CHEMICAL ENGINEERING TRANSACTIONS VOL. 69, 2018
A publication of
The Italian Association of Chemical Engineering Online at www.aidic.it/cet Guest Editors: Elisabetta Brunazzi, Eva Sorensen
Copyright © 2018, AIDIC Servizi S.r.l.
ISBN 978-88-95608-66-2; ISSN 2283-9216
Enhanced Biobutanol Separation by a Heat Pump Assisted Azeotropic Dividing-Wall Column
Iulian Patrascu
a, Costin Sorin Bîldea
a, Anton A. Kiss
b,c,*
aUniversity “Politehnica” of Bucharest, Polizu 1-7, 011061 Bucharest, Romania
bThe University of Manchester, School of Chemical Engineering and Analytical Science, Centre for Process Integration, Sackville Street, The Mill, Manchester M13 9PL, United Kingdom
cUniversity of Twente, Sustainable Process Technology, PO Box 217, 7500 AE Enschede, The Netherlands tony.kiss@manchester.ak.uk
Stronger sustainability needs for the production of fuels and chemicals have spurred extensive research to substitute fossil fuel sources by renewable sources. Yet, the major cost of biorefineries is in the downstream processing. This issue has to be addressed properly to make biofuels an economically viable alternative.
As a renewable fuel, biobutanol is produced from biomass feedstocks. But after the fermentation step it has a very low concentration (less than 3 %wt) that leads to high energy requirements for onventional downstream separation. To reduce the energy penalty, we describe here a new hybrid separation process based on a heat pump assisted azeotropic dividing-wall column (A-DWC). CAPE tools and Pinch analysis were used for the process synthesis, design and optimization of the process. The plant capacity considered here is 40 ktpy butanol (99.4 %wt). Remarkably, the energy requirement for butanol separation using heat integration and vapour recompression assisted A-DWC is reduced by 58% from 6.3 to 2.7 MJ/kg butanol.
1. Introduction
Due to its remarkable properties (e.g. low water miscibility, flammability and corrosiveness) biobutanol can replace gasoline in existing car engines. But its current production costs prohibit biobutanol use as a biofuel.
In the fermentation process of acetone-butanol-ethanol (ABE), diluted biobutanol is obtained with a concentration of less than 3 %wt. The productivity, yield and concentration can be improved by genetic engineering, but this is a longer-term goal to be achieved. A higher butanol yield is achieved in fermentation using anaerobic bacteria as Clostridium acetobutylicum and Clostridium beijerinckii (Tashiro et al., 2013).
The low concentration of butanol obtained by fermentation leads to significant penalties in the energy required for downstream processing, typically in the range of 14.7-79.05 MJ/kg butanol (Patrascu et al., 2017). This has a major impact on the costs for separation, which have to be drastically reduced. Many separation techniques are available for the ABE separation, e.g. distillation, reverse osmosis, adsorption, liquid-liquid extraction and others (Abdehagh et al., 2014; Sanchez-Ramirez et al., 2017). Another way to increase the concentration of ABE in the outlet stream of fermentation is by in-situ product recovery (ISPR), e.g. by gas stripping (Lodi and Pellegrini, 2016) which can lead to ABE: 4.5 %wt acetone, 18.6 %wt butanol and 0.9 %wt ethanol (Xue et al., 2013). Using this stream as start of the downstream processing, distillation becomes more reasonable.
The conventional separation sequence using three distillation columns along with one decanter (Figure 1, left) requires 6.3 MJ/kg butanol. By using heat integration and combining two columns into a dividing-wall column (Figure 1, right), about 29 % reduction of the energy requirement was achieved (Patrascu et al, 2017). This is a significant reduction of the energy requirements, but can the energy savings be pushed any further? To achieve more savings, a novel process is proposed in this work. The azeotropic DWC combines three distillation columns into one unit and reduces the energy used for separation by employing a heat pump (vapor recompression) and heat integration. (Kiss, 2013; 2014). The decanter is not used here as the first separation unit, as the organic phase (rich in butanol) has a high impact on the reboiler duty for butanol purification and makes heat pumping very inefficient. By using a highly integrated azeotropic dividing-wall column (A-DWC) assisted by vapor recompression (VRC) technology, significant energy savings are possible.
