ENGR 103 - Spring 2013 Freshman Engineering Design Lab Biodiesel Fuel Purification Through Electric Field Assisted

Washing Project Design Proposal

Date Submitted: April 29, 2013

Submitted to:

Kenneth Lau, klau@drexel.edu Nathan Taylor, nt65@drexel.edu

Group Members:

Esmail Hamidi, egh35@drexel.edu Blake Piccolo, bmp62@drexel.edu Louis Sacks, las464@drexel.edu Dong Zhao, dz92@drexel.edu Jiaqi Zhou, jz442@drexel.edu

Abstract Conventional methods of biodiesel fuel purification involve washing with distilled water. An alternative method of purification uses electric field assisted washing. Precipitate composed of soap and excess catalyst, by-products of transesterification, are formed when the biodiesel fuel is subjected to an electric field. Electrolysis will serve as the technique to precipitate excess material. An apparatus will be built to conduct electrolysis on the crude biodiesel. Firstly, crude biodiesel will be synthesized from an oil feedstock. Conventional water washing, the alternative electric field method, and a combination of the two methods will be used to purify six biodiesel fuel samples. The samples will be tested according to the American Society of Testing Materials (ASTM) D 6751-11a Standard [1] to determine the quality of the samples. A final report and presentation will be generated to discuss results.

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Introduction Biodiesel is a fuel composed of long-chain alkyl esters. An alternative to conventional

diesel fuel, made using fossil fuels, biodiesel is made by reacting lipids (animal fats and vegetable oils) with an alcohol. This breaks triglyceride compounds present in the oil feedstock into various alkyl esters and glycerol. In the process of making crude biodiesel, glycerol and excess reagent remain in the mixture. Before biodiesel is suitable for use in a diesel engine, it must be purified of these unwanted contaminants. Conventional biodiesel production uses distilled water washing to rid the mixture of these contaminants. The water is poured off and the mixture is then dried with heat. This process is repeated at least five to ten times per sample of crude biodiesel. A downside of this process is that making and transporting large quantities of distilled water is expensive. The goal for this project is to modify the purification process, using electrolysis as an alternative to the common method of distilled water washing. An apparatus can be constructed out of two electrodes, a high voltage power supply, and a jig (Figure 1). By applying current to the crude biodiesel, positively charged soaps and excess reactants are pulled out of solution and precipitate on the electrodes. From this process refined biodiesel will be produced using less or no water. This concepts viability was proven by NASA in a 2010 patent [2]. This process can save water and increase the yield of refined biodiesel. It can even be applied to large-scale manufacture. This project is designed to explore the capabilities of electrolysis both alone and used in conjunction with distilled water washing.

Deliverables Three types of refined biodiesel will be produced. The first type will be washed with

conventional distilled water as a control, and the second type will be refined using electrolysis. The third type will be purified using electrolysis and distilled water washing. Each sample will be analyzed to determine the efficiency of these methods. For samples washed with distilled water, the volume of water used will be translated into a cost. For samples purified by electrolysis, the power consumption will be recorded.

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An assembly used to conduct electrolysis will be constructed. A blog will be created using Blogger and updated weekly to track progress and display final results. A final presentation and report will be compiled that summarizes and evaluates the project. The project will be evaluated based on the quality of fuel produced and the cost-effectiveness of the methods used.

Technical Activities Major tasks of the project are divided into five categories: Initial Preparations, Crude

Biodiesel Production, Purification, Final Product Testing, and Final Report Preparation. Initial preparations of the project include background study, obtaining the oil feedstock, processing the feedstock, and preparing the experimental setup. The production of crude biodiesel involves the process of transesterification. Purifying the crude biodiesel contains multiple steps where three different washing methods will be used to produce samples. Testing the refined biodiesel samples will determine the success of the experiment. A final report and presentation will then be developed to compare results. 3.1 Initial Preparations Background research will be done on the process of biodiesel production. About one gallon of used canola oil feedstock will be obtained from a local Chick-fil-A restaurant. Initial purification of the feedstock will be conducted. Pretreatment methods will involve filtration through a Buchner funnel if solid material is present and determination of the feedstocks free fatty acid (FFA) content by a titration experiment. After initial processing, reagents will be prepared for the experimental process phase. The quantities of the reagents will depend on the feedstocks FFA content. Pure liquid methanol will be used as the alcohol for the reaction. The base catalyst will be solid potassium hydroxide. Calculations will be done to determine specific amounts of reagents that will be used. An excess amount of potassium hydroxide will be used to ensure that the reaction goes to completion. Lab space for the experiment and specific lab equipment will be needed. The lab equipment needed for the experiment can be found in section 5, Facilities and Resources. 3.1.1 Circuit Configuration and Experimental Setup of Electric Field Washing Device An electric field washing device will be constructed and used in the purification process of the biodiesel (Figure 1). The device will contain carbon electrodes made from mechanical 2

