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Environmental Technology (United Kingdom) • Volume , Issue , Pages - • November

Phosphate recovery through struvite-family

crystals precipitated in the presence of citric acid:

mineralogical phase and morphology evaluation

Perwitasari D.S. , Edahwati L. , Sutiyono S. , Muryanto S. , Jamari J., Bayuseno A.P.

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Department of Chemical Engineering, Universitas Pembangunan Nasional ‘Veteran’ Jawa Timur, Surabaya, Indonesia

Center for Waste Management, Department of Mechanical Engineering, Diponegoro University, Semarang, Indonesia

Department of Chemical Engineering, UNTAG University, Semarang, Indonesia

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Phosphate recovery through struvite-family crystals precipitated in the presence of citric acid: mineralogical phase and morphology evaluation

D. S. Perwitasariâ,b, L. Edahwatiâ,b, S. Sutiyonoâ,b, S. Muryanto^b,c, J. Jamari^band A. P. Bayuseno^b

aDepartment of Chemical Engineering, Universitas Pembangunan Nasional‘Veteran’Jawa Timur, Surabaya, Indonesia;^bCenter for Waste Management, Department of Mechanical Engineering, Diponegoro University, Semarang, Indonesia;^cDepartment of Chemical Engineering, UNTAG University, Semarang, Indonesia

ABSTRACT

Precipitation strategy of struvite-family crystals is presented in this paper to recover phosphate and potassium from a synthetic wastewater in the presence of citric acid at elevated temperature. The crystal-forming solutions were prepared from crystals of MgCl₂and NH₄H₂PO₄with a molar ratio of 1:1:1 for Mg⁺², NH⁺₄, and PO⁻³₄ , and the citric acid (C₆H₈O₇) was prepared (1.00 and 20.00 ppm) from citric acid crystals. The Rietveld analysis of X-ray powder diffraction pattern confirmed a mixed product of struvite, struvite-(K), and newberyite crystallized at 30°C in the absence of citric acid.

In the presence of citric acid at 30° and 40°C, an abundance of struvite and struvite-(K) were observed. A minute impurity of sylvite and potassium peroxide was unexpectedly found in certain precipitates. The crystal solids have irregular flake-shaped morphology, as shown by scanning electron microscopy micrograph. All parameters (citric acid, temperature, pH, Mg/P, and N/P) were deliberately arranged to control struvite-family crystals precipitation.

ARTICLE HISTORY Received 5 September 2016 Accepted 31 December 2016 KEYWORDS

Precipitation; struvite-family crystals; citric acid; elevated temperature; XRPD Rietveld analysis

1. Introduction

Precipitation of phosphate minerals, namely struvite (MgNH4PO4·6H2O), occurs commonly in process pipes, pumps, and other industrial equipment [1,2]. This occur- rence could lead to significant problems, as the mineral may form scale deposit and thus blocking the pipes. In contrast, engineered struvite precipitation could be carried out to the phosphate and ammonium compounds from effluent of urban wastewaters, liquid manure, and industrial organic waste streams [3]. The resulted struvite crystals may be used as either fertilizer or raw material for the production of phosphorus, and therefore the struvite precipitation is now becoming economically interesting [1].

Extensive research on struvite precipitation has been conducted with the aim at inhibiting scaling problems of pipelines including precipitation in tanks [2]. All reviews conductedso farhave been focused on: (i) struvite solubility product of crystal dissolution patterns of both pure water and water solutions at controlled laboratory conditions [4]; (ii) understanding of the spontaneous struvite precipitation conditions based on the thermo- dynamic modeling of wastewater [5]; and (iii) modeling of struvite precipitation conditions for minimum struvite solubility by an approach of the pH solution [1].Struvite crystals are generallymade up of 9.8 wt.% magnesium,

7.3 wt.% ammonium, 38.8 wt.% phosphate, and 44.1%

water and organic compounds [1]. Struvite usually precipitates as stable white orthorhombic crystals according to the following equation (withn= 0, 1, and 2) [1]:

Mg²⁺+NH⁺₄ +H_nPOⁿ⁻₄ ³+6H₂O

MgNH4PO4·6(H2O)+nH⁺. (1) Struvite is only slightly soluble in water, but its solubility may be greatly enhanced in dilute acidic solutions [6].

Because it has low solubility in alkaline solution, the reac- tion solution may exhibit struvite precipitation. Moreover, factors controlling struvite crystallization in a piping system may include surface roughness of interior pipes.

For example, slower precipitation of struvite may be found in the polyvinyl chloride (PVC), polyethylene plastic pipes, and PVC fittings, but higher, increasing struvite formation may take place in metal pipes [7]. Struvite precipitation may be influenced by an increase in energy caused by vibration or turbulent flow [3] and increasing pH from the released CO2as a result of pressure drop in pipes [8].