DOI: 10.3303/CET1869035
Please cite this article as: Patrascu I., Bildea S., Kiss A., 2018, Enhanced biobutanol separation by heat pump assisted azeotropic dividing wall columns, Chemical Engineering Transactions, 69, 205-210 DOI: 10.3303/CET1869035
Feed
Aqueous Organic
Azeotrope
Azeotrope Decanter Cooler
Blower
Mixer
Butanol COL1
Acetone
COL4
Ethanol COL3
Water COL2 Feed
Aqueous Organic
Azeotrope
Azeotrope Decanter Cooler
Blower
Mixer
Butanol COL1
Butanol COL1
Butanol Butanol COL1
Acetone
COL4
Ethanol COL3
COL3 COL3
Water COL2
Water COL2
Water Water COL2
Feed
Aqueous
Organic Azeotrope
Water
Azeotrope
Decanter Cooler
Blower
Mixer
Butanol COL1
DWC Hex1
Hex3 Hex2
Acetone
COL4
Ethanol Feed
Aqueous
Organic Azeotrope
Water
Azeotrope
Decanter Cooler
Blower
Mixer
Butanol COL1
Butanol COL1
Butanol Butanol
COL1
DWC DWC Hex1
Hex3 Hex2
Acetone
COL4
Ethanol Acetone
COL4
Ethanol Acetone
COL4
Ethanol Acetone
COL4 Acetone Acetone
COL4
Ethanol
Figure 1. Process flowsheet of ABE downstream separation sequences (Patrascu et al., 2017)
2. Modeling approach
The downstream process was rigorously simulated in Aspen Plus, using the NRTL as suitable property model.
As the fourth column (COL-4) shown in Figure 1 separates only the light components (acetone and ethanol, which could be also used directly as fuel), it is not included in the energy requirement for butanol separation.
To account for a realistic composition of the ABE mixture, impurities are taken into account: 0.1 % wt. CO2, as well as small amounts of acetic acid and butyric acid. Several basic assumptions and design specifications are used for the optimization and heat integration: butanol purity is 99.4 % wt.; each side of the dividing wall has the same number of stages; feed streams are preheated to 97 °C; product streams are cooled to 25 °C; the (left) side reboiler is not considered in optimization process of A-DWC because will be replaced with a heat exchanger. Pinch analysis was used to determine the energy targets and the design of the heat exchange network (HEN). The investment and operation costs of the novel process were evaluated to show the benefits of this design (Dimian et al., 2014). The coefficient of performance (COP) was used to evaluate the feasibility of heat pumping, while taking into account the additional costs for compression and the limited payback time.
3. Results and discussion
3.1 Process design and development
Figure 2 shows the transition process configurations used to arrive eventually to the new process based on an azeotropic dividing-wall column (A-DWC). Based on the overlap of operating conditions and composition match, the three distillation columns can be conveniently integrated into just a single A-DWC unit. Heat pump and energy integration is considered in the next design step. Figure 3 illustrates the flowsheet of the heat integrated process with a heat pump assisted A-DWC at heart. The mass and energy balance is also included.