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pencil lead (graphite sticks) and aluminum foil, held together by a constructed jig. Epoxy will hold the graphite sticks together. The jig will be made out of a wooden block and serve to ensure uniform distance between electrodes for the experiment. This will be done by drilling two holes into the block, each with a diameter equal to the width of the electrodes. An ohmmeter will be used to measure resistance to detect for breaks in the electrodes. The electrodes will be

connected to a high voltage power supply and an ammeter to measure the amount of current that will flow between the electrodes.

Figure 1 Electric Field Washing Device [2]

3.2

Crude Biodiesel Production The transesterification reaction begins with the mixing of methanol (alcohol) and

potassium hydroxide (base catalyst). This mixture will need to be stirred until all of the solid potassium hydroxide dissolves in the methanol. This will form a methoxide solution which will then be mixed with the processed oil feedstock. During the reaction, methoxide will combine with the triglycerides contained in the pretreated oil feedstock. The mixture will be left to react in a water bath shaker at a temperature of 40C for approximately 14 hours. During this time the glyceride chains will be cut off and replaced with the alcohol, producing glycerol and methyl esters as a by-product
[3]

. The methyl esters will be the crude biodiesel and are expected to be

less viscous than the triglycerides. Once completed, the crude biodiesel will be placed in a

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separating flask, where it will rise to the top of the mixture. The glycerol will settle to the bottom and then drained from the mixture. 3.3 Purification of Crude Biodiesel The crude biodiesel will contain excess catalyst and soap formed from the transesterification reaction. Three different washing methods will be used to purify three

samples of the synthesized crude biodiesel into biodiesel fuel. The control method will consist of washing by use of heated distilled water only. The second method will only involve the use of the electric field washing device and no distilled water will be added. The third method will include the use of both washing by heated distilled water and with the electric field washing device. Once thoroughly washed, all three mixtures will then be heated and dried to remove excess water from the biodiesel. complete. 3.4 Final Testing of Product The quality of the produced biodiesel will be determined by tests based on clarity, purity, and viscosity. The results of the tests will be compared to the American Society of Testing Materials (ASTM) D 6751-11a Standard: Standard Specification for Biodiesel Fuel (B100) Blend Stock for Distillate Fuels
[1]

These processes will take approximately two weeks to

. According to these standards the biodiesel must not contain

more than 0.24% glycerin. Too much glycerin indicates that the reaction went in reverse or that the crude biodiesel was not properly washed. By mixing biodiesel samples with methanol, the 3/27 test
[4]

will show if there is any trace of triglyceride present by a chemical reaction. The

biodiesel cannot exceed a maximum of 0.05% water. If this reading is high, then the fuel was not properly dried and will appear cloudy or turbid. If a newspaper can be read through the biodiesel sample then it is fit to put into an engine
[5]

. The biodiesel will have a viscosity limit

between 1.9-6.0 cst at 40 C. If the biodiesel is too thick, then there is an excessive amount of feedstock still present in the fuel. This test will be conducted with the aid of a viscometer. Additionally the Cold Soak Filtration Test
[6]

will determine if the biodiesel works in cold

climates. When biodiesel is chilled, as in cold climates, High Melting Point Esters (HMPE) are sometimes formed. HMPEs have high melting points, and therefore will not melt back into the fuel at room temperature. In the test the biodiesel samples will be cooled for 16 hours at 40 F,

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warmed to room temperature, and then filtered using a Buchner funnel. If all of the fuel does not pass through the funnel within 6 minutes then it will clog fuel filters. 3.5 Final Report Preparation After testing has been conducted, a final report and presentation deliverable will be made. The final report will thoroughly document the progress and end results of the project. The presentation will be based on the material within the final lab report.

