Accepted Manuscript

Integrated production of biodiesel and bioethanol from sweet potato

Joab Oliveira Virgnio e Silva, Manuel Fonseca Almeida, Maria da Conceio Alvim-
Ferraz, Joana Maia Dias

PII: S0960-1481(17)30666-3
DOI: 10.1016/j.renene.2017.07.052
Reference: RENE 9027

To appear in: Renewable Energy

Received Date: 21 February 2017

Revised Date: 2 June 2017
Accepted Date: 11 July 2017

Please cite this article as: Virgnio e Silva JO, Almeida MF, da Conceio Alvim-Ferraz M, Dias JM,
Integrated production of biodiesel and bioethanol from sweet potato, Renewable Energy (2017), doi:
10.1016/j.renene.2017.07.052.

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 ACCEPTED MANUSCRIPT
1 Integrated production of biodiesel and bioetanol from sweet potato

2 Joab Oliveira Virgnio e Silva a, Manuel Fonseca Almeida a, Maria da

3 Conceio Alvim-Ferraz b, Joana Maia Dias a

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a
4 LEPABE, Departamento de Engenharia Metalrgica e de Materiais, Faculdade de Engenharia,

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5 Universidade do Porto, R. Dr. Roberto Frias, 4200-465 Porto, Portugal
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6 LEPABE, Departamento de Engenharia Qumica, Faculdade de Engenharia, Universidade do

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7 Porto, R. Dr. Roberto Frias, 4200-465 Porto, Portugal
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8 Corresponding author. E-mail address: jmdias@fe.up.pt (J. M. Dias)
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9 ABSTRACT

10 In the present study, the production of sweet potato bioethanol was conducted at a small industrial

11 plant in Brazil and integrated in biodiesel production through ethanolysis. The specific objectives

12 were: (i) monitor bioethanol production at a small industrial plant, considering production yield; (ii)

13 study the ethanolysis of sunflower oil using sweet potato bioethanol with different grades (98, 99

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14 and 99.4 GL), with focus on biodiesel yield and pu rity. Bioethanol was produced under the

15 following conditions: Sweet potato dilution in water (1:1 in wt.%); enzymatic hydrolysis with alpha-

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16 amylase (90 C) and glucoamylase (60 C) enzymes (700 mL/t); and, fermentation (30 C) with

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17 saccharomyces cerevisiae (3.3 kg/t). Ethanolysis was performed as follows: 6:1 ethanol:oil molar

18 ratio; 1.0 wt.% NaOH; 45 C; 1 h. The average yield of bioethanol was 161.4 L/t, corresponding to

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19 10 598 L/ha. Biodiesel synthesis using bioethanol of different grades showed that both the yield
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20 and purity of the product increased with the grade of the ethanol used, with values ranging from 63

21 to 83 wt.%, and 50 to 94 wt.% for yield and purity, respectively. Results show that a high alcohol
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22 grade is required to make viable integrated production of biodiesel and bioethanol.

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23 Keywords: Bioethanol; sweet potato; biodiesel; ethanolysis.

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24

25 ABBREVIATIONS
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26 ABNT - Brazilian Association of Technical Standards; BD Biodiesel; Exp.- Experiment; GHG -

27 Greenhouse Gases; IEA - International Energy Agency; ISO - International Organization for
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28 Standardization; LASPER - Laboratory of Energy Production Systems from Renewable Resources;

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29 N.A. Not applied; NBR - Brazilian Standard; UFT - Federal University of Tocantins; GL -

30 Alcoholic degrees Gay Lussac; Bx - Degrees brix.

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31 1. Introduction

32 World population growth has practically doubled in the last five decades, increasing energy

33 consumption due to the development of new technologies and processes, which, having brought

34 great benefits to mankind, are based on a rather insecure and limited energy matrix, derived from

35 fossil fuels (coal, oil and natural gas), which are mainly responsible for greenhouse gases (GHG).

