Accepted Manuscript

Beverage dealcoholization processes: Past, present, and future

Dave Mangindaan, K. Khoiruddin, I.G. Wenten

PII: S0924-2244(17)30381-3
DOI: 10.1016/j.tifs.2017.10.018
Reference: TIFS 2105

To appear in: Trends in Food Science & Technology

Received Date: 16 June 2017

Revised Date: 21 September 2017
Accepted Date: 29 October 2017

Please cite this article as: Mangindaan, D., Khoiruddin, K., Wenten, I.G., Beverage dealcoholization
processes: Past, present, and future, Trends in Food Science & Technology (2017), doi: 10.1016/
j.tifs.2017.10.018.

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 ACCEPTED MANUSCRIPT
1 Beverage Dealcoholization Processes: Past, Present, and Future

2 Dave Mangindaan1, K. Khoiruddin2, I.G. Wenten*,2

1
3 Department of Food Technology, Faculty of Engineering, Bina Nusantara University, Binus Alam Sutera Main
4 Campus, Jalan Jalur Sutera Barat Kav. 21, Tangerang 15143, Indonesia
2
5 Department of Chemical Engineering, Institut Teknologi Bandung, Jl. Ganesha 10, Bandung 40132, Indonesia
6 *Corresponding Author: igw@che.itb.ac.id

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7 Abstract
8 Background
9 It is clearly observed that there is a highly significant increase on the demand of non-alcoholic

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10 beverages (such as beer and wine) for the last few years. However, there is a huge issue faced by the
11 market, where most of the available non-alcoholic beverages are not organoleptically accepted, as
12 they exhibit lack of flavor and aroma, and also different taste compared to the regular brews.

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13 Therefore, it is imperative to have appropriate processes or methods to selectively remove ethanol
14 while retaining the volatile components that are related with flavor and aroma of original brew.
15 Scope and Approach
16 To present a clear background about the dealcoholization and its importance, this paper will bring a

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17 brief discussion on the nutrient and health aspects related to the beer and wine. Furthermore, some
18 conventional approaches for dealcoholization in the past will be discussed, mainly on the thermal-
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19 based processes. Moreover, the state of the art and the present status of the beverage dealcoholization
20 processes will be discussed in detail, focusing on the approaches utilizing membranes along with
21 some miscellaneous dealcoholization methods. In addition, the dealcoholization employing the
22 membrane processes is the spotlight for the future perspective and development.
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23 Key Findings and Conclusions

24 The membrane processes demonstrate promising results for beverage dealcoholizations while
25 preserving the sensorial properties. However, there is still a lot effort to be placed on the research for
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26 the development of the prospective separation process that may produce brews that are both healthy
27 (dealcoholized) and delicious.
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29 Keywords: beer; dealcoholization; membrane; non-alcoholic beverage; wine.

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31 1. Introduction
32 Beer and wine are beverages produced via fermentation process. With the assistance of yeast, the
33 mixture of malt and hops are converted into beer, while those of grape juices are transformed into
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34 wine, both having alcoholic content up to around 5 and 15 %, respectively. Recently, there is an
35 increasing global demand for the alcohol-free beer (ranging from 0.05 to 1.2% ABV (alcohol by
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36 volume) or dealcoholized wine (less than 7% ABV) (Figure 1), due to improved paradigm aiming for
37 healthy lifestyle, consciousness of moderate consumption of beer or wine, and also due to religious
38 reasons. This is such a positive attitude where consuming beer or wine, especially when the
39 disadvantageous alcohol content is sharply reduced, will let one to enjoy beneficial bioactive
40 compounds, namely vitamins, minerals, antioxidants to anticancer agents.
41 Despite the increasing worldwide demand, producing such low-alcohol beverages are quite
42 challenging. The manufacturer could just use grape with lower sugar content, perform arrested
43 fermentation with special yeast that produces low alcohol concentration, or without any fermentation
44 at all continued with blending with artificial aroma, but the products are quite disappointing, as they
45 are organoleptically different with those of standard beer or wine. Physical separation processes are
46 also employed in the post-fermentation stage to remove alcohol from the beverages, although facing
47 the same obstacle in the quality of the end product (Figure 1). In this paper, a brief detail on the

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48 nutritive substances of the brews will be introduced, continued with overview on the production of
49 low alcoholic beverages, and then focused on the membrane-based processes and the challenges
50 countered for the removal of alcohol while maintaining the quality of taste and flavor, and taking as
51 low energy as possible. By observing Figure 1, we could also notice that the membrane-based
52 dealcoholization processes are the common ones nowadays (almost 50%). Furthermore, our main
53 focus in this review is only on categorizing some advancements in the dealcoholization processes for
54 the last 30 years, without promoting much on the feasibility study of those processes.
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57 Figure 1. Number of annual publications related to the search terms “non-alcoholic beverage” and
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58 “dealcoholization” over the past 30 years. Indexed by Scopus (TITLE-ABS-KEY (terms); June 2017).

