PAMANTASAN NG LUNGSOD NG MAYNILA College of Engineering and Technology Bachelor of Science in Chemical Engineering (BS ChE)

Extraction of Linoleic Acid from Tuba-tuba (Jatropha curcas) and Lumbang (Aleurites moluccana) for the production of Quick Drying Oil via Condensation Polymerization
Submitted by: BARCELONA, Margarette Kaye D. BAUTISTA, Well Known L. GALANGUE, Bernard F. ZUBIRI, Gladys Anne T.

BS ChE V Submitted to: Engr. Milagros R. Cabangon CHAPTER 1 INTRODUCTION A study on jatropha (Jatropha curcas) indicates that it can produce more than 30 percent oil yield and that it is more environment-friendly as fuel source than diesel. Based on an article in the Philippine Daily Inquirer, Energy Secretary Jose Rene Almendras recently disclosed that the Arroyo administration had already spent P1 billion of a P1.4 billion allocation for the project, covering the cost of planting some 4,000

hectares of land with jatropha plant. While established studies had found that jatropha oil could be converted into methyl ester, a material suitable as blend for diesel fuel according to DOST, commercial production is said to be not viable. (Tarra Quismundo, November 2011). According to the United Nations Food and Agriculture Organization, the Jatropha fruit contains 62.5 % seeds. Lumbang (Aleurites moluccana) or also known as candlenut is a flowering tree and distributed throughout tropical regions. It grows to a height of 15-25 meters and has a nut that is round for about 4-6 cm and the seed (kernel) inside has a very hard seed coat (nutshells) and has a high oil content, which allows its use as a candle. According to the research made by Hong TD et al., the lumbang kernels yields 57-80 percent of inedible oil. According to Bureau of Agricultural and Statistics the production of lumbang seeds in San Alfonso, Cavite has an average of 50-150 kilograms per tree annually. Quick Drying oils are any group of oily, organic liquid that, when applied as a thin coating, can absorb atmospheric oxygen and polymerize, forming a though and elastic layer. These quick drying oils are being used in the paint industry as a raw material to quick drying enamel products, raw material in the production of varnish, and in nail polish enamels. The processes involved in the production of Quick Drying Oil includes the extraction of the oil from the lumbang kernel and tuba tuba seeds, degumming, alkali refining, bleaching, and the heart of the process polymerization. From these cases, the researchers are triggered to formulate a study entitled Extraction of Linoleic Acid from Tuba-tuba (Jatropha curcas) and Lumbang (Aleurites moluccana) for the production of Quick Drying Oils via Condensation Polymerization

RATIONALE The thousand hectares of planted tuba-tuba for the jatropha biodiesel project turned out to be a problem as the plan was considered to be commercially unviable. Lumbang seeds are unutilized agricultural material abundant here in the country.

Linseed, the most commonly used raw material for quick drying oils is not native in our country. In 2009, 80,865 kilograms of linseed oil were imported to the Philippines. In an effort to supply this demand without resorting to importation, and to minimize waste brought about by tuba-tuba and lumbang, this research is projected.

The proposed study, pertaining to producing quick drying oil tuba-tuba and lumbang looks forward to providing a way in which the said agricultural materials will be of use. The manufacture of a oilseed industrial plant will also prove its significance in the countrys economy.

COMPANY PROFILE Vision Jatrumbang Corporation aims to be the leader in the production of Quick Drying Oil in the Philippines that renders world class quality products and services. An institution led by the by waste utilization under the impression of technology innovation.

The corporation is equipped with the latest technology application through outstanding manufacturing plant and sites. It envisioned its staffs, employee, and workers the spirit of true service and everlasting care for the environment and to the public it serve. Mission In the light of the corporation vision, we commit ourselves to: 1. Make the Jatrumbang Corporation a home of excellence in working relations and to be guided by our core values and with professional conduct. 2. To make the Jatrumbang Corporation an ambiance of service and genuine concern with the customers overall satisfaction. 3. Provide trainings to the employee to make the globally competitive and effective with any demands of work. 4. And to stress the use of waste utilization and to protect the environment and the public we serve. Core Values y Teamwork The employees do not only work individually but he can blend in a team or group y Integrity We value integrity through taking care of the name of the company as we take care of our names integrity. y Honesty We show honesty through work right all the times even without anyone looking or praising his work. He works at his best all the time. y Safety We put safety the top priority of the company. We make sure that all the employees are taken the proper care while inside the company vicinity. y Professionalism We set aside differences while working in the manufacturing plant and site.

PRODUCT LOGO

The

company

logo

constitutes 5 parts. First is the circular formation of the logo, symbolizes the unity of the corporation as seen in the organization of the company. The second is the two raw materials of the company, the Jatropha (Jatropha curcas) seeds and Lumbang (Aleurites moluccana) kernel, signifies that the product Quick Drying Oil is made from the utilization of the two waste raw materials. Third is the oil drop that gives the product of the Jatrumbang Corporation which is Quick Drying Oil. Fourth and fifth is the leaves that surround the logo and the earth that gives emphasize on the aim of the Jatrumbang Corporation which is to create Quick Drying Oil that uses waste utilization as a part of promoting environmental awareness and the public health.