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36 Such an energy model makes the planet progressively less healthy, so it is extremely important

37 that the next generations encourage the use of renewable energies such as solar, wind, thermal,

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38 hydroelectric and biomass, among others. The use of biomass in the production of biofuels

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39 (bioethanol and biodiesel) can meet the energy needs in a sustainable manner, conserving

40 biodiversity and becoming an alternative for small farming communities, which should be adapted

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41 to regional constraints and characteristics to ensure sustainability, namely through absence of
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42 competition with food sources and reduced land use impacts [1-3].

43 In 2015, for the first time in history, some developing countries (such as China, India and Brazil)
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44 invested more in renewable energy and biofuels than other developed economies, and 19 % more

45 than in 2014 [4]. The International Energy Agency (IEA) proposes to increase investments in
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46 renewable energy to reach US $ 400 billion by 2030 [5] as it is recognized that the promotion of
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47 renewable energy contributes decisively to an environmentally sustainable future [6]. Biofuels,

48 including biodiesel and bioethanol, already play an important role in the current supply of
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49 renewable energy, and it is estimated that there will be a continued growth in the use of these

50 biomass sources; in agreement, the demand for bioethanol may increase by 108 % between 2015
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51 and 2050 [3].

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52 1.1. Bioethanol

53 In 2015, world bioethanol production was approximately 98.3 Mm3, corresponding to about 74 % of

54 all biofuels produced, showing the potential and relevance of the production of this renewable

55 energy source [4]. The bioethanol currently used is mainly produced from sugarcane in Brazil, corn

56 in the United States and sugar beet in Europe. Recent studies indicate that sweet potato is a highly

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57 promising complementary alternative raw material for the production of this biofuel because of high

58 yields of ethanol, between 5 859 and 10 467 L/ha [7-10], when compared to sugarcane, between 6

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59 281 and 7 224 L/ha [11-13], and corn, between 1 598 and 4 250 L/ha [14, 15].

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60 By 2014, the International Potato Center [16] refers to sweet potato [Ipomoea batatas (L.) Lam.]

61 as the sixth most cultivated food crop on the planet, after rice, wheat, potatoes, maize and

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62 cassava. In 2016, the world production was 105 million tons, about 95 % of which was originated in
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63 developing countries and Brazil ranked the 18th place, with approximately 0.5 % of world

64 production [17]; the northern region produced only around 1 %, despite the high potential [18].
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65 Sweet potato is a perennial crop of wide adaptation, easy growth and high resistance to drought,

66 with low production cost when compared to other conventional crops, being resistant to pests and
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67 also contributing to soil erosion prevention. Taking into account the harvesting practices, it is very
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68 versatile, allowing mechanical processes adapted from existing technologies, or manual

69 harvesting, creating local jobs, with high relevance for the country [10, 19].
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70 The energy source contained in the sweet potato is in the form of starch; bioethanol production

71 from starch involves 3 steps: hydrolysis (acid or enzymatic), fermentation and distillation [20]. The
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72 hydrolysis process causes the total unfolding of the amylose molecules, which break down and
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73 transform into dextrins, and finally into glucose. At the fermentation phase, the simple sugars are

74 transformed into ethanol. To obtain high yields it is extremely relevant to optimize pre-treatmens

75 and fermentation conditions [21-23]. The bioethanol produced is separated from the wet residue by

76 the distillation process to obtain the final ethanol product [10]; this step is responsible for the

77 highest energy consumptions in the bioethanol production process [22] and dictates the final grade

78 of the product.

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79 The overall energy consumption and production in ethanol production depends upon raw

80 material production and transport, bioethanol production (sugars obtention, fementation and

81 distillation) as well as final product energy content and associated yields [22]. The use of locally

82 available raw materials has the potential to reduce transport costs, also affecting positively the

83 energy balance.

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84

85 1.2. Biodiesel

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86 Currently, almost all biodiesel produced worldwide is based on the transesterification process

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87 using the methylic route (methanolysis), due to low production costs and operational simplicity [24].

88 The kinetics of the methanolysis reaction is also usually referred to as faster compared to

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89 ethanolysis [25]. However, the use of methanol for the production of biodiesel is environmentally
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90 less favorable because it is mostly obtained from fossil resources. On the opposite, ethanol has

91 low toxicity and becomes more environmentally sustainable as it is easily obtained from renewable
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92 biomass sources [26].