Further formation and crystal growth of struvite may be controlled by eliminating the driving force of the reac- tion or restricting the access of ionic species to the growing face of crystals. To some extent, struvite precipitation in the supersaturated solution can be adjusted by additives, which eventually control the characteristics of

CONTACT A. P. Bayuseno [email protected] The Center for Waste Management, Mechanical Engineering Graduate Program, Diponegoro University, Tembalang Campus, Semarang 50275, Indonesia

ENVIRONMENTAL TECHNOLOGY, 2017

http://dx.doi.org/10.1080/09593330.2017.1278795

(18)

Influence of Mn valence state and characteristic of TiO

₂

on the performance of Mn–Ti catalysts in ozone decomposition

Dong Wook Kwon, Geo Jong Kim, Jong Min Won and Sung Chang Hong

Department of Environmental Energy Engineering, Graduate School of Kyonggi University, Youngtong-ku, Suwon-si, Gyeonggi-do, Republic of Korea

ABSTRACT

The effects of physicochemical properties of Mn–Ti catalysts on O₃conversion were examined. The catalysts were prepared by a wet impregnation method that gave manganese supported on various commercial sources of TiO₂. The properties of the catalysts were studied using physicochemical techniques, including Brunauer–Emmett–Teller (BET) surface area analysis, X-ray diffraction (XRD), H₂ temperature-programmed reduction (H₂-TPR), X-ray photoelectron spectroscopy (XPS), and thermal gravimetric analysis (TGA). The O₃decomposition tests of Mn–Ti catalysts with various manganese loadings revealed that the 10 wt% manganese catalyst exhibited optimal, excellent activity. The O₃ conversion and Mn valence state of the Mn–Ti catalysts were different, depending on the structure of the TiO₂source. Increasing the O/Ti surface atomic ratio in TiO₂ increased the Mn³⁺ ratio. The Mn³⁺ ratio directly affected the O₃decomposition activity of the Mn–Ti catalyst. When the Mn³⁺ratio was the largest, the catalyst showed the highest activity in O₃ decomposition. The valence state of Mn exposed to the surface was a critical factor in O₃ decomposition by Mn–Ti catalysts.

ARTICLE HISTORY Received 4 March 2016 Accepted 26 December 2016 KEYWORDS

Mn valence state; manganese oxide; ozone; catalytic decomposition; MnOx oxide

1. Introduction

Ozone (O3) has been widely used for oxidation and puri- fication in wastewater treatment and drinking water manufacturing process [1,2]. The tail gas contains ozone that remains after use, so it needs to be removed before discharge. Ozone also occurs in various sources such as office equipment such as laser printers, facsimile machines, and copiers. Ozone in the atmosphere, formed by photochemical reactions between nitrogen oxides and volatile organic compounds (VOCs), can be harmful to humans [3], as it causes photochemical smog and leads to respiratory dis- eases [4]. Ozone has adverse effects on humans and the environment, contributing to asthma, headaches, damaged mucous membranes, and interfering with leaf discoloration and plant growth [5–7]. Ozone concen- trations between 0.1 and 1 ppm can cause the adverse health effects as described above.

Ozone removal methods using adsorption by porous materials such as activated carbon and zeolite have been reported. However, the necessity of replacing used adsorbent due to reduced adsorption capacity is disadvantageous. An alternative, catalytic decomposition, could overcome this disadvantage. Catalytic decomposition has been extensively studied. For

example, Imamura et al. [8] reported that metal oxide catalysts were effective in O3 decomposition, with manganese being the most active among them. Hoke et al. [9] used Pt, Pd, and MnOx as active materials, and coated the catalysts on hot patches on automobile water tanks (surface temperatures of 45–105°C) [10].

Dhandapani and Oyama [11] and Hao et al. [12] prepared manganese and Au/Fe2O3to decompose O3at high con- centrations. In addition, MnOx catalysts with added Pd resisted relative humidity (RH) and slowed the depletion of catalyst activity [13,14]. The above studies revealed that the MnOx-based catalyst showed excellent catalytic activity in O3decomposition. This activity was promoted by the addition of precious metals such as Pt, Pd, and Au to the MnOx-based catalysts. However, further study of the correlation between activity and catalytic characteristics of MnOx-based catalysts is required.

