Waste Management 33 (2013) 1339–1344

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Waste Management
journal homepage: www.elsevier.com/locate/wasman

Treatment of digestate from a co-digestion biogas plant by means of vacuum

evaporation: Tests for process optimization and environmental sustainability
A. Chiumenti ⇑, F. da Borso, R. Chiumenti, F. Teri, P. Segantin
Department of Agricultural and Environmental Sciences (DISA), University of Udine, Italy

a r t i c l e i n f o a b s t r a c t

Article history: Vacuum evaporation consists in the boiling of a liquid substrate at negative pressure, at a temperature
Received 21 September 2012 lower than typical boiling temperature at atmospheric conditions. Condensed vapor represents the so
Accepted 15 February 2013 called condensate, while the remaining substrate represents the concentrate.
Available online 4 April 2013
This technology is derived from other sectors and is mainly dedicated to the recovery of chemicals from
industrial by-products, while it has not been widely implemented yet in the field of agricultural digestate
Keywords: treatment. The present paper relates on experimental tests performed in pilot-scale vacuum evaporation
Anaerobic digestion
plants (0.100 and 0.025 m3), treating filtered digestate (liquid fraction of digestate filtered by a screw-
Digestate treatment
Biogas
press separator). Digestate was produced by a 1 MWe anaerobic digestion plant fed with swine manure,
Vacuum evaporation corn silage and other biomasses. Different system and process configurations were tested (single-stage
Concentration and two-stage, with and without acidification) with the main objectives of assessing the technical feasi-
bility and of optimizing process parameters for an eventual technology transfer to full scale systems.
The inputs and outputs of the process were subject to characterization and mass and nutrients balances
were determined.
The vacuum evaporation process determined a relevant mass reduction of digestate.
The single stage configuration determined the production of a concentrate, still in liquid phase, with a
total solid (TS) mean concentration of 15.0%, representing, in terms of mass, 20.2% of the input; the
remaining 79.8% was represented by condensate. The introduction of the second stage allowed to obtain
a solid concentrate, characterized by a content of TS of 59.0% and representing 5.6% of initial mass.
Nitrogen balance was influenced by digestate pH: in order to limit the stripping of ammonia and its
transfer to condensate it was necessary to reduce the pH. At pH 5, 97.5% of total nitrogen remained in
the concentrate. This product was characterized by very high concentrations of total Kjeldhal nitrogen
(TKN), 55,000 mg/kg as average.
Condensate, instead, represented 94.4% of input mass, containing 2.5% of TKN. This fraction could be
discharged into surface water, after purification to meet the criteria imposed by Italian regulation. Most
likely, condensate could be used as dilution water for digestion input, for cleaning floor and surfaces of
animal housings or for crop irrigation.
The research showed the great effectiveness of the vacuum evaporation process, especially in the two
stage configuration with acidification. In fact, the concentration of nutrients in a small volume deter-
mines easier transportation and reduction of related management costs. In full scale plants energy con-
sumption is estimated to be 5–8 kWhe/m3 of digestate and 350 kWht/m3 of evaporated water.
Ó 2013 Elsevier Ltd. All rights reserved.

1. Introduction Muller, 2011). Anaerobic digestion process determines transforma-

Anaerobic digestion of organic waste and/or livestock manure
represents a great opportunity, not only for the revenues related
to the production of energy from renewable sources, but also from
environmental point of view. (Burton and Turner, 2003; Rehl and
⇑ Corresponding author. Address: DISA Department of Agricultural and Environ-
mental Sciences, University of Udine, Via delle Scienze 208, 33100 Udine, Italy. Tel.:
+39 0432 558650; fax: +39 0432 558603.
E-mail addresses: achiumenti@hotmail.com, alessandro.chiumenti@uniud.it
(A. Chiumenti).
tions of nitrogen compounds but total nitrogen content of dige-
state and, hence, nitrogen load for agricultural utilization, result
unvaried: where surplus nitrogen is a problem, dedicated solutions
must be implemented (Chiumenti et al., 2010). Nitrogen reduction
and/or its concentration in different fractions, in limited quantity
and easier to store and transport, is becoming a key factor for the
land spreading of livestock manure in many Nitrate Vulnerable
Zones of Europe (Flotats and Magrì, 2011).
The treatment of digestate in order to produce effluents with
high fertilizing potential is the core of the ‘‘conservative