Project Timeline
Week Task 1 x 2 x 3 x x x x x x x x x x x x x x x x x x 4 5 6 7 8 9 10

Background/Procedure Study and Obtain Materials Construction of Electric Field Washing Device Crude Biodiesel Production Purification of Crude Biodiesel Testing of Biodiesel Samples Final Report/Presentation Preparation

Table 1 - The project timeline is divided into six major parts: Background/Procedure study and obtaining materials, Crude Biodiesel Production, Purification, Testing of Biodiesel Samples, and Final Report/Presentation Preparation

Facilities and Resources Research space, lab equipment, specific chemicals, and other materials will be needed to The research space should come stocked with the following lab

complete the project. equipment:

Graduated cylinders Beakers Erlenmeyer flasks Magnetic stirrers Stirrer plates (with heating component) Reaction vessels (seal-able plastic containers) Filter paper Funnels 5

ENGR-103 Freshman Design Proposal Gloves, safety glasses and lab coats. Burette and burette stand Test tubes Work space

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Items that may need to be acquired elsewhere are listed below: High Voltage Power Supply Multimeter (to measure current and resistance) Water bath shaker Viscometer

The chemicals that will be needed to produce the reaction are: Sodium hydroxide (NaOHaq) Potassium hydroxide Methanol Used canola oil Distilled Water Phenolphthalein indicator Isopropyl alcohol Toluene

Other essential materials that are needed for the project include: Aluminum foil Mechanical pencil lead (graphite) Scrap wood (for apparatus construction) Epoxy Alligator clips

Expertise Knowledge of basic circuit theory Use of machine tools (i.e. band saw) Analytical Chemistry o Basic stoichiometry Information Literacy o Finding good information of the topic 6

ENGR-103 Freshman Design Proposal Biodiesel Production o Feedstock pretreatment

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o Determination and treatment of free fatty acids through titration o Reactions involved in synthesis process (i.e. transesterification) o Product purification methods Basic Use of Laboratory Equipment o Laboratory analysis o Safety in the laboratory Environmental Awareness Microsoft Office

Budget The budget was composed under the assumption that lab equipment would be provided. It

was split into four main sections: Basic lab equipment, advanced lab equipment, chemicals, and other materials. Category Basic lab equipment Advanced lab equipment Chemicals Other Materials Projected Cost $0.00 $200.00 $0.00 $26.25

TOTAL

$226.25

Table 2 - Freshman design project budget.

7.1

Basic Lab Equipment Item Graduated cylinders Beakers Erlenmeyer flasks 7 Cost $0.00 $0.00 $0.00

ENGR-103 Freshman Design Proposal Magnetic stirrers Stirrer plate (with heating component) Reaction vessels (sealable plastic containers) Filter paper Buchner funnel Gloves, safety glasses, and lab coats Burette and burette stand Test tubes
Table 3 - Essential Lab Equipment

Section 075, Group 01 $0.00 $0.00 $0.00 $0.00 $0.00 $0.00 $0.00 $0.00

The above lab equipment is essential. They will be needed for every step in the project. 7.2 Advanced Lab Equipment

Item Pasco Scientific Model SF9585 High Voltage Power Supply Multimeter Viscometer Water bath shaker
Table 4 - Advanced Lab Equipment

Cost $100.00 $0.00 $100.00 $0.00

These items will be used during the purification steps of the experiment. 7.3 Chemicals Item Sodium hydroxide (NaOHaq) Liquid Methanol Used canola oil Distilled Water Phenolphthalein Potassium Hydroxide (KOH) Isopropyl Alcohol Toluene
Table 5 - Chemicals

Cost $0.00 $0.00 $0.00 $0.00 $0.00 $0.00 $0.00 $0.00

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These chemicals will be used as basic reagents in the experiment. 7.4 Other Materials

Item Aluminum foil Mechanical pencil lead (graphite) Wooden blocks (for apparatus construction) Epoxy adhesive material 3 16 gauge double wiring material Alligator clips
Table 6 - Other Material

Cost: $6.00 $10.25 $0.00 $3.00 $3.00 $4.00

These materials will be used to construct the electrodes and the apparatus. 8 References

[1]

Utah Biodiesel Supply. (2013). ASTM Tests Explained [Online]. Available: http://www.utahbiodieselsupply.com/astmtests.php

[2]

T. Abdel-Fattah, A.C. Siochi, A.L.J. Siochi, E.J. Siochi, W.T. Yost, Method for Purifying Biodiesel Fuel, Patent 20100212219, Aug. 26, 2007. Available: http://www.faqs.org/patents/app/20100212219

[3]

K. Lau. (2013, April 5). ENGR 103: Biofuels & Biodiesel. Available: PDF

[4]

M. Alovert. (2012). The 3-27 Conversion Test [Online]. Available: http://make-biodiesel.org/Quality-Testing/the-3-27-conversion-test.html

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[5]

Rickdatech. (2012). The Important Tests Testing Finished biodiesel for water [Online]. tests.html Available: http://make-biodiesel.org/Quality-Testing/the-important-

[6]

Rickdatech. (2012). Cold Soak Filtration Test [Online]. Available: http://make-biodiesel.org/Quality-Testing/cold-soak-filtration-test.html

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