Decanter Feed
Aqueous
Organic AEW
+ Butanol
water
AEW
Water
COL1
Butanol water
Butanol COL3
Butanol water COL2
Cooler
AEW
Water Feed
DWC-L
A-DWC Butanol
Aqueous
Aqueous Organic
DWC-R
Azeotrope
Decanter Cooler
Condenser
AEW
Water Feed
DWC-L
A-DWC Butanol
Aqueous
Aqueous Organic
DWC-R
Azeotrope
Decanter Cooler
Condenser
Figure 2. Alternative distillation-decanter configuration (left) and corresponding azeotropic DWC (right)
AEW
Feed
1
13
DWC-L
25°C, 1.13 bar 26971 kg/h 04.50%w A 18.54%w B 00.91%w E 75.83%w W 00.04%w Acetic Acid 00.08%w Butiric Acid 00.10%w CO2
Water
25°C, 1.44 bar 20425 kg/h 99.86%w H2O 00.2%w Acids
RR= 27.02 Diam= 2.09 m Qreb= 1971 kW
31.73°C, 1 bar 1515.87 kg/h 80.16%w A 16.14%w E 01.98%w W 01.72%w CO2
Qcond = –7790 kW
A-DWC
25°C, 1.44 bar 5030.14 kg/h 99.4%w B 00.5%w W 00.1%w Acids
Butanol Aqueous
Organic
DWC-R
15 1
Diam = 1.22 m Qreb = 3012 kW
45 32
Qc = –1634 kW
Aqueous
38.35°C, 1.12 bar 8476.56 kg/h 00.53%w A 07.11%w B 00.53%w E 91.80%w W 00.03%w Acids 38.35°C, 1.12 bar
9072.94 kg/h 00.72%w A 76.32%w B 00.93%w E 21.95%w W 00.08%w Acids
Azeotrope
40°C, 1.12 bar 17549.5 kg/h 00.63%w A 42.89%w B 00.74%w E 55.69%w W 00.05%w Acids
Qh = 5777 kW Qh = 814 kW
Qh = 661 kW
Qc = –2098 kW Qc = –471 kW
97°C, 1.13 bar 97°C, 1.13 bar
59.43°C, 1 bar
98.11°C, 1.12 bar
110.177°C, 1.44 bar 127.961°C, 1.44 bar 97°C, 1.14 bar
Decanter
Figure 3. Flowsheet of the new process using azeotropic DWC, including mass and energy balance
Heat integration leads usually to significant reduction of heating and cooling requirements. Pinch analysis was used to determine the energy targets as well as the configuration of the optimal heat exchanger network. As shown in Figure 3, the vapor stream from the top of the A-DWC has low temperature hence it cannot be used for heat integration. However, by recompressing the vapor to 5.8 bar, the temperature increases to 150 °C, which is useful for heat integration. The maximum energy savings are given by (Blahusiak et al., 2018):
. (%) 100 reb reb/
reb
Q HR Q COP Max savings
Q
− ⋅
= ⋅ (1)
Figure 4 shows the dependence on pressure of the log-mean temperature difference (LMTD) and compressor power (Patrascu et al., 2018). The LMTD must exceed 5 K to obtain an acceptable heat exchange area and hence not an expensive heat exchanger (HEX). The compressor is limited by the compression ratio (up to 2.5- 4.0) and also by the discharge temperature which should not exceed 150°C for safety reasons: at higher temperatures the system may fail from worn rings, acid formations, oil breakdown (Luo et al., 2015).
0 0.1 0.2 0.3 0.4 0.5
1500 1550 1600 1650 1700 1750
5.1 5.2 5.3 5.4 5.5 5.6 5.7 5.8 5.9 6 6.1 6.2 6.3
1/LMTD / [1/K]
Compressor duty / [kW]
Pressure / [bar]
Tcomp,out=150°C Compressor duty
LMTD=7.21 1/LMTD
Figure 4. Dependence of compressor duty and the long-mean temperature difference (LMTD) on the pressure
3.2 Heat integrated heat pump assisted A-DWC process
The complete process flowsheet – including the main design parameters and the energy balance – is shown in Figure 5 (Patrascu et al., 2018). The A-DWC column has 45 stages in total, with 13 stages for the fractionation section and 32 stages for the stripping section. Butanol and water are the two bottom products, while a mixture of acetone and ethanol with some water (AEW) is removed as distillate. The ABE feed and the aqueous phase recycled from the decanter are fed on 1st stage of the stripping section (14th stage of A- DWC), which separates water as bottom product. The top vapor stream is compressed to 5.8 bar (150 °C), provides heat to the (left) side reboiler (HEX1), preheats the diluted ABE feed (HEX2) and is finally condensed. The liquid flowing down the column is routed to the right stripping section. From the 13th stage, a mixture close to the azeotropic composition is withdrawn as side stream, cooled, and sent to the decanter.
