Phosphorus Transformation from Municipal Sewage Sludge

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Phosphorus Transformation from Municipal Sewage Sludge Incineration with Biomass: Formation of Apatite Phosphorus with High Bioavailability Yazhou Zhao, Qiangqiang Ren, and Yongjie Na Energy Fuels, Just Accepted Manuscript • DOI: 10.1021/acs.energyfuels.8b01915 • Publication Date (Web): 08 Sep 2018 Downloaded from http://pubs.acs.org on September 9, 2018

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Energy & Fuels

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Phosphorus Transformation from Municipal Sewage Sludge Incineration with

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Biomass: Formation of Apatite Phosphorus with High Bioavailability

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Yazhou Zhaoa,b, Qiangqiang Rena,b,*, Yongjie Naa,b

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a

Institute of Engineering Thermophysics, Chinese Academy of Sciences, Beijing 100190, China b

University of Chinese Academy of Sciences, Beijing 100049, China

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ABSTRACT

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Phosphorus (P) is an essential and limited nutrient element for all life. The recovery

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and reuse of P from municipal sewage sludge (MSS) incineration fly ash are

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considered to be practical and economical. Addition of biomass into MSS was

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proposed to enhance the P bioavailability during incineration. The speciation

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conversion of P during MSS incineration with different types of biomass was studied

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in this work. The chemical reactions between P-containing model compound (AlPO4)

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and mineral model compounds in biomass (CaO and KCl) were investigated to

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simulate the conversion mechanism of non-apatite inorganic phosphorus (NAIP) to

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apatite phosphorus (AP) during MSS incineration with biomass. It is shown that the

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addition of biomass increases the P mass percentage and facilitates the

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transformation of NAIP to AP in fly ash. Cotton stalk has the most positive effect on

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the P transformation in the four biomass samples. Ca, Cl, K, and/or Mg compounds

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in biomass promote the conversion of NAIP (such as AlPO4) to AP (such as Ca2P2O7,

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Ca5(PO4)3Cl, and Ca10K(PO4)7) during MSS incineration. Higher temperature

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stimulates the transformation of NAIP to stable AP. The primary reaction pathway

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ACS Paragon Plus Environment

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between phosphorus and the main components in biomass is revealed. AlPO4 can

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react with CaO to form Ca2P2O7 and Ca3(PO4)2 at 900 oC, and two new P-containing

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compounds, Ca5(PO4)3Cl and Ca10K(PO4)7, are formed in the presence of KCl.

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1. INTRODUCTION

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Phosphorus (P) is a fundamental element for all organisms.1 Particularly,

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sustainable food production for meeting the demands of fast-increasing population

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depends largely on P fertilization in agriculture.2,3 These P fertilizers are mainly

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produced from geological phosphate rocks, which are globally limited4 and will be

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exhausted in 50-100 years at the current mining rate.2 Municipal sewage sludge

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(MSS), a kind of waste, contains a considerable amount of P.5,6 The P recovery from

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MSS is critical.7 However, MSS, containing a variety of organic/inorganic

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contaminants, heavy metals and pathogens, cannot be directly used in agriculture.8,9

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MSS incineration is a frequently employed disposed method because it not only can

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decompose organic contaminants and pathogens, but can dramatically reduce MSS

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volume.10 The reduction of MSS volume can decrease the costs of post-processing

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of MSS, such as its transportation costs. In addition, P is highly concentrated in the

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MSS incineration ash, giving enormous potential for P recovery.11,12

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P speciation in MSS incineration ash is a fundamental factor affecting P recovery

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and reuse, because it greatly determines the mobility and bioavailability of P. In

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incineration ash, inorganic phosphorus (IP) is the predominant phosphorus form and

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apatite phosphorus (AP, Ca/Mg-P), which is bound to Ca/Mg ions, shows high

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bioavailability and can be absorbed directly by plants or used as a raw material in

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fertilizer manufacture.11 In recent years, there has been an increasing number of

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studies on P speciation conversion during thermal treatment of MSS and the

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secondary treatment of the incineration fly ash with various additives. Li et al.7

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confirmed that calcium phosphate (Ca3(PO4)2) and calcium pyrophosphate (Ca2P2O7)

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were generated by the addition of calcium oxide (CaO) into MSS during incineration.