0956-053X/$ - see front matter Ó 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.wasman.2013.02.023
1340 A. Chiumenti et al. / Waste Management 33 (2013) 1339–1344

approach’’: typically, in fact, input nitrogen is diverted into differ-

ent fractions, easier to be managed and with higher concentration
of nutrients, if compared to raw digestate.
The vacuum evaporation process consists in the creation of neg-
ANAEROBIC
ative-pressure conditions in dedicated equipment, maintaining
boiling temperature at that pressure. Water evaporation takes DIGESTION
place and consequent concentration of treated substrate occurs;
evaporated water, then, is condensed by cooling and collected in DIGESTATE
the condensate tank. This technology is implemented in other sec-
tors, mainly in the fields of the treatment of residuals from indus- L/S SEPARATION
trial production, in some cases with the aim of recovering
chemicals, like in the galvanic industry. Vacuum evaporation has SOLID FRACTION
been applied for years also to the treatment of landfill leachate
(Marks et al., 1994; Birchler et al., 1994).
In the agro-industry sector, this technology was tested on the
dairy industry, for the recovery of proteins from serum (Altieri FILTERED DIGESTATE
et al., 2003), in the olive oil industry, for the treatment of wastewa-
ter from mills (Vitolo et al., 1999) and of olive husks (Barbari et al.,
2005). Other tests were performed on residues from the produc-
tion of wood pulp and paper (Nilsson and Strand, 1994; McKeough CONDENSATE
and Fagernäs, 1999) and on pig slurry (Palatsi et al., 2004).
VACUUM
CONCENTRATION
Up to date the vacuum evaporation technology has not been
1 st STAGE
widely implemented yet in the field of agricultural digestate
treatment.
CONCENTRATE
The main objective of the present research was the assessment
of the technical feasibility of the process in this field.
Tests were conducted on single and two stage pilot-scale sys-
tems, with and without acidification of digestate, through the deter-
mination of process parameters: chemical–physical characteristics VACUUM CONDENSATE
of input and output materials, mass balance and nutrients balance. CONCENTRATION
2 nd STAGE

2. Materials and methods

The tests were performed in a fattening pigs farm (10,000
heads) with a 1 MWe codigestion plant. The biogas plant was fed
with swine manure (90 m3/day), corn silage (20 t/day), triticale si-
lage (10 t/day), maize flour (2 t/day) and limited quantities of other
biomasses.
The thermal regime of the plant was mesophilic (39 °C) and the
produced biogas was about 12,000 m3/day. The digestate produced
by the biogas plant was subject to liquid/solid separation by means
of a screw-press separator (1 mm screen).
The experimental tests were performed on the liquid fraction
from the separator (filtered digestate) by means of pilot scale vac-
uum evaporators. A schematic of the process is depicted in Fig. 1.
The single stage system was composed by an evaporation
chamber, with a volume of 100 l, heated by means of a heat ex-
changer, connected to a heat pump system (Fig. 2). The operation
was semi-discontinuous, with continuous loading of digestate,
continuous discharge of condensate and discontinuous discharge
of concentrate.
The functioning of the system was automatic and managed by a
programmable logic controller (PLC).
The two-stage system was composed by the previous equip-
ment, as first stage, and a second unit represented by a unit featur-
ing an evaporation chamber (capacity of 25 l), with conic base,
equipped with scraper for the movement of the product, heat
pump system, with heat exchanger installed under the floor of
the boiling chamber itself (Fig. 2) The second unit was capable of
handling also solids. The operation was semi-discontinuous, with
discontinuous loading of digestate, continuous discharge of con-
densate and discontinuous discharge of concentrate. Also the sec-
ond unit was controlled by PLC.
The pH correction unit was represented by a stainless steel tank,
with a volume of about 100 l, equipped with maximum and
CONCENTRATE
Fig. 1. Schematic of the process, including anaerobic digestion, liquid solid
separation pre-treatment and the two evaporation stages. Tests were performed
both in single stage and two stage configuration.
minimum levels, mixing system, pH meter, acid tank and pump
and PLC. Tank was filled with filtered digestate until the set upper
level was reached and then acid was pumped automatically till the
desired pH value was achieved. Filtered digestate loading started
when minimum level was reached in the pH correction tank.
Three different series of tests were performed varying the con-
figuration of the process:
– In the test series n.1 filtered digestate, without acidification,
was subject to vacuum concentration in the single stage
configuration.
– The test series n.2 were performed in single stage configuration,
with acidification to pH 3.5 by means of sulfuric acid (35%).
– The test series n.3 were performed in two stage configuration,
with acidification. In this case the strategy was to achieve a
compromise between acid consumption and stripping of
ammonia, with a pH reduction to 5.0.
Each concentration cycle was operated until the production of
condensate stopped, indicating that evaporation ceased.
For each cycle, mass and volume of input and outputs were
determined, including, in particular, filtered digestate, concentrate
and condensate. Samples of each product were collected at the
beginning, during the process at variable intervals (3–5 h), and at
the end of each cycle. The samples were subject to analyses for
the determination of: total solids (TSs), volatile solids (VSs), pH,
 A. Chiumenti et al. / Waste Management 33 (2013) 1339–1344 1341