The organic phase is recycled on 2nd stage of the right stripping section (15th stage of A-DWC), from which butanol is obtained as bottom product. Additional heat is recovered by using the water product stream to preheat the aqueous and organic phases (HEX3, HEX4).
AEW
Feed
1
13
DWC-L
RR= 27.02 Diam= 2.43 m Qreb= 1971 kW
Qcond = –647 kW
A-DWC
Aqueous DWC-R15
1
45 32
Qc = –1634 kW
Azeotrope A = 301 m2
A = 74 m2
A = 59 m2
Qc = –622 kW
Qc = –471 kW
97°C, 1.14 bar
P = 1646 kW
Comp
59.43°C, 1 bar
149.63°C, 5.8 bar
98.11°C, 1.12 bar
115.89°C, 5.79 bar 97°C, 1.13 bar
110.177°C, 1.44 bar
127.961°C, 1.44 bar
Water
Butanol Organic
Aqueous
40°C, 1.12 bar 97°C, 1.13 bar
31.735°C, 1 bar
54.55°C, 5.78 bar 38.35°C, 1.12 bar
25°C, 1 bar 25°C, 1 bar
110.177°C, 1.44 bar
110.177°C, 1.44 bar
97°C, 1.12 bar
51.09°C, 1.43 bar
51.54°C, 1.43 bar
51.09°C, 1.43 bar 38.35°C, 1.12 bar
Decanter
25°C, 1 bar
A = 491 m2
110.177°C, 1.44 bar
110.177°C, 1.44 bar 110.176°C,
1.44 bar
vap
vap
vap
vap
Hex2 Feed
Hex1
Hex3 Hex4 P1
P2
Cond
Cool1
Cool2 Cool3
FL
Splitter Mixer
AEW
Feed
1
13
DWC-L
RR= 27.02 Diam= 2.43 m Qreb= 1971 kW
Qcond = –647 kW
A-DWC
Aqueous DWC-R15
1
45 32
Qc = –1634 kW
Azeotrope A = 301 m2
A = 74 m2
A = 59 m2
Qc = –622 kW
Qc = –471 kW
97°C, 1.14 bar
P = 1646 kW
Comp
59.43°C, 1 bar
149.63°C, 5.8 bar
98.11°C, 1.12 bar
115.89°C, 5.79 bar 97°C, 1.13 bar
110.177°C, 1.44 bar
127.961°C, 1.44 bar
Water
Butanol Organic
Aqueous
40°C, 1.12 bar 97°C, 1.13 bar
31.735°C, 1 bar
54.55°C, 5.78 bar 38.35°C, 1.12 bar
25°C, 1 bar 25°C, 1 bar
110.177°C, 1.44 bar
110.177°C, 1.44 bar
97°C, 1.12 bar
51.09°C, 1.43 bar
51.54°C, 1.43 bar
51.09°C, 1.43 bar 38.35°C, 1.12 bar
Decanter
25°C, 1 bar
A = 491 m2
110.177°C, 1.44 bar
110.177°C, 1.44 bar 110.176°C,
1.44 bar
vap
vap
vap
vap
Hex2 Feed
Hex1
Hex3 Hex4 P1
P2
Cond
Cool1
Cool2 Cool3
FL
AEW
Feed
1
13
DWC-L
RR= 27.02 Diam= 2.43 m Qreb= 1971 kW
Qcond = –647 kW
A-DWC
Aqueous DWC-R15
1
45 32
Qc = –1634 kW
Azeotrope A = 301 m2
A = 74 m2
A = 59 m2
Qc = –622 kW
Qc = –471 kW
97°C, 1.14 bar
P = 1646 kW
Comp
59.43°C, 1 bar
149.63°C, 5.8 bar
98.11°C, 1.12 bar
115.89°C, 5.79 bar 97°C, 1.13 bar
110.177°C, 1.44 bar
127.961°C, 1.44 bar
Water
Butanol Organic
Aqueous
40°C, 1.12 bar 97°C, 1.13 bar
31.735°C, 1 bar
54.55°C, 5.78 bar 38.35°C, 1.12 bar
25°C, 1 bar 25°C, 1 bar
110.177°C, 1.44 bar
110.177°C, 1.44 bar
97°C, 1.12 bar
51.09°C, 1.43 bar
51.54°C, 1.43 bar
51.09°C, 1.43 bar 38.35°C, 1.12 bar
Decanter
25°C, 1 bar
A = 491 m2
110.177°C, 1.44 bar
110.177°C, 1.44 bar 110.176°C,
1.44 bar
vap
vap
vap
vap
Hex2 Feed
Hex1
Hex3 Hex4 P1
