LLMC is an innovativ e and eco - friendly technology for ammonium salts production ; ED can concentrate efficient ly ammonium salts ; Concentrated ammonium salts can be obtained by means of integration processes ( LLMC and ED ) ; Ammonium salts produced can be used as liquid fertilizersPostprint (author's final draft

Bhushan, Brij

Cortina Pallás, José Luís

Gibert Agulló, Oriol

López Rodríguez, Julio

Reig i Amat, Mònica

Valderrama Angel, César Alberto

Vecino Bello, Xanel

UPCommons. Portal del coneixement obert de la UPC

waterenergynexus.org							ISSN:		XXXX-XXXX		2nd	WaterEnergyNEXUS	–	International	Conference	  Integration	of	liquid-liquid	membrane	contactors	and	electrodialysis	for	ammonia	recovery	from	urban	wastewaters	X.	Vecino	1,	M.	Reig	1,	B.	Bhushan	1,	J.	López	1,	O.	Gibert	1,	C.	Valderrama	1,	J.L.	Cortina	1,2	1	Chemical	Engineering	Department,	UPC-Barcelona	TECH;	Barcelona	Research	Center	for	Multiscale	Science	and	Engineering,	C/	Eduard	Maristany	10-14,	Campus	Diagonal-Besòs,	08930	Barcelona,	Spain.	2	CETaqua,	Carretera	d'Esplugues,	75,	08940	Cornellà	de	Llobregat,	Spain.	 Highlights:	LLMC	is	an	innovative	and	eco-friendly	technology	for	ammonium	salts	production;	ED	can	concentrate	efficiently	ammonium	salts;	Concentrated	ammonium	salts	can	be	obtained	by	means	of	integration	processes	(LLMC	and	ED);	Ammonium	salts	produced	can	be	used	as	liquid	fertilizers.	Keywords:	ammonium	valorization;	ammonium	salts;	wastewater	treatment;	liquid	fertilizers;	liquid-liquid	contactors;	electrodialysis	concentration.	1. Introduction	Nowadays,	reactive	nitrogen	compounds	are	excesive	released	into	the	environement	due	to	industrial	and	urban	wastewaters.	A	huge	environmental	 challenge	exists	due	 to	 these	compounds,	 such	as	nitrogen	oxides	 (NO	and	NO2),	 nitrous	 oxide	 (N2O),	 ammonia	 (NH3),	 ammonium	 (NH4+)	 and	 nitrate	 (NO3)	 pollute	 the	 environement	 and	endanger	human	health	 (Sareer	 et	 al.	 2016).	 In	 addition,	 the	 circular	 economy	policy	proposes	 actions	 that	will	contribute	to	"closing	the	loop"	of	product	 lifecycles	through	greater	recycling	and	re-use,	and	bring	benefits	for	both	 the	 environment	 and	 the	 economy.	 From	 this	 point	 of	 view,	 two	 innovative	membrane	 technologies	 are	proposed	 to	 valorizate	 the	 ammonia	 present	 in	 urban	 wastewaters	 by	 separating	 and	 concentrating	 it	 as	ammonium	 salts:	 liquid-liquid	 membrane	 contactors	 (LLMC)	 (Licon	 Bernal	 et	 al.,	 2016)	 and	 electrodialysis	 (ED)	(Reig	et	al.,	2014).	Using	 LLMC	 is	possible	 to	 separate	and	 recover	 the	ammonia	 from	urban	wastewater	as	ammonium	phosphate	(NH4H2PO4),	using	an	acid	stripping	solution	(e.g.,	phosphoric	acid).	Besides,	ED	allows	to	 increase	the	NH4H2PO4	concentration	 in	 order	 to	 reach	 the	 required	 nitrogen	 and	 phosphorous	 concentration	 to	 be	 used	 as	 liquid	fertilizer.	Environmental challenge Eutrophication Industrial application Liquid fertilizers ED process LLMC process 1 2 3 	Figure	1.	Integration	of	LLMC	and	ED	membrane	technologies	for	ammonia	revalorization	as	liquid	fertilizers.	Xanel	Vecino/	Proceedings	of	WaterEnergyNEXUS-2018	2. Material	and	Methods	A	liquid-liquid	membrane	contactor	was	supplied	from	3M	Company	(USA)	to	conduct	the	experiments	at	lab-scale	(2.5x8	 Liqui-Cel	 X-50	 PP	 fiber).	 Urban	 wastewaters	 from	 regenerated	 zeolites	 were	 used	 as	 feed	 solution,	containing	1.6	g	NH3/L	at	pH	12	in	a	60	L	tank	(lumen	side),	whereas	0.5	L	of	0.4	mol/L	phosphoric	acid	were	used	as	 stripping	 solution	 (shell	 side).	 Both	 streams	 circulated	 through	 the	 LLLMC	 pumped	 at	 450	 mL/min	 and	recirculated	back	into	its	respective	tanks	at	room	temperature	during	12	h.		