93 In 2015, biodiesel was the second most produced biofuel in the world, with 30.1 Mm3,
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94 corresponding to 22 % of the total biofuels produced [4]. Biodiesel is a mixture of esters that can
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95 be produced by various processes [27]. The most commonly used is transesterification, whereby

96 triglyceride molecules react with an alcohol (methanol or ethanol), generating esters of fatty acids
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97 (biodiesel) and glycerol, usually using a homogeneous alkaline catalyst (NaOH, KOH and

98 respective methoxides between others). As already mentioned, the biodiesel production industries
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99 generally follow the methanolic route, due to the lower cost and operational simplicity [28].
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100 Amongst the problems arising from the use of ethanol, the difficulty in products separation and

101 purification is considered the most relevant [29] since it can lead to lower biodiesel yield and purity.

102 Several studies indicate ethanol as a promising alternative for the production of biodiesel [29-

103 33], mainly from an environmental point of view, due to the replacement of methanol (from fossil

104 derived resources) by a renewable energy source. Sweet potato is also indicated as a good

105 substrate for the production of a more sustainable bioethanol [7, 9, 10, 21, 34-36]. Most of the

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106 existing studies focus on the laboratory production o biofuels, with little emphasis on the pilot and

107 industrial scale productions, with related difficulties and developments. The development of small

108 scale production plants has high relevance in remote regions of several countries, including Brazil

109 (North, with large territorial area and rich biodiversity), adding value to regional raw materials and

110 making processes more economically-viable, contributing to local sustainable development. In

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111 particular, for the production of bioethanol at a small scale, the purity of the product is a key factor,

112 that strongly conditions the production cost.The integrated production of biodiesel and bioethanol

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113 lis not a new topic [29], but in this study, the startup of a bioethanol small industrial plant using

114 sweet potato was followed and the integration of bioethanol for biodiesel production was

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115 evaluated, considering different bioethanol grades, to assess technical integration constrains. Such

116 approach has without doubt novelty, without similar studies being found in the literature.

117
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The specific objectives were established as: (i) bioethanol production in the start-up phase of
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118 the process at a small industrial plant in Palmas (Brazil), with focus on production yield; and, (ii)

119 the ethanolysis of sunflower oil using sweet potato bioethanol with different grades (98, 99 and
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120 99.4 GL), with focus on biodiesel yield and purity .

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121 2. Materials and methods

122 2.1 Production of Sweet Potato Ethanol

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123 Sweet potato (Cultivar Duda) was harvested in the city of Edia - Gois, and transported for 850
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124 km to the small scale bioethanol production plant (3 000 L/day of capacity) of the LASPER/ UFT,
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125 located in the city of Palmas (Brazil), used in the present study. The process occurred as follows.

126 The total amount of processed sweet potato was 4.2 t; 300 kg of washed and fragmented

127 biomass was used per batch (approximate size 4 mm, using a hammer mill), being further diluted

128 at an 1:1 w/w ratio with water. For the enzymatic h198ydrolysis, a concentration of 700 mL/t(Sweet

129 potato) of each enzyme (alpha-amylase and glucoamylase, from Novozymes) was used. In the

130 fermentation stage, 3.3 kg(Yeast)/t(Sweet potato) of a commercial yeast (Saccharomyces cerevisiae) of

131 the Fleischmann brand was used. The operational conditions were selected in agreement with

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132 previous optimization studies by Silveira et al. [10], using the same raw material.

133 To pH of the hydrolysate was maintained by neutralizing with an 1 M hydrochloric acid from

134 MERCK. The alcohol content was determined by densitometry.

135 The experiments were conducted during a period of 19 days. Five sets of experiments were

136 performed and each lasted approximately two days and were made in triplicate or duplicate.

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137 Variations were always less than 5%.

138 Table 1 summarizes the operational conditions for bioethanol and biodiesel production. Detailed

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139 information is presented in the following sections.