Fig. 2. Schematics of the first stage (upper scheme) and of the second stage of the system (source: Italschell).

total Kjeldhal nitrogen (TKN) (APHA, AWWA, WPCF Standard
methods, 1992) (Table 1).
Preliminary analyses performed on digestate allowed excluding
the presence of nitrites and nitrates, allowing to consider TKN as an
indication of total nitrogen content.
Acid consumption, when applicable, was determined manually
by mass and volume determinations.
3. Results and discussion
3.1. Process parameters
The concentration units were set to operate at a temperature of
35 °C and at a relative pressure of 96 kPa, equivalent to an
absolute pressure of 5.3 kPa. Pressure and temperature were

Table 1
Synthesis of monitored parameters and methods. (TS = total solids, VS = volatile solids, TKN = total Kjeldhal nitrogen).

Parameter Measurement points Frequency Method

Mass and volume Input and output products Beginning and end of each cycle Manual determination of mass
and volume
Temperature Input and output products, evaporation chamber(s) Beginning, end of each cycle and intermediate Portable thermometer
periods
pH Input and output products Beginning, end of each cycle and intermediate Portable pH-meter
(concentrate and condensate) periods
TS, VS, pH, TKN Input and output products Beginning, end of each cycle and intermediate Lab analysis
(concentrate and condensate) periods
Acid consumption Acidification tank Beginning of the cycle Manual determination of mass
and volume
1342 A. Chiumenti et al. / Waste Management 33 (2013) 1339–1344

