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Committee of the Global Engineers & Technologists Review Chief Editor Ahmad Mujahid Ahmad Zaidi, MALAYSIA Managing Editor Mohd Zulkifli Ibrahim, MALAYSIA Editorial Board Dr. Arsen Adamyan Yerevan State University ARMENIA

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ŠPUBLISHED 2012

Global Engineers and Technologists Review GETview ISSN: 2231-9700 (ONLINE) Volume 2 Number 12 December 2012 All rights reserved. No part of this publication may be reproduced, stored in a retrieval system, or transmitted, electronic, mechanical photocopying, recording or otherwise, without the prior permission of the Publisher.

Printed and Published in Malaysia


CONTENTS Vol.2, No.12, 2012 1.

A STUDY OF THE CORROSION INHIBITOR OF MILD STEEL IN SULPHURIC ACID USING MUSA SAPIENTUM PEELS EXTRACT SALAMI, L., WEWE, T.O.Y., AKINYEMI, O.P. and PATINVOH, R.J.

7.

HEXANE ECONOMIZATION IN PALM KERNEL OIL PLANT: A STUDY AFTER PROCESS DESIGN IMPROVEMENT SIVARAO, KUMAR, N., WIDODO, W.S. and HAERYIP SIHOMBING

© 2012 GETview Limited. All right reserved

ISSN 2231-9700 (online)


GLOBAL ENGINEERS & TECHNOLOGISTS REVIEW www.getview.org

A STUDY OF THE CORROSION INHIBITOR OF MILD STEEL IN SULPHURIC ACID USING MUSA SAPIENTUM PEELS EXTRACT SALAMI1, L., WEWE2, T.O.Y., AKINYEMI3, O.P. and PATINVOH4, R.J. 1, 2, 3, 4

Department of Chemical and Polymer Engineering Lagos State University Epe, Lagos, NIGERIA 1 salamilukumon@yahoo.com ABSTRACT

The use of local wastes which are organic in nature for the production of green corrosion inhibitor is no doubt the trend of the day. The aim of this study is to produce corrosion inhibitor from Musa Sapientum peels extract with a view of determining the effectiveness of the corrosion inhibitor. Musa Sapientum peels extract produced was used as a corrosion inhibitor on mild steel in concentrated tetraoxosulphate (vi) acid using weight loss method. The results of the study showed that as the concentration of the produced inhibitor increases, the rate of corrosion decreases. It also showed that as the concentration of the inhibitor increases, the inhibitor efficiency also increases up to a optimum of approximately 71 % for 0.8 g/l extract in 2.0M H2SO4 which is encouraging. It was concluded that Musa Sapientum peels extract can be used as corrosion inhibitor as this will reduced the importation cost, increase the gross domestic product (GDP) of the nation and make the environment free of toxic chemical inhibitor. The use of the peels extract as corrosion inhibitor was recommended for use in the process industries Keywords: Corrosion, Inhibitor, Musa Sapientum, Extract, Mild Steel.

1.0

INTRODUCTION

Musa Sapientum which is commonly called banana is a herbaceous plant known to have originated from the tropical region of southern Asia, belong to the family of Musaceae (Anhwange et al., 2009). It is cultivated throughout the tropic primarily for its fruits and to a very few extent for the production of fibre. Musa Sapientum typically grows up to a height of about 6 to 25 feet with large leaves of about 11 feet in length. It has a tuberous subterranean rhizome, from which leaves are folded within themselves (Erunoso, 2011). The stem is called pseudostem, produces a single bunch of banana before dying and replaced by new pseudostem. The fruit grows in clusters with about twenty fruits to a tier and having 3 to 20 tiers to a bunch. The fruit is a source of protein and is protected by its peel which is discarded as waste after the inner fleshy portion is eaten (Anhwange et al., 2009). The Musa Sapientum peels when discarded constitute solid waste which is a problem in African continent inclusive in Nigeria because of lack of solid waste management (Olafadehan and Salami, 2011). These peels are part of organic waste and organic waste is about 62 % of solid waste generated in Lagos, Nigeria (Adogame, 2009). The Musa Sapientum peels comprises nutritional and anti-nutritional contents. According to Anhwange et al., (2009) the peels contain potassium, calcium, sodium, iron, manganese, bromine, rubidium, strontium, zirconium and niobium of concentration 78.10, 19.20, 24.30, 0.61, 76.20, 0.04, 0.21, 0.03, 0.02 and 0.02 mg/g respectively. These peels in Nigeria constitute environment nuisance because Nigeria is not proactive in the management of her solid waste. These peels accumulate and form heap especial in non-engineered landfill sites. The contaminants from these peels percolate the subsoil and contaminate the groundwater. In order to avert this problem, this paper looked at how the extract from these peels can be used as corrosion inhibitors in the ambient temperature of Nigeria thereby creating wealth from wastes. Corrosion is the gradual destruction of materials usually metals, by chemical reaction with its environment which means electrochemical oxidation of metals in reaction with an oxidation such as oxygen. Corrosion occurs not only in metals but also in non metals like plastics and glass. A lot of money is lost every year due to corrosion. In United State, industries and government loss approximately 276 dollars annually or 3.1 percent of the GDP (Gerhardus et al., 2002). It was estimated that about 25 to 30 % of this total could be avoided if corrosion prevention technologies are put in place (Gerhardus et al., 2002). In Australia, Great Britain and Japan, the cost of corrosion is approximately 3 to 4 percent of the GDP (Kruger, 2000). Therefore, a way of preventing or avoiding corrosion is not only timely but also important. If corrosion is prevented, the money loss to corrosion can be channeled to other uses like creation of employment especially in developing countries like Nigeria where poverty level is above 70 %. There are several methods of corrosion control and prevention but this work looked at corrosion inhibitor as a way of preventing corrosion. Corrosion inhibitor is a chemical -

