 − + 2OH− → Ca10(PO4 )6 (OH)2 ↓

Table 1. Chemical Composition of a Concrete Sludge Sample composition [wt %] a

CaO

SiO2

Al2O3

Fe2O3

othersa

17.2

3.2

0.6

1.9

77.1

Others are mainly water and hydration water.

shows the chemical composition of typical concrete sludge samples measured with an X-ray fluorescence analyzer (XRF, Rigaku ZSX Primus II). The concrete sludge is mainly composed of water and hydration water, while the major solid component is calcium (the calcium oxide (CaO) weight fraction is 17.2 wt %). Thus, the dilution ratio of cement can be estimated to be about four times, based on the normal calcium content of Portland cement of (64.4 wt %). This is as expected, since cleaning a cement production facility usually causes water dilution of the sludge. It should be noted that concrete sludge samples could be entirely hardened after several hours without further treatment. This hardening occurs because of hydration reactions of the cement components. To avoid the hardening, the concrete sludge was further diluted with water, and the dilution ratio is expected to be one of the key factors determining the phosphorus recovery performance of PAdeCS. Reagent grade or higher quality chemicals were purchased from Wako Pure Chemical Industries Ltd., Osaka, Japan, and used for all experiments. 2.2. Methods. 2.2.1. Preparation of Phosphorus Adsorbent from Concrete Sludge. The concrete sludge was first diluted with distilled water. Dilution ratio by weight varied from 1 (undiluted) to 15. The dilution ratio is expected to affect the products of hydration of the cement components in concrete sludge. Then, the diluted concrete sludge was stirred at 1000 rpm with a magnetic stirrer for 60 min. During this treatment, cement compounds in concrete sludge were hydrated and partially dissolved into the water phase. Hydrated concrete sludge was then filtered with a filter press (Nihon Rokasouchi Co. Ltd., φ80 × 1 room, test filter press). The pressure and time for the filter press were 0.5 MPa and about 25 min, respectively. A filter fabric with air permeability of 420 mL/ cm2/min was used. The obtained concrete sludge cake was then dried overnight. Two drying methods were investigated: natural drying (at 25 °C) and forced drying (at 105 °C). The drying methods are also expected to affect the hydration products of the cement components in the concrete sludge. Dried samples were pulverized in a mortar and classified with a sieve of 106 μm. The fine particles, with diameter of less than 106 μm, were used as phosphorus adsorbents. Table 2 summarizes the preparation conditions for each adsorbent and the resultant Brunauer−Emmett−Teller (BET) surface areas. BET surface areas were analyzed with a nitrogen-adsorption BET analyzer

(1)

Alkali calcium compounds in concrete sludge, such as calcium hydroxide or unhydrated cement compounds are dissolved in water, and generate calcium and hydroxide ions. Phosphorus ions in wastewater are then precipitated as HAP. As far as the solubility products are concerned, hydroxyapatite (HAP) has the lowest solubility product among the possible compounds in the present system. It is also clear that calcium hydroxide, a main compound of the cement hydration with a relatively high solubility product, could be dissolved into water. However, precipitates of the phosphorus recovery reaction could be other chemical forms including dicalcium phosphate dihydrate (DCPD), dicalcium phosphate anhydrous (DCPA), octacalcium phosphate (OCP), tricalcium phosphate (TCP), hydroxyapatyte (HAP), and amorphous calcium phosphate (ACP). Among these compounds, the solubility product of HAP is the smallest among these compounds under the pH above 4.5.42 However, it has been reported that ACP or DCPD could precipitate under the conditions with higher degrees of oversaturation, and they would be gradually transformed to HAP.43−45 Generation of these other calcium phosphates should be also considered. 11267

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Table 2. Preparation Conditions for Each Adsorbent, and Resultant BET Surface Areas adsorbent

dilution ratio [g/g]

hydration time [min]

drying temp. [°C]

BET surface area [m2/g]

N-UT N-5 N-10 N-15 F-UT F-5 F-10 F-15

not diluted 5 10 15 not diluted 5 10 15

− 60 60 60 − 60 60 60

25 25 25 25 105 105 105 105

16 a 23 a 11 17 27 17

a

Not measured.