constant during the tests and did not vary significantly from the set Digestate from the biogas plant was characterized by TS content
values. from 5.6% to 5.7%, TKN varying from 4700 to 3510 mg/kg and pH
The first unit operated with treatment cycles of about 40–45 h, from 7.6 to 7.9.
the second unit was characterized by 10–15 h of operation: tests Filtered digestate used for the tests was characterized by
were interrupted when the production of condensate stopped, limited variations of the TS content (3.3–3.4%), while relevant
indicating that the evaporation ceased. variations were detected in terms of volatile solids content,
The treatment capacity was of about 500 kg of filtered digestate 54.2–70.0%TS, and of TKN, ranging from 3380 to 4550 mg/kg. The
per cycle for the first unit and 20–25 kg/cycle for the second unit. value of pH varied from 7.6 to 7.9. The variability of TS and TKN
The relevant difference is mainly related to the continuous load of in digestate and, hence, in filtered digestate, was detected in
the first unit and the discontinuous of the second. several monitored plants, depending on several factors related to
the management of the biogas plant, such as quality and quantity
3.2. Mass balance of feedstocks and mixing level in digesters (Chiumenti et al., 2010).
Filtered digestate quality, furthermore, varies from plant to
In terms of mass balance a significant effect was determined by plant depending on the type of separation equipment. Also in this
the configuration of the plant. In case of single stage treatment, in particular case the feeding of the monitored plant was subject to
fact, it was possible to obtain a concentrate characterized by being variations in the 2 years’ time span of the study, but the variations
liquid, even if dense. In terms of mass, concentrate represented of digestate quality did not affect the vacuum evaporation process.
20.2% of input, while the condensate represented the remaining The first stage of the process determined an increase of TS up to
79.8%. 15.0%, as average. The resulting concentrate was a dense liquid
The introduction of the second stage determined a significant fraction.
increase of the concentration rate, so that the final product re- This result is related to the configuration of the system, in par-
sulted solid. The reduction of mass was also increased: the solid ticular to the static conditions of the product (not stirred) and to a
concentrate represented 5.6% of initial mass, while condensate progressive reduction of the efficiency of the heat exchangers dur-
from the second stage resulted of 14.6% of the input, with a com- ing the process, due to the formation of deposits over the surface of
prehensive production (both from first and second stage) repre- exchangers.
senting 94.4% of input mass. Experimental tests carried out by other authors, with single
stage systems, demonstrated that the highest content of solids that
3.3. Chemical characteristics can be achieved in the concentration of animal manure was be-
tween 20% and 25% TS (ten Have and Chiappini, 1993).
Tables 2 and 3 report the most representative characteristics of The two stage process allowed to obtain a solid concentrate
input and outputs of the process, in relation to test series n.1 and with an average TS content of 59.0%. Other authors underline that
n.2 (single stage treatment, with and without acidification) and the vacuum evaporation process is not capable to achieve complete
to test series n.3 (two stage process with acidification). drying of the product (Bonmatí and Flotats, 2003).
In particular, the evolution of TS with time was monitored to
evaluate the performance of the process: in Fig. 3 representative
Table 2 plots are depicted. The first unit reached the highest concentration
Average characteristics of input and output streams in case of test series n.1 and n.2:
of TS after 27–32 h of operation. The second unit determined a
single-stage process with and without acidification (n.d. = not determined). (TS = total
solids, VS = volatile solids, TKN = total Kjeldhal nitrogen).
steep increase of the concentration rate, reaching the highest TS
concentrations (63%) in 10–15 h of operation (Fig. 3).
Sample TS (%) VS (%TS) pH TKN
The chemical characteristics of concentrate and of condensate
(mg/kg)
(first stage), resulted strongly influenced by pH of filtered dige-
Test series n.1: single stage – without acidification state. Digestate itself, in fact, was characterized by a pH in the
Digestate 5.7 53.8 7.6 4700
Filtered digestate 3.4 54.2 7.6 4550
range of 7.5–7.9, resulting in chemical conditions favorable to
Condensate (without acidification) n.d. n.d. 7.7 3730 the stripping of gaseous ammonia. In these conditions, in fact, con-
Concentrate 15.1 75.8 8.6 5350 densate showed significant concentration of TKN, 3730 mg TKN/kg,
Test series n.2: single stage – with acidification compared to 4550 mg TKN/kg of filtered digestate; the
Digestate 5.6 71.0 7.9 3780
Filtered digestate 3.3 70.0 7.9 3660
Condensate (with acidification) n.d. n.d. 3.2 10
Concentrate 15.0 84.7 4.6 18,700

Table 3
Average characteristics of input and output streams in case of test series n.3: two-
stage process with acidification (n.d. = not determined). (TS = total solids, VS = volatile
solids, TKN = total Kjeldhal nitrogen).

Sample TS (%) VS (TS%) pH TKN (mg/kg)

Digestate 5.6 61.2 7.6 3510
Filtered digestate 3.3 62.8 7.6 3380
1st Stage
Condensate (with acidification) n.d. n.d. 5.2 98
Concentrate 14.8 69.5 6.0 16,890
2nd Stage
Condensate (with acidification) n.d. n.d. 3.2 46
Concentrate 59.0 68.5 n.d. 55,000
Fig. 3. Typical evolution of TS in concentrate, in the first and second stages.
 A. Chiumenti et al. / Waste Management 33 (2013) 1339–1344 1343