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60 2. Nutritive substances in beer and wine

61 It is true that beer or wine have alcohol content that might deliver adverse effect to human, if it is
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62 consumed excessively. Some possible health disadvantages due to overconsumption of beer or wine
63 (mainly due to ethanol content and some allergens) are allergy induction, increasing uric acid (gout),
64 cancer induction, dementia, obesity, cirrhosis, and other liver problems (Sohrabvandi, Mortazavian, &
65 Rezaei, 2012). However, less is consciously known about the nutritive substances inside the brews
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66 that are beneficial to the health, but need to be accompanied with moderate amount of consumption. It
67 is therefore a great advantage to consume dealcoholized brews to get nutrition from beer or wine,
68 without the drawback effects of alcohol.
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69 In the literature, it is found that beer has significant quantities of B vitamins (thiamine, riboflavin,
70 niacin, B6, folate, and B12) that would be important to reduce the risk of having beriberi and nerve-
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71 degenerating diseases. Beer also possesses minerals such as Ca, P, Mg, Fe, Zn, high K over low Na
72 (4:1 ratio), and Se, as the active components for the active site in the intercellular antioxidant enzymes
73 (Bamforth, 2002; Sohrabvandi et al., 2012). As a fermentation product, beer is enriched with
74 significant phenolic compounds that is beneficial as antioxidant and free-radical scavengers, namely
75 phenols, benzoic acid, cinnamic acid derivatives, coumarins, catechins, di-, tri-, and oligomeric
76 proanthocyanidins, and flavonoids that is believed to be able to prevent cancer, tumor, diabetes, aging,
77 and neurological diseases(Sohrabvandi, Mousavi, Razavi, Mortazavian, & Rezaei, 2010).
78 On the other hand, although wine has higher ethanol content compared to beer, but it is also enriched
79 with antioxidants such as hydroxycinnamic acids, tyrosol and hydroxytyrosol (Lugasi & Hóvári,
80 2003) and several health-improving bioactive phenolic substances, namely caffeic acid, catechin (Li,
81 Cao, & Zhu, 2006; Norata et al., 2007), resveratrol, hydroxytyrosol, and melatonin (Fernández-Mar,
82 Mateos, García-Parrilla, Puertas, & Cantos-Villar, 2012). Those three compounds are both

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83 simultaneously capable as impressive antioxidants, anticancer substances, and
84 neuroprotectivebiochemicals. Resveratrol is a stilbene phenolic compound commonly found in red
85 wines. It is also found applications as cardioprotective, anti-diabetic, and anti-aging agent.
86 Hydroxytyrosol is a phenyl ethyl alcohol, having similar power to that of resveratrol (although not an
87 anti-aging substance), with additional antimicrobial activity. Melatonin is an indolamine that acts as a
88 neurohormone, with further ability for improving immune system (Fernández-Mar et al., 2012). In
89 conclusion, both beer and wine are not totally health-degenerative, in account of their nutritive and
90 bioactive compounds, accompanied with moderate amount of consumption, and even greater positive
91 impact for the health if the alcohol components could be extracted to a safe level (while expectedly
92 with maintained taste and aroma/flavor).

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93 3. Methods in producing low or free alcoholic beverages
94 There are several methods possible to produce low alcohol or free alcohol beverages, which are the
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pre-production and post-production techniques (Andrés-Iglesias, Blanco, García-Serna, Pando, &
96 Montero, 2016; Brányik, Silva, Baszczyňski, Lehnert, & Almeida e Silva, 2012; Erten & Campbell,
97 2001; Lehnert et al., 2009; Lehnert, Brânvik, Vicente, Dostálek, & Teixeira, 2006; Lehnert, Kuřec,
98 Brányik, & Teixeira, 2008; Montanari, Marconi, Mayer, & Fantozzi, 2008; Navrátil, Dömény,

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99 Šturdík, Šmogrovičová, & Gemeiner, 2002; Pickering, 2000; Schmidtke, Blackman, & Agboola,
100 2012; Strejc, Siříšťová, Karabín, Almeida e Silva, & Brányik, 2013; van Iersel, Meersman, Swinkels,
101 Abee, & Rombouts, 1995). In the first method, the fermentation process is modified in some aspects
102 such as using raw materials of grape juice with low sugar content; by utilizing special or immobilized

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103 yeasts that produces low ethanol content; or by blending malt juice (with no fermentation process at
104 all) with several aroma compounds in order to create a product resembles to its alcoholic counterpart.
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105 However, these processes definitely have an obvious drawback where the aroma and taste of the
106 products are not acceptable, where the color might change (Gambuti, Rinaldi, Lisanti, Pessina, &
107 Moio, 2011), some worty off-flavor might be involved, and lack of fruity aroma (Liguori, Russo,
108 Albanese, & Di Matteo, 2013b). Therefore, these days a lot of effort is placed on the post-production
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109 method (Schmidtke et al., 2012) where it is still involving the production of brews having high-
110 alcoholic composition, where the alcohol content is to be separated later and some aroma compounds
111 might be added up again (Belisario-Sánchez, Taboada-Rodríguez, Marín-Iniesta, Iguaz-Gainza, &
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112 López-Gómez, 2012; del Olmo, Blanco, Palacio, Prádanos, & Hernández, 2012).
113 The traditional post-production alcohol separation processes from brews are heat treatment processes,
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114 such as evaporation and distillation (Andrés-Iglesias, García-Serna, Montero, & Blanco, 2015; Eckert,
115 Baumann, & Gierschner, 1990; Gómez-Plaza, López-Nicolás, López-Roca, & Martínez-Cutillas,
116 1999; Pickering, 2000). As ethanol is more volatile compared to water, it is logical to remove ethanol
117 from the brews by heating. However, the product is significantly differ with the regular beer in terms
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118 of taste and flavor as some volatile components are thermally degraded during the dealcoholization
119 process, and not to mention that these processes are consuming extensive amount of energy (Blanco,
120 Andrés-Iglesias, & Montero, 2016; Pickering, 2000). An improvement to the distillation process is the
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121 spinning-cone column (SCC) method. SCC is a column having a stack of specially-designed cones
122 connected to a shaft that enables them to be rotated. These movable cones are intercalated with the
cones fixed onto the column’s wall. This meticulous design of SCC clearly combines high contact
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124 area and also mass transfer rate, thus low pressure drop in the column (Schmidtke et al., 2012). The
125 beer or wine is flowed from the top of the SCC, while water vapor is introduced from the bottom of
126 the column as the stripping agent in order to create a contact that allow water vapor to extract the
127 alcohol content from the brews. Nevertheless, as ethanol is rapidly removed, the volatile aroma
128 compounds are also extracted out, rendering the final product flavor to be reduced extensively.
129 Furthermore, the SCC process is also an energy extensive process, as water as the stripping agent
130 needs to be heated and vaporized. The SCC applications can be found in several literatures (Belisario-
131 Sánchez et al., 2012; Bellsario-Sánchez, Taboada-Rodríguez, Marín-Iniesta, & López-Gómez, 2009).
132 Another option is by partial removal of alcohol during the fermentation process (Aguera, Bes, Roy,
133 Camarasa, & Sablayrolles, 2010).This option was reported could improve the fermentation rate.
134 However, simultaneous removal of alcohol during the fermentation was stressful for the yeast. It can