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140 Table 1

141 Operational conditions of bioethanol and biodiesel production

Variables
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Bioethanol production Biodiesel
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Production
Enzymatic Hydrolysys Fermentation Transesterification
Step 1 Step 2
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Temperature (C) 90 60 45

Time (h) 1.5 1 20 1

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Enzyme Type Alpha-amylase Glucoamylase

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Enzyme Concentration 700 700

(mL/tsweet potato)
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Yeast Type Saccharomyces

cerevisiae
Yeast Concentration 3.3
(kg/tsweet potato)
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Catalyst Type NaOH

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Catalyst concentration 1
(wt.%, relative to oil mass)
Ethanol:oil Molar ratio 6

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143 2.1.1. Enzymatic Hydrolysis Stage

144 The diluted biomass was added to the hydrolisis bioreactor. First, the temperature was set at 90 C

145 and 700 mL/t(Sweet potato) of alpha-amylase were added and hydrolysis occurred for 90 minutes under

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146 constant mechanical stirring. The reactor was then naturally cooled to 60 C and the pH of the

147 medium was adjusted to 4.0 - 4.5 by addition of the required volume of 1M HCl solution. Then, the

148 enzyme glucoamylase was added (700 mL/t(Sweet potato)) to promote the saccharification process

149 which occurred at 60 C during 60 minutes under co nstant mechanical stirring.

150 2.1.2. Fermentation Stage

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151 The pulp resulting from the enzymatic stage was added to the fermentation reactor and naturally

152 cooled down to 30 C. Based on the sugar content, w ater was added to ensure an 13 Bx, value

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153 considered more favorable to the fermentation process [10]. The commercial yeast

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154 (Saccharomyces cerevisiae, 3.3 kg(Yeast)/t(Sweet potato)) was then added and the process occurred

155 during 20 h.

156 2.1.3. Distillation Stage

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157 The product resulting from the fermentation stage was finally conveyed to the distillation tower for

158 ethanol recovery. Throughout the process, the volume of recovered ethanol was monitored and the
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159 grade was measured by densitometry using a Gay Lussac alcoholometer (brand INCOTERM,

160 readings in the range of 0 100 GL) in agreement with ABNT, NBR-5992 [37]. The distillate
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161 presented an average grade of 90 GL, being further purified to obtain higher grades (section
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162 2.1.4).The yield of the final product (LEthanol / tsweet potat)) was determined.
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163 2.1.4. Ethanol Upgrade

164 To obtain bioethanol of higher purity, respectively 98, 99 and 99.4 GL, laboratory distillation in
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165 a rotary evaporator (Heidolph laboratory) was performed, at 78 C, 600 mBar, 30 rpm, during 1 h
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166 and; if needed, calcium oxide (Quimirraia, lot 3/2016). The concentration of 0.4 g CaO/mLethanol,

167 allowed to reach the maximum ethanol grade (99.4 GL). Anhydrous ethanol, by Panreac, was also

168 used for comparison.

169

170 The complete process described above is shown in Figure 1.

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171

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172 Fig. 1. Process flow diagram of bioethanol production and purification.
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173
174 2.2. Ethanolysis of Sunflower Oil
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175 2.2.1 Raw Materials

176 Commercial sunflower oil, of Fula brand was used as raw material; the homogeneous catalyst
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177 applied in the transesterification reaction was sodium hydroxide (Powder, 98 wt.%, Sigma-Aldrich).
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178 2.2.2. Biodiesel Production

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179 In each experiment, 50 g of oil were used. Transesterification was performed under the following

180 standard conditions: Ethanol:oil molar ratio of 6:1; 1 wt.% of NaOH (relative to oil mass), 45 C and
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181 1 hour of reaction time. The experiments were performed aiming to evaluate the influence of the
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182 ethanol purity towards biodiesel syhthesis through ethylic route. In agreement, for each type of

183 alcohol (98, 99, 99.4 GL and anhydrous) at least two experiments were performed and results

184 were only considered if variations were less than 5 wt.%. Taking into account that only one

185 variable was studied, and that the ethanol purities to study were established, no experimental

186 design tools were used.