(BEL Japan BELSORP II mini). The surface area of the adsorbent may depend on various factors. The surface area of these adsorbents would be the reflection of the particle size of the adsorbent: no porous structure in the adsorbent. The difference of the BET surface area is due to the difference in the particles size, which is not strictly controlled during the preparation process. The phosphorus adsorbent was named “PAdeCS”, short for “Phosphorus Adsorbent derived from Concrete Sludge”. 2.2.2. Phosphorus Recovery Experiments. Phosphorus recovery experiments were conducted using a polymethylpentane (PMP) beaker with an inner volume of 1.5 L. The solution was stirred at approximately 650 rpm with a three-bladed propeller (φ = 80 mm). All experiments were conducted at room temperature (25 °C). The synthetic wastewater (100 mgP/L) was prepared using potassium dihydrogen phosphate (KH2PO4) and deionized water. After the addition of adsorbent (3 g) to the synthetic wastewater (1.5 L), aliquots of the mixture were collected intermittently and filtered through a polyethersulfone membrane filter having a 0.2 μm mesh (Puradisc 25 AS, Whatman, Ltd.). The concentrations of phosphorus and calcium were determined by inductively coupled plasma-atomic emission spectrometry (ICP-7510, Shimadzu Corp., Kyoto, Japan). The pH of the solution was intermittently measured with a pH meter (TES-1380, Custom Corp., Tokyo, Japan). After phosphorus recovery experiments, adsorbents were filtered with filter paper and dried overnight at 25 °C. The adsorbents before and after the experiments were also analyzed using X-ray diffraction (XRD; Ultima IV, Rigaku Ltd., Tokyo, Japan) and observed by scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM-EDX, S-4800, Hitachi, Tokyo, Japan). All the runs were conducted once for a given experimental condition except some conditions, and it was confirmed from the repeated experiments that experimental error for the phosphorus removal experiments was lower than10%.

Figure 1. Time variation of phosphorus concentration in water after addition of naturally dried concrete sludge-derived adsorbents.

Figure 2. Changes of calcium concentration during phosphorus recovery experiments using naturally dried samples.

Figure 3. Changes of pH during phosphorus recovery experiments using naturally dried samples.

3. RESULTS AND DISCUSSION 3.1. Filterability of Adsorbent. Filterability of the adsorbent is practically important for the treatment of the concrete sludge. A shorter filtration time is better for the treatment and preparation of the adsorbent. The filtration experiments showed that the filtration time increased with the dilution ratio, that is, the water content in the concrete sludge. After filtration, the sludge cake was obtained; the cake obtained from the sludge with dilution ratio of 15 contained the least amount of water. The dehydration of the concrete sludge with lower dilution ratios, such as 5, was difficult, and only a slurry

form cake with a relatively high-water content was obtained. From the viewpoint of filtration, a higher dilution ratio is favorable. 3.2. Phosphorus Recovery Experiments. Figure 1 shows the time variation of the phosphorus concentration in the synthetic wastewater treated with the naturally dried concrete sludge-derived adsorbents (N-UT to N-15, prepared using different dilution ratios). For all cases, the phosphorus 11268

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Figure 4. Time variation of phosphorus concentration in water after addition of force dried concrete sludge-derived adsorbents.

Figure 7. XRD patterns of the prepared adsorbents before phosphorus recovery experiments.

Figure 5. Changes of calcium concentration during phosphorus recovery experiments using force dried samples.