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135 affect the final concentration of the compounds in the final product including the lowered volatile
136 compounds content.
137 As the aforementioned processes are lack of sensorial satisfaction due to high loss of volatile aroma
138 compounds accompanying the removed alcohol, membrane-based separation process is emerged in
139 this field as a type of ethanol-selective separation process which is expected to produce low alcoholic
140 beer or wine with acceptable aroma and taste (Schmidtke et al., 2012). The following discussion is
141 devoted to describe some of the membrane-based technologies to produce low-alcohol beer or wine.
142
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4. Membrane technologies in dealcoholization
144 Membrane technology has been widely used in various industrial sectors and started to replace
145 conventional processes due to interesting features such as low energy consumption, high separation
146 efficiency, selective and molecular separation, relatively low cost, easy to scale-up, and smaller

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147 footprint (D. Ariono, Khoiruddin, Subagjo, & Wenten, 2017; Aryanti, Yustiana, Purnama, & Wenten,
148 2015; Belyaev et al., 2003; Bernardo & Drioli, 2010; Himma, Anisah, Prasetya, & Wenten, 2016;
149 Himma, Wardani, & Wenten, 2017a, 2017b; Khoiruddin, Hakim, & Wenten, 2014; Khoiruddin,

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150 Ariono, Subagjo, & Wenten, 2017; Wenten, Dharmawijaya, Aryanti, Mukti, & Khoiruddin, 2017;
151 Wenten & Khoiruddin, 2016a). In addition, it is also possible to combine membrane technology with
152 other processes into an integrated process thus the separation steps could be reduced (intensified
153 process) (Danu Ariono, Purwasasmita, & Wenten, 2016; Drioli, Criscuoli, & Curcio, 2002; Drioli &

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154 Curcio, 2007; Khoiruddin, Widiasa, & Wenten, 2014; Purwasasmita, Nabu, Khoiruddin, & Wenten,
155 2015; Wardani, Hakim, Khoiruddin, & Wenten, 2017; Wenten, Julian, & Panjaitan, 2012; Wenten,
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156 Khoiruddin, Arfianto, & Zudiharto, 2013; Wenten & Widiasa, 2002). Furthermore, since membrane-
157 based separation can be operated at the mild condition, it is beneficial for maintaining the nutritive
158 compounds in food and beverage processing (Cuperus & Nijhuis, 1993; Mohammad, Ng, Lim, & Ng,
159 2012; Snape & Nakajima, 1996). In this section, we will discuss exclusively on the membrane-based
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160 technologies, such as reverse osmosis, nanofiltration, dialysis, membrane contactor, osmotic
161 distillation, and pervaporation.
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(a) Reverse Osmosis and Nanofiltration (batch (b) Dialysis, Osmotic distillation, Membrane
or diafiltration mode) Contactor

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(c) Pervaporation

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163 Figure 2. Schematic of membrane-based processes for beverage dealcoholization

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165 4.1. Reverse osmosis (RO)
166 RO can be promising alternative for dealcoholization process replacing the thermal-based processes
167 because it can remove alcohol under mild temperature (Wenten & Khoiruddin, 2016b). The low

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168 molecules, namely ethanol and water, are permeated across the membrane while the taste and
169 nutritive components of beverages are retained in the product. Since RO is operated under low
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170 operating temperature, it offers advantages over traditional distillation which include reduction of
171 energy consumption, high quality of beverage, low damage to temperature sensitive compounds, and
172 alcohol removal without phase change (Catarino, Mendes, Madeira, & Ferreira, 2007). Reported
173 studies of RO applications in beverage dealcoholization are shown in Table 1.
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174 RO has been used in several works to remove ethanol from fermented beverage such as beer, wine,
175 and cider (Catarino & Mendes, 2011a; Gil et al., 2013; Leeper & Tsao, 1987; Lisanti, Gambuti,
176 Genovese, Piombino, & Moio, 2013; López, Alvarez, Riera, & Alvarez, 2002; Pilipovik & Riverol,
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177 2005). In dealcoholization, RO process can be operated as batch, continuous, or diafiltration mode.
178 According to those studies, beverage dealcoholization using RO process can be summarized as
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179 follow:
180 - RO can be used in beverage dealcoholization with insignificant change of flavor and quality.
181 - Producing dealcoholized beverage with alcoholic content < 0.45% is not feasible.
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182 - Feed dilution is recommended to keep the levels of carbohydrate content, extract percentage,
183 and salts in acceptable range.
184 - Considerable flux declining is found for beverage with higher pH.
185 - Cellulose acetate membrane exhibits the highest flux and the lowest ethanol rejection. The
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186 highest rejection of polyamide membrane is considered as the effect of its hydrophobicity.
187 - A higher ethanol removal and rejection of desirable aroma compounds can be obtained via
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188 diafiltration mode rather than batch operating mode.

