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Oil Recovery from Palm Kernel Meal Using Subcritical Water Extraction in a Stirred Tank Reactor

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Oil Recovery from Palm Kernel Meal Using Subcritical Water Extraction in a Stirred Tank Reactor processes Article Oil Recovery from Palm Kernel Meal Using Subcritical Water Extraction in a Stirred Tank Reactor Johnnys Bustillo Maury 1,* , Andrés Aldana Rico 1,*, Cindy García Pinto 1, Ingrid Hernández Medina 2, Juan Urueta Urueta 3, Jerry W. King 4 and Antonio Bula Silvera 1 1 Departamento de Ingeniería Mecánica, Universidad del Norte, Km 5 vía Puerto Colombia, Barranquilla C.P. 080001, Colombia; [email protected] (C.G.P.); [email protected] (A.B.S.) 2 Departamento de Ingeniería Industrial, Universidad del Norte, Km 5 vía Puerto Colombia, Barranquilla C.P. 080001, Colombia; [email protected] 3 Departamento de Innovación, Aceites S.A., Santa Marta C.P. 470001, Colombia; [email protected] 4 Critical Fluid Symposia, Fayetteville, AR 72071, USA; [email protected] * Correspondence: [email protected] (J.B.M.); [email protected] (A.A.R.) Received: 13 August 2019; Accepted: 16 October 2019; Published: 2 November 2019 Abstract: Palm kernel meal (PKM) is one of the main byproducts of the oil palm industry. PKM can be obtained as the result of solvent or mechanical extraction of palm kernel oil; in both cases, meal has a remaining oil content that could be recovered. In this work, PKM coming from a mechanical pressing extraction system with an initial oil content between 7 to 8% (wt.) was treated with subcritical water in a batch stirred reactor. To find the proper operational conditions, a three-step experimental process was performed. Extraction temperature, reaction time, particle size and alkaline catalyst usage were selected as process factors. After subcritical extraction, the system was cooled down and depressurized; then oil phase was separated by centrifugation. After extraction, meal was oven-dried at 80 ◦C. A maximum recovery of 0.034 kg-oil/kg-meal was obtained at 423 K, 720 s and particles smaller than 0.001 m. The experimental procedure showed consistent extraction yields of 40% without modifying the quality of the obtained oil. Keywords: palm kernel meal; subcritical water extraction; oil recovery; clean separation 1. Introduction In recent years, interest in improving sustainability of agricultural material processing has been increasing. In addition, environmental phenomena have become significantly unstable, directly impacting agricultural business competitiveness. Palm kernel oil processing hasn’t been sheltered from that reality, so trying to improve oil recovery has become a necessity for this sector. Palm kernel meal (PKM) is a by-product in the palm kernel oil (PKO) production process. PKM is used as a basis for the manufacture of animal feed [1]. Palm kernel oil represents between 46% and 53% of the weight of the kernel [2]. Its chemical composition is different from crude palm oil and it is semi-solid at room temperature [3]. Worldwide, Colombia it is ranked as the fifth-largest palm kernel meal producer; its 148,000 MT in 2016 placed Colombia as the first American maker of this feedstock. The commercial value of this material it is rated at approximately 46.7USD/ton, which is lower than other competitors, such as rice bran or soybean meal. However, pressed palm kernel meal still has an oil content between 7 to 8% wt, this vegetable oil has a market value around 617.15USD/ton. One option that could become a valid sustainable alternative is subcritical water processing [4]. Subcritical water refers to a region where fluid temperature varies between 373 K and 547 K in a liquid state. At those conditions some properties, like polar moment shift, make water more similar Processes 2019, 7, 797; doi:10.3390/pr7110797 www.mdpi.com/journal/processes Processes 2019, 7, 797 2 of 11 to conventional organic solvents, making it suitable for lipid extraction and hydrolysis [5], creating a sustainable method to decrease hazardous organic solvent consumption. The thermodynamic properties of water are based on the strength and structure of their hydrogen bonds [6]; which are governed by the relations between water atoms [7]. Therefore, a minimum change in one of the bonds affects the entire volume of water. Particularly at the subcritical region, changes in the resistance of these bonds are reflected in the dielectric constant and heat of vaporization change [6]. At lower temperature, the hydrogen bonds are stronger implying a high dielectric constant. The opposite occurs at high temperatures, since the dielectric constant is decreased [8,9], leading to an increase in the solubility of a normally hydrophobic compound [6]. Oil recovery from previously pressed fibers using subcritical water, using different catalysts, has been investigated in pervious studies [10,11]. Also, the complementary use with different solvents was evaluated in [12]. Studies on palm empty fruit bunch liquefaction using alkaline catalysts have also been conducted [13,14]. Subcritical water has also been used for phenolic compound extraction from several oil palm byproducts [15], carotenoids [16], and carbohydrates, such as sugars [17] and cellulose [18] from palm fibers and leaves. This study presents the findings from tests of an experimental batch extraction process of oil from palm kernel meal using subcritical water under different experimental conditions. 