KAUTILYA INSTITUTE OF TECHNOLOGY & ENGINEERING

JAIPUR

Session 2013-2014A Synopsis

On

EXTRATION OF BIODIESEL FROM SOYBEAN OIL AND INVESTIGATE EMISSIONS PARAMETER ON A SINGLE CYLINDER

DIESEL ENGINE

Submitted to: - Submitted by:-Mr. Rakesh Mahavar Sonu Pareekh Mechanical engg. Dept. Shashank Pathak Ram Naresh Suthar Pooran Mal Yadav

Mechanical Engineering Department Kautilya Institute of technology & Engineering

ACKNOWLEDGEMENT

It is really matter of great pleasure for me to present this creative and practical work. Project which is important part of learning and every engineering student prepares it in final year of his B.tech.

In preparation of this report I have received encouragement and support from various persons. I would like to express my helpful thanks and gratitude to all of them.

I am thankful

TO Mr. Rakesh mahavar (Asst. prof. ME department) for guiding me for preparation of this report.

Thank you

ABSTRACT

Due to limited resource of fossil fuel and high rise in the demand of them the need for

alternative fuels is all time high. Where countries are trying to find the best alternative fuel

and to encourage the domestic production of fuels for self efficiency.

The article gives a condensed overview of biodiesel extraction from cotton

seed oil with caliberation in their catalyst content and alcohol content, viscocity, density,

flash point, fire point, calorifc value and abopve all cost efficiency are measured and

determined. The process of conversion of vegetable oil into biodiesel employed is

transesterification. And the production method employed is base catalyzed. Alcohol used for

this process is methanol and a base catalyst catalyst is used for the prcess i.e. potassium

hydroxide (KOH). The paper tries to throw some light on the best and most biodiesel

obtaioned with varitions in the amount of catalyst and alocohol with the help in iteration

process of finding out the best combination for maximum biodiesel and less amount of

residual substitute.

INTRODUCTION

In todays world where the population is increasing marginally and the demand to have

automobiles is also at all time high and further only going to increase. With tthis scenario the

demand of fossil fuel and its consumption is increasing exponentialy and is a matter of

concern for developing countries who are not self sufficient. Vegetable oil is the most desired

alternative fuel available at the present scenario and in near coming future. Also the pollution

caused by the combustion of these fossil fuels is a major concern for the enviroment and the

search of alternative fuel has gained much importance.

Biodiesel is also named as Methyl Esters. Methyl esters are clean burning fuel with no

sulfur emission. Although its heat of combustion is slightly lower than that of the petro-

diesel, there is no engine adjustment necessary and there is no loss in efficiency . Methyl

esters are non-corrosive and are produced at low pressure and low temperature conditions.

Direct use of vegetable oils or animal fats as fuel can cause numerous engine

problems like poor fuel atomization, incomplete combustion and carbon deposition

formation, engine fouling and lubrication oil contamination, which is due to higher viscocity.

Through this paper we try to make the idea of biodiesel more feasible by running

some iterations in the production process of biodiesel from cotton seed oil. The process used

for the production is transestrification metchod. The production process involved is base

catalyzed and the alcohol used in the production is methanol as it is cheap and provides better

and has easy recovery. The catalyst being used in this process is potassium hudroxide (KOH).

EXPERIMENTAL SETUP

The experimental setup is shown in figure 1. A 2000 ml three-necked round-bottomed flask

was used as a reactor. The flask was placed in a water bath, whose temperature could be

controlled within + 2 oC. One of the two side necks was equipped with a condenser and the

other was used as a thermowell. A thermometer was placed in the thermowell containing

little glycerol for temperature measurement inside the reactor. A blade stirrer was passed

through the central neck, which was connected to a motor alongwith speed regulator for

adjusting and controlling the stirrer speed. Esterification: A known amount of Cottonseed oil

was taken in the above-mentioned setup. Required amount of sulphuric acid and methanol

were added to the oil and stirred continuously maintaining a steady temperature of 640C.

Intermittently samples were collected at regular intervals (30min) and acid value was

determined. After the confirmation of complete reduction of acid valve to less than 1.0, the

heating was stopped and the products were cooled. The unreacted methanol was separated

by separating funnel. The remaining product was analyzed for acid value and it was found

that the acid value varied from 1.0 to 0.5. This oil sample was for transesterified to obtain

methyl esters. Transesterification: In the same setup, known amount of esterified

Cottonseed oil was charged. Required amount of catalyst NaOH was desolved in methanol

and the rest amount of methanol alongwith the catalyst solution was added to the oil

sample. After proper closing of the flask it was put on the water bath.The system was

maintained airtight to prevent the loss of alcohol. The reaction mix was maitained at

temperature just above the boiling point of the alcohol i.e. around 70°C to speed up the

reaction rate.