189 - It requires a relatively high operating pressure to exceeds osmotic pressure of the beverage
190 solution.
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192 4.2. Nanofiltration (NF)
193 NF is a pressure driven membrane process that uses semipermeable membrane which has
194 characteristics between RO and ultrafiltration (UF) membranes. A more loose pores of NF membrane
195 compared to RO allows to provide higher fluxes than RO (Figure 3) while exhibits better rejection for
196 small molecules than UF membrane. Several studies on NF application in wine processing have been
197 reported (Table 1). Banvolgyi and co-workers (Szilvia Banvolgyi, Kiss, Bekassy-Molnar, & Vatai,
198 2006) have investigated the performance of NF (XN45 from Trisep) for concentrating red wine.

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199 During the concentration of valuable components, water and ethanol permeated through the
200 membrane resulting in permeate with similar alcoholic content of the original wine. The alcoholic
201 content of permeate was 10.75% ABV (at 20 bar and 30 °C) which was slightly lower than the
202 original wine (12.81% ABV) while the rejection was 9.7%. Furthermore, the valuable components
203 such as sugar, total acid, total extract and sugarless extract were increased to about two times larger
204 from the initial concentrations with low aroma loss.
205 Comparison of NF and RO membranes for dealcoholization of wine containing 12% ABV were
206 conducted under 16 bar and 30 °C of feed pressure and operating temperature, respectively (Catarino
207 & Mendes, 2011a). The results showed that NF membranes exhibited higher flux than RO membrane

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208 and acceptable ethanol rejection (7 to 10 %). NF membrane showed the effectiveness in
209 dealcoholization of wine due to their high ethanol permeability, high rejection of aroma compounds,
210 and promising organoleptic properties of the product. Similar results was found in another study
211 (Labanda, Vichi, Llorens, & López-Tamames, 2009). In addition, another approach in producing low

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212 alcohol-contents could be applied by reducing sugar content of musts with NF membrane (N García-
213 Martín et al., 2010; Noemi García-Martín et al., 2011; Massot, Mietton-Peuchot, Peuchot, & Milisic,
214 2008; Salgado et al., 2017). The advantage of the method is easier to preserve the organoleptic

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215 properties resulting from fermentation. Despite of the effective performance on dealcoholizing wine,
216 NF applications on the beer dealcoholization are not very commonly reported in the literature. With
217 higher flux and high rejection of aroma compounds, NF could be promising alternative to RO on
218 beverage dealcoholization.

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221 Figure 3. Permeate flux and ethanol rejection of several NF and RO membranes in wine
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222 dealcoholization (Data labels: membrane; pressure [bar]; temperature [oC]; Data from refs. (Szilvia
223 Banvolgyi et al., 2006; Catarino & Mendes, 2011a; Labanda et al., 2009; Takács, Korány, & Vatai,
224 2010)).

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225
Process Membrane
RO Renew spiral wound
membrane, no available
information of the material
Cellulose acetate, DSS-
CA995P, Alfa Laval
Cellulose acetate, DSS-
CA995P, Alfa Laval
Osmonics - SE
Cellulose acetate, CA995PE
- Red Wines (AOC
Polyester-sulfone
Polyamide, AF99
NF Polyamide, NF99 HF, Alfa
Laval
Polyamide, XN45 (Trisep)
Polyamide, XN45 (Trisep)
NF200, DOW Filmtec
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Table 1. Typical example of beverage dealcoholization using RO and NF membranes
Beverage Operating conditions Results Ref.
Home-made C0:5.5%; P: 35 bar; T: 0oC; Alcohol concentration in final product: (Pilipovik & Riverol, 2005)
alcoholic beverage 0.5%
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Beer C0:5.45%; P: 40 bar; T: 10oC; Alcohol concentration in permeate: (Catarino, Mendes, Madeira, &
3.84% Ferreira, 2006)
Beer C0:5.26%; P: 40 bar; T: 5oC; Alcohol concentration in final product: (Catarino et al., 2007)
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~0.5%
Model Wine C0:12%; P: 29 bar; T: 15oC; Alcohol rejection: 36% (Labanda et al., 2009)
C0:12%; P: 16 bar; T: 30oC;
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Red Wine Alcohol concentration in final product: (Catarino & Mendes, 2011a)
8.4%; in permeate: 11.6%;
- Dealcoholization cost: 0.15 €/L for (Gil et al., 2013)
Penede`s & AOC removing 1 % of ethanol. No
Priorat) significant change in wine
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characteristics
Stout beer C0:6.6%; P: 4.9 bar; T: 20oC; Alcohol concentration in product: 0%; (Alcantara et al., 2016)
Sample dilution gives a better
performance.
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Apple cider C0:8%; P: 45 bar; T: 15oC; Alcohol removal: 75% (in diafiltration (López et al., 2002)
mode)
Red Wine C0:12%; P: 16 bar; T: 30oC; Alcohol concentration in product: (Catarino & Mendes, 2011a)
9.11% (120 h);
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Red Wine (from The C0:12.8%; P: 20 bar; T: 30oC; Alcohol concentration in product: (Szilvia Banvolgyi et al., 2006)
Bojt Laszlo wine 9.8%; Cost: 4.8 €/m3
cellar)
Red Wine (from The
Bojt Laszlo wine
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C0:12%; P: 20 bar; T: 20oC; Alcohol concentration in product: 4-6%
(reconstitution);
(S Banvolgyi, Savaş Bahçeci,
Vatai, Bekassy, & Bekassy-
cellar) Molnar, 2016)
Tokaji árslevel C0:13.1%; P: 20 bar; T: 25oC; Alcohol concentration in permeate: (Takács et al., 2010)
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wine 9.72%; Alcohol rejection: 17.06%;
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226 4.3. Dialysis
227 An early study on the beer dealcoholization by using dialysis processes have been conducted by
228 Moonen and Niefind using a pilot unit with capacity of 1500 l/h (Moonen & Niefind, 1982). In the
229 dealcoholization via dialysis, ethanol is removed using the principle of selective diffusion through
230 semipermeable membrane. Alcohol diffuses through the membrane from beer into water as a result of
231 concentration gradient between both solutions (see Figure 2 b). It was suggested that the dialysis
232 should be operated at pressure above the CO2 saturation pressure, virtually zero difference to the
233 transmembrane pressure, and the water stream is enriched with CO2 to prevent CO2 release. By using
234 hollow fiber membrane (Cuprophan® from cotton cellulose) with 90 m2 area, with dialysis