187 The reaction was performed in a glass reactor (three-necked batch reactor) which was

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188 immersed in a temperature controlled water bath, equipped with a water-cooled condenser, both

189 under atmospheric pressure. Mixture was made by magnetic stirring (stirring plate regulated to 600

190 rpm). Biodiesel and glycerol phases were separated by gravitational settling and, following, the

191 excess ethanol was removed from both phases in a rotary evaporator at reduced pressure. The

192 conditions of transesterification and purification by water washing and drying were previously

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193 described in detailed studies including optimization, using the same raw material [29, 38]. The

194 biodiesel production yield was calculated by considering the mass of the final product obtained in

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195 each test, after purification, divided by the mass of oil used, and expressed as a percentage.

196 The biodiesel production process is depicted in Figure 2.

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197
198 Fig. 2. Process flow diagram of biodiesel production.
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199
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200 2.2.3. Biodiesel key parameters

201 Three parameters were measured to assess biodiesel quality: acid value, viscosity and ethyl ester

202 content. EN14214 comprises several other parameters; the ones selected were considered to be

203 key parameters taking into account the raw material and studied process to evaluate viability [28,

204 29, 38].

205 The biodiesel acid value was determined by volumetric titration using KOH according to EN14104

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206 and the kinematic viscosity at 40 C was determined using capillary viscometers immersed in a

207 water bath according to ISO 3104.

208 The purity of the biodiesel, expressed as the percentage of ethyl esters in the final product, was

209 determined by gas chromatography according to EN 14103 using as the internal standard ethyl

210 pentadecanoate instead of methyl heptadecanoate. Methodology was previously described [29].

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211 3. Results and Discussion

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212

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213 3.1 Production of sweet potato ethanol

214 Figure 3 presents the bioethanol yields obtained in the 5 sets of experiments carried out at the

215
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startup of the pilot scale plant. The average yield was 161.4 L/t with a minimum of 149.2 L/t and a
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216 maximum of 184.0 L/t being observed. The mean value obtained was slightly higher than those

217 reported in two studies [7, 10], as well as lower by up to 15 % in two other studies [34, 36]. Two
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218 studies presented similar conditions than the present, with better results being found only in one
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219 study at a laboratory scale [10, 36]. The maximum value of the literature [34] relates with the use of
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220 cheese whey instead of water. In agreement, the results of the present study were considered

221 satisfactory, taking in to account that relate to the startup of the pilot plant, opening up a range of
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222 optimization opportunities for the industrial process.

223 The yields presented in Figure 4, in L/ha, refer to the sweet potato cultivation area in the study
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224 and were obtained based on the field productivity of the sweet potato (Duda cultivar), which is 65.5
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225 t/ha [10]. Thus, the average value obtained for the bioethanol produced in this work was 10 598

226 L/ha, with the minimum of 9 772 L/ha and the maximum of 12 052 L/ha being registered.

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228

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229 Fig. 3. Yield of bioethanol from sweet potato (L / t) at the start of the pilot scale plant of Palmas (Brasil).
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230
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231
232 Fig. 4. Yield (L/ha) of bioethanol of sweet potato and comparison with reference values: sweet potato [7, 9,

233 10], Corn [14, 15], Sugar Cane [11-13], Sweet Sorghum [39, 40] and Sugar Beet [41, 42].

234

235 The differences in ethanol yield, although expressive, do not reflect process efficiency variation

236 during the different batches. They reflect the natural moisture loss of the raw material throughout

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237 the experimental period because the same amount of as received material was used in each

238 experiment. In fact, the total moisture loss was found to be around 15%, which agrees with the

239 variations in bioethanol yield. Such results were also observed in other studies [10].

240 The mean yield results obtained are about 46 % higher than those obtained with sugarcane, 34 %

241 higher than those obtained with sugarbeet and about 149 % higher than those obtained with corn.

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242 They are only about 22 % lower than that obtained for sweet sorghum, but in that study [39]

243 bagasse of sorghum was also used which allowed a significant increase in ethanol yield. Taking

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244 into account the sweet potato productivities and the experimental yields obtained, such crops

245 seem to be in fact promising to produce bioethanol at the studied scale.