Afterwards,	the	ammonium	phosphate	solution	obtained	from	LLMC	was	fed	into	an	ED	system	supplied	by	PCCell	GmbH	(Germany),	named	PCCell	ED	64-004.	The	ED	system	worked	with	5	cell	pairs	of	membranes	(64	cm2	active	area	each	one)	from	two	different	companies:	Fujifilm	and	PCCell.	1L	of	NH4H2PO4	solution	was	used	to	feed	the	electrode	rinse,	diluate	and	concentrate	compartments.	The	first	one	was	pumped	at	90-100	L/h,	while	the	others	were	pumped	at	15-20	L/h	through	the	ED	stack.	Experiments	were	carried	out	at	constant	voltage	of	7.5	V,	taking	into	account	the	voltage	drop	of	the	system	(2.5	V	across	the	electrodes	and	1	V	for	each	chell	pair	(5	V)),	using	a	power	cell	HCS-3202	supplied	by	Manson	Engineering	Industrial	(Hong	Kong).	The	 liquid	fertilizer	composition,	after	these	processes,	was	expressed	for	ammonia	as	%N	and	for	phosphate	as	%P2O5.		3. Results	and	Discussion	Ammonia	removal	from	urban	wastewaters	using	LLMC	was	86±3%	(at	the	lumen	side),	whereas	its	concentration	factor	was	34±2%	after	12	h	(in	the	shell	side).	Moreover,	it	was	possible	to	recover	it	as	ammonium	phosphate	at	the	shell	side,	containing	5.0±0.1%	of	N	and	14.9±2.2%	of	P2O5.	a)	 b)	0	200	400	600	800	1000	1200	1400	1600	1800	0	 4	 8	 12	NH3	(mg/L)	Time	(h)	 	0 4 8 12 16 20 0 4 8 12 Mass concentration (%) Time (h) P2O5 N 		Figure	2.	a)	Ammonia	evolution	in	the	feed	side	and	b)	N	and	P2O5	evolution	in	the	stripping	side	over	time.		The	 ammonia	 phosphate	 produced	 in	 the	 LLMC	 was	 subsequently	 concentrated	 by	 ED.	 It	 was	 possible	 to	concentrated	the	ammonium	salt	by	51±1	%	and	54±2	%	using	PCCell	and	Fujifilm	membranes,	respectively,	after	almost	4	h	of	operation	process.	0 2 4 6 8 10 0 1 2 3 4 NH4H2PO4  concentration (%) Time (h) PCCell Fujifilm 	Figure	3.	NH4H2PO4	evolution	in	concentrated	stream	by	ED	process.	Xanel	Vecino/	Proceedings	of	WaterEnergyNEXUS-2018	4. Conclusion	To	summarize,	by	the	integration	of	LLMC	and	ED	as	innovative	membrane	technologies	was	possible	to	separate,	concentrate	 and	 valorize	 ammonia	 present	 in	 urban	 wastewaters	 as	 ammonium	 phosphate.	 This	 salt	 solution	could	be	used	as	liquid	fertilizer	in	the	agriculture	sector,	promoting	in	this	way	a	circular	economy	scheme.	References	Licon	Bernal	E.E.,	Maya	C.,	Valderrama	C.,	Cortina	J.L.,	Valorization	of	ammonia	concentrates	from	treated	urban	wastewater	using	liquid-liquid	membrane	contactors,	Chem.	Eng.	J.	302	(2016)	641-649.	Reig	 M.,	 Casas	 S.,	 Aladjem	 C.,	 Valderrama	 C.,	 Gibert	 O.,	 Valero	 F.,	 Centeno	 C.M.,	 Larrotcha	 E.,	 Cortina	 J.L.,	Concentration	 of	 NaCl	 from	 seawater	 reverse	 osmosis	 brines	 for	 the	 chlor-alkali	 industry	 by	 electrodialysis,	Desalination	2	(2014)	107-117.	Sareer	O.,	Mazahar	S.,	Al	Khanum	Akbari	W.M.A.	and	Umar	S.,	Nitrogen	pollution,	plants	and	human	health,	Plants,	Pollutants	and	Remediation	1	(2016)	27-61.	Acknowledgments	This	research	was	supported	by	the	Waste2Product	project	(CTM2014-57302-R)	and	by	R2MIT	project	(CTM2017-85346-R)	 financed	 by	 the	 Spanish	 Ministry	 of	 Economy	 and	 Competitiveness	 (MINECO)	 and	 the	 Catalan	Government	(ref.	2017-SGR-312),	Spain.	As	well,	Xanel	Vecino	thanks	MINECO	for	her	Juan	de	 la	Cierva	contract	(ref.	IJCI-2016-27445)	and	Julio	López	for	his	pre-doctoral	grant	(ref.	BES-2015-075051).	

Integration of liquid-liquid membrane contactors and electrodialysis for ammonia recovery from urban wastewaters

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Integration of liquid-liquid membrane contactors and electrodialysis for ammonia recovery from urban wastewaters

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