Excess alcohol was used to ensure total conversion of the oil to its esters. The formation of

methyl ester was monitered by using thin layer chromatography (TLC) technique. Coated

silicagel glass plates were spotted with Cottonseed oil and the sample of ester. The spotted

samples were developed in solvent system in glass chamber using solvent ratio of 80:20

hexane/ether by volume. This confirms the formation of methyl esters. This procedure was

followed for all the samples collected at regular interval of time to check the formation of

methyl ester. After the confirmation of completion of methyl ester formation, the heating

was stopped and the products were cooled and transferred to a separating funnel. Where

the ester layer containing mainly methyl ester and methanol and glycerol layer containing

mainly glycerol and methanol were separated. The pH level of both layers were measured

and neutralised seperately. For neutralisation a known amount of sulfuric acid in methanol

was added to both the layers seperately to neutralize the sodium methoxide present in

them. The traces of methanol present in ester layer was recovered in a distillation column

under control vacuum. Distilled methanol was weighed and stored in sample bottle. Similar

procedure was adopted to recover the traces of methanol present in glycerol layer. The

methyl ester was washed and dried under vacuum to remove traces of moisture. A sample

of esters were analyzed for acid value by using standard AOCS procedures for

standardization. The sample of glycerol layer was analyzed for glycerol content by using

AOCS procedure. The glycerol content was found from 80 to 85 %.

TRANSESTERIFICATION PROCESS

The most common way of producing biodiesel is the transesterification of vegetable

oils and animal fats . Oil or fat reacts with alcohol (methanol ). This reaction is called

transesterification. The reaction requires heat and a strong catalyst (alkalis, acids, or

enzymes) to achieve complete conversion of the vegetable oil into the separated esters and

glycerin. The reaction is shown below:

A major problem in carrying out the alcoholysis of oil is to limit the presence of water

and free fatty acids (FFA) in the oils. The excess presence of FFA may lead to formation of

soap in presence of certain catalyst, hence decreasing the yield, as shown by the following

reaction.

CATALYST

Transesterification reaction can be catalyzed byboth homogeneous (alkalies and acids) and

heterogeneous catalysts. The used alkali catalysts are NaOH, CH3ONa, and KOH for

producing biodiesel13,14. The alkali-catalyzed transesterification of vegetable oils proceeds

faster than the acid-catalyzed. But the use of base catalyzed transesterification is only limited

to oil having low water and FFA content. This reaction is the most widely used process for

production of biodiesel worldwide. To keep check on the water and FFA content of the oil,

they are first pretreated with an acid catalysed transesterification process, which converts the

FFA to esters.

MATERIALS AND METHODS

1. COTTON SEED OIL

India is fifth largest cotton producing country in the word, the first-four being the U.S,

China, Russia, and Brazil. Our country produces about 8-9% of the world cotton .

Cottonseed oil has a red–brown color because of the presence of pigments, the most

important being gossypol. Gossypol is known to have antioxidant properties that may

potentially increase the shelf life of the oil and biodiesel .

CSO a rich vegetable oil obtained from the seeds of the cotton plant (Gossypium) by

pressing or extraction. The specific component of CSO is the pigment gossypol. The

gossypol content determines the color and quality of the oil. The darker the color and the

more stable is the biodiesel . Unrefined cottonseed oil is a reddish brown liquid,

sometimes almost black in color, with a unique odor and bitter taste.

2. ALCOHOL

In transesterification reaction, an alcohol in the presence of catalyst lyses oil into

methyl esters and glycerol. The commonly used alcohols for the transesterification include

methanol, ethanol, propanol, butanol, and amyl alcohol. Ethanol and methanol is commonly

used for transesterification. Methanol is widely used for producing biodiesel compared to

other alcohols, as it is not expensive, Prevent soap formation, its reactivity is high even

methanol recovery is comparatively easier.

3. CATALYST

Based on the use of catalyst the transesterification can be divided in to three

types, they are acid catalyzed, base catalyzed and enzyme catalyzed method. In the

case of base catalyst potassium hydroxide (KOH) or sodium hydroxide (NaOH) are

used, because it is less expensive, easy to handle in storage and transport.