G.L.O.B.A.L E.N.G.I .N.E. E.R.S. .& . .T.E.C. H.N.O.L.O.G.I.S.T.S R.E.V.I.E. W

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compounds that when added to a liquid or a gas, decreases the corrosion rate of a material (Yuhazri et al., 2011a; Hubert, 2002). The performance of a corrosion inhibitor depends on quality of water, fluid composition and flow regime. The common mechanism for inhibiting corrosion involves formation of a coating, passivation which prevents access of the substance to the metal. Inhibitors are added to many systems such as cooling systems, chemical, oil and gas production unit, boilers and refinery unit to prevent corrosion. In most cases, the effective inhibitors used contain heteroatom such as oxygen, nitrogen, sulphur and multiple bonds in their structure through which they are adsorbed on the surface of the metal (Singh et al., 2012; Yuhazri et al., 2011b). It was observed by Singh et al., (2012) that adsorption depends solely on certain physiochemical properties of the inhibitor groups such as functional groups, electronic skeleton of the molecules and electron density at the donor atom. Many manufactured inhibitors have shown to have good anticorrosive ability but majority of them are toxic to human and environment. As a result of the adverse effects of synthetic inhibitors, plant extracts which are organic are now substituting the chemical inhibitors because they are environmental friendly, cheap, readily available and ecologically acceptable which make them to be green corrosion inhibitors. Naturally occurring substances have been used successfully as corrosion inhibitor and have been reported by some researchers (Eddy and Ebenso, 2008; Okafor et al., 2005, 2007; Okafor and Ebenso, 2007; Chetouani et al., 2004; Abiola et al., 2007; El-Etre, 2003, 2006; Umoren and Ebenso, 2008; Abdallah, 2004; Rajendran et al., 2005; Bouyanzer and Hammouti, 2004; Oguzie, 2005; Oguzie et al., 2006, 2007: Bendahou et al., 2005). Several works have been done on banana peels, for the production of biogas (Ilori et al., 2007), production of ethanol by fermentation and hydrolysis (Sirkar et al., 2008), biomass production (Essien et al., 2005) natural solid fuel for combustion (Yuhazri et al., 2012), antacid and diuretic activities of the ash and extracts of the peesl (Jain et al., 2007) and antibacterial and antioxidant activities (Mokbel and Hashinage, 2005). However, the aim and objective of this study is to produce corrosion inhibitor from local banana peel with a view of determining the effectiveness of the corrosion inhibitor produced on mild steel in concentrated tetraoxosulphate (vi) acid medium. The production of corrosion inhibitor from local waste will not only reduce the huge amount of money normally spend by the process industries on the importation of corrosion inhibitor but will also increase the GDP of the nation which justifies this work. This work in addition will make corrosion inhibitors that are non toxic and harmless to the environment to be available in the country which further justifies the study.

2.0

EXPERIMENTAL PROCEDURES 2.1 Materials Preparation Mild steel bar of composition Mn (0.6), P (0.36), C (0.15), Si (0.03) in wt. % and the rest Fe was used for the study. Five mild steel bars each of weight 35.50 grams were mechanically cut and washed with ethanol to remove any form of grease or oxide. The bars were then dried in acetone and preserved in a desicator to prevent a reaction with the environment or the formation of a passivation layer which might interfere with the results of the experiment. All reagents used in this study were analytical grade. 2.2 Musa Sapientum Extract Two kilograms of fresh samples of Musa Sapientum peels were collected from Ayetoro market in Epe area of Lagos State and were washed carefully with distill water to remove any form of dirt from the peels. The peels were dried under the sun and weighed at intervals until a constant weight of 1.20 kg was attained. This was to ensure complete removal of water from the peels. The dried Musa Sapientum peels were grounded using an industrial scale grinder to powdered form. The powdered Musa Sapientum peels was then run through wire mesh sifter to obtain very fine powdered samples and to separate the shaft of the peels. The fine powdered were completely soaked in ethanol solution for 96 hours after which the mixture was stirred properly in order to have homogenous solution and then filtered. The filtrate was subjected to evaporation process to remove the ethanol in the filtrate. The inhibitor was obtained in its pure form at the end of the evaporation process. The stock solution of the extract obtained were used in preparing different concentrations of the extract by dissolving 0.2, 0.4, 0.6 and 0.8 gram of the extract in one litre of 2.0 M H2S04 respectively. 2.3 Weight Loss Method One of the mild steel bars was inserted in 2.0M H2S04 without Musa Sapientum extract which was removed and weighted at 24 hours to determine loss of weight. It was inserted again and at 48 hours, it was removed and reweighed. This was done for 72 hours, 96 hours and 120 hours. It was ensured all inhibitor solution dropped from the bar before weighing. The same procedure was carried out for 0.2 g/l, 0.4 g/l, 0.6 g/l and 0.8 g/l of 2.0M H2S04. All experiments were performed at ambient temperature.