STATEMENT OF THE PROBLEM

Lumbang (Alurites moluccana) kernel represents an agricultural crop with importance as it is being used as one alternative in candles and often called candlenut. An interview made by the researchers revealed that years and years ago when there is no electricity yet, the oil was being extracted in the lumbang kernel using a piece of cotton. Mr. Dimacuja, a resident of Barrio Sinaliw San Alfonso, Cavite told the researchers that the oil extracted from the lumbang kernel was being ignited and will be a source of light. But upon the discovery of electrical technology lumbang kernel was left unutilized, scattered in the ground, and if not germinated will be rotten. Meanwhile according to ABS-CBN news on the 4th of November 2011, the Department of Energy is claiming the Arroyo administration wasted P1.4 billion on a project to cultivate the jatropha (Jatropha curcas) plant, which was hailed as a future source of fuel. More than 4,000 hectares of idle land was planted with the Jatropha curcas during the Arroyo administration. The program has been running for several years now, but there is one problem according to the Aquino administration - jatropha is not commercially viable. In Pila, Laguna, there used to be 5,000 to 6,000 jatropha trees planted in this 2-hectare property. The researchers aimed to conduct further studies on the other uses of jatropha and jatropha oil, aside from petroleum additives. With all these considerations, the researchers are triggered to use the Lumbang and Tuba Tuba Seeds as the primary raw material: which are considered as unutilized waste. The researchers indulge in this study entitled Extraction of Linoleic Acid from Tuba-tuba (Jatropha curcas) and Lumbang (Aleurites moluccana) for the production of Quick Drying Oils via CondensationPolymerization

OBJECTIVE OF THE STUDY: General: The main objective of this research is to develop a technology that would produce organic based Quick Drying Oil from the utilization of tuba-tuba (Aleurites moluccana) and lumbang (Jatropha curcas) seeds. Specific: y To obtain a Quick Drying Oil that has properties like density of 929 kg/m3, pH of 6.5-7.5 and viscosity of 25-35 centipoises. y To determine the market feasibility of the proposed project by providing analyses of the historical and projected demand and supply and the market stability by constituting marketing strategies and market plans y To develop a equivalent manufacturing process of experimental procedures for the production of Quick Drying Oil from tuba-tuba and lumbang seeds y To develop an economic feasibility for the proposed project.

SIGNIFICANCE OF THE STUDY

To the Students This study would give an insight to the students of the notion such that crops like tuba-tuba and lumbang could be a multipurpose crop providing both energy and feed (as a raw material) which, in one way or another, could relate it to their future research studies in cases like utilizing the same raw material for the production of a different product and vice versa.

To the Nation By utilizing tuba-tuba oil and lumbang oil for the production of useful products, such as Quick Drying Oil, can respectively be an alternative use for the raw material to paint, varnish and nail polish. This could possibly be a way to make more job opportunities possible.

To the ChE Profession Advance researches and process developments from Chemical engineers about this study, which explores tuba-tuba and lumbang oil as a viable source of Quick Drying Oil, could boost up the country's economic and scientific development.

To the Industry If proven feasible, both the material and method used could be utilized and developed by other institutions so that it could help increase incomes not only for resin industry but also for agricultural industry. This could benefit the domestic economy and could help be diverted to both the farmers and local agro industry.

SCOPE AND LIMITATIONS This study entitled Extraction of Linoleic Acid from Tuba tuba (Jatropha curcas Linn.) and Lumbang (Jatropha Mollucana Linn.) for the Production of Quick Drying Oil via Condensation Polymerization centers on tuba-tuba seeds and lumbang kernels as raw materials for the production of quick drying oil. The product is proposed to be an alternative to linseed oil. For the experimental part of the research, tuba-tuba seeds are obtained from LOCATION and lumbang kernels are from San Alfonso, Cavite. The production is composed of four steps; (1) Preparation and Conditioning of Raw Materials, (2) Extraction, (3) Refining and (4) Polymerization.

A market study was included to institute feasibility of the product sales. Analysis of the historical and projected demand and supply was done for the market allocation. For the marketability of the quick drying oil, product distribution techniques were also accounted.

Technical study was also integrated in order to have the required specifications and designs of the necessary equipment for the process. Careful selection and design of essential equipment for the production of cellophane was included in this study. Part of this study was the wastewater facility for the treatment of process wastewater. Also, the appropriate instrumentation and process control and piping system fitting the actual

manufacturing process were identified. Laboratory scale was used for the experimental procedures. Human and instrument errors may be inevitable during the experiment but can be corrected in the actual operation.

Financial study was built-in to establish the economic feasibility of the project.

METHODS OF RESEARCH Throughout the comprehensive study, the researchers used two methods for the collection of data. Facts and figures gathered were for the properties and availability of the raw materials, characteristics of the product and its market statistics and/or records; and experimental procedures and manufacturing processes. These two methods were the following:

A. Descriptive Method

The researchers went to the following institutions to gather the most recent information and statistical data accessible for the raw materials, namely, tuba-tuba and lumbang, and the product, quick drying oil.

 National Statistics Office (NSO) - Sta. Mesa, Manila Historical statistical data on the import and export of quick drying oil from year 2005 to 2010

 Department of Trade and Industry (DTI) - Buendia, Makati Provided the lists of the consuming and competing industries and their local production  Supplementary reading and facts National Library PLM Library Cavite Municipal

B. Experimental Method The experimental method is the scientific undertaking of the research. Laboratory scale experimentation in view of various parameters was made to arise with the optimum operating conditions and best quality of the product.  Adamson University Chemistry Laboratory Laboratory apparatus, equipment and facilities were provided for experimentation.