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235 temperature of 5 °C, alcohol content was reduced from 6.29 to 3 %v/v under continuous operation.
236 Leskošek and Mitrović studied an optimization of beer dealcoholization using Cuprophane
237 membranes (I. J. Leskošek & Mitrović, 1994), where the clearance and the permeability of ethanol as
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the relevant penetrant were optimized. The optimal selectivity could be obtained by tuning an
239 appropriate average velocity of beer to achieve an adequate residence time at specific hydrodynamic
240 regime (related to a specific Reynold number). Furthermore, membrane thickness and transmembrane
241 pressure also influence alcohol and beer separation using dialysis process (I. Leskošek, Mitrović, &

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242 Nedović, 1995). An 8 µm thick Cuprophane hollow fiber membrane showed higher ultrafiltration
243 coefficient, permeability, and higher selectivity for ethanol than that of 11 µm thick membrane. By
244 applying transmembrane pressure higher than 40 Pa, removal of essential volatile flavor components
245 might be minimized thus improved the quality of the dealcoholized beer. Moreover, the ethanol

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246 concentration could be reduced from 3.8 to 0.35%w/w (when operated at 2 bar and 5 °C).
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247 Experimental studies of beer dialysis with transmembrane pressure were performed to investigate
248 mass transfer of the process (Leskoŝek, Nedović, & Petkovska, 1997; M Petkovska, Leskošek, &
249 Nedović, 1997; Menka Petkovska, Leskošek-Čukalović, Vukosavljević, & Krstić, 1996). Two
250 different membrane materials i.e. Cuprophane (regenerated cellulose) and polysulfone were used. By
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251 applying transmembrane pressure, two simultaneous mass transfer processes took place, namely
252 diffusion and convection. Contribution of convection induced by transmembrane pressure was found
253 to be depend on membrane type, beer flow rate, and molecular size of solute. Elimination of ethanol
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depended on diffusion mechanism while convection contributed to large molecule transfer and extract
255 loss which diminished the efficiency of selective alcohol/extract separation in beer dialysis.
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256
257 4.4. Osmotic distillation (OD)
258 In the process of dealcoholization of beverages using OD, microporous hydrophobic membrane is
259 utilized. An ethanolic feed is contacted onto the surface of the membrane at atmospheric pressure and
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260 room temperature, while the opposite side of the membrane is contacted to a stripping solution flowed
261 in counter-current mode (see Figure 2 b). As ethanol is permeating through the membrane, the
262 stripping solution is tasked to capture the ethanol. There are different names for this process, such as
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263 membrane contactor, isothermal membrane distillation, or evaporative pertraction, but they are
264 actually bear the similar principles with OD. With the OD process, both beer and wine can be
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dealcoholized to some extent of control of the product concentration (Diban, Athes, Bes, & Souchon,
266 2008; Liguori, De Francesco, Russo, Perretti, et al., 2015; Liguori, Russo, Albanese, & Di Matteo,
267 2013a; Liguori et al., 2013b). A successful pilot plant test of OD for beer dealcoholization has also
268 been reported (De Francesco, Sileoni, Marconi, & Perretti, 2015).
269 A handful numbers of OD or membrane contactor for the application of dealcoholization of beer or
270 wines are shown in Table 2. It can be observed that the dealcoholization process by using OD is
271 dominated by the utilization of polypropylene-based microporous hollow fiber membrane, operated at
272 about ambient temperature, using water as an inexpensive and biologically safe stripping agent.
273 Moreover, OD is able to perform partial dealcoholization of wine (final concentration of ethanol of
274 8% to 11% ABV), total dealcoholization of wine (< 2% ABV), and dealcoholization to < 1% ABV,
275 either from real brews or synthetic ethanol-water mixtures. There are some variations of the
276 temperature and types of stripping agent, but commonly the optimum conditions are room
277 temperature with water as stripping agent.