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RESULTS AND DISCUSSION

Table 1 shows the weight of mild steels bar in different concentration of Musa Sapientum extract in 2.0M H2S04 at different time interval. Table 2 which shows the weight loss of mild steel bar in different concentration of Musa Sapientum extract in 2.0M H2S04 at different time interval was generated using Table 1. Table 1: Weight of steel bar in different concentration of Musa Sapientum extract in 2.0M H2SO4 at different time interval. Concentration of Musa Sapientum extract 0.00 0.20 0.40 0.60 0.80

Weight of bar in grams at Initial 35.50 35.50 35.50 35.50 35.50

24 hours 35.32 35.49 35.41 35.42 35.44

48 hours 35.29 35.34 35.37 35.40 35.43

72 hours 35.25 35.32 35.35 35.39 35.42

96 hours 35.20 35.28 35.32 35.38 35.41

120 hours 35.16 35.25 35.30 35.36 35.40

Table 2 revealed that as the concentration of inhibitor increases, the weight of mild steel bar loss decreases. This means that the inhibitor concentration is inversely proportional to weight loss of materials. It also showed that corrosion is a function of time. That is as time increases, the rate of corrosion also increases at a specified condition. This supports the findings of Eddy and Ebenso, (2008); El-Etre (2003); Kliskic et al., (2000). Table 2: Weight loss of steel bar in different concentration of Musa Sapientum extract in 2.0M H2SO4at different time interval. Concentration of Musa Sapientum extract 0.00 0.20 0.40 0.60 0.80

Weight of bar in grams at Initial 35.50 35.50 35.50 35.50 35.50

24 hours 0.18 0.11 0.09 0.08 0.06

48 hours 0.21 0.16 0.13 0.10 0.07

72 hours 0.25 0.18 0.15 0.11 -.08

96 hours 0.30 0.22 0.18 0.12 0.09

120 hours 0.34 0.25 0.20 0.14 0.10

Table 3 shows the inhibitor efficiency for various concentration of Musa Sapientum extract in 2M H2S04 at different time interval. It shows that as the inhibitor concentration increases, percentage of inhibitor efficiency also increases which means inhibitor efficiency is directly proportional to inhibitor concentration at a particular time. It also revealed that at a specified concentration, percentage inhibitor efficiency is inversely proportional to time that is as time increases, percentage inhibitor efficiency decreases. The optimum inhibitor efficiency was approximately 71 % which corresponds to 0.80 g/l Musa Sapientum extract in 2.0M H2S04 at 120 hours. Table 3: Inhibitor efficiency for various concentration of Musa Sapientum extract in 2.0M H2SO4 . Concentration of Musa Sapientum extract 0.00 0.20 0.40 0.60 0.80

% IE at 24 hours 0.00 38.89 50.00 55.56 66.67

48 hours 0.00 23.81 38.10 52.38 61.90

72 hours 0.00 28.00 40.00 56.00 64.00

96 hours 0.00 26.67 40.00 60.00 70.00

120 hours 0.00 26.47 41.18 58.82 70.59

Figure 1(a) shows a graph of weight loss in mild steel bar against concentration of Musa Sapientum in 2.0M H2S04 at different time while Figure 1(b) shows the graph of weight loss in mild steel bar against time. From Figure 1(a), the graph shows a downward slope from left to right which supports the inverse relationship between weight loss and inhibitor concentration. From Figure 1(b), the graph shows an upward slope from left to right which is in line with the direct relationship between weight loss and time. Figure 2(a) shows the graph of percentage inhibitor efficiency against inhibitor concentration for various time while Figure 2(b) shows the graph of percentage inhibitor efficiency against time for different inhibitor concentration. The graph of % IE against time has distinct features for various inhibitor concentration unlike the graph of % IE against inhibitor concentration which interfere at various time. The results of the experiment have shown that the Musa Sapientum extract reduced the corrosion rate as high as approximately 71 % for this particular study. The inhibitor efficiency is encouraging and this can be used in the industries as a substitute for the imported chemical inhibitors which will save the country a huge amount of money use for importation of inhibitors annually. In addition, using the Musa Sapientum peels extract is a way of managing waste because the peels constitute solid waste which its management is a problem in Nigeria. The fact that the Musa Sapientum extract is a natural extract which is environment friendly and non toxic to human Š 2012 GETview Limited. All rights reserved

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is also a reason why the industries should key into it especially in this era where there is a big environmental challenge in the world as a whole.

(a)

(b)

Figure 1: Graph of weight loss against (a) concentration at different time interval, (b) different concentration.