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Han et al.13 found that CaO could stabilize P in incineration ash. Adam et al.14

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indicated that during thermochemical treatment of sludge ashes and Cl-based

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additives, P was converted into new mineral phases with high bioavailability and

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toxic trace metals were removed simultaneously. Additionally, the P speciation was

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reported to be dramatically influenced by the temperature, as high temperatures can

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promote the formation of Ca3(PO4)2, Ca2P2O7, and Ca5(PO4)3(OH).15,16

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MSS incineration with biomass as the new additive was proposed to enhance the

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P bioavailability in the incineration ash and reduce the toxicity of heavy metals. It

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can both eliminate the consumption of mineral resources and avoid the secondary

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pollution in the ash treatment process. Our previous studies demonstrated that the

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addition of cotton stalk (CTS) containing multifarious mineral elements could

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effectively facilitate the P transformation to highly available forms by plants, such as

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Ca18Mg2H2(PO4)14 and Ca2P2O7.17 Meanwhile, MSS combustion with CTS could

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also greatly stimulate the stabilization of Zn and speciation transformation of arsenic

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to arsenates (As5+), dramatically decreasing the toxicity of fly ash.18,19 It is

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advantageous for P utilization and recovery in fly ash. Furthermore, there was not

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corrosion problem during MSS incineration with biomass.20

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However, the P speciation conversion mechanism during MSS incineration with

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biomass remains unknown. Therefore, this work focuses on the effects of biomass

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type and incineration temperature on the speciation conversion of P during MSS

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incineration. To further understand the influences of addition of biomass on the P

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transformation mechanism, the chemical reactions between P-containing model

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compound (AlPO4) and mineral model compounds (CaO and KCl) were studied.

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2. EXPERIMENTAL PROCEDURES

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2.1. Materials. In this work, dewatered MSS was collected from Qinghe

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wastewater treatment plant in Beijing, China. Four kinds of biomass, corn stalk

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(CRS), cotton stalk (CTS), wheat straw (WS), and wood, were obtained from

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Baoding in Hebei Province, China. Raw biomass samples were circular cylinder

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particles (length: 5-10 mm, diameter: 8 mm). MSS and biomass samples were

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crushed into particles less than 4 mm in size and dried for 8 h at 105 oC prior to tests.

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Major chemical compositions of the fuel samples were determined using inductively

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coupled plasma optical emission spectroscopy (ICP-OES). Prior to the ICP-OES

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experiments, the raw fuel samples were broken and sieved to less than 0.2 mm. The

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experiments were performed in the Institute of Process Engineering of China. The

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ultimate analysis, proximate analysis, and major chemical compositions of the fuel

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samples were given in our previous report.21 It was found that the biomass contained

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higher content of Cl than MSS.21 Model compounds (analytical reagent), AlPO4,

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CaO and KCl, were sieved to less than 125 µm before tests.

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The crystal structures in raw fuel samples were analyzed by X-ray powder

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diffraction (XRD). Prior to the XRD test, the raw fuel samples were first ashed.22

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The XRD results of MSS and biomass ash are presented in Figure 1. It is indicated

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that mineral chemical forms in the fuels are obviously different. CaO, MgO, and

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KCl were found in biomass and not in MSS. In particular, CaO could effectively

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promote the transformation of P to phosphates with high bioavailability.11

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2.2. Equipment and Analytical Methods. The incineration tests were performed

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in a 5 kW bubbling fluidized bed. The details of test apparatus and experimental

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procedure were described elsewhere.17,20 Each test was continuously conducted for 4

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h. The reaction tests between model compounds were conducted in an electrically

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heated tube furnace under atmospheric air. The schematics and operation procedure

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of the test system were detailed elsewhere.23 Each test lasted for 1 h in the tube

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furnace.