Preparation and Conditioning of Raw Materials

I. Washing of the Tuba tuba A. Materials and Apparatus:

Materials and Apparatus Tuba Tuba Seeds Tap Water Analytical Balance Basin

B. Objective: To remove the dirt that adheres on the tuba-tuba that may affect the process in producing quick drying oil. C. Hypothesis: The dirt (eg. soil) on tuba tuba seeds that may affect the purity of the oil extracted, the colour of the wash water will determine the amount of water tha will be used in the process. D. Procedures: 1. Weigh 50 grams of tuba tuba seeds, put in a beaker and label for trials. 2. Use 100 g of tap water for each washing of the raw materials. Mix the components. 3. Record the appearance of wash water. 4. Repeat step 2 for tuba tuba until the washings exhibit a clear coloration. 5. Record the total water used. E. Data and Results: Appearance of the Wash Water of Tuba tuba seeds Weight 50 g 1st Wash Dark brown 2nd Wash Dark brown 3rd Wash Brown 4th Wash Light brown 5th wash Light brown

F. Analysis: The color of the wash water after the process exhibits a dark color and settleable solids. The dirt removed may affect the purity of oil that will be obtained. G. Conclusion: The preliminary treatment of tuba-tuba seeds such as washings eliminates dirt that adheres in the seeds. H. Equivalent Unit Operation Laboratory Scale Water and Basin Plant Scale Washer

Preparation and Conditioning of Raw Materials 1. Washing Laboratory Scale Basin Plant Scale Washer

A. Deshelling of Lumbang nut A. Materials and Apparatus: Materials and Apparatus Lumbang Seeds Spatula Hammer Analytical Balance

B. Objective: To remove the shell that may not contribute to the amount of oil extracted during the extraction process C. Hypothesis:

The hard shells of lumbang will not contribute to the amount of oil to be extracted.

D. Procedures: 1. Weigh several pieces of lumbang seeds. 2. Use a hammer to break the hard shells 3. Remove the kernel from the shells. 4. Weigh the total amount of kernels obtained. E. Data and Results: Weight of seeds (g) 149.89 Weight of kernels (g) 44.31

F. Analysis: The kernel obtained was observed to be saturated with oil due to its greasy feeling leaving the shells barely dry. The oil content of the lumbang seeds is concentrated on its white kernel. G. Conclusion: The hard shells of the lumbang seeds do not contribute to the oil content and it needs to be eliminated. H. Equivalent Unit Operations: Laboratory Scale Hammering Plant Scale Milling

Preparation and Conditioning of Raw Materials 1. Deshelling Laboratory Scale Hammer Plant Scale Hammer mill

B. Crushing of Tuba tuba Seeds A. Materials and Apparatus:

Materials and Apparatus Tuba Tuba Seeds Spatula Beaker Mortar and Pestle Analytical Balance

B. Objective: The crushing of tuba tuba seeds will extract more oil in solvent extraction. The solvent will have a good contact with the crushed tuba tuba seeds in solvent extraction. C. Hypothesis: The increase in the surface area of the seeds especially its kernel in contact with solvent will increase the oil yield of the seeds.

D. Procedures: 1. Prepare samples of 30 g of cleaned tuba tuba seeds. 2. Use mortar and pestle to grind the samples 3. Transfer the samples into beaker and label each beaker accordingly. E. Data and Results: Weight of seeds (g) 88.98 Weight of crushed seeds (g) 88.62

F. Analysis: The crushing process increases the surface area of the sample and at the same time exposing the oil rich kernel of the seeds to the solvent. G. Conclusion: The oil yield of the seeds is improved by increasing the surface area and exposing the kernel to the solvent. H. Equivalent Unit Operations: Laboratory Scale Mortar and Pestle Plant Scale Milling

2. Solvent Extraction I. Variation of Solvent used in Extraction Materials and Apparatus: Materials, Reagents, and Apparatus Crushed Lumbang Kernels Crushed Tuba Tuba Seeds Methanol Acetone Petroleum Ether Beakers Analytical Balance Stirring Rod Rotary Evaporator

A. Objective: To determine the appropriate solvent that will yield optimum amount of extracted oil. B. Hypothesis: The appropriate solvent will yield the optimum amount of oil from the samples. D. Procedures: 1. Weigh the 30 g sample prior to solvent extraction. 2. Prepare 100 mL of acetone, methanol and petroleum ether. 3. Mix the samples plus the solvent and allow the contact process for 10 minutes. 4. Separate the miscella (solvent plus oil) from the cake. 5. Weigh the miscella and record the data. 6. Separate the oil from the solvent using the rotary evaporator. 7. Record the temperature of the boiling point of the mixture. 8. Record both the volume of the oil collected and the recovered solvent 9. Repeat steps 1-8 using now methanol as the solvent. 10. Record the data and determine which solvent is appropriate for the extraction of oil from seeds. E. Data and Results:

Variation of Solvent Solvent used Volume of solvent (ml) 100 100 100 Weight of lumbang kernel (g) 30 30 30 Soaking time (min) Boiling point of solvent ( C) 60 60 65 Vol. of oil plus solvent (mL) 90 90.5 88.3 Volume Volume of solvent of oil recovered recovered (mL) (mL) 61 60.5 74 6 17.8 16

Acetone Methanol Petroleum ether

10 10 10

Variation of Solvent Solvent used Volume of solvent (ml) 100 100 100 Weight of jatropha seed (g) 30 30 30 Soaking time (min) Boiling point of solvent ( C) 59 68 65 Vol. of oil plus solvent (mL) 90 90.5 88.3 Volume Volume of solvent of oil recovered recovered (mL) (mL) 73 72 69.8 5.6 4.4 16

Acetone Methanol Petroleum ether

10 10 10

F. Analysis: In this procedure, three different solvents were used: acetone, methanol and petroleum ether, the optimum condition will be determined to the amount of oil the solvent can extract. In these variations applied to both raw materials separately, petroleum ether yields the maximum amount of oil (both 16 ml for lumbang and tuba-tuba) with very high purity compared to acetone( 6 and 5.6 ml) and methanol (17.8 and 4.4 ml) in which two layer of liquids were observed.

