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We deliver Phosphorus made in

Europe

PHOSPHORUS RECOVERY FROM DRIED SLUDGE WITH REACTIVE EXTRACTION TO REMOVE IMPURITIES 5th ECSM, 08.10.19, Liège, Belgium

Shariff Z.A., Fraikin L., Léonard A., Pfennig A.

[email protected]

PEPs - Department of Chemical Engineering, Université of Liège

mailto:[email protected]

agenda

• PULSE process concept

• process development

– SLE modelling

– cascaded option tree

• experimental results

• summary

8th October 2019, Liège | 5th ECSM | Zaheer Shariff | PEPs - ULiège | Slide n° 2

PULSE (Phosphorus University of

Liege Sludge Extraction) process


acid

organicsolventbase/Ca

drying leaching separation

reactiveextraction

re-extractionCaP

solid waste

metals

precipitation

dewateredsludge

wastewater

re-extraction agent/NH3

P + impurities

solid-liquid-liquid equilibrium

• aqueous phase speciation:– mass balance

– law of mass action

– charge balance

• solid precipitation:

– saturation index

• activities instead of concentration to account for ionic interactions

• degree of reactive extraction with organic solvents

• evaluation of model parameters by data fitting




-1 0 1 2 3 4 5 6 7 8 91E-6

1E-5

1E-4

0.001

0.01

0.1

1

CaHPO4

FeCl4-

FeHPOFe2+

PO4

3-

CaHPO4(S)

AlPO4(S)

FePO4(S)

CaH2PO

4+

FeH2PO

4

2+

H3PO

4

H2PO

4-

HPO4

2-

FeH2PO

4+

Ca2+

Cl-

Al3+

Fe3+

co

nce

ntr

atio

n m

ol/l

pH



0 1 2 3 4 5 6 7 8 9 10 110.0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1.0

estimated log Kextraction

= 3.2

2) model

measured

deg

ree o

f iron

extr

actio

n

Cl- concentration mol/L

cascaded option tree: drying


P-recovery

from sludge

drying

conditions

- dewatered sludge 0 0 0 -

+ convective air drying + 0 0 0 0

slow drying (no air) + + 0 0

extraction compatibility

filtrability

P leaching

operation cost

transport/handling/storage

- not feasible

0 acceptable

+ good

not evaluatedBednarz, A. et al. 2014

driedsludge

dewateredsludge

P leaching- different acids and pH


-1 0 1 2 3 4 5 60.0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

degre

e o

f P

leachin

g

equilibrium pH

HCl

H2SO

4

HNO3

HCl+HNO3

HCl+H2SO

4

HNO3+H

2SO

4

H3PO

4

model

sludge leach liquor


P Fe K Mg Ca Al Mn Zn Na Cr Cu Ni Co Pb Cd0.1

1

10

100

1000

10000

ce

nce

ntr

atio

n (

mg

/L)

in le

ach

liq

uor H2SO4

HCl

reactive extraction with HCl

conc. 1mol/L


D2E

PHA

TBP

D2E

PHA-T

BP

A33

6

A33

6-D2E

PHA

A33

6-TBP

A33

6-D2E

PHA-T

BP

0

20

40

60

80

100

pe

rce

nta

ge

of

extr

actio

n P

Ca

Cd

Cu

Pb

Zn

Fe

reactive extraction of Fe with

A336 + TBP


1 2 3 4 5 6 70.0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1.0

extraction without H2O

2

extraction with H2O

2

deg

ree o

f iron

extr

actio

n

Cl- mol/L

Alamine 336:

𝐹𝑒𝐶𝑙4−+ 𝑅3𝑁𝐻

+𝐶𝑙−= 𝐹𝑒𝐶𝑙4𝑅3𝑁𝐻+ 𝐶𝑙−

TBP:

𝐹𝑒𝐶𝑙4−+ 𝑇𝐵𝑃= 𝐹𝑒𝐶𝑙4𝑇𝐵𝑃

PULSE product


Comp. Conc.

P2O5 29.2%

CaO 21.7 %

Total C 6 %

Al2O3 2.61 %

MgO 1.84 %

Fe 0.325 %

Mn 10800ppm

Cr 1530 ppm

Cu 294 ppm

Ni 51.6 ppm

Pb 38,8 ppm

Zn 8.97 ppm

Cd 0.735ppm

Hg 0.054 ppm

leaching of dried sludge

filtration

metal removal by reactive extraction

CaP precipitation with NaOH(pH = 6 - 7)

summary

• no significant difference between P leaching from wet or dry sludge

• P leaching depends only on pH and not on the type of acid

• extraction of metals at low pH only achieved with Alamine 336

• metals concentration in product is within the limits set by the EU fertilizer regulations except in case of Cr


acknowledgements

• funding– Interreg North-West Europe

– SPW Région Wallonne

• analytics– Faculty of Bioscience Engineering, Ghent University,

Belgium

– Prayon S.A., Belgium


8th October 2019, Liège | 5th

ECSM | Zaheer Shariff | PEPs -

ULiège | Slide n°

15

PHOSPHORUS RECOVERY FROM DRIED SLUDGE WITH REACTIVE EXTRACTION TO REMOVE IMPURITIES 5th ECSM, 08.10.19, Liège, Belgium

Shariff Z.A., Fraikin L., Léonard A., Pfennig A.

[email protected]

PEPs - Department of Chemical Engineering, Université of Liège

mailto:[email protected]

references

• http://www.nweurope.eu/projects/project-search/phos4you-phosphorus-recovery-from-waste-water-for-your-life/

• Doetsch, P., Pinnekamp, Johannes, Montag, D., Rath, W., Grömping, M., 2010. Rückgewinnung von Pflanzennährstoffen, insbesondere Phosphor aus der Aschevon Klärschlamm (Abschlussbericht PASCH). Institut fürSiedlungswasserwirtschaft der RWTH Aachen, Aachen.

• Bednarz, A., Rüngeler, B., Pfennig, A., 2014. Use of Cascaded Option Trees in Chemical-Engineering Process Development. Chem. Ing. Tech. 86, 611-620.


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