(a)

(b)

Figure 2: Graph of % IE against (a) concentration at different time, (b) different concentration.

5.0

CONCLUSION

This study has shown that Musa Sapientum peels extract can be used as corrosion inhibitor. As the concentration of inhibitor produced increases, the corrosion rate decreases and the inhibitor has an optimum efficiency of about 71 % which proved that its usage in the process industries will reduce drastically the corrosion rate. If the Musa Sapientum peels extract is used as corrosion inhibitor, it will increase the GDP of the nation hence the standard of living and also make our environment less prone to pollution. ACKNOWLEDMENTS The contribution of Erinoso Oluwaseun Mathew during the experiment has made this study to be successful. We really appreciate your efforts.

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[4] Anhwange, B.A., Ugye, T.J. and Nyiaatagher, T.D. (2009): Chemical Composition of Musa Sapientum (Banana) peels. Electronic Journal of Environment, Agricultural and Food Chemistry, Vol.8, No.6, pp.437-442. [5] Bendahou, M.A., Benadellah, M.B.E and Hammouti, B.B.(2006): A Study of Resomary Oil as A Green Corrosion Inhibitor for Steel in 2M H3P04. Pigment and Resin Technology. Vol.35, pp.95-100. [6] Bouyanzer, A. and Hammouti, B. (2004): A study of Anticorrosion Effects of Artemisia Oil on Steel. Pigment and Resin Technology, Vol.33, pp.287-292. [7] Chetouani, A., Hammouti, B. and Benkaddour, M. (2004): Corrosion Inhibition of Iron in Hydrochloric Acid Solution by Jojoba Oil. Pigment and Resin Technology, Vol.33, pp.26-31. [8] Eddy, N.O. and Ebenso, E.E. (2008): Adsorption and Inhibitive Properties of Ethanol Extracts of Musa Sapientum Peels as A Green Corrosion Inhibitor for Mild Steel in H2S04. African Journal of Pure and Applied Chemistry, Vol.2, No.6, pp.46-54. [9] El-Etre, A.Y. 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(2007): Eco-Friendly Corrosion Inhibitors: Inhibitive Action of Ethanol Extract of Garcinia Kola for The Corrosion of Aluminium in Acidic Medium. Pigment and Resin Technology, Vol.36, pp.299-305. [25] Olafadehan, O.A. and Salami, L. (2011): Proactive Solid Waste Management and Control: A Way of Environmental Sustainability in Nigeria. Nigeria Journal of Engineering Management, Vol.12, No.1, pp.26-32. [26] Rajendran, S., Ganga, S.V., Arockiasevi, J. and Amalraj, A.J. (2005): Corrosion Inhibition by Plant Extracts – An Overview. Bulletin of Electrochemical, Vol.21, pp.367-377. [27] Singh, A., Ebenso, E.E. and Quraishi, M.A. (2012): Corrosion Inhibition of Carbon Steel in Hydrochloric Acid Solution by Some Plant Extract. International Journal of Corrosion, Vol.2012, pp.1-20. [28] Sirkar, A., Das, R., Chowdhury, S. and Sahu, S.J. (2008): An Experimental Study and Mathematical Modeling of Ethanol Production from Banana Peels by Hydrolysis And Fermentation. IE Journal, Vol.88, pp.4-10. [29] Umoren, S.A. and Ebenso, E.E. (2008): Studies of Anti-Corrosive Effect of Raphia Hookeri Exudates GumHalide Mixtures for Aluminium Corrosion in Acidic Medium. Pigment and Resin Technology, Vol.37, pp.173182. [30] Yuhazri, M.Y., Haeryip Sihombing, Umar, N., Saijod, L. and Phongsakorn, P.T. (2012): Solid Fuel from Empty Fruit Bunch Fiber and Waste Papers Part 1: Heat Released from Combustion Test, Global Engineers and © 2012 GETview Limited. All rights reserved

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Technologists Review, Vol.2, No.1, pp.7-13. [31] Yuhazri, M.Y., Jeefferie, A.R., Haeryip Sihambing and Siti Rahmah, S. (2011a): Effect of Coating Controlled in Tin Coating on the Mild Steel Substrate. International Journal of Engineering Science and Technology. Vol.3, Iss.3, pp.2113-2117. [32] Yuhazri, M.Y., Jeefferie, A.R., Haeryip Sihambing, Nooririnah, O. and Warikh, A.R. (2011b): Coating effect Condition on the Corrosion Properties of Mild Steel Substrate. International Journal of Applied Science and Technology. Vol.1, Iss.1, pp.45-49.