G. Conclusion: Petroleum ether is the appropriate solvent that yielded the optimum amount of oil

during the extraction period.

II.

Variation of Ratio of Raw Materials (Tuba tuba to Lumbang) A. Materials and Apparatus: Materials and Apparatus Crushed Lumbang Kernels Crushed Tuba Tuba Seeds Petroleum Ether Stop watch Beakers Stirring Rods Rotary Evaporator Analytical Balance

B. Objective: To determine the optimum ratio of raw materials that will yield the desired property of oil extracted. C. Hypothesis: The appropriate ratio of raw materials provides the desired property of oil being extracted. D. Procedures: 1. Prepare five (5) sets of 132.93 grams of combined crushed tuba-tuba seeds and lumbang kernel for a 1:1, 1:2, 2:1, 1:3 and 3:1 ratio. 2. Place 266 mL of petroleum ether in each beaker. 3. Allow the mixture to dissolve the oil to the solvent for 10 minutes. 4. Separate the liquid portion of the mixture and record the initial volume. 5. Record the boiling point of the mixture 6. Record the volume of both the oil collected and the recovered solvent 7. Weigh the mass of cake 8. Observe the appearance and compared the results.

E. Data and Results Variation of Ratio of Raw Materials (Tuba tuba to Lumbang) Ratio of Ratio of Volume Weight Soaking Volume Boiling Vol. of Vol. of oil tuba solvent of of raw time of oil point solvent recovered tuba to to raw solvent materials (min) plus of recovered (mL) lumbang materials used (g) solvent solvent (mL) (J:L) (S: RM) (mL) (mL) 1:1 1:2 2:1 1:3 3:1 2:1 2:1 2:1 2:1 2:1 266.00 266.00 266.00 266.00 266.00 132.93 132.93 132.93 132.93 30 10 10 10 10 10 177.40 177.40 182.40 212.8 186.20 67 68 71 72 78 175.10 175.10 133.00 186.20 181.80 15.70 32.60 20.00 54.10 47.80 Wt. Of cake (g)

174.89 174.67 176.97 172.76 174.36

F. Analysis: In this procedure, five different ratios of raw materials were used to determine the appropriate ratio that will give the desired property of drying oil but not very fast that may cause difficulty in manufacturing process. Obviously, the greater the proportion of lumbang to tuba-tuba (1:2 and 1:3) yielded the maximum amount of oil but the consequence was that they easily solidifies upon transferring from one container to another right after their volume and mass were recorded. On the other hand, the greater the proportion of tuba tuba oil to lumbang, the slower the drying of oil since tuba tuba oil dries much slower than the lumbang oil. In this case, 2:1 is the chosen one although yield has lower volume compared to 3:1. G. Conclusion: The 2:1 ratio of raw materials is the appropriate ratio that will yield the desired property of the oil.

III.

Variation of Ratio of Solvent to Seeds (Tuba tuba to Lumbang, 1:1) A. Materials and Apparatus:

Materials, Reagent, and Apparatus Crushed Lumbang kernels Crushed tuba tuba seeds Petroleum ether Analytical balance Beakers Stirring rods Stop watch Rotary evaporator

B. Objective: To determine the optimum ratio of solvent to seeds that will yield the optimum amount of oil extracted. C. Hypothesis: The appropriate ratio of solvent to seeds provides the optimum amount of oil being extracted. D. Procedures: 1. Prepare three (3) sets of 132.93 grams of combined crushed tuba tuba seeds and lumbang kernel (2:1) for a 1:1, 2:1, and 3:1 solvent to raw material ratio. 2. Place 133 mL of petroleum ether in one beaker, 266 mL for another and 399 mL for the third. 3. Allow the crushed tuba tuba seeds and lumbang kernels to have contact with the solvent for 10 minutes. 4. Separate the miscella from the mixture and record the initial volume. 5. Record the boiling point of the mixture. 6. Record the volume of both the oil collected and the recovered solvent. 7. Weigh the mass of cake. 8. Observe the appearance and compared the results.

E. Data and Results Variation of Ratio of Solvent to Seeds Ratio Wt. of Ratio of Vol.of Contact Boiling Vol. of tuba of sample solvent time pt. oil plus tuba to solvent Used (mL) (min) (C) solvent lumbang to (g) (mL) (J:L) seeds Vol. of oil (mL) Vol. of recovered solvent (mL) Wt. of cake (g)

(ml:g)

1:1 2:1 3:1

132.93 132.93 132.93 F. Analysis:

1:2 1:2 1:2

133.00 266.00 399.00

10 10 10

67 68 72

102.00 177.40 314.80

10.50 18.00 53.80

93.10 175.10 243.80

175.20 174.89 176.80

In this procedure, three variations ratio of solvent to seed were used. Obviously, increasing the amount of solvent also increases the amount of oil recovery. In this case, the ratio 3:1 is the most appropriate.