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X-ray fluorescence spectrometry (XRF, PANalytical, Netherlands) was employed

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to determine the major chemical components of fly ash samples. The crystal

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structures of the ash samples were identified by XRD. The Standards, Measurements,

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and Testing (SMT) protocol was applied for the analyses of phosphorus speciation in

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the ash samples, including total phosphorus (TP), organic phosphorus (OP),

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inorganic phosphorus (IP), non-apatite inorganic phosphorus (NAIP, Fe/Al/Mn-P),

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and apatite phosphorus (AP, Ca/Mg-P).24 The contents of P in different forms were

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analyzed by the molybdenum blue colorimetric method.25

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3. RESULTS AND DISCUSSION

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3.1. Distribution and Speciation of P during MSS Incineration with Biomass.

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It is found that co-firing of 70% MSS with 30% biomass could greatly decrease the

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toxicity of As and Zn in the incineration ash.18,19 The experiment was continued to

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study P behavior on the basis of the experimental results. The distribution of P in

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flue gas, fly ash, and bottom ash during co-firing of 70 wt.% MSS with 30 wt.%

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biomass at 900 oC was studied, as illustrated in Figure 2. Distribution of P was

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defined as the mass ratio of the P content in bottom ash, fly ash or flue gas to the

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total P content in fuel combusted. The P fraction in flue gas was calculated by P

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balance.

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As shown in Figure 2, the sum of P fractions distributed in fly ash and bottom ash

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is as high as 84.70% during MSS incineration alone. The P fraction present in

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bottom ash decreases after co-firing of MSS with biomass, especially with WS, CTS,

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and CRS, while the P fractions distributed in both fly ash and flue gas increase

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slightly. During MSS combustion with biomass, the OP is highly volatile and

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converts to P oxides like P2O5, which is the main source of P in flue gas.26 In this

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work, the fluidization velocity was low to get sufficient residence time and high

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combustion efficiency during incineration in the test bed. This resulted in a

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considerable fraction of ash being discharged in the form of bottom ash. Thereby,

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most P is present in bottom ash, as depicted in Figure 2.

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The P species in bottom ash from MSS incineration with different biomass was

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analyzed through the SMT protocol. It was found that the addition of biomass

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showed little influences on the distribution of P speciation in bottom ash during

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MSS incineration, which was supported by our previous studies.17 To further assess

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the influences of addition of different biomass on the P speciation transformation

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during MSS incineration, the P speciation in co-firing fly ash was studied.

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The main components of fly ash samples from MSS combustion with biomass can

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be found elsewhere.21 The P speciation in fly ash from MSS combustion with

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different biomass at 900 oC was examined according to the SMT protocol. The mass

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ratios of IP/TP, OP/TP, AP/IP, and NAIP/IP in the co-firing fly ash are displayed in

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Figure 3a. IP is the predominant P form in the fly ash. During MSS incineration

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alone, the ratio of NAIP/IP is up to 59.97% while the ratio of AP/IP is only 40.03%,

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showing low bioavailability. The AP/IP ratio in fly ash is enhanced obviously after

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MSS combustion with biomass, especially CTS, with the highest ratio of 56.08%.

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The results confirm that adding biomass into MSS can effectively promote the

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conversion of NAIP to AP while CTS gives a better effect, enhancing the P

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bioavailability in the fly ash.

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The major phosphate minerals in fly ash from MSS combustion with different

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biomass are examined by XRD, as presented in Figure 3b. It is shown that NAIP

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compounds such as AlPO4 are present in the fly ash from MSS combustion alone.

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With the addition of wood, Ca compounds such as CaO in wood can react with

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AlPO4 to form Ca2P2O7 in the fly ash. For the addition of WS, AlPO4 is transformed

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into Ca5(PO4)3Cl and Ca10K(PO4)7 in the co-firing fly ash. In the process of MSS

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combustion with CTS, the Ca, Mg, and Cl matters in CTS stimulate the conversion

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of P to AP, including Ca-Cl-P and Ca-Mg-P compounds. By adding CRS into MSS,

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the abundant elements of Mg and Ca in CRS favor the transformation of AlPO4 to

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new phosphates like Ca2P2O7. Overall, the Ca, Cl, Mg, and K compounds in biomass

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can promote the conversion of NAIP like AlPO4 to AP, such as Ca2P2O7,

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Ca5(PO4)3Cl, and Ca10K(PO4)7, during MSS incineration. In conclusion, the addition

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of biomass is beneficial for P utilization from the fly ash during MSS combustion.