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GLOBAL ENGINEERS & TECHNOLOGISTS REVIEW www.getview.org

HEXANE ECONOMIZATION IN PALM KERNEL OIL PLANT: A STUDY AFTER PROCESS DESIGN IMPROVEMENT SIVARAO1, KUMAR2, N., WIDODO3, W.S. and HAERYIP SIHOMBING4 1, 2

Department of Manufacturing Process Department of Manufacturing Design 4 Department of Manufacturing Management Faculty of Manufacturing Engineering Universiti Teknikal Malaysia Melaka Hang Tuah Jaya, 76100, Durian Tunggal, Melaka, MALAYSIA 1 sivarao@utem.edu.my 3 wswidodo@utem.edu.my 4 iphaery@utem.edu.my 3

ABSTRACT Hexane (C6H14) is used as a solvent to extract oil from palm kernel to produce crude palm kernel oil (CPKO) which is a common cooking ingredient. The main intention of this research work is to reduce hexane loss during the extraction process of oil from palm kernel. This research project was carried out in a leading vegetable factory in Malaysia. Although this plant managed to get high yield (average 48.5 %) compare with other similar conventional plants in Malaysia but the hexane loss is very high, 8.5 litre/Metric Ton (l/MT) in average. To reduce the hexane loss, few modification jobs were carried out; adding of new shell and tube condenser, sealing of leakages and developed a set of standard operating procedures. Preliminary investigation after the improvement steps found that, reduction of hexane loss showed a decrease of about 30 % from the average of 9.5 % litre/MT of palm kernel 6.5 litre/MT of palm kernel after the improvement. This amounted of hexane savings of 3 litre/MT of palm kernel which is equivalent to about RM 727,660 for 8 months after the process improvement taken into effect. Keywords: Palm Kernel, Hexane, Extraction, Condenser.

1.0

INTRODUCTION

Solvent extraction as a process utilizes solvents to extract the residual oil from oil-bearing seeds, cakes and brans (Dacera et al., 2003). Vegetable oil has been the main source of fat for human consumption. Most edible oils and fats are soluble in liquid hydrocarbons and hexane is the most commonly used hydrocarbon fraction for solvent extraction (Dacera et al., 2003). The solvent used in this process is not expanded, but is used over and over again in the process of recycling and a large volume of the solvent always remains in various stages of the closed processing cycles. Reducing production cost by reducing the hexane loss during the process is the key point of this study. The main aim of this research work is to reduce hexane losses during the oil extracting process from palm kernel and to study how effectively hexane and oil in the form of mischella can be separated in order to reduce the production cost while increasing the profit. Using Hexane to extract oil is called solvent extraction or solvent extraction plant. Solvent is a liquid, solid, or gas that dissolves another solid, liquid, or gaseous solute, resulting in a solution that is soluble in certain volume of solvent at a specified temperature. In solvent extraction plant, hexane is commonly used as a solvent to extract the oil from the palm kernel. Hexane is a hydrocarbon with the chemical formula C6H14; that is, an alkane with six carbon atoms. According to a report by the Cornucopia Institute, hexane is used to extract oil from grains as well as protein from soy, to such an extent that in 2007, grain processors were responsible for more than two-thirds of hexane emissions in the United States (NVO Hexane Report, 2010). The report also pointed out that the hexane can persist in the final food product created; in a sample of processed soy, the oil contained 10 ppm, the meal 21 ppm and the grits 14 ppm hexane. Using hexane to extract oil is commonly used for oil-cake extraction (soya bean meal, groundnut meal, rice bran meal, cotton seed meal, sells seed, guar meal, copra meal), oilseeds (soya bean, sunflower seed, groundnut, cotton, sal, niger, mustard, castor), vegetable oils (palm olefins, soya bean oil, rap seed oil, sunflower seed oil), grains (wheat, corn, rice, sorghum, millets, barley) (Yuhazri et al., 2012) and (House et al., 1981). In Malaysia there is a leading vegetable oil plant using hexane to extract oil from palm kernel. This is the only plant in Malaysia using hexane for direct extraction from palm kernel flakes. This plant is divided into two sections where the first section is preparation plant and the second section is a solvent extraction plant. In the -

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preparation plant, the palm kernels will be hammered, crushed, flaked and conditioned by indirect steam and then, this flaked meal will be sent to the second section, solvent extraction plant where hexane will be pumped and flushed to these flakes to extract the oils. By using hexane about 48 % of crude palm kernel oils and 52 % of by-product, palm kernel meal can be produced. By using this technology this plant is able to extract more crude palm kernel oils, yield an average 48 % compared with conventional press which would only be 44.5 % in average (Hai, 2002). Although this plant uses hexane for solvent extraction from palm kernel and gain higher yield compared with other conventional methods, but they are facing problem to recover hexane efficiently. Average hexane loss at the end of the day is about 9.5 of hexane per ton of palm kernel losses encountered. Basically this plant faces problem with high hexane losses during the process of extracting oils from palm kernels. Complete process flow of preparation and extraction sections are show in the form of flow chart in Figure 1.

Figure 1: Preparation plant flow chart.