G. Conclusion: The 3:1 ratio of raw materials to solvent is the appropriate ratio that will yield the optimum amount of the oil.

IV.

Variation of contact time A. Materials and Apparatus: Materials and Apparatus Crushed Lumbang kernels Crushed tuba tuba seeds Petroleum ether Analytical balance Stop watch Beakers Stirring rods Rotary evaporator

B. Objective: To determine the optimum ratio of raw materials that will yield the desired property of oil extracted

C. Hypothesis: The appropriate ratio of raw materials provides the desired property of oil being extracted. D. Procedures:

1. Prepare five (5) sets of 30 g samples of combined crushed tuba tuba seeds and lumbang kernel of 1:1 ratio. 2. Place 90 mL of petroleum ether in each beaker. 3. Allow the samples to have contact in the solvent at a varying time (5, 10, 15, 20, and 25 minutes) respectively. 4. Separate the miscella from the mixture and record the initial volume. 5. Record the boiling point of the mixture. 6. Record the volume of both the oil collected and the recovered solvent. 7. Weigh the mass of cake. 8. Observe the appearance and compared the results.

E. Data and Results Variation of the Contact Time Time of Soaking (min) 5 10 15 20 25 Wt. of sample Used (g) 132.93 132.93 132.93 132.93 132.93 Vol.of solvent (mL) 399 399 399 399 399 Vol. of oil plus solvent (mL) 385.70 346.00 336.30 322.10 321.80 Boiling point (C) 65 68 72 71 75 Vol. of oil (mL) Vol. of recovered solvent (mL) 277.10 243.80 239.40 246.10 242.90 Wt. of cake (g) 174.67 176.57 174.89 172.76 174.36

46.80 53.10 55.30 56.03 54.60

F. Analysis: In this procedure, five different soaking times were used to determine the minimum time required to extract the maximum amount of oil from the samples.

In these results, the maximum amount of oil was obtained after 20 minutes (56.03 ml) but the result in the 15-min soaking time (55.30ml) is not very far from the maximum value. G. Conclusion: A minimum soaking time of 15 minutes is required the optimum amount of oil extracted in the extraction process.

H. Solvent Extraction Laboratory Scale Beaker, Rotary evaporator Plant Scale Evaporator, Condenser

III. Alkali Refining i. y Alkali Refining Variation of Refining Time

A. Materials and Apparatus: Materials and Apparatus Iron stand Sodium hydroxide Water Bunsen burner Stirrer Analytical balance Dropper Beaker Clamp

B. Objective: To determine the minimum time required to react any free fatty acids in the oil to the caustic solution

C. Hypothesis:

The minimum time required allows the complete reaction of any free fatty acids present in the oil to the caustic solution. D. Procedures: 1. Prepare 50.77 g oil 2. Prepare a caustic solution for 12 degrees Baume (8%w/w NaOH solution) 3. Add the 4 ml caustic solution to the oil 4. Mix for 5 minutes 5. Heat mixture to 55-60C (131-140F) as rapidly as possible 6. Allow the solution to be heated for 5 minutes. 7. Allow the soap to settle for 1 hour. 8. Suck the refined oil layer (top layer) out of the tank from the top down being careful not to remove any of the soap-stock that has settled to the bottom of the tank. 9. Wash the oil with warm water 10. Record the mass of the obtained oil 11. Repeat steps 1 to 10 with different reaction times: 10, 15, 20, 25 and 30 min and compare the results.

F. Data and Results Weight of oil (g) Variation of the Time of Mixing Vol. of Molarity Time of Mass of soap Caustic of mixing formed (g) solution (mL) Caustic (min) Solution 4.00 2.17 5 5.40 4.00 2.17 10 6.38 4.00 2.17 15 6.39 4.00 2.17 20 6.40 4.00 2.17 25 6.40 4.00 2.17 30 6.41 Mass of neutralized oil (g) 49.72 48.74 48.73 48.72 48.72 48.71

50.77 50.77 50.77 50.77 50.77 50.77

F. Analysis:

The oil obtained was proven to be acidic in nature. This is due to the presence of free fatty acids (FFA) in the solution. Based on the results, a minimum of 10 minutes is enough to neutralize most of the FFAs in the sample. A significant amount of soap was recorded. This is may be accounted to other mechanisms involved aside from neutralization such as hydration of phophatides by the water in the lye and adsorption of colour elements on to soap. Further neutralization results almost negligible changes in the mass of solutions which also indicates that the solution almost reach a pH of neutrality.

G. Conclusion: 10 minutes is the minimum time required to neutralize the oil sample given a specific amount of lye going to be add.

H.

Alkali Refining Laboratory Scale Beaker, stirring rod Plant Scale Neutralization Tank and Retention Mixer Centrifuge Centrifugal Separator

Bleaching A. Materials and Apparatus: Materials and Apparatus Neutralized oil Stirring rod Activated Carbon Analytical balance Bunsen burner Centrifuge

B. Objective: To determine the minimum amount of bleaching agent that will remove most of colour-carrying component of oil. C. Hypothesis:

The appropriate bleaching agent will removed most of colour-carrying component of oil. D. Procedures: 1. Prepare 48.74 g of neutralized oil 2. Add 1g of activated carbon and add to the neutralized oil 3. Heat the solution at 100 C 4. Centrifuge the solution to settle the activated carbon residues in the bottom. 5. Carefully separate the oil from the residue. 6. Repeat steps 2 to 5 using 2 and 3 g activated carbon 7. Record the weight and compare the results.