concentrate, compared to the input, was characterized by a con- DIGESTATE

centration of 5350 mg TKN/kg (test series n.1).
In order to limit the stripping of ammonia from digestate, the L/S SEPARATION
pH of the input was lowered to pH 3.5 by means of sulfuric acid
(35%). In this condition the concentration of nitrogen in condensate FILTERED DIGESTATE
100% MASS
resulted very low, 10 mg TKN/kg. As consequence of the solubiliza- 100.0% N
tion of ammoniacal nitrogen in digestate, TKN in concentrate re- VACUUM CONDENSATE
sulted increased to 18,700 mg/kg (test series n.2). CONCENTRATION 79.8% MASS
The tests with the two-stage process were performed with acid- 1ST STAGE 78.1% N without acidification
0.8% N with acidification
ification (test series n.3): pH was lowered from 7.6 of filtered dig- CONCENTRATE
estate to 5.0, by means of sulfuric acid (35% solution). In this case a 20.2% MASS
higher pH was adopted (instead of pH 3.5 of the previous test) in 21.9% N without acidification
99.2% N with acidification
order to obtain a compromise between stripping effect and acid
consumption. Filtered digestate used in test series n.3 was charac-
terized by TKN content of 3380 mg/kg. DIGESTATE
The first stage determined the production of a condensate char-
acterized by TKN concentration of 98.0 mg TKN/kg) even if slightly L/S SEPARATION

higher than that of the test with lower pH. The concentrate was
FILTERED DIGESTATE
characterized by high TKN concentration, 16,890 mg/kg, slightly 100.0% MASS
lower than the concentration obtained with lower pH. The second 100.0% N
stage determined the production of a condensate characterized by VACUUM
CONDENSATE
TKN concentration of 46 mg/kg. CONCENTRATION
1st STAGE 79.8% MASS
Considering the potential destination of the condensate, dilu- 2.3% N
tion of biomasses to be destined to anaerobic digestion, necessary CONCENTRATE
in case of high ST feedstocks, this result appears to be satisfactory. 20.2% MASS
97.7% N
For a discharge on surface water of this fraction a higher acidificat-
ion is preferable. VACUUM CONDENSATE
CONCENTRATION 14.6% MASS
The final product of the two stage process was a solid concen- 2nd STAGE 0.2% N
trate characterized by very high concentration of TKN, 55,000 mg
CONCENTRATE
TKN/kg. Other authors obtained a concentrate characterized by a
5.6% MASS
TKN between 18,100 and 41,200 mg/kg (Bonmatí and Flotats, 97.5% N
2003).
Acid consumption varied from 30 to 40 kg/m3. Other authors re- Fig. 4. Average mass and nitrogen balances in the single stage system, test series
n.1 and n.2 (upper scheme). Average mass and nitrogen balance for the two stage
ported a consumption of 3.0–3.3 kg/m3 of H2SO4 for the acidificat-
vacuum concentration process with acidification, test series n.3 (lower scheme).
ion of digestate, in laboratory tests, but no indication was given
about the concentration of acid and pH shift (Panvini et al., 2009).

