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Titanium Dioxide As a Catalyst in Biodiesel Production

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Titanium Dioxide As a Catalyst in Biodiesel Production catalysts Review Titanium Dioxide as a Catalyst in Biodiesel Production Claudia Carlucci *, Leonardo Degennaro and Renzo Luisi Flow Chemistry and Microreactor Technology FLAME-Lab, Department of Pharmacy–Drug Sciences, University of Bari “A. Moro” Via E. Orabona 4, 70125 Bari, Italy; [email protected] (L.D.); [email protected] (R.L.) * Correspondence: [email protected]; Tel.: +39-080-544-2251 Received: 30 November 2018; Accepted: 20 December 2018; Published: 11 January 2019 Abstract: The discovery of alternative fuels that can replace conventional fuels has become the goal of many scientific researches. Biodiesel is produced from vegetable oils through a transesterification reaction that converts triglycerides into fatty acid methyl esters (FAME), with the use of a low molecular weight alcohol, in different reaction conditions and with different types of catalysts. Titanium dioxide has shown a high potential as heterogeneous catalyst due to high surface area, strong metal support interaction, chemical stability, and acid–base property. This review focused on TiO2 as heterogeneous catalyst and its potential applications in the continuous flow production of biodiesel. Furthermore, the use of micro reactors, able to make possible chemical transformations not feasible with traditional techniques, will enable a reduction of production costs and a greater environmental protection. Keywords: titanium dioxide; heterogeneous catalyst; biodiesel; continuous flow 1. Introduction Public attention to energy consumption and related emissions of pollutants is growing. The constant increase in the cost of raw materials derived from petroleum and the growing concerns of environmental impact have given considerable impetus to new products research from renewable raw materials and to technological proposal solutions that reduce energy consumption, use of hazardous substances and waste production, while promoting a model of sustainable development and social acceptance [1–3]. In recent years, titanium complex catalytic systems consisting of several catalysts or containing one catalyst with functional additives have found wide applications [4–6]. This application is very promising, since it appreciably widens the possibility of controlling the activity and selectivity of catalysts. Titanium containing catalysts can be divided into organic, inorganic, mixed, and complex catalysts. Both organic and inorganic titanium compounds represent the main components of the complex catalysts for esterification and transesterification reactions [7]. Recently, titanium oxide (TiO2) was introduced as an alternative material for heterogeneous catalysis due to the effect of its high surface area stabilizing the catalysts in its mesoporous structure [8]. Titania-based metal catalysts have attracted interest due to TiO2 nanoparticles high activity for various reduction and oxidation reactions at low pressures and temperatures. Furthermore, TiO2 was found to be a good metal oxide catalyst due to the strong metal support interaction, chemical stability, and acid–base property [9]. Catalysts 2019, 9, 75; doi:10.3390/catal9010075 www.mdpi.com/journal/catalysts Catalysts 2019, 9, 75 2 of 25 Catalysts 2019, 9, x FOR PEER REVIEW 2 of 28 2 This review focuses on TiO2 as an excellent material for heterogeneousheterogeneous catalysis, with potential applications in biodiesel production. Applications of titanium dioxide as he heterogeneousterogeneous catalyst for continuous flowflow processes havehave beenbeen considered.considered. 2. Titania-Based Catalysts in TransesterificationTransesterification ReactionReaction Homogeneous basedcatalystsbasedcatalysts in in the the transesterification transesterification reaction reaction have somehave disadvantages,some disadvantages, among whichamong are which high are energy high consumption,energy consumption, expensive expensive separation separation of the catalyst of the fromcatalyst the from reaction the mixture,reaction andmixture, the purificationand the purification of the raw of material.the raw material. Therefore, Therefore, to reduce to the redu costce ofthe the cost purification of the purification process, heterogeneousprocess, heterogeneous solid catalysts solid suchcatalysts as metal such oxidesas metal were oxides recently were used, recently as they used, can as be they easily can separated be easily fromseparated the reaction from the mixture reaction and mixture reused. and reused. Titanium dioxide used as a heterogeneousheterogeneous catalystcatalyst shows a wide availabilityavailability and economical synthesis modalities. 