E. Data and Results

Mass of Bleaching agent (g) 1 2 3

Variation of mass of bleaching agent Mass of Temperature (C) Mass of bleached neutralized oil (g) oil (g) 48.74 100 47.99 48.74 100 48.05 48.74 100 47.98

Appearance

Clear Clear Clear

F. Analysis: The added activated carbon removes almost all the colour bodies present in the sample. This is due to the clear appearance exhibited by the oil. In the results, 1g of the bleaching agent is enough to adsorbed this elements. No further significant changes in the mass of the oil was obtained. G. Conclusion: 1g of activated carbon (approx.2% w/w of oil) remove significant amount of color material present in the oil. H. Bleaching Laboratory Scale Beaker, stirring rod Plant Scale Bleaching Tank

Washing A. Materials and Apparatus: Materials and Apparatus Neutralized oil Stirring rod Water Analytical balance Centrifuge

B. Objective: To determine the minimum amount of bleaching agent enough to remove most of colour carrying component of oil.

C. Hypothesis: The oil obtained may still contain contaminants from the neutralization and bleaching process

D. Procedures: 1. Prepare 47.99 g of neutralized oil 2. Add 5 ml of water and add to the neutralized oil 3. Centrifuge the solution to separate the oil and water 4. Record the weight and compare the results. 5. Repeat steps 2 to 3 for 2nd and 3rd trial E. Data and Results

Trial

1 2 3 F. Analysis:

Mass of neutralized oil (g) 47.99 47.99 47.99

Mass of washed oil (g)

Appearance

47.97 47.98 47.96

Clear Clear Clear

The purpose of this step is to remove the remaining soap stocks and activated carbon in the oil. A slight change in the mass of oil was observed. It signifies that contaminants in the oil are still present and should be eliminated.

G. Conclusion: The remaining contaminants in the oil from neutralization and bleaching process are removed through washing.

H. Washing Laboratory Scale Beaker, stirring rod Centrifuge Plant Scale Wash Tank Centrifugal Separator

Polymerization Variation of Time of Polymerization A. Materials and Apparatus Beakers (5) Stirring rod Thermometer Bunsen burner Rubber tubing Graduated cylinder Wire gauze Tripod

B. Objectives The purpose of this process is to determine the polymerization time that would gain higher volume of viscous product C. Hypothesis The final mass of the solution after the process will determine the optimum time of the polymerization. D. Procedures 1. Prepare the five set of 47.97-g samples. 2. Place them into different erlenmeyer flasks and allow them to heat up to 110oC. 3. Heat the sample in 30, 35, 40, 45, and 50 minute variation. 4. Observe the viscosity of the solution and record the recovered product mass.

E. Data and Results Weight of bleached oil (g) 47.97 47.97 47.97 47.97 47.97 F. Analysis: The polymerization reaction of the oil results the formation of water in the sample. Since the operating temperature exceeds the boiling temperature of water, they vaporize that results a decrease in the mass of oil. 40 minutes of the reaction shows that the mass of the oil starts to remain almost constant. This indicates that the reaction approaches to almost completion (47.65 ml). Polymerization in varying Time Time Weight of the sample (min) (g) 30 35 40 45 50 47.77 47.69 47.65 47.64 47.64 Observations

G. Conclusion: 40 minutes is the minimum time to complete the polymerization process. H. Polymerization Tank Laboratory Scale Beaker, stirring rod Plant Scale Polymerization Tank

REVIEW OF RELATED LITERATURE

RELATED LITERATURE

Tuba-tuba Jatropha curcas L. is found throughout the Philippines. In fact, different regions have their own common name for Jatropha. In the Tagalog region it is known as tubingbakod, tuba and sambo. Among the Bicolanos, it is called tuba and tuba-tuba; in

Pangasinan and Nueva Ecija, it is called tagumbao; tawa-tawa in Ilocos and kalunay in Cagayan Valley. In the Visayas and Mindanao, it is also known as tuba-tuba; kasla among the Ilonggos and tangan-tangan in Lanao region.

Jatropha is a drought resistant perennial shrub or small tree that has an economic life of up to 35 years and can live for 50 years. It grows fast, with little or no need for maintenance and can reach a height of 3 to 8 meters.

It has a smooth gray bark which exudes whitish color, watery, latex when cut. The size of the leaves ranges from 6-15 cm in length and width. The leaves are green to pale, alternate to sub-opposite with 3 to 5 lobes. It sheds leaves in the dry season and rejuvenates during rainy season.
Jatropha curcas is a tropical and subtropical plant. It grows almost anywhere even on sandy, gravelly and saline soils and does well on high temperatures. Jatropha is well adapted

to marginal soils with low nutrient content but the use of organic fertilizer would result to higher yield. Its water requirement is extremely low and can stand long periods of drought by shedding most of its leaves. It grows best when planted at the start of the rainy season.

