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

Washing Project Design Proposal

Date Submitted: April 11, 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 generate the electric field. 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 and the alternative electric field method will be used to purify 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.

ENGR-103 Freshman Design Proposal

Section 075, Group 01

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 triglycerides present in the oil feedstock down 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. 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 water. This concepts viability was explored 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 A blog will be created on the Internet and updated weekly to track progress. Three types of

refined biodiesel will be produced. The first type will be washed with conventional distilled water, and the second type will be refined using only electrolysis. The third type will be purified using electrolysis and distilled water washing. Each sample will be chemically analyzed to determine the efficiency of these methods. An assembly used to conduct electrolysis will be constructed. A final presentation and report will be compiled that summarizes and evaluates the project.

ENGR-103 Freshman Design Proposal 3 Technical Activities

Section 075, Group 01

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 three gallons of oil feedstock will be obtained from local restaurants. If needed, initial purification of the feedstock will be conducted. These pretreatment methods may involve filtration, if solid or other material is present, water removal, by drying or absorption, and determining the feedstocks free fatty acid (FFA) content. After initial processing, reagents will be prepared for the experimental process phase. The quantities of the reagents will depend on the condition of the feedstock after pretreatment. Pure methanol or HEET, gas-line antifreeze, will be used as the alcohol for the reaction. The base catalyst will be sodium hydroxide (NaOH) or Drano, liquid clog remover. Excess amounts of methanol and sodium hydroxide in fuel can be harmful to engines; therefore calculations will be done to determine specific amounts of reagents that will be used. If pure reagents cannot be obtained then generic products that contain high percentages of methanol and sodium hydroxide (i.e. HEET and Drano) will be used. Other chemical compounds in these products and their effects in the reaction will then have to be considered. 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 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 three wooden blocks, and serve to 2

ENGR-103 Freshman Design Proposal

Section 075, Group 01

ensure uniform electrodes for the experiment. This will be done by gluing two smaller wooden blocks on top of a larger block with a gap 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 sodium

hydroxide (base catalyst). This mixture will need to be stirred until all of the sodium hydroxide dissolves in the methanol. This will form a methoxide solution which will then be mixed with the processed oil feedstock at a high temperature. During the reaction, methoxide will combine with the triglycerides contained in the pretreated oil feedstock. The mixture will be left to react 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 rise to the top of the mixture, while the glycerol will settle to the bottom. The crude biodiesel will be decanted from the mixture and taken out of the reaction vessel.

ENGR-103 Freshman Design Proposal 3.3 Purification of Crude Biodiesel

Section 075, Group 01

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. The soap from each sample will be removed by filtration. Once washed, all three mixtures will then be heated and dried to remove excess water from the biodiesel. These processes will take approximately three days to complete. 3.4 Final Testing of Product The quality of the produced biodiesel will be determined by tests based on purity, viscosity, distillation temperature, and cetane number. 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]

. According to these

standards the biodiesel must not contain more than 0.24% glycerin. Too much glycerin indicates that the reaction did not work or that the crude biodiesel was not properly washed. The biodiesel cannot exceed a maximum of 0.05% water. If this reading is high, then the fuel was not properly dried. 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. The biodiesel will have a maximum distillation temperature of 182.22 C. Exceeding this point in the

distillation process means there is oil in the sample. Biodiesel must also have a minimum cetane number of 47. This is a measure of how well the fuel will ignite. 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.

ENGR-103 Freshman Design Proposal 4 Project Timeline

Section 075, Group 01

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

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 Gloves, safety glasses and lab coats. Burette and burette stand Test tubes Work space

Items that may need to be acquired elsewhere are listed below: High Voltage Power Supply Small centrifuge An ohmmeter (to measure resistance) An ammeter (to measure current) A fume hood 5

ENGR-103 Freshman Design Proposal

Section 075, Group 01

The chemicals that will be needed to produce the reaction are: Sodium hydroxide (NaOH) or Drano (as an equivalent) Methanol or HEET (as an equivalent) Soybean oil/canola oil/vegetable oil/grease Distilled Water

Other essential materials that are needed for the project include: Aluminum foil Mechanical pencil lead (graphite) Wood blocks (for apparatus construction) Toothpicks Epoxy (or a similar acting adhesive)

Expertise Knowledge of basic circuit theory Use of machine tools (i.e. band saw, centrifuge) Analytical Chemistry o Basic stoichiometry Information Literacy o Finding good information of the topic Biodiesel Production o Feedstock pretreatment o Determination and treatment of free fatty acids 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

ENGR-103 Freshman Design Proposal 7 Budget

Section 075, Group 01

The budget was composed under the assumption that no 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 $238.00 $296 $20.00 $33.00

TOTAL

$587.00

Table 2 - Freshman design project budget.

7.1

Basic Lab Equipment Item Graduated cylinders Beakers Erlenmeyer flasks Magnetic stirrers Stirrer plate (with heating component) Reaction vessels (sealable plastic containers) Filter paper Funnels Gloves, safety glasses, and lab coats Burette and burette stand Test Tube
Table 3 - Essential Lab Equipment

Cost $5.00 $20.00 $18.00 $0.00 $86.00 $0.00 $11.00 $5.00 $20.00 $55.00 $18.00

The above lab equipment is essential. They will be needed for every step of project.

ENGR-103 Freshman Design Proposal 7.2 Advanced Lab Equipment

Section 075, Group 01

Item Paso Scientific Model SF9585 High Voltage Power Supply Small centrifuge An Ohmmeter (to measure resistance) An ammeter (to measure current)
Table 4 - Advanced Lab Equipment

Cost $150.00 $120.00 $20.00 $6.00

These items will be used during the purification steps of the experiment. 7.3 Chemicals Item Sodium hydroxide (NaOH) or Drano (as an equivalent) Methanol or HEET (as an equivalent) Soybean oil/canola oil/vegetable oil/grease Distilled Water
Table 5 - Chemicals

Cost $10.00 $10.00 $0.00 $0.00

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)
Table 6 - Other Material

Cost: $33.00

$0.00

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

ENGR-103 Freshman Design Proposal 8 References

Section 075, Group 01

[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