1.1 Preparation Plant Preparation plant is the place where daily production is set by key in the required flow rate (MTs/hour) of palm kernels in the weigher machine. In this plant, after past the magnetic separator to separate metal pieces, palm kernels from silos will send to weigher to produce required flow rate per hour. After the weigher machine, the palm kernels will enter to hammer mill where the palm kernels will be hammered to reduce the size and for further reduction the kernels will past to the cracking roller machine where the kernels will be crushed and break further. To get high yield of crude palm kernel oils (CPKO), the kernels must be soft and small size. So to get that result, the broken kernels will send to 1st operation flaker where all these kernels will be flaked to below 1.5 mm thickness and then all these materials will send to conditioner where these flakes will be heated up with jacketed steam to get temperature about 70 °C. After the conditioner these soft flakes will enter to 2nd operation flaker to get flakes thickness below 0.3 to 0.5 mm. Finally these flakes are ready to extract oil. All these process are online continuous process. 1.2 Extraction Plant After the final process in preparation plant, the flakes will be transferred to the extractor with 2 compartments. In this extractor, the fresh hexane will be pumped into these flakes to extract the oil. This oil called miscella, means oil and hexane mixed together where miscella contains about 60 % of hexane. To separate oil and hexane, this miscella will go through another process in distillation plant. After the oils were extracted from the flakes, the by-product, palm kernels meals from the 2nd compartment will be produced. This by-product, palm kernel meals contains around 40 % of hexane. To separate meals and hexane, these by products will be sent to another plant, meal de-solventizing. Process flow of the extraction plant is shown in Figure 2. Distillation is the process to separate the miscella into crude palm kernel oil and hexane. In this plant the mischella will be heated up in three different stages and temperature till capture all the hot hexane vapor and this hot vapor will be vacuumed to three different condensers to cool it and regain the hexane in liquid form and will be re-used. In this meal de-solventizing plant, the by-product will be heated Š 2012 GETview Limited. All rights reserved

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up by going through a super heater and by using vacuum about –0.5bar, the hot hexane vapor will be sucked into condenser where, heat transfer will take place to convert the hexane into vapor to liquid form. This liquid hexane will be stored in working tank and will be recycled to the extractor. Whatever hexane missed to collect in distillation and meal de-solventizing process, will be sent to absorption plant where, in this plant absorption oil will be used to trap whatever missing hexane. The hexane, which dilute with abruption oil, will send to absorption column and followed by heat exchanger to heat up the hexane to separate it from absorption oil and then will past to 2nd heat exchanger to bring back the hexane to liquid form and finally all the collected hexane will be transferred to the hexane working tank. After the hexane removed through the above process, the oil called crude palm kernel oil, CPKO and the by-product is palm kernel meal. By this extraction process around 48 % Crude palm kernel oils and 52 % of by-product, palm kernel meals is produced. The CPKO will be transferred to main storage tank to sell out or further process in the refinery plant. The palm kernel meal will send to palletizing plant to produce palm kernel pallets and palm kernels meal.

Figure 2: Extraction plant flow chart.

2.0

MATERIALS AND METHODS 2.1 Pre-assessment Pre-assessment audit were carried out on high hexane loss followed an assessment to focus the major problems and implementation to reduce the hexane loss and finally monitoring and evaluation of the final result. The pre-assessment audit was conducted in May, 2011. Pre-assessment audit was conducted to focus area of high hexane loss based on fish bone diagram as shown in Figure 3. Input details were collected through current result, parameters, interviews, questionnaires and brain storming sections.

Figure 3: Fishbone analysis. Š 2012 GETview Limited. All rights reserved

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Based on the pre-assessment findings, the audit was focused on: (i)

Excess loss Excess loss is the amount of additional loss through: (a) (b) (c) (d) (e) (f)

oil from the final oil stripper. air from the meal dryer cooler. meal from meal dryer cooler. air from the mineral oil system. water from waste water evaporator. inconsistent operation.

The excess loss due to inconsistent operation occurs during the period starting when the input conditions change and ending when the input conditions change back to normal, or during the period starting when the input condition change and ending when steady state is achieved after the operating parameters have changed. (ii)

Fugitive loss Fugitive loss is the amount of solvent loss from the process equipment through flanges, doors, packing glands, pump seals, valves stems, sight glasses, etc. This loss occurs when the pressure inside the vessel is higher than atmospheric pressure, causing solvent vapour inside the vessel to leak out through any orifice.

(iii)

Purging loss Purging loss is amount of solvent loss from process equipment resulting from freeing the process equipment of solvent vapour for inspection or maintenance. This loss occurs as a result of opening up the process equipment and as a result of using purge fans to pull air through the process equipment. During normal operation, purging loss does not exist. Purging loss only exists when the plant is shutdown. Thus, the solvent loss as a result of purging can not be quantified in terms of litters of solvent loss per ton of palm kernel processed on a direct basis, as with other categories of solvent loss.

2.2 Assessment Based on findings in the fish bone diagram, the assessment audit was conducted in July 2011. The assessment was focused on excess loss, fugitive loss and purging loss. The purpose of the assessment was to collect detail information on high hexane loss due to excess loss, fugitive loss and purging loss. 2.2.1 Assessment phase 1: excess loss Excess loss is the only area able to do analyse the quantity of hexane contains in crude palm kernel oil, palm kernel meal, vent gases from absorption and water from waste water system. Hexane contains in crude palm kernel oil measured by flash point temperature meanwhile hexane contain in palm kernel meal and waste water measured by mg/kg or ppm and hexane contain in vent gases from absorption measured by kg/ or ppm. According to Solvent Extractors Association Handbook of India 9th revised edition 2009, the allowable range for for flash point is min 100 °C, hexane contain in palm kernel meal is 170 ppm, hexane contain in vent gases is 50 mg/ and hexane contain in waste water is 10 ppm. Detail audit of analyzing the hexane contains were carried on January till May 2011 and the average for these 5 months are as per in Table 1. Table 1: Detail audit data.