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278 From several researches in the Table 2, there are some studies regarding the quality of the volatile
279 aroma compounds in the dealcoholized beer, conducted using organoleptic testing or spectrometric
280 study. Generally, for the partially dealcoholized wine (reduction from 2% to 5% ABV), the aroma and
281 flavor are not significantly different to that of original wine. However, for the total dealcoholized
282 wine and beer (reduction more than 10%, and 5%, respectively), left a hole for the taste and need
283 additional aroma components, such as ethyl acetate, isoamyl acetate, and so on (Liguori, De
284 Francesco, Russo, Perretti, et al., 2015; Liguori et al., 2013b).
285
286 4.5. Pervaporation (PV)

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287 PV is a concentration-driven membrane-based process, which works with the principle of permeation
288 and evaporation over a membrane (Wenten et al., 2017). At first the liquid feed is contacted onto the
289 membrane, without any additional pressure, at mild temperature (around 50 °C). The component that
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is intended to be separated will then interacts with the membrane material due to the activity
291 coefficient and themodynamical affinity, and later permeates through the membrane, evaporates and
292 leaves the membrane. The permeate stream may then be collected with the assistance of liquid
293 nitrogen cold trap (Feng & Huang, 1997). PV is actually a common membrane-based process for

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294 alcohol dehydration (removal of water from ethanol mixture, to produce alcohol with purity>98%,
295 and usually combined with distillation column) due to its superiority in breaking the azeotropic point
296 between water-ethanol. For the pervaporation dehydration, usually the membranes of interest are the
297 hydrophilic ones, capable of drawing water and get the ethanol dehydrated. However, for the

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298 dealcoholization of beer the hydrophobic membranes play a vital role (Feng & Huang, 1997; Jiang,
299 Wang, Chung, Qiao, & Lai, 2009).
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300 Takács et al. (Takács, Vatai, & Korány, 2007) reported dealcoholization of semi-sweet
301 TokajiHa´rslevelu (Linden leaves) of vintage 1997 quality wines (provenance Tolcsva having 13.11%
302 ABV) using PERVAP.Sulzer 1060 type pervaporation (organophilic flat composite membrane).
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303 Results of the study showed that temperature plays the important role in pervaporation performance
304 i.e. flux and separation ability. Meanwhile, economic analysis implies that the high cost of investment
305 was due to the relatively high price of non-porous pervaporation membrane. Tan et al. (Tan et al.,
306
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2003) used a pervaporation with flat composite PDMS membrane for wine dealcoholization. The
307 dealcoholization process was conducted at 40oC and 1.3 kPa of permeate pressure. The process could
308 produce wine with 3-7% of ethanol while the average flux was 1.5 kg.m-2.h
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309 Catarino and Mendes (Catarino & Mendes, 2011b) reported the application of PVfor dealcoholization
310 using hydrophobic POMS/PEI membrane (polyoctylmethylsiloxane/supported onto polyetherimide)
311 only for extracting aroma and volatile components from Pilsner beer (5.5% ABV), namely ethanol,
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312 propanol, isobutanol, amyl alcohol, ethyl acetate, isoamyl acetate, and acetaldehyde. The main step
313 for dealcoholization was conducted by using SCC process, where the ethanol from the Pilsner beer
314 could be reduced to 0.45% ABV. After following the SCC distillation, the pervaporated aroma is then
315 re-blended into the dealcoholized beer in order to obtain beer with acceptable taste. Similar strategy
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316 on recovering amyl alcohol, ethyl acetate, isoamyl acetate from Special (5.5% ABV) and Reserve
317 beer (6.5% ABV) was carried out by pervaporation using hydrophobic PDMS/PET
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318 (polydimethylsiloxane/supported onto polyethylene terephtalate, from Pervatech BV), continued with
319 blending the pervaporated aroma onto the non-alcoholic beer, resulting in organoleptically
320 satisfactory beer (del Olmo et al., 2012).
321 A membrane distillation using non-porous membrane which is similar to pervaporation process has
322 been used by Indonesian scientists for the dealcoholization of Anker beer, a local Indonesian beer
323 (Purwasasmita, Kurnia, Mandias, Khoiruddin, & Wenten, 2015). The dealcoholization process was
324 carried out by using non-porous spiral wound membrane from DOW Filmtec, composed of polyamide
325 thin film composite membrane, at room temperature and 2-3 bar gauge, and permeate of alcohol was
326 drawn by vacuum ranged from 0.49-0.66 bar. This process was successfully reduced ethanol from 5%
327 ABV to 2.45% ABV in 6 h, without meaningful loss of several nutritious components (maltose and
328 glycerol).
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330 Table 2. Performance of OD during dealcoholization
Operating conditions Results
Membranes Type of beverage Ref.
Time C0 T Qf Qs Cf
Liqui-cel 1x5.5, PP hollow fiber Red wine, Aglianico 255 13 20 0.07 0.14 0.19 (Liguori et al., 2013b)

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Liqui-cel 0.5x1, PP hollow fiber Red wine, Aglianico 170 12.5 20 1.2 2.4 10.65 (Liguori et al., 2013a)
Ethanol-water mixture 170 12.5 20 1.2 2.4 10.6
170 10 20 1.2 2.4 7.8
340 10 20 1.2 2.4 5

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510 10 20 1.2 2.4 4
680 10 20 1.2 2.4 3
850 10 20 1.2 2.4 2

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Liqui-cel Extra-flow, PP hollow fiber Red wine, Merlot 60 13.35 20 5.8 8.1 11 (Diban et al., 2008)
Ethanol-water mixture 20 13.02 20 5.5 8.7 10
20 10.78 20 5.4 8.8 8
60 13.32 20 5.6 9.6 11