Accordingly, in this study, the catalysts were prepared by the addition of manganese to various TiO2sources to enhance the activity of MnOx-based catalysts in O3

decomposition. The study examined the effects of physicochemical properties of MnOx/TiO2and different Mn valence states on the catalytic activity. It also studied that the catalyst properties using physiochemical ana- lyses, including Brunauer–Emmett–Teller (BET) surface

CONTACT Sung Chang Hong [email protected]; [email protected] Department of Environmental Energy Engineering, Graduate School of Kyonggi University, 94-6 San, Iui-dong, Youngtong-ku, Suwon-si, Gyeonggi-do 443-760, Republic of Korea

ENVIRONMENTAL TECHNOLOGY, 2017

http://dx.doi.org/10.1080/09593330.2016.1278274

(19)

Tailoring the properties of a zero-valent iron-based composite by mechanochemistry for nitrophenols degradation in wastewaters

Giovanni Cagnettaâ, Jun Huangâ, Igor O. Lomovskiy^band Gang Yuâ

aSchool of Environment, State Key Joint Laboratory of Environment Simulation and Pollution Control (SKJLESPC), POPs Research Center, Tsinghua University, Beijing, People’s Republic of China;^bInstitute of Solid State Chemistry and Mechanochemistry, Novosibirsk, Russia

ABSTRACT

Zero-valent iron (ZVI) is a valuable material for environmental remediation, because of its safeness, large availability, and inexpensiveness. Moreover, its reactivity can be improved by addition of (nano-) particles of other elements such as noble metals. However, common preparation methods for this kind of iron-based composites involve wet precipitation of noble metal salt precursors, so they are often expensive and not green. Mechanochemical procedures can provide a solvent-free alternative, even at a large scale. The present study demonstrates that it is possible to tailor functional properties of ZVI-based materials, utilizing high-energy ball milling.

All main preparation parameters are investigated and discussed. Specifically, a copper-carbon- iron ternary composite was prepared for fast degradation of 4-nitrophenol (utilized as model pollutant) to 4-aminophenol and other phenolic compounds. Copper and carbon are purposely chosen to insert specific properties to the composite: Copper acts as efficient nano-cathode that enhances electron transfer from iron to 4-nitrophenol, while carbon protects the iron surface from fast oxidation in open air. In this way, the reactive material can rapidly reduce high concentration of nitrophenols in water, it does not require acid washing to be activated, and can be stored in open air for one week without any significant activity loss.

ARTICLE HISTORY Received 8 July 2016 Accepted 10 January 2017 KEYWORDS

Mechanochemistry; ball milling; zero-valent iron;

ternary composite;

nitrophenols

1. Introduction

Zero-valent iron (ZVI) is a versatile material that has been utilized over the past 20 years for treatment of various organic and inorganic pollutants in wastewater and groundwater [1,2]. Iron is the fourth most abun- dant element by mass in the Earth’s crust, so it is largely available and can be safely spread into the environment [3]. In addition, ZVI can be coupled with other elements, like noble metals (e.g. Pd, Ag, Cu, Ni, etc.), also in nano-particle form [4], or carbonaceous material [5,6], to produce composite materials. In this way, electron transfer from ZVI is boosted by massive formation of galvanic micro-cells [7]. Such composites can be prepared by several methods, but usually they necessitate large volumes of water under controlled conditions [4,8], so their production is expensive and not green. Moreover, due to ZVI perishability in open air, reactive materials are normally stored under inert atmosphere after preparation, determining further costs. Hence, cheaper and greener preparation methodologies are highly required.

High-energy ball milling (HEBM) is a promising technology that allows design and production of enhanced

materials by facile solvent-free procedures [9–12]. Mech- anical energy provided by special milling devices can be used to introduce extraordinary amounts of crystal defects into solids, which acquire very peculiar properties [13]. Moreover, it is possible to carry out at environmental temperature and pressure solid-state mechanochemical (MC) reactions that require high activation energies. Therefore, HEBM can be a green and cost-effective alternative for ZVI-based materials production [14]. Occasionally, HEBM has been applied with success to the preparation of materials for pollutant degradation in water. In some works, properties and reactivity of metal alloys (e.g. Fe–Si, Mg–Al, Mg–Zn- based alloy, etc.) were improved by enhancement of amorphization degree [15–18]; in other works, HEBM was employed to produce catalytic nano-particles (e.g.

Pd, Cu, Ni) supported on other materials (prevalently ZVI, but also AC) [19–21]. In each case, HEBM was simply utilized to aggregate two different components with intrinsic reactivity to form a stable composite or alloy with superior pollutant degradation effectiveness.

Nonetheless, MC methodologies permit a finer tuning of the properties of the milled material. Theoretically, it

CONTACT Jun Huang [email protected] School of Environment, State Key Joint Laboratory of Environment Simulation and Pollution Control (SKJLESPC), POPs Research Center, Tsinghua University, Beijing 100084, People’s Republic of China

Supplemental data for this article can be accessed here:http://dx.doi.org/10.1080/09593330.2017.1282985 ENVIRONMENTAL TECHNOLOGY, 2017

http://dx.doi.org/10.1080/09593330.2017.1282985