Palm Kernel thru put (MT) CPKO-Flash Point (°C) Hexane in Palm Kernel Meal (ppm) Vent gases from absorption (mg/ltr) Water (ppm)

January 2011

February 2011

March 2011

April 2011

May 2011

Acceptable

12,250

11,510

12,505

12,500

12,498

-

120

120

120

120

120

Min 100

210

300

250

225

220

170

600

500

550

580

570

50

8

6

10

8

8

10

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Base on data from Table 1, four independent plots were developed to have a clear picture of the improvement in better hexane recovery.

(a) (b) Figure 4: (a) comparison of actual & allowable with PK thru put, (b) comparison of hexane contain in palm kernel meal with PK thru put.

From Figure 4(a), 4(b), 5(a) and 5(b), it was found that there is high hexane loss in vent air from absorption compare with other hexane losses in CPKO, palm kernel meal and waste water. Decision was made to focus on hexane loss in vent air and to draft an action plan and improvement. Detail studies and audits were carried out in distillation section as shown in Figure 6.

(a) (b) Figure 5: Comparison of hexane contain in (a) vent air with PK thru put, (b) waste water with PK thru put.

The vent air blows through absorption section but the unrecovered hexane vapor comes mainly from distillation section, while small amount from extractor. To save 50 % steam of the distillation is achieved using hot De-solventizer vapors in a unique falling film economizer. This reduces the steam consumption and the load on the final condenser. This is followed by a steam heated rising film evaporators and stripping column operating under vacuum.

Figure 6: Distillation section before modification.

The vapors from falling film economizer, rising film evaporators 1 and 2 and from stripper column will be sucked into condensers to condense hexane vapor to liquid form. The hexane vapor that is not condensed in the last condenser is typically passed through a mineral oil absorption system. The hexane liquid will be transferred into special water separator to remove the waste water. After maximum recovery by condensation further hexane content in the exhaust air can be further reduced only by an absorption by intimate contact with chilled mineral oil in specially designed packed column. Thereafter the air is exhausted to the atmosphere with the maximum hexane content and the absorber oil is stripped with direct stream to remove the traces of hexane and send for re-circulation to cold absorber. The special absorber unit is a packed column. The air aspirated with the feedstock into the plant has to be evacuated. This air is a carrier of hexane at its saturation vapor pressure. So the Š 2012 GETview Limited. All rights reserved

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exhaust air is cooled first in chilled water vent condenser to a temperature around 20 °C for maximum recovery by condensation. To reduce the hexane content in vent air, there are two options considered: upgrade complete absorption section and add 1 more condenser to increase the condensation capacity. Since the cost is high to upgrade the complete absorption system, recommendation given to management to add 1 more condensers in the distillation plant. Table 2 shows the existing and the recommendation. Table 2: Existing and proposed distillation installation. Water Temperature (°C) In Out C1 450 200 32 38 C2 450 200 32 38 C3 450 200 32 38 *Recommendation: Add new condenser of 450m2 Condenser

Area (m2)

Water Flow Rate (m3)

Hexane Vapour Temperature (°C) In Out 120 44 90 40 90 40

2.2.2 Assessment phase 2: fugitive loss Decisions taken to carry out pressure test all equipment and piping with pressurized water to ensure that the system is free of leaks prior to start operation. 2.2.3 Assessment phase 3: purging loss Purging loss only exist once the plant is starting back after the shutdown. Case study was carried for the year 2010 of high hexane losses during the plant start back after more than 1 day shutdown as shown in Figure 7. The actions that can be taken to minimize the purging loss are: (i)

(ii) (iii)

Improve equipment reliability through design improvement and trough preventive maintenance processes. This will reduce the frequency for which maintenance and inspection are required, thus reducing the frequency of vapor freeing and its related purging solvent loss. Allow the normal vapor recovery system to run as long as possible prior opening up the process equipment. This will recover the majority of the solvent prior to vapor freeing, thus reducing purging loss. Discharge the purge fan through a condenser to recover as much as the solvent vapor as possible, thus reducing purging solvent loss.

Decision was taken to carry out action plant no 2 due to able to carry out the action immediately without any major cost.

Figure 7: Hexane loss after plant starting back from shut down.

2.3 Implementation Once the action plans were selected for excess, fugitive and purging loss, decision taken to implement the action plans in stages, 1st excess loss followed by fugitive loss and finally purging loss. 2.3.1 Excess loss On 23 December 2011, added 1 more condenser, 450 m2 to increase the cooling capacity from 1350m2 to 1800m2 (refer to Figure 8). This mainly to condense the vapor from economizers, evaporators and stripper and reduce the excess load in absorption section.