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246 In addition, because for bioethanol production not all the plant was used (ex. branches) and the

247 overall process leads to wastewaters, the ethanol yield could be improved by using the cellulose

248
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and even combined with other bioenergy production schemes (eg. biogas production) using
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249 wastewater and residues from the production, adding value to the overall process [43].

250
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251 3.2 Biodiesel Synthesis by Ethylic Route

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252 Table 2 shows the results regarding biodiesel yield and quality after its production from sunflower
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253 oil using ethanol of different grades.

254
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255 Table 2

256 Quality parameters of biodiesel obtained from ethanolysis of sunflower oil with sweet potato
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257 bioethanol of different degrees of purity and with absolute commercial ethanol.
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Parameters BD-98a BD-99a BD-99.4a BD-P.Ab EN 14214c

Yield (wt.%) 63.23 1.38 70.52 0.51 73.03 0.62 83.34 0.53 NA
Purity (wt.%) 50.31 2.33 60.11 0.50 75.11 1.82 94.05 0.10 > 96.5c
Viscosity (mm2 s-1) 13.70 0.25 9.75 0.49 4.64 0.08 4.40 0.22 3.50 5.00
Acid value (mg KOH g-1) 0.61 0.02 0.57 0.04 0.56 0.03 0.31 0.01 < 0.50

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258 Biodiesel produced with sweet potato ethanol of different grades (98 99.4 GL).

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b
259 Absolute commercial ethanol.

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260 Established for methyl esters.

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262 With 98 GL sweet potato ethanol, the yield of biod iesel was 63.23 1.38 wt.%, the lowest value

263 obtained, while for 99.4 GL the yield obtained was 73.03 0.62 wt.%, being the highest with such

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264 ethanol type. Using absolute commercial ethanol, the yield reached 83.34 0.53 wt.%, 4 % higher

265 than that obtained by Santana et al. [44], which was 80 wt.%. In such study [44], an yield of 90

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266 wt.% for biodiesel production thourgh a methylic route was obtained, 7.4 % higher than that

267 observed in the present study.

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268 Viscosity is a property used to evaluate the evolution of the transesterification reaction,

269 decreasing as it proceeds, as the triglycerides have higher viscosity than the resulting ethyl esters.

270
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The results show high viscosity of the biodiesel obtained when using sweet potato ethanol with
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271 purity 99 GL, outside the requirements of the European m ethyl biodiesel standard, which might

272 indicate less product conversion, expressed by the purity results.

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273 In fact, purity also increased with the use of higher purity ethanol, from about 50 wt.% for 98
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274 GL bioethanol to 94 wt.% for absolute ethanol. A p urity greater than 75 wt.% corresponds to
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275 biodiesel with a viscosity that meets the requirements of the European standard. For the higher

276 quality biodiesel obtained, the viscosities agree with the values of the literature, with differences of
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277 no more than 10 % [29, 45].

278 The acid value of the product only agreed with standard EN14214 for methylic biodiesel
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279 obtained using absolute ethanol being in agreement with the results found in the literature [29, 45].
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280 It can be seen that the acid value also decreased with increasing purity of the alcohol used in the

281 experiments. Such fact might be due to difficulties during product purification, which means that

282 using a lower grade ethanol requires a greater amount of washing steps to ensure separation of

283 the product and removal of the catalyst, which may lead to the ester hydrolysis causing the release

284 of fatty acids and the acid value increase.

285 In Table 3, the purity of the best biodiesel obtained in the present work can be compared with

286 the literature results.

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287 The values of the present study are close to the minimum established by the European

288 standard for methylic biodiesel and to the best results reported in the literature.

289 Figure 5 summarizes the results of yield and purity obtained in the study, clearly showing the

290 increase of both parameters with ethanol grade.

291

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292 Table 3

293 Purity of biodiesel obtained in the present study and others reported in the literature.

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Reference Alcohol Purity biodiesel (wt.%)

EN 14214a; [37]; [39] Methanol > 96.5; 97.3; 99.5

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Present study; [29]; [33]; [32] Ethanolb 94.05 0.10; 98.7; 90.0; 83.0

294

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a
295 European standard for biodiesel of methyl esters.
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b
296 Absolute commercial.