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60 12.88 20 5.4 7.6 10
60 13.39 20 1.7 5 8
Liqui-cel Extra-flow, PP hollow fiber Red wine, Aglianico 2007 60 15.46 20 0.583 0.183 13.46 (Gambuti et al., 2011)
120 20 0.583 0.183 12.46
180 20 0.583 0.183 10.46

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Red wine, Aglianico 2008 60 13.81 20 0.583 0.183 11.81
120 20 0.583 0.183 10.81
180 20 0.583 0.183 8.81
Red wine, Merlot 60 13.88 20 0.583 0.183 11.88

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120 20 0.583 0.183 10.88
180 20 0.583 0.183 8.88
Red wine, Piedirosso 60 13.67 20 0.583 0.183 11.67

Liqui-cel Extra-flow, PP hollow fiber

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Red wine, Aglianico 2007
120
180
88 15.46
20
20
20
0.583
0.583
0.583
0.183
0.183
0.183
10.67
8.67
13.54 (Lisanti et al., 2013)
140 20 0.583 0.183 12.04
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246 20 0.583 0.183 10.84
331
332
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333
334 Table 2. (Continued)
Liqui-cel Extra-flow Red wine, Aglianico 2008 86 13.81 20 0.583 0.183 11.65 (Lisanti et al., 2013)

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Polypropylene hollow fiber 147 20 0.583 0.183 10.52
283 20 0.583 0.183 8.83
Liqui-cel Extra-flow Aglianico wine 180 12.8 - - - 0.42 (Liguori, Attanasio, Albanese,
& Di Matteo, 2010)

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Polyvinylidene fluoride (PVDF) Red wine (Siam Winery) 360 13.2 30 0.066 0.053 8.1 (Varavuth, Jiraratananon, &
Memcor Ethanol-water mixturea 60 13 30 0.053 0.093 11.92 Atchariyawut, 2009)
Ethanol-water mixtureb

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60 13 30 0.053 0.093 11.89
Ethanol-water mixturec 60 13 30 0.053 0.093 11.77
Polypropylene hollow fibers (JU.CLA.S. Langhe Rosè (C0:13.2% v/v), 360 13-15 10 1.6 0.8 5 (Motta et al., 2017)
LTD, Verona, Italy) VerdunoPelaverga red wine

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(C0:15.2% v/v) and Barbera red
wine (C0: 14.6% v/v)
Liqui-cel ExtraFlow Xarelo wine 20 11.5 10 10 10.1 (Diban et al., 2013)
Garnacha wine 60 13.9 5 5 9.3

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Tempranillo wine 60 13.3 5.8 5.8 9.0
Liqui-cel mini module 1.7x5.5 Lager beer A 60 4.53 10 0.5 0.5 1.5 (De Francesco, Freeman, Lee,
Membrana GmbH 120 10 0.5 0.5 1.06 Marconi, & Perretti, 2014)
Lager beer B 60 5 10 0.5 0.5 1.2

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120 10 0.5 0.5 0.79
Lager beer C 60 4.81 10 0.5 0.5 1.1
120 10 0.5 0.5 0.51
Liqui-cel 1x5.5
Polypropylene
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Italian lager beer, Vs/Vf = 1

Italian lager beer, Vs/Vf = 2

200

200
5

5
10

10
0.07

0.07
0.14

0.14
0.89

0.47
(Russo, Liguori, Albanese,
Crescitelli, & Di Matteo, 2013)
(Liguori, De Francesco, Russo,
Perretti, et al., 2015)
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Liqui-cel polypropylene hollow fiber Craft beer 270 4.3 - 0.7 0.14 0.7 (Liguori, De Francesco, Russo,
Albanese, et al., 2015)
Liqui-cel polypropylene hollow fiber Weiss beer 285 5.7 1.0 (Liguori et al., 2016)
Liqui-cel polypropylene hollow fiber Bitter beer 285 3.6 10 0.07 0.14 0.7
Liqui-cel ExtraFlow Beer 150 5.2 24 30 30 0.9 (De Francesco et al., 2015)
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335 Note: C0 – initial concentration of alcohol; Cf – alcohol concentration in the final product; Qf – feed flow rate; Qs – flow rate of stripping agent (most of the times, water); T – temperature; PP –
336 polypropylene;
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337 Units: Concentration - (%v/v); Pressure – bar; Rejection - %; T - °C; Flowrate – l/min;Time – minutes;
338 a
Water as stripping solution; b Glycerol 50% w/w as stripping solution; c CaCl2 40% w/w as stripping solution

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339 5. Miscellaneous technologies
340 Besides the conventional thermal-based and membrane-based process, there are some several new
341 emerging technologies that are noteworthy in the application of the dealcoholization process. A
342 relatively new technology that is quite exciting for its product quality in aroma recovery, and
343 cleanliness/food safety, is the supercritical fluid extraction, with CO2 as the most common solvent
344 (Fornari, Hernández, Ruiz-Rodriguez, Javier Señorans, & Reglero, 2009; Medina & Martínez, 1997;
345 Rizvi, Yu, Bhaskar, & Chidambarra Raj, 1994; Ruiz-Rodriguez, Fornari, Hernández, Señorans, &
346 Reglero, 2010; Schmidtke et al., 2012). This process acts with the thermodynamic principles, where at
347 above its critical pressure and temperature, a matter could be a phase where both densities of liquid