P2
Cond
Cool1
Cool2 Cool3
FL
Splitter Mixer
Figure 5. Process flowsheet of the new downstream separation heat-integrated process based on A-DWC Figure 6 plots the temperature and the liquid composition profiles in the A-DWC unit. Note that the bottom of the column shows two temperatures due to the use of two reboilers, for the water and butanol products.
50 60 70 80 90 100 110 120 130
0 5 10 15 20 25 30 35 40 45 50
Temperature / [°C]
Stage
LEFT SIDE RIGHT SIDE
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
0 5 10 15 20 25 30 35 40 45 50
Mass fraction
Stage
Water
Butanol
Acetone Ethanol
LEFT SIDE RIGHT SIDE
Butanol Water
Figure 6. Temperature and liquid composition profiles along the A-DWC unit (Patrascu et al., 2018)
The temperature difference between the two sides of the dividing-wall does not exceed 20 K hence there is no need for special insulating measures. In terms of composition, the liquid composition profiles confirm the high purity of the bottom products, while a ternary mixture (AEW) is obtained as distillate stream. On the 13th stage it can be observed the composition of the heterogeneous azeotrope (butanol-water), while the aqueous and organic phase can be observed on the 14th stage for both sides of the dividing wall.
Despite the high degree of integration, such processes combining vapor recompression with (extractive) DWC technology have been reported to be also controllable (Patrascu et al., 2017; Luyben, 2017).
4. Process evaluation
The process is optimized using the total annual cost (TAC) as the objective function to be minimized.
CapEx TAC OpEx
Payback period
= + (2)
where a payback period of 3 years is considered, with 8000 hours/year operating time.
The main design parameters (e.g. number of trays, feed tray location) are used as decision variables in the optimization (Patrascu et al., 2017). The capital expenditures (CapEX) include the heat exchangers, coolers, heat pump, flash unit, distillation column, and the decanter. The heating and cooling costs considered are standard: LP steam (at 6 bar, 160 °C, $7.78/GJ), cooling water (at 25 °C, $0.72/GJ) and chilled water (at 5 °C,
$4.43/GJ). The compressor power cost taken into account is 15.5 $ per GJ electrical power.
Table 1 provides details of the economic evaluation of the new process for butanol recovery, based on a heat- integrated heat pump assisted A-DWC (Patrascu et al., 2018). The total equipment cost is evaluated at 5250 k$/year. The optimal operating cost is 1435 k$/year, including also the cooling of the products.