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3.2. Effect of Temperature on P Transformation in Fly Ash from MSS

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Incineration with CTS. The results of the SMT protocol for the fly ash from

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co-firing of MSS with and without CTS at different temperatures are indicated in

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Figure 4. It can be observed from Figure 4a that with the temperature increasing

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from 800 oC to 950 oC, the TP and IP concentrations in fly ash initially increase

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slightly and then decrease, reaching a maximum value at 850 oC. The OP

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concentration is small. The NAIP concentration decreases gradually while the AP

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concentration increases gradually with the increase in temperature. NAIP is highly

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volatile at 950 oC, leading to the decrease in TP and IP contents in the fly ash. In

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contrast, AP is more stable at 950 oC. The fraction of NAIP/IP decreases obviously

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with increasing the fraction of AP/IP at the temperature range from 800 oC to 950 oC,

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as displayed in Figure 4b. This result shows that a higher temperature favors the

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transformation of NAIP to AP. In addition, the results presented in Figure 4a and

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Figure 4b indicate that both the AP content and AP/IP fraction in fly ash, during 70%

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MSS/30% CTS incineration, are larger than those during MSS combustion

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separately at each temperature. This further demonstrates that the addition of CTS

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into MSS can favor the conversion of NAIP to AP during incineration.

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Figure 5 displays the main phosphate phases in fly ash from MSS and 70%

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MSS/30% CTS incineration at different temperatures. As displayed in Figure 5a,

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during MSS incineration alone, NAIP compounds such as AlPO4 and Ca9(Fe,

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Al)(PO4)7 are detected in the fly ash at 800 oC. Increasing the temperature to 950 oC

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promotes the conversion of NAIP to AP (such as Ca3(PO4)2 and Ca2P2O7). For the

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70% MSS/30% CTS incineration case (shown in Figure 5b), with the temperature

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increasing from 800 oC to 950 oC, NAIP like AlPO4 can react with Ca/Cl compounds

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to produce new AP, including Ca5(PO4)3Cl and Ca3(PO4)2. Thereby, a higher

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temperature stimulates the conversion of NAIP to AP by forming new phosphate

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minerals. Combined Figure 5a with Figure 5b, it is concluded that Ca, Cl and/or K

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compounds in CTS can afford additional active sites for P to generate AP at different

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temperatures.

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3.3. Conversion Mechanism of NAIP to AP for Addition of CTS into MSS

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during Incineration. As stated previously, AlPO4 is the major NAIP form in fly ash

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from MSS incineration alone detected by XRD. It can be observed from Figure 1

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that CaO and KCl are detected in CTS. AlPO4, CaO, and KCl were selected as the

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model compounds to analyze the transformation mechanism of NAIP to AP for

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addition of CTS into MSS during incineration. Compared with co-firing of 70%

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MSS and 30% CTS, our previous study found that more AP was formed in the

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combustion process of 50% MSS and 50% CTS.17 To simulate the P reaction

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mechanism during co-firing of MSS with CTS, the mixture of AlPO4 and CaO at a

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molar ratio of 1:1.8, and the mixture of AlPO4, CaO, and KCl at a molar ratio of

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1:1.8:1.4, were heated at 900 oC under atmospheric air for 1 h. The molar ratio of

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AlPO4, CaO, and KCl was determined by the molar ratio of P, Ca, and K in the

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mixture of 50% MSS and 50% CTS.

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The XRD results of model compounds heated at 900 oC are illustrated in Figure 6.

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Ca2P2O7, Ca3(PO4)2 and Al2O3 are detected in the heated product of AlPO4 and CaO,

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showing that AlPO4 can react with CaO to generate Ca-P at 900 oC. In the heated

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mixture of AlPO4, CaO, and KCl, the AlPO4 and Ca3(PO4)2 peaks are not detected,

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while the mineral phases of Ca2P2O7, Ca5(PO4)3Cl, and Ca10K(PO4)7 are observed.