Much research has been conducted on the composition and properties of Jatropha seeds by others ((Openshaw, 2000, 1-19), (Heller, 1996), (Henning, 2004) and (Sirisomboom, 7 A.D.)). These studies also provide insight in the

possibilities of using Jatropha oil for uel purposes. Knowledge of the physical and mechanical

properties of Jatropha is required for adequate design of machines for de-hulling, drying and pressing of the seeds. Restrictions on how to store the seeds are linked to these properties. Mechanical properties such as rupture force and energy required for rupturing fruit, nut and kernel provide insights on how to adapt the pressing process to Jatropha seeds. The seeds contain 27-40% oil (average: 34.4%). The seeds are also a source of the highly poisonous toxalbumin curcin.

Jatropha Curcas or "Tuba tuba" is a non-edible plant that grows mostly in tropical countries like the Philippines. Jatropha Curcas is resistant to drought and can easily be planted or propagated through seeds or cuttings. It starts producing seeds within 14 months, but reaches its maximum productivity level after 4-5 years. The plant remains useful for around 30-40 years. As potential source for biodiesel, the Jatropha plant can produce an oil content of 30-58%, depending on the quality of the soil where it is planted. Its seeds yield an annual equivalent of 0.75 to 2 tons of biodiesel per hectare. Based on a March 2006 study commissioned by the Department of Science and Technology (DOST), potential areas for jatropha plantation in the Philippines is at 2 million hectares. If farmers will be encouraged to plant even in field boundaries or hedges and to practice intercropping, a total of 5 million hectares can be utilized for the jatropha plant. With 1.1 million hectares dedicated to jatropha, 5.5 million metric tons (MMT) of biodiesel feedstock can be produced. Five million hectares can yield up to 25 MMT of biodiesel feedstock. At present, a total of 360 hectares of land are planted with Jatropha in the country, found in the following areas: 200 hectares in General Santos, 27 hectares in Camarines Sur, 120 hectares in Fort Magsaysay, Nueva Ecija, 5 hectares in Dacong Cogon, Negros Occidental, and aside from locally-grown jatropha in Quezon Province.

Lumbang

Lumbang is a large tree reaching a diameter of 80-150 cm with an average height of 24.0 m in the dense stand and 21.4 m in the open stand. The outer bark is grayish white, while the inner bark is reddish when cut and slightly exuding a reddish sap when wet.

The seeds are only about 3 cm long and 3.5 cm broad with 1 or 2 hand shells. The shell of the seed is very hard, rough, ridged and about 2.5 mm in thickness. Within the seed is a white, oily and fleshy kernel consisting of a very thin embryo surrounded by a large endosperm.

Lumbang is also grown in plantations as shade for growing plants. The wood is used in the manufacture of matches and wooden shoes. The juice of the nuts can be taken internally to eradicate worms. Its seeds serve as mild purgative.

Lumbang is found throughout the Philippines at low and medium altitudes in secondary forests. It is widely planted in the provinces of Cavite and Laguna. It apparently grows well in a variety of tropical climates. It grows in dry localities as well as in regions where rainfall is very heavy and in provinces where rainfall is fairly well distributed. In the Philippines, it grows in 6 provinces with climatic type 1 (6 months dry from November-April and the rest wet season) namely, Antique, Cavite, Laguna, Zambales, Cebu, and Davao.

Solvent Extraction

Solvent Extraction is a process which involves extracting oil from oil-bearing materials by treating it with a low boiler solvent as opposed to extracting the oils by mechanical pressing methods (such as expellers, hydraulic presses, etc.) The solvent extraction method recovers almost all the oils and leaves behind only 0.5% to 0.7% residual oil in the raw material. In the case of mechanical pressing the residual oil left in the oil cake may be anywhere from 6% to 14%. The solvent extraction method can be applied directly to any low oil content raw materials. It can also be used to extract prepressed oil cakes obtained from high oil content materials. Because of the high

percentage of recovered oil, solvent extraction has become the most popular method of extraction of oils and fats. Fat is one of the essential components of the human diet, therefore the demand for oils and fats are increasing with the in-crease in population and standards of living. Today large quantities of oil cakes such as peanut, cottonseed, linseed, kardiseed, neem, castor, mowha, copra, sunflower, etc. are extracted. Direct extraction of rice bran, salseed and soybean is also used. Solvent Extraction is basically a process of diffusion of a solvent into oil-bearing cells of the raw material resulting in a solution of the oil in solvent (www.srsbiodiesel.com/SolventExtraction.aspx). Alkali Refining

The nonglyceride components contribute practically all the colour and flavour to fats. In addition, such materials as the free fatty acids, waxes, colour bodies, mucilaginous materials, phospholipids, carotenoids, and gossypol (a yellow pigment found only in cottonseed oil) contribute other undesirable properties in fats used for edible and, to some extent, industrial purposes.

Many of these can be removed by treating fats at 40 to 85 C (104 to 185 F) with an aqueous solution of caustic soda (sodium hydroxide) or soda ash(sodium carbonate). The refining may be done in a tank (in which case it is called batch or tank refining) or in a continuous system. In batch refining, the aqueous emulsion of soaps formed from free fatty acids, along with other impurities (soapstock), settles to the bottom and is drawn off. In the continuous system the emulsion is separated with centrifuges. After the fat has been refined, it is usually washed with water to remove traces of alkali and soapstock. Oils that have been refined with soda ash or ammonia generally require a light re-refining with caustic soda to improve colour. After water washing, the oil may be dried by heating in a vacuum or by filtering through a dry filteraid material. The refined oil may be used for industrial purposes or may be processed further to edible oils. Usually, the refined oils are neutral (i.e., neither acidic nor alkaline), free of material that separates on heating (break material), lighter in colour, less viscous, and more susceptible to rancidity (www.britannica.com).