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2.3.2 Fugitive Loss On 02 June 2012, the complete solvent extraction plant was shutdown for annual maintenance works. The action taken to pressure tests all the equipment including economizers, evaporators, stripper, vapors lines and vessels. The pressure test carried out by using water and found the water leaking from economizer top manhole, evaporators transfer line flange, several piping flange and 1 elbow cracked. Gaskets were changed to all the leaking area and replaced new elbow. 2.3.3 Purging Loss A shutdown procedures was planned and a case study was carried out from June to August 2012, decision taken that vacuum pump, steam and cooling tower need to be operated continuously for 3 hours before the plant completely shut down. This due to allow the normal vapor recovery system and recover the majority hexane vapor to be condensed.

Figure 8: Distillation section after modification.

3.0

RESULTS AND DISCUSSION

The results after the improvement were recorded in three different stages. The findings and discussion are focused on hexane loss in excess loss, purging loss and fugitive loss. 3.1 Excess Loss After installed new condenser to increase the cooling capacity from 1350 m2 to 1800 m2, results are monitored for hexane content in ventilated air from January 2012 to May 2012. Based on the results, a graph was plotted as per Figure 9(a). This graph shows hexane contains in vent reduced from average 560 mg/litre taken in January-May 2011 to average 132 mg/litre. Detail analysis of hexane loss also carried in the same period. Figure 9(b) is the results and found after the installed new condenser, the hexane loss reduced from average 9.5 litre/MT to 7.5 litre/MT.

Figure 9: (a) Monitoring hexane in vent air, (b) hexane excess loss before and after modification.

3.2 Fugitive Loss After rectified all the leakages especially from economizer, evaporators’ flanges and elbows and fittings, detail analysis was carried for 3 months. A graph was plotted base on the results. Figure 10(a) clearly shows the improvement and saving about 1 litre/MT after stop the leakages.

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Figure 10: Hexane before and after modification, (a) fugitive loss, (b) Purging loss.

3.3 Purging Loss Although the hexane loss due to purging cannot be quantified in terms of litre of solvent loss per ton of palm kernel processed on a direct basis but it’s very important to keep the hexane loss as low as possible during the plant start up after shutdown. Following the specific shutdown and start-up procedures complying detailed checklists, the results have been improved as shown in Figure 10(b).

4.0

CONCLUSION

Hexane loss has always been the significant reason incurring cost for operating of an extraction plant. Perhaps, in the past, there were times when additional solvent usage was accepted as part of having lower residual oils in the meal and mill feed or even lower energy costs in steam production, but discarded by recent food and safety regulations. However excessive expenditure for additional solvent recovery or pollution control equipment would not be necessary if a plant is properly operated and maintained. Table 3 clearly shows the total saving of RM 727, 660 from January 2012 to August 2012 after the improvements we implemented. Table 3: Total saving of hexane

PK throughput (mt)

January 2012

February 2012

March 2012

April 2012

May 2012

June 2012

July 2012

August 2012

7,943

13,652

12,723

12,557

15,086

14,066

14,754

12,840

Hexane Loss (/mt)

7.3

7.8

7.4

7.5

7.5

6.6

6.5

6.5

Hexane Price (RM/s)

2.89

2.82

2.82

2.43

3.17

3.22

3.05

2.94

Average Hexane loss in year 2011

9.5

9.5

9.5

9.5

9.5

9.5

9.5

9.5

50,494

65,536

75,450

61,020

95,704

131,261

134,871

113,324

Saving (RM)

ACKNOWLEDMENTS Authors would like to thank Faculty of Manufacturing Engineering and Universiti Teknikal Malaysia Melaka for supporting this research Special thanks to Ministry of Higher Education (MOHE) for awarding research grants (GLuar/2012/FKP(1)/G00010) and (PRGS/2012/TK01/FKP/02/1/T0003) which very much helped in completing the study without much hurdles.

REFERENCES [1] Dacera, D., Jenvanitpanjakul, P., Nitisoravut, S. and Babel, S. (2003): Hexan Reduction in a Thai Rice Bran Oil factory: A Cleaner Technology Approach. Thammasat Int. Journal of Science and Technology, Vol.8, No.4, pp.6-16. [2] NVO Hexane Report (2010): Soy Protein and Chemical Solvents in Nutrition Bars and Meat Alternatives, Cornucopia Institute. [3] Hai, T.C. (2002): The Palm Oil Industry in Malaysia: From Seed to Frying Pan, Plantation Agriculture - WWF Malaysia. [4] House, R.J.R., Harcombe, A.O. and Guinness R.G. (1981): Hexane Losses in Solvent Extracted Soya Meal: Measurement by Gas Chromatography and Brief Evaluation. Journal of the American Oil Chemist’ Society, pp.626-629. [5] Yuhazri, M.Y., Haeryip Sihambing, Umar Nirmal, Saijod Lau and Phongsakorn Prak Tom. (2012): Solid Fuel from Empty Fruit Bunch Fiber and Waste Papers part1: Heat Released from Combustion Test. Global Engineers and Technologists Review. Vol.2, No.1, pp.7-13.

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