Figure 8. XRD patterns of the adsorbents after phosphorus recovery experiments.

during the phosphorus recovery experiments. The calcium concentration rapidly increased immediately after the addition of the adsorbents. This result indicates that calcium ions were dissolved into water from the adsorbent. After the initial increase, the calcium concentration decreased, presumably owing to the deposition of hydroxyapatite via reaction with phosphorus ions. The calcium concentration in the solution is determined by the material balance of the calcium dissolution rate and the HAP precipitation rate. Thus the increase of calcium concentration can be attributed to the fact that the calcium elimination rate is smaller than the calcium dissolution rate from the adsorbents. On the other hand, pH of the solution increased rapidly after addition of adsorbent, and then decreased gradually, which corresponds to dissolution into the aqueous phase from the adsorbent and consumption of hydroxyl ions up taken in hydroxyapatite, respectively. The final pH of the solution was almost 9 for all cases. Figure 4 shows the time variation of the phosphorus concentration in synthetic wastewater treated with force dried concrete sludge-derived adsorbents (F-UT to F-15, prepared with different dilution ratios). The phosphorus recovery performance of the force-dried adsorbents was superior to that of the naturally dried adsorbents. The phosphorus concentration rapidly decreased to 1 mg-P/L, except for the F-15 system. The best performance was observed for the adsorbent with the dilution ratio at 10 (F-10), as also found for

Figure 6. Changes of pH during phosphorus recovery experiments using force dried samples.

concentration decreased rapidly within the initial 5 min, and gradually decreased after that. The best performance was observed for the adsorbent with 10-times dilution (N-10). However, no clear effects of the dilution ratio on the phosphorus recovery performance were observed within the conditions studied. The phosphorus adsorption amounts after 4 h were in the range of 31−37 mg-P per g-adsorbent. Figures 2 and 3 show changes in the calcium concentration and pH 11269

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Figure 9. SEM images of the adsorbents before and after phosphorus recovery. (a) N-10, (b) N-10 after phosphorus recovery, (c) F-10, and (d) F10 after phosphorus recovery.

Figure 10. SEM and elemental mapping images of the adsorbent N-10 after phosphorus recovery experiment.

ent, and decreased for all dilution ratios. In general, the observed calcium concentrations are higher than those observed for the cases using naturally dried adsorbents. Figure 6 shows the change of pH of the solution. The pH is higher than observed in the tests with naturally dried adsorbents. These results suggest that the dissolution rate of alkali calcium compounds, such as calcium hydroxide, Ca(OH)2, should be accelerated by the forced drying at 105 °C. This is the reason for the higher phosphorus recovery performance of the forcedried adsorbents. 3.3. Characterization of the Adsorbents, PAdeCs. Figure 7 shows the XRD patterns of the prepared phosphorus adsorbents. The observed reflections in the XRD patterns could not be assigned well, and the influence of dilution ratio and

the naturally dried adsorbents. The phosphorus concentration rapidly decreased during the initial few minutes, and the final phosphorus concentration was 0.83 mg/L after 4 h. The amounts of phosphorus adsorbed after 4 h were in the range of 36−50 mg-P per g-adsorbent. The adsorption amount obtained under the present conditions is not the maximum adsorption capacity, because an excess amount of adsorbent was used. The lowest phosphorus recovery performance was observed for F15. The influence of dilution ratio on phosphorus recovery performance was also unclear. Figure 5 shows the change of calcium concentration during the phosphorus recovery experiments using force-dried adsorbents prepared with different dilution ratios. The calcium concentration increased immediately after adding the adsorb11270

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Figure 11. SEM and elemental mapping images of the adsorbent F-10 after phosphorus recovery experiment.

method thus can be applicable to the capturing process of phosphorus from wastewater stream. The present method is essentially the same and based on the HAP method, in which alkaline, calcium, and seed crystals are used to form HAP from the dissolved phosphorus ions. The adsorbents derived from concrete sludge can simultaneously work as alkaline, calcium, and seed crystal simultaneously. Although the present adsorbents would not exceed the ones derived from pure chemicals compared by weight base because waste concrete contains many kinds of inactive compounds in it, the adsorbent developed in this study has a great advantage in terms of cost reduction. Concrete sludge is basically free of charge, and the adsorbent preparation cost is low because of its simple operation. In addition, the use of waste concrete sludge can lead to further cost reduction because waste treatment cost of this alkaline waste can be reduced. In this study, synthetic wastewater was used for the phosphorus removal experiments. It has been reported that some coexisting chemicals, such as carbonate ions, organic acids, and magnesium ions could retard the crystallization of HAP, and these effect shall be elucidated in future work.