Quick Drying Oil

The drying oils can absorb oxygen and on exposure dry into thin elastic films. These oils are of importance in the paint and varnish industries.

RELATED STUDIES

Chemical Composition and Antioxidant Properties of Candlenut Oil Extracted by Supercritical CO2 (Siddique, B. M., et. al., 14 April 2011)

Candlenut oil was extracted using supercritical CO2 (SC-CO2) with an optimization of parameters, by the response surface methodology. The ground candlenut samples were treated in 2 different ways, that is, dried in either a heat oven (sample moisture content of 2.91%) or dried in a vacuum oven (sample moisture content of 1.98%), before extraction. An untreated sample (moisture content of 4.87%) was used as a control. The maximum percentage of oil was extracted from the heatoven-dried sample (77.27%), followed by the vacuum-oven-dried sample (74.32%), and the untreated sample (70.12%). At an SC-CO2 pressure of 48.26 Mpa and 60 min of extraction time, the optimal temperatures for extraction were found to be 76.4 C, 73.9 C, and 70.6 C for the untreated, heat-oven-dried, and vacuum-oven-dried samples, respectively. The heat-oven-dried sample contains the highest percentage of linoleic acid, followed by the untreated and vacuum-oven-dried samples. The antiradical activity of candlenut oil corresponded to an IC50 value of 30.37 mg/mL. Crude Candlenut Oil Ethanolysis to Produce Renewable Energy at Ambient Condition (Sulistyo, H., et. al., 20-22 October 2009)

Transesterification reaction of crude candlenut (aleurites moluccana) oil with ethanol to form fatty acid ethyl ester by using a potassium hydroxide as catalyst was studied. Experiments were performed at ambient condition. The

operation variables employed for transesterification were ethanol to oil molar ratio and catalyst concentration. The objective of the present investigation was to produce a renewable energy that the ethyl ester formed was used as biodiesel. Pretreatment process was undertaken to reduce the free fatty acid to less than 2% by esterification with ethanol. The optimal triglyceride conversion was attained by using ethanol to oil ratio of 7.5:1, potassium hydroxide as catalyst was of 1.50%. Ethyl ester formed was characterized by its density, viscosity, cloud and pour points. The ethyl ester viscosity of 5.593 cSt was close to the viscosity of diesel oil of 5.8 cSt, and other properties have also similar to those of diesel oil.

Solid Liquid Extraction of Jatropha Seeds by Microwave Pretreatment and Ultrasound Assisted Methods (Sayyar, S., et. al., 28 May 2011)

Jatropha curcas has a variety of uses which are of great economic significance. Jatropha oil can be used as fuel alternative and for making biodiesel that is supposed to overcome the source limitation problem. In this study, conventional, ultrasound assisted and microwave pretreatment solid liquid extraction of Jatropha seed were studied in terms of amount and quality of the extracted oil. The free fatty acid content which is an important oil quality index was also investigated for the obtained oil. Both ultrasonication and microwave pretreatment of the seeds had a positive effect on amount of yield. However, by application of ultrasound, more oil could be extracted compared with that obtained by conventional and microwave pretreatment extraction methods. The maximum amount of oil which could be extracted by conventional, ultrasound assisted and microwave pretreatment methods were 47.33, 51.4 and 49.36%, respectively. Regarding the quality, oil extracted by conventional, ultrasound assisted and micmicrowave pretreatment extraction methods did not show any significant difference in terms of Free Fatty Acids (FFA) content.

COMPARISON OF RELATED STUDIES

UNIQUENESS OF THE STUDY The study Extraction of Linoleic Acid from Tuba tuba (Jatropha curcas Linn.) and Lumbang (Jatropha Mollucana Linn.) for the Production of Quick Drying Oil via Addition Polymerization is considered unique due to the reason of utilizing main raw materials which are tuba-tuba and lumbang seeds which have not been used before for the production of quick drying oil.

Different studies were tied with careful analyses of researches and methodical experimentations. Various parameters were taken into account to suit the properties of the raw materials and to achieve the optimum operating conditions. Solvent extraction was used in obtaining the oil from the raw materials that is then alkali refined to produce quick drying oil.

CONCEPTUAL FRAMEWORK

PROJECT STUDY

MARKET STUDY

TECHNICAL STUDY

CONCLUSION and RECOMMENDATION

FINANCIAL STUDY ANALYSIS OF THE CONCEPTUAL FRAMEWORK

The research aims to design a manufacturing process for the production of Quick Drying Oil from the utilization of lumbang and jatropha oil for industrial applications. In the market study historical data of demand and supply of Linseed oil was taken from 2004-2010 in line for the projection of values in the next six years. The projected values were the basis for computing the market share, plant rated capacity and daily production capacity. Market study also includes all the most effective marketing strategies, programs, advertisement, promotions and the like. For the technical study, the raw material lumbang and jatropha seeds were introduced. Material balances were calculated based on from the values obtained from all the parameters tested in the experiment. It also takes into consideration the ideal parameters that were chosen in each process. Equipment design, piping system, instrumentation and process control, safety measures, plant location, wastewater treatment were also included in the technical study. The financial study covers the balance sheet, the cost of the equipment designed, and total production cost.

PROJECT STUDY CONCLUSION