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Based on the results and element balance, the primary reactions between AlPO4 and

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CaO/KCl at 900 oC are concluded to be represented by the following reactions:

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2AlPO4 + 2CaO → Ca2P2O7 + Al2O3

(1)

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2AlPO4 + 3CaO → Ca3(PO4)2 + Al2O3

(2)

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10AlPO4 + 15CaO + KCl → Ca5(PO4)3Cl + Ca10K(PO4)7 + 5Al2O3

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4. CONCLUSION

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(3)

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This present work investigated the P speciation conversion in the combustion

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process of MSS with different biomass. Simultaneously, AlPO4, CaO, and KCl were

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used as model compounds to analyze the conversion mechanism of NAIP to AP

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during MSS incineration with biomass. The results indicate the addition of biomass

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increases the P fraction in fly ash and stimulates NAIP conversion to AP. Cotton

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stalk has the best effects on P transformation out of the four different biomass

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samples. Ca, Cl, K, and/or Mg matters in biomass provide additional reactive sites

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for P to promote the transformation of NAIP like AlPO4 to AP, such as Ca2P2O7,

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Ca5(PO4)3Cl, and Ca10K(PO4)7, during MSS incineration. More NAIP is transformed

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to stable AP with increasing temperature from 800 oC to 950 oC. AlPO4 can react

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with CaO to form Ca2P2O7 and Ca3(PO4)2 at 900 oC. The reactions between AlPO4,

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CaO and KCl occur by producing Ca2P2O7, Ca5(PO4)3Cl, and Ca10K(PO4)7. This

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work proposes a new idea that is used for P recovery and reuse from MSS

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incineration fly ash. Based on the study results, it is potential to find new additives

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to gain higher P bioavailability in the fly ash in the future research work.

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AUTHOR INFORMATION

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Corresponding Author

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*E-mail: [email protected]. Fax: +86-10-82543119. Phone: +86-10-82543055.

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ACKNOWLEDGEMENTS

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This research was supported by Youth Innovation Promotion Association, Chinese

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Academy of Sciences (No. 2015120), and National Natural Science Foundation of

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China (No. 51476169).

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during carbothermic reduction. ISIJ Int. 2008, 48, 912-917.

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Figures 20000

1

MSS

10000

13

Diffracted intensity (CPS)

0 Wood 3000 1

1500 0 20000

4 4 3 5 2 52 1 1 48 6 4 77

WS

0 20000

1 77

CRS 1 8

0 10

1 9

1

10 12 8

10

6

12

1

1 9 6 61

10

10 12 6 12 8 77 8 6 1 11 19 1 6 1

1

15000

1

10

1

CTS

10000

1

6

10 11 8

10000

0 30000

20

13

4 13 8 6

16 1

30

40

19

1

1

50

60

1 70

80

2θ/(°)

1-SiO2; 2-Ca9Fe(PO4)7; 3-NaAlSi3O8; 4-KAlSi3O8; 5-MgCa2(PO4)2(H2O)2; 6-CaO; 7-K2SO4;

8-CaAl2Si2O8; 9-MgO; 10-KCl; 11-KAl3Si3O10(OH)2; 12-Ca2SiO4; 13-CaSO4 Figure 1. XRD results of municipal sewage sludge and biomass ash.

Bottom ash

70 Distribution of phosphorus (%)

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60

Page 16 of 20

Fly ash

Flue gas

60 50 40 30 20 10 0

MSS

70% MSS /30% Wood

70% MSS /30% WS

70% MSS /30% CTS

70% MSS /30% CRS

Figure 2. Distribution of P in flue gas, fly ash, and bottom ash during co-combustion of MSS with biomass at 900 oC.

16


Page 17 of 20

OP/TP

(a) 100

IP/TP

NAIP/IP

AP/IP

Fraction (%)

80

60

40

20

0

(b)

MSS

70% MSS /30% Wood

70% MSS /30% WS

70% MSS /30% CTS

70% MSS /30% CRS

1

20000

MSS

10000

1 66 52 70% MSS 1 /30% Wood

2

4

0 12000 Diffracted intensity (CPS)