297
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100 100
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90 Yield Purity 90
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Purity (wt.%)
Yield (wt.%)

80 80
70 70
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60 60
50 50
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40 40
BD-98 BD-99 BD-99.4 P.A
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Grade Ethanol
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299 Fig. 5. Production yield and purity of ethyl biodiesel obtained from sunflower oil using sweet potato

300 bioethanol with different degrees of purity and also absolute ethanol (BD-98, BD-99, BD-99.4 e P. A.).

301 The presence of water in the ethanolic reaction mixture significantly influenced the conversion of

302 the product, as previously reported [31]. A higher amount of water in the mixture leads to the

303 formation of stable emulsions during the reaction, which can cause difficulties in separating the

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304 phases of ethanol and glycerol [30], also influencing the step of catalyst removal with water. In the

305 present study, it was shown that even a small amount of water in the sweet potato bioethanol of

306 99.4 GL purity was sufficient to reduce the yield by about 10 % and the purity by 19 %, compared

307 to results obtained using absolute ethanol.

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308 4. Conclusion

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309 Bioethanol production at the LASPER / UFT pilot scale plant in Palmas, Tocantins / Brazil, was

310 considered to be sactisfactory. An yield of 161.4 L/t in average was obtained, with minor

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311 differences to that obtained at a laboratory scale, under the same conditions and with margin for

312 progression taking into account additional reported studies. The yield of bioethanol production per

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313 unit area of cultivation, taking into account the average yield of sweet potato crop of the Duda
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314 cultivar, was 10 598 L/ha, approximately 46 % higher than that obtained from sugarcane and 149

315 % higher than that resulting from corn production, showing the high relevance of its use and
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316 application at the studied scale.

317 The bioethanol obtained from the pilot plant was not suitable for the production of ethylic
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318 biodiesel due to the low grade, of 90 GL. Biodiese l yield and purity increased proportionally with
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319 ethanol grade. The biodiesel obtained from ethanolysis using 99.4 GL sweet potato bioethanol

320 allowed to obtain a product yield of 73 wt.% and a purity of 75 wt.%. Such result was still very low
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321 compared to that required by the European standard for methylic biodiesel (> 96.5 wt.%) and to

322 what was obtained using commercial absolute ethanol, which enables the production of biodiesel
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323 with quality close to that specified by the mentioned standard (83 wt.% of yield and 94 wt.%. of
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324 purity).

325 Accordingly, the production of absolute ethanol is essential for subsequent use of this more

326 sustainable raw material for ethylic biodiesel production.

327

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328 Limitations and Future Directions of Present Work

329 The following limitations were found by performing the present study:

330 Difficulties in controlling / maintaining uniform moisture content of the raw material

331 (sweet potato);

332 Difficults in achieving high bioethanol grade at the small industrial plant;

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333 Difficulties in biodiesel production process with ethanol of low grade.

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334 The following future directions are indicated:

335 Evaluation of different potato cultivars as well as other starchy crops using the small

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336 scale industrial process;

337 Integration of other biofuels (biogas) in the process by taking advantage of residual

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338 streams;
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339 Evaluation of the dry by-product for animal feed;

340 Evaluation of the use of waste oils for biodiesel production throught ethylic route;
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341

342 Aknowledgments
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343 This work was supported by the UED / EQU / 00511/2013 Project - LEPABE (Laboratory of
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344 Process, Environment, Biotechnology and Energy Engineering - EQU / 00511) by ERDF funds

345 through the Competitiveness and Internationalization Operational Program - COMPETE 2020 and
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346 national funding Of FCT - Foundation for Science and Technology. Joab Silva thanks IBRASIL

347
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Project - Erasmus Mundus Program (ibrasil@univ-lille3.fr), for the PhD scholarship (IB - 14DF /

348 0138). Joana Dias thanks FCT for the scholarship SFRH/BPD/112485/2015.
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349

350

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