3.4. Nitrogen balance
Nitrogen balance was not only influenced by the pH of the input
product (filtered digestate) but also by the configuration of the sys-
tem (one or two stage process).
In the test series n.1 (single stage, without acidification), filtered
digestate was characterized by a pH in the range 7.5–7.9,
conditions favorable to the stripping of ammonia from the product.
As a result 78.1% of nitrogen was removed from digestate by strip-
ping, and was lately recovered in the condensate, representing
79.8% of input mass. The concentrated fraction contained the
remaining 21.9% of nitrogen (Fig. 4). This configuration, hence,
determined the production of significant quantity of condensate
containing most of TKN and did not determine a significant con-
centration of TKN in concentrate.
These tests resulted useful for a first determination of the distri-
bution of TKN in the different output fractions and showed that to
achieve the main goal of concentrating nutrients in limited quanti-
ties of product the vacuum evaporation process must be performed
with acidification.
The acidification to pH 3.5 performed in test series n.2 (single
stage) limited the stripping of ammonia by shifting the chemical
equilibrium between gaseous ammonia and soluble ammonium
to the soluble form: 99.2% of nitrogen was maintained in the liquid
concentrate, while only 0.8% of N was detected in condensate
(Fig. 4). The results obtained with this level of acidification could
be considered satisfactory in terms of concentration of nutrients
and quality of condensate, since almost all input TKN was collected
in concentrate.
Test series n.3 (two stage) were performed with a pH reduction
to 5.0 to achieve a compromise between acid consumption and
stripping of ammonia.
In this case the first stage determined a separation in the con-
densate of 2.3% of TKN, while the second stage determined a sep-
aration of 0.2% of TKN. At the end of the two stage process,
hence, the concentrate, representing 5.6% of input mass, contained
97.5% of TKN (Fig. 4). Since the process was performed in enclosed
reactors, the loss of nitrogen in the atmosphere was prevented.
These results were confirmed, by other Authors that performed
tests on digestate: with a correction of pH < 6.5 removal of 25% of
nitrogen from the feedstock was obtained, while with a pH of 8.4
more than 50% of nitrogen passed to condensate even at 33% of
evaporated mass (Bonmatí et al., 2003; Bonmatí and Flotats,
2003; Panvini et al., 2009).
4. Conclusions
The performed experimental tests allowed to have indications
on the possibility to implement the vacuum evaporation process
in anaerobic digestion plants for a sustainable management of
digestate.
The most evident outcome is represented by the significant
reduction of the mass of digestate to be destined to agricultural
utilization. This result was more evident in case of a two stage pro-
cess that transformed digestate in a solid product, containing 97.5%
of input TKN, in 5.6% of mass.
1344 A. Chiumenti et al. / Waste Management 33 (2013) 1339–1344
The fertilizing potential of this product is expected to be higher
than the potential of digestate itself, for the higher content of
nutrients (TKN), and the reduction of volume represents an advan-
tage in terms of easier transportation and reduction of related
management costs.
Anyway, it is important to underline that to obtain an effective
reduction of nitrogen load on the territory part of these products
has to be transported elsewhere or, eventually, sold.
The emissions from the process are prevented, since the treat-
ment is performed in enclosed reactors.
Acidification of input digestate appeared a necessary step in or-
der to limit the stripping of ammonia from digestate and its trans-
fer to the condensate.
The condensate represented, in terms of mass, the main output
of the process. The quality of this fraction depended on many fac-
tors, including the characteristics of digestate (TKN, ammonia con-
centration, pH), and the configuration of the process (with or
without acidification). In order to reach discharge limits stated
by European law further treatments are required, such as mem-
brane filtration. The most interesting application could be repre-
sented by the use for the dilution of biomasses with high TS
content, such as litter from livestock farms, in order to obtain a
feedstock suitable for the anaerobic digestion process. This fraction
would not determine an increase of TKN of digesters input because
of its low content of nitrogen. Other possible uses are represented
by cleaning of floor and surfaces of animal housings or irrigation of
crops.
Energy consumption was monitored by means of the PLC, but
was not considered a valid reference because could not be consid-
ered as proportional to energy demand of a full scale system. On a
full scale system, in fact, thermal energy would be recovered by
Combined Heat and Power (CHP) unit and not produced by a heat
pump system.
Energy consumption of a full scale plant, treating agricultural
digestate, is estimated by the manufacturer to be of 5–8 kWhe/
m3 of digestate and of 350 kWht/m3 of evaporated water. Thermal
energy produced by a CHP unit would be sufficient to treat the en-
tire production of digestate of a biogas plant, result that is not
obtainable with other technologies such as digestate drying, that
allows to treat a maximum of 50% of digesters output.
Other technologies can be used to concentrate digestate nutri-
ents, such as membrane filtration, but in this case mass reduction
is lower (99% of nitrogen is concentrated in 55% of mass repre-
sented by solid and concentrated fractions) (Chiumenti et al.,
2010). Energy consumption of membrane systems results double
compared to vacuum evaporation; thermal energy is not required
by the membrane process, but this is penalizing considering that
Italian regulations in matter of renewable energies require the uti-
lization of thermal energy from CHP units.
The results of the tests allow to give a first positive evaluation of
the technical feasibility of the process. The extension of the moni-
toring to full scale plants, for prolonged periods of operation,
would allow to perform a significant evaluation of the feasibility
of the vacuum evaporation technology, in relation, in particular,
to the effective requirements for the management of the process
(energy, acid consumption), and, hence, about its economic
sustainability.
Acknowledgements
The present research was conducted in the frame of the Ridu-
CaReflui Project, financed by the Veneto Region, Italy, and coordi-
nated by Veneto Agricoltura. The authors would like to thank
Italschell S.r.l. that provided the test plants, Mr. Duilio Calura,
Mr. Francesco Mombelli, Mr. Carlo Guidi, and Mr. Bizzoni Paolo
and Diego for their kind and professional support.
Appendix A. Supplementary material
Supplementary data associated with this article can be found, in
the online version, at http://dx.doi.org/10.1016/j.wasman.2013.02.
023.
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