drying method were unclear. This is because the hydration products of cement are fundamentally very complex, and generally have low crystallinity. Only reflections for the calcite type calcium carbonate (CaCO3), calcium hydroxide [Ca(OH)2], and silica (SiO2) were observed. The calcite would be derived from dissolved carbonate ions in the water. Figure 8 shows the XRD patterns of the adsorbents after the phosphorus recovery experiments. Very weak amorphous halos, which can be assigned to hydroxyapatite, were observed at 32°. Reflections which can be assigned to other calcium phosphates were not clearly observed. No obvious influence of dilution ratio or drying method on phosphorus recovery products was observed. From the above results of XRD patterns, the formation of HAP was confirmed, which is consistent with the thermodynamic consideration that the solubility product of HAP is smallest among the possible phosphates for the present system. However, the formation of other phosphate such as amorphous calcium phosphate (ACP) or dicalcium phosphate dehydrate (DCPD) could occur prior to HAP formation. Figure 9 shows the SEM images of the adsorbents before and after phosphorus recovery. After phosphorus recovery by the adsorbent N-10, plate-like products were generated [Figure 9b]. These plate-like products were not observed for F-10 [Figure 9d]. Thus, there must be some differences in the chemical or physical form of the phosphorus recovery products produced by naturally dried and force dried adsorbents. The shape of these plate-like products was completely different from the shape of the original adsorbent particles [Figure 9b]. Thus, in this case, nucleation and growth of calcium phosphates, mainly HAP with low crystallinity, must also occur at sites other than the surface of the phosphorus adsorbent N-10. Figures 10 and 11 show the elemental mapping images of N-10 and F-10 after phosphorus recovery. In both cases, phosphorus element is distributed over all surfaces of the solid particles, along with calcium and oxygen. The plate-like products observed in Figure 9b seem to contain only calcium, phosphorus, and oxygen. Thus, these plate-like products have been generated by homogeneous nucleation in the bulk solution. 3.4. Process Feasibility. The above results of the phosphorus removal experiment showed that the adsorbent derived from real concrete sludge showed phosphorus removal performances without any other additional chemicals. This

4. CONCLUSIONS The adsorbent prepared from real concrete sludge (PAdeCS) showed phosphorus recovery capacity from synthetic wastewater of which the initial phosphorus concentration was 100 ppm. The recovery mechanism is the crystallization of HAP from the phosphorus in the wastewater and calcium ions and hydroxyl ions dissolved from the adsorbent. The phosphorus recovery capacity depended on the preparation conditions such as the dilution ratio and the drying temperature. The drying at 105 °C greatly improved the phosphorus recovery capacity of the adsorbents. The effect of the dilution ratio of water is not clear, but the adsorbent with dilution ratio 10 showed the highest phosphorus recovery performance. These results demonstrated that the adsorbent, of which the production cost is much lower than other sorbents for phosphorus recovery, can be applicable to the phosphorus recovery process from wastewater stream for fertilization use. 11271

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AUTHOR INFORMATION

Corresponding Author

*Phone: +81 222175214. Fax: +81 222175214. E-mail: iizuka@ tagen.tohoku.ac.jp. Notes

The authors declare no competing financial interest.

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ACKNOWLEDGMENTS

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REFERENCES

The authors would like to gratefully acknowledge Mr. Yusuke Tsunashima of Seikei University and Ms. Miyuki Takahashi of Tohoku University for their support in the phosphorus recovery experiments and analytical work.

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dx.doi.org/10.1021/ie301225g | Ind. Eng. Chem. Res. 2012, 51, 11266−11273