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60

Energy & Fuels

6000

1

0 6000

70% MSS /30% WS 1

3000 0 20000 10000 0 8000

45 3 3 1 6

1

1

1

4 2 7 4 3 37 61 1 7 1

1

1

1

1

1

1

1

1

1

1

50

60

9 2

2 4

8 8 3 931 11 1 70% MSS 1 /30% CTS 1 11 2 11 10 10 10 2 8 3 31 1 1 8 70% MSS 1 /30% CRS 7

1

4000

2 12 7 2 7 3 31 1 1

1

1

0 10

20

30

40

70

80

2θ/(°)

1- SiO2; 2-KAlSi3O8; 3-Fe2O3; 4-Ca9(Fe, Al)(PO4)7; 5-Ca4(Fe, Mg)5(PO4)6; 6-AlPO4; 7-Ca2P2O7; 8-Ca5(PO4)3Cl; 9-Ca10K(PO4)7; 10-Ca18Mg2H2(PO4)14; 11-KH5(PO4)2; 12-Ca9MgK(PO4)7 Figure 3. Speciation of P in the fly ash from MSS combustion with biomass at 900 oC: (a) SMT results, (b) XRD results.

17


Energy & Fuels

TP

(a) 60

OP

MSS

IP

NAIP

AP

OP/TP

(b) 120

IP/TP

MSS

70% MSS/30% CTS

50

100

40

80

Fraction (%)

Phosphorus concentration (g/kg)

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60

Page 18 of 20

30 20 10

NAIP/IP

AP/IP

70% MSS/30% CTS

60 40 20

0 800

850

900

950 800 850 o Temperature ( C)

900

0

950

800

850

900

950 800 850 o Temperature ( C)

900

950

Figure 4. Fraction of P in the fly ash from MSS combustion with CTS at different temperatures: (a) P concentration, (b) SMT results.

18


Page 19 of 20

(a)

800 C

2 1 55

0 10000


1

o

10000 5000

o

850 C

5000

2 4 4 3 35 5 1

1 5 5 62 24 46 3 31 5 o 1 900 C 2

0 20000 10000

1 55 7 2

0 10000

1

1

1

1

1

1

1

1

1

1

1

1

50

60

1

1

1

1

1

4

1 473 3 5

1

o

950 C

5000

19 2 2 8 89 3 31 1 9 1 0 10

20

30

40

70

80

2θ/(°) (b)

1

o

800 C

10000 5000


1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60

Energy & Fuels

1

0 10000

10 10 1 2 9 2 9 3 3 5 1

1

o

850 C

2 11 1 9 9 9 2 3 31

5000 0 20000

1 11

1

o

900 C

11 1 13 13 12 2 12 11 12 2 3 31 1 1

10000 0 10000

1

1

1

50

60

1

1

o

950 C

1 14 11 14 1 2 8 83 3 1

5000

1

11

1

0 10

20

30

40

70

80

2θ/(°)

1-SiO2; 2-KAlSi3O8; 3-Fe2O3; 4-Ca9(Fe, Al)(PO4)7; 5-AlPO4; 6-Ca4Mg5(PO4)6; 7-Ca4(Fe, Mg)5(PO4)6; 8-Ca3(PO4)2; 9-Ca2P2O7; 10-Ca9Fe(PO4)7; 11-Ca5(PO4)3Cl; 12-Ca18Mg2H2(PO4)14; 13-KH5(PO4)2; 14-Ca10K(PO4)7 Figure 5. XRD results of the fly ash from MSS combustion with CTS at different temperatures: (a) MSS, (b) 70% MSS/30% CTS.

19


Energy & Fuels

8800 Diffracted intensity (CPS)

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60

0 8800

2

AlPO4+CaO

2

2 1 3 5 345 1

4400

Page 20 of 20

2 2

2

AlPO4+CaO+KCl

6 4400

0

3 2 6 7 2 7 8 8 7 37 75 5 10

20

30

40

50 2θ/(°)

60

2 65

6

70

80

90

1-AlPO4; 2-CaO; 3-Ca2P2O7; 4-Ca3(PO4)2; 5-Al2O3; 6-KCl; 7-Ca5(PO4)3Cl; 8-Ca10K(PO4)7 Figure 6. XRD patterns of model compounds heated at 900 oC.

20


Phosphorus Transformation from Municipal Sewage Sludge

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