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348 and gas are the same and no interphase between them. In other words, supercritical fluid acts both as
349 liquid and gas. Therefore, supercritical CO2 may extract organic components due to its affinity from
350 the carbon chain (as liquid), and then it will immediately evaporate (as gas) and leave the extracted
351 substances, without any residue. CO2 has critical temperature of 31 °C and critical pressure of 73 atm

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352 (Atkins & De Paula, 2006). Although the advantages of clean, no toxic residue, nonflammable, cheap
353 and recyclable CO2 are interesting, however the supercritical CO2 extraction are still limited for the
354 dealcoholization of beverages due to economical infeasibility for preparing an industrial scale

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355 supercritical fluid reactor/container, that must be built form materials that is able to withstand >75
356 atm, while the extracted component is quite small, only 5% ethanol ABV for beer.
357 Another carbon dioxide based technology which has been used for dealcoholization of beverage is
358 extraction with solid carbon dioxide. A pilot scale of wine dealcoholization (capacity of 10 L/h) using

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359 this extraction process has been reported by Antonelli et al. (Antonelli, Carnacini, Marignetti, &
360 Natali, 1996). The system was applied to remove the alcohol from six samples of red and white wines.
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361 In this process, wines were sprayed over the solid carbon dioxide and extraction process was
362 conducted at 5oC and 5 min. retention time. The alcohol content of white wines was successfully
363 reduced to 1.1-1.4% from initial 9.4-10.7% of concentrations. Meanwhile, for the red wines, the
364 alcohol content was reduced to 4-6%. However, similar to distillation, a loss of major volatile
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365 compounds was observed in this technique. In addition, the energy consumption of the process is also
366 relative high (12 kW/kg wine).
367
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Recently, a microbial fuel cell (MFC) is proposed by Szollosi et al. (Szollosi et al., 2016) to produce a
368 non-alcoholic beer. Generally, MFC is used to simultaneously produce energy and to treat wastewater
369 in a single process (Khoiruddin, Aryanti, Hakim, & Wenten, 2017). MFC consists of one or two
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370 chambers separated by proton exchange membrane and equipped with a pair of electrode. In their
371 study, two-chamber MFC was used wherein about 107 CFU/mL yeast cell was employed to inoculate
372 the anode chamber. In addition, Riboflavin was used as a non-toxic extracellular mediator. They
373 found that a low-alcoholic beer (alcohol content < 2%) could be produced by fermentation in an MFC
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374 as well as an electricity. Furthermore, they proposed that non-alcoholic beer could be produced in
375 MFC by increasing anode surface and/or controlling the amount of electron shuttles.
376
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377 6. Challenges
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378 As the world paradigm over beer or wine is shifted from excessive drinking to moderate drinking, and
379 followed by healthy drinking (to avoid ethanol, and looking for nutrition and bioactive components
380 such as anticancer and antioxidants), the production of low alcohol or even alcohol free beverages
381 (beer or wine) is increased. However, the production of such beer or wine has its own challenges,
382 especially in preserving volatile aroma compounds that are important to give delicious and fruity like
383 taste/aroma. Unfortunately, those volatile organic components are soluble in ethanol, an organic
384 solvent, where simultaneous removal of ethanol and aroma will definitely occur (Bartolomé, Peña-
385 Neira, & Gómez-Cordovés, 2000; Liguori, De Francesco, Russo, Perretti, et al., 2015; Liguori et al.,
386 2013b) (see Figure 4). Therefore, it is imperative for the research and development in the field of
387 membrane science and technology, especially, to explore new exciting possibilities for the selective
388 removal of ethanol while retaining the aroma components. Membrane-based separations have the
389 advantage in energy-saving process (mild temperature), a type of process with relatively high
390 selectivity and productivity, but it is still limited with the thermodynamics of the solubility. Hopefully

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391 in the near future this barrier, along with the energy consumption, and productivity will be gradually
392 tackled.
393

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394
395 Figure 4. Loss of volatile compounds in dealcoholized beer produced from different methods
396

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(Catarino et al., 2006; De Francesco et al., 2015; Liguori et al., 2016)

397
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398 7. Conclusions
399 With increasing demand of alcohol-free beer or wines (less than 1.2 and 7% ABV, respectively), it
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400 opens up opportunity for both scientists and engineers in the field of fermentation or separation
401 processes to make such products available, with comparable taste and flavor to that of standard brews,
402 and sustaining the beneficial bioactive components (listed previously) inside both beverages. This
403 review has discussed the state of the art for production of alcohol-free beverages. It is initially
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404 developed from several past pre-fermentation technologies. Currently, post-fermentation

405 dealcoholization technologies has also been reviewed, with deep focus on the emerging membrane-
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406 based dealcoholization processes. It is believed that the membrane-based processes will also be the
407 preferred methods in the future for the removal of alcohol (besides supercritical fluid extraction, albeit
408 its high pressure requirement) due to their promising properties of high selectivity to ethanol, mild
409 operation temperature thus saving vast amount of energy, and combined with high productivity.
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410 However, there is still a lot effort to be placed on the research for development of the finding the
411 prospective separation process that may produce brews that are both healthy (dealcoholized) and
412 delicious (acceptable sensory and organoleptic aspects).
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413 References
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Title: Beverage Dealcoholization Processes: Past, Present, and Future

Authors: D. Mangindaan, K. Khoiruddin, I.G. Wenten

Highlights
• There is a highly significant increase on the demand of non-alcoholic beverages.
• It is imperative to have appropriate processes to produce dealcoholized brews.
• The present status of beverage dealcoholization processes are discussed in detail.

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• The membrane processes demonstrate promising results for dealcoholization.

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