2.1. Sulfated TiO 2 A solid superacidic catalyst used in the petrochemical industry and petroleum refining refining process was sulfatedsulfated doped doped TiO TiO2 [102 [10,11].,11]. This This catalyst catalyst showed showed better better performances performances compared compared to other to sulfated other metalsulfated oxides metal due oxides to the due acid to strengththe acid ofstrength the TiO of2 particles the TiO2 which particles further which enhanced further withenhanced loading with of 2− SOloading4 groups of SO4 on2− groups the surface on the of surface TiO2. The of TiO higher2. The content higher of content sulfate groupsof sulfate determined groups determined the formation the offormation Brönsted of acid Brönsted sites which acid sites caused which the supercaused acidity the super of the acidity catalyst of [ 12the]. Somecatalyst studies [12]. Some reported studies that thereported enhancement that the ofenhancement the acidic properties of the acidic after theproperti additiones after of sulfate the addition ions to metalof sulfate oxides, ions caused to metal less deactivationoxides, caused of less the catalystdeactivation [13,14 of]. the catalyst [13,14]. 2− 2.1.1. SO 42−/TiO/TiO2 2 Hassanpour et al. described sulfated doped TiO 2 asas a solid super-acidic catalyst which is also used in the petrochemical industry and petroleum refiningrefining process and shows better performances compared to other sulfated metal oxides [[15,16].15,16]. This is due to the acid strength of the TiO22 particles 2− which further enhanced enhanced with with loading loading of of SO SO42−4 groupsgroups on the on surface the surface of TiO of2. TiO The2. synthesized The synthesized nano- nano-catalystcatalyst Ti(SO Ti(SO4)O (Figure4)O (Figure 1) is 1used) is used for the for production the production of biodiesel of biodiesel deriving deriving from from used used cooking cooking oil oil(UCO). (UCO). Figure 1. TEM images of (a) TiO2 and (b) Ti(SO4)O (Copyright of Elsevier, see [15]). Figure 1. TEM images of (a) TiO2 and (b) Ti(SO4)O (Copyright of Elsevier, see [15]). The esterificationesterification of free fatty acids (FFAs) andand transesterificationtransesterification of oils were conducted simultaneously using the titanium catalyst (1.5(1.5 wt.%),wt.%), inin methanol/UCOmethanol/UCO in in 9:1 ratio, a temperature reaction of of 75 75 °C,◦ C,and and a reaction a reaction time of time 3 h, of yiel 3ding h, yielding97.1% of fatty 97.1% acid of methyl fatty acid esters. methyl The authors esters. Theinvestigated authors investigatedthe catalytic the activity catalytic activityand re-usability and re-usability of the of theTi(SO Ti(SO4)O4 )Ofor for the esterification/transesterificationesterification/transesterification ofof UCO.UCO. AfterAfter eighteight cycles cycles under under optimized optimized conditions conditions the the amount amount of 2− 2− SOof 4SO4species species in thein the solid solid acid nano-catalystacid nano-catalyst slowly slowly decreased decreased and this and data this resulted data higherresulted compared higher tocompared other functionalized to other functionalized titania reported titania in thereported literature. in the The literature. formation The of polydentate formation of sulfate polydentate species insidesulfate thespecies structure inside of TiOthe2 enhancedstructure theof TiO stability2 enhanced of synthesized the stability Ti(SO 4of)O synthesized nanocatalyst Ti(SO and also4)O nanocatalyst and also presented a higher tolerance to ≤6 wt.% percentage of free fatty acids in raw material for biodiesel production (Table 1). Catalysts 2019, 9, 75 3 of 25 presented a higher tolerance to ≤6 wt.% percentage of free fatty acids in raw material for biodiesel Catalysts 2019, 9, x FOR PEER REVIEW 3 of 28 production (Table1). Table 1. The effect of free fatty acid (FFA) in feedstock on the percentage of fatty acid methyl esters Table 1. The effect of free fatty acid (FFA) in feedstock on the percentage of fatty acid methyl esters (FAME) yield. (FAME) yield. Oleic acid to oil, wt.% 0.5 1 2 3 4 5 5.5 6 6.5 7 Oleic acid to oil, wt.% 0.5 1 2 3 4 5 5.5 6 6.5 7 FAMEFAME yield% yield% 97.197.1 9797 97.1 97.1 97.01 97.01 96.14 96.14 95.69 95.69 93.42 93.42 91.37 91.37 75.39 75.39 64.5 64.5 Zhao and co-workers have recently studied the catalytic activity of sulfated titanium oxide 2− (TiO2-SO-SO442−). ).The The authors authors reported reported that that the the high high surfac surfacee acidity acidity of of titanium titanium dioxide dioxide increased the yield ofof butylbutyl acetate acetate to to about about 92.2% 92.2% in esterificationin esterification reaction, reaction, and theand selectivity the selectivity of the of catalyst the catalyst mostly mostlydepended depended on the degreeon the of degree exposure of exposure of reactive of crystal reactive facets crystal [17]. facets In this [17]. paper, In athis high-surface-area paper, a high- surface-areamesoporous
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