2. Materials and Methods 2.1. Raw Material Mechanically pressed palm kernel meal was collected from PALMACEITE S.A. (Aracataca, Magdalena, Colombia) in 5 kg plastic bags that were stored at approximately 23 ◦C to prevent lipidic photo-oxidation. Potassium hydroxide (85% of purity) was provided by Riedel de Haen (Wunstorfer Str. 40, 30926 Seelze, Germany). High performance liquid chromatograph (HPLC) grade hexane was supplied by EMD Millipore corporation (Billerica, MA, USA). Ultra high purity argon gas was used as inert gas for reactor headspace during the extractions and Ultra high purity helium, hydrogen, air and nitrogen, all supplied by The Linde Group (Klosterhofstrasse 1, Munich, Germany) were used as carrier and detection gases during the chromatographic analysis. Distilled water from the experimental laboratory was used during the experiments. 2.2. Meal Preparation Palm kernel meal was separated in 5 fractions using number 8, 20, 40 and 60 standard American Society for Testing and Materials (ASTM) sieves and a shaker all provided from Pinzuar Ltd.a. (Carrera 108 No. 18-31, Bogota, Colombia). The sieving process produced 2.38 10 3 m, 0.84 10 3 m, × − × − 0.42 10 3 m, 0.25 10 3 m and a fine size particle fractions that were labeled and stored separately × − × − for further processing. 2.3. Subcritical Water Extraction Subcritical water extraction was performed in a 2.5 10 4 m3 stirred tank batch reactor Model × − 3230 (Figure1) supplied by AMAR Equipments Pvt. Ltd. (6, Parmar Industrial Estate, Kale Marg, Bail Bazaar, Kurla (West) Mumbai–400 070, India). Palm kernel meal, catalyst, and water mixture were added. Argon gas was introduced to replace the air on the reactor headspace and establish a 6 105 Pa base pressure. Reaction temperature and agitation were established using a NEURO100 PPI × Controller (Process Precision Instruments, 101 Diamond Industrial Estate, Navghar, Vasai Road (E), Dist. Palghar—101210, Maharashtra, India) and a frequency inverter (Schneider Electric Co., 43-45, bd Franklin Roosevelt 92500 Rueil Malmaison, France) respectively. Pressure was elevated from base level to operational condition by temperature action, and was monitored also using a NEURO100 PPI Controller. After the determined reaction time passed, temperature was decreased using the water cooling system of the vessel. After the system was cooled, vessel was depressurized, and the mixture Processes 2019, 7, 797 3 of 11 wasProcesses poured 2019, 7 in, x FOR 15 PEER10 6 REVIEWm3 centrifuge tubes. Later, the tubes with the samples were centrifuged3 of at11 × − 1262 g for 1200 s in a Thermo Scientific CL-22 bench centrifuge (168 Third Avenue, Waltham, MA, USA Waltham,× MA, USA 02451). After centrifugation, oil layer was extracted by pipetting and separated 02451). After centrifugation, oil layer was extracted by pipetting and separated for further analysis. for further analysis. Figure 1. StirredStirred tank batch reactor. 2.4. Soxhlet Soxhlet Extraction 6 3 Between 0.005 and 0.01 kg ofof palmpalm kernelkernel mealmeal werewere mixedmixed withwith 150150 × 1010−−6 m3 of hexane for × standard Soxhlet extraction at 343 K for 6h inin orderorder toto determinedetermine totaltotal oiloil contentcontent ofof thethe material.material. 2.5. Gas Chromatography Gas Chromatography with Thermal Conductivity Detector (GC-TCD) was performed with a Hewlett-Packard 58905890 series series II, II, a TCDa TCD detector detector (135 (135 mL/min mL/min He), usingHe), ausing DB-23 a AgilentDB-23 TechAgilent capillary Tech capillarycolumn with column a 0.25 with mm a internal0.25 mm diameter, internal 60diameter, m length 60 and m length 0.25 µ mand film 0.25 thickness. μm film Thethickness. Fatty acids The Fattycomposition acids composition was performed was by performed oil conversion by oil to conver fatty acidssion methylto fatty esters,acids methyl according esters, to Cocks according and Van to CocksRede [ 19and]. AboutVan Rede 50mg [19]. of oilAbout and 50mg mixed of with oil and 950 µmixedm of n-hexane,with 950 μ thenm of was n-hexane, added 50thenµm was of CH3NaO,added 50 μandm of the CH3NaO, mixture was and stirred the mixture in a vortex was mixerstirred and in a let vort it restex mixer for 60 minand afterlet it 1rest uL for collected 60 min supernatant after 1 uL wascollected injected supernatant in the GC was for injected 40 min andin the 30 GC◦C. for The 40 Standards min and used30 °C. (fatty The Standards acids oleic, used myristic, (fatty lauric, acids oleic,linoleic, myristic, linolenic, lauric, palmitic, linoleic, palmitoleic, linolenic, arachidic, palmitic, caprylic,palmitoleic, caproic, arachidic, capric caprylic, and stearic) caproic, were ancapric analytic and stearic)grade (Sigma-Aldrich were an analytic Inc., grade St. Louis, (Sigma-Aldrich MO, USA).
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