Table 1. Economic evaluation of the heat pump assisted A-DWC for butanol recovery
Item description (unit) DWC Decanter Coolers Exchangers Flash &Comp
Shell / [103 US$] 718.1 71.6 - - 1618.9
Trays / [103 US$] 94.6 - - - -
Condenser / [103 US$] 266.7 - 1179.5 - -
Reboiler / [103 US$] 497.8 - - 803.4 -
Heating / [103 US$/year] 441.8 - - - 737.3
Cooling / [103 US$/year] 82.5 - 173.2 - -
TAC / [103 US$/year] 1050.0 23.9 566.4 267.8 1276.8
A quick comparison of the energy efficiency for various process alternatives reveals the following results:
• 6.30 MJ/kg butanol, for the optimized conventional decanter-distillation process (Patrascu et al., 2017)
• 4.46 MJ/kg butanol, for the dividing-wall column process (Patrascu et al., 2017)
• 8.78 MJ/kg butanol, for the azeotropic DWC process (without heat integration and vapor recompression)
• 7.78 MJ/kg butanol, for the azeotropic DWC process (with heat integration, but no vapor recompression)
• 2.70 MJ/kg butanol, for the heat-integrated heat pump assisted A-DWC process (this work)
Remarkable, the heat-integrated heat pump assisted A-DWC process requires only 2.7 MJ/kg butanol (58%
less than in conventional separation sequence). This energy efficiency is better than liquid-liquid extraction or supercritical extraction processes (Salemme et al., 2016). However, using a heat pump increases the capital cost due to the expensive compressor (1581.5 k$). Nonetheless, considering the energy savings (1.69 MJ/kg butanol) evaluated at 1893 k$/year, the payback time is less than a year (about 10 months).
The potential environmental impact was evaluated in Aspen Plus using Carbon Tracking to calculate the CO2
emissions. The fuel source considered is natural gas and the CO2 emission factor data source used is the US Environmental Protection Agency Rule of ‘E9-5711’ (CO2 E-US) proposed in 2009. The standard used for the Global Warming Potential is USEPA (2009) with a carbon tax of 5 $/ton. The CO2 emissions are estimated at 1429 kg/h (11.43 ktpy) for the complete downstream process (heat-integrated heat pump assisted A-DWC).
The total net carbon tax has been evaluated at 7.87 $/h (62.96 k$/year). CO2 emissions were calculated as:
2
[ ] %
100
fuel emissions
Q C
CO = NHV α (3)
(
419) ( (
0) )
proc FTB
fuel proc
proc FTB stack
Q T T
Q h
T T
λ
−
= − − (4)
where α = 3.67 is the ratio of molar masses of CO2 and C; NHV (net heating value) is 48900 kJ/kg for natural gas; C% (carbon content) is 0.41 kg/kg; Qproc is the heat duty required by the process and duty provided by the stripping steam (kW); λproc is the latent heat of steam delivered to the process (kJ/kg); hproc is the enthalpy of steam delivered to the process (kJ/kg); T0 is the ambient temperature; TFTB (K) and Tstack (K) are the flame and stack temperature, respectively.
5. Conclusions
The novel process proposed here was effectively designed, optimized, and heat integrated allowing the bio- butanol recovery (from the ABE mixture obtained by fermentation) in only few separation units: three classic distillation columns are combined into one azeotropic dividing-wall column (A-DWC) and one decanter is used for the liquid-liquid split of the heterogeneous azeotrope. The energy requirements (and the associated CO2
emissions) are drastically reduced further by applying heat integration and vapor recompression. The economic evaluation proves that it is feasible, with the investment costs of the downstream process (40 ktpy capacity) of 5250 k$, and the operating cost of 1434 k$/year. Although, the cost of the compressor (required for VRC) is rather high (1581.5 k$), the payback period is less than one year (10 months). The highly integrated process reduces by 58% the energy usage for butanol separation to only 2.7 MJ/kg butanol.
Acknowledgments
The financial support of the European Commission through the European Regional Development Fund and of the Romanian state budget, under the grant agreement 155/25.11.2016 Project POC P-37-449 (ASPiRE) is appreciatively recognized. AAK thankfully acknowledges the Royal Society Wolfson Research Merit Award.
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