Transesterification reaction can be catalyzed byboth homogeneous (alkalies

and acids) and heterogeneous catalysts. The used alkali catalysts are NaOH,

CH3ONa, and KOH for producing biodiesel. The alkali-catalyzed transesterification

of vegetable oils proceeds faster than the acid-catalyzed. But the use of base catalyzed

transesterification is only limited to oil having low water and FFA content. This

reaction is the most widely used process for production of biodiesel worldwide. To

keep check on the water and FFA content of the oil, they are first pretreated with an

acid catalysed transesterification process, which converts the FFA to esters.

CALCULATION OF CATALYST AND ALCOHOL

Amount of catalyst and alcohol to be added depends on the FFA value.

Methanol: For 1 liter of vegetable oil 200 ml of methanol is added.

NaOH is added based on FFA as given in below table 1.

To calculate FFA% from a titration value the formula is: FFA%=28.2∗0.1N NaOH∗Burette

readingW Where, Burette Reading: Volume in ml of titration solution. N is the normality of

the titration solution (0.1 gram/liter). W is the weight of the sample of oil in grams (10

grams). 28.2 is the molecular weight of oleic acid divided by ten.

Table 1: Calculation of NaOH based on FFA

FFA AMOUNT OF NAOH IN GMS.01234

PREPARATION

1. WASHING OF PRODUCTS

After transesterification the upper ester layer may contain traces of NaOH,

methanol and glycerol. Since the remaining unreacted methanol in the biodiesel has

safety risks and can corrode engine components, the residual catalyst (NaOH) can

damage engine components, and glycerol in the biodiesel can reduce fuel lubricity

and cause injector coking and other deposits. [2].These being water soluble is

removed by washing (4-6 times) the biodiesel with water maintained at 40-50ºC as

shown in fig 2. Washing is carried out by spraying hot water over the biodiesel;

precautions were taken to avoid soap formation.

2. HEATING PRODUCTS

After the completion of washing process the biodiesel may contain some

traces of water. Biodiesel is heated to 1100C to remove the trapped traces of water.

3. YIELD OF BIODIESEL BY TRANSESTERIFICATION

The main objective is biodiesel production from vegetable oil. In the present

study the vegetable oil was successfully converted into biodiesel by transesterification

process using base catalyst. We could obtain around 70% biodiesel yield from both

cotton seeds and mahua seeds and 80% from neem seeds respectively by base

catalyzed method. The biodiesel yield for different batches was presented in table 2,

table 3 and table 4. The main factors affecting the transesterification are FFA, reaction

time, temperature, amount of alcohol and catalyst, catalyst concentration, and rate of

mixing. It was observed, FFA increases if the precaution is not taken to store the

vegetable oil. Since higher amount of FFA can directly react with the base catalyst to

form soaps, and prevents separation of the biodiesel from the glycerol and decrease

the yield, it is better to select reactant oils with low FFA content, or reduce FFA by

some means. Experiment was conducted at the FFA range of 3 to 4.6 for cotton, 1.5 to

3 for mahua and 2 to 3.5 for neem seeds. It was found during experiment that

separating glycerol from cotton seed biodiesel was bit difficult because both are dark

in color.

Table 2. Yield of Biodiesel by transesterification (CSOME)

BATCH

FFA

CSO(ml.)

Glycerol(ml.)

Biodiesel from washing(ml.)

Biodiesel after washing(ml.)

Biodiesel after heating (ml.)

IIIIIIIVVVIVIIVIII

Conclusion

I am thankful to the Mr. rakesh mahavar to provide me to provide me chance for

producing own bio diesel and enhance my knowledge in I.C. engine field.

As fossil fuels are limited, and biodiesel will play very important role in future

industry, understanding this fact I decided to work on biodiesel so that after getting

sufficient base from college level I can continue my research in this field.

Thanking you

Sonu Parekh

Shashank Pathak

Ram Naresh Suthar

Pooran Mal Yadav

References:-

Braz. J. Chem. Eng. vol.27 no.4 São Paulo Oct./Dec. 2010

Journal of the Brazilian Chemical Society

Transesterification of Vegetable Oils: a Review

Ulf Schuchardta, Ricardo Serchelia, and Rogério Matheus Vargas*b

Instituto de Química, Universidade Estadual de Campinas, C.P. 6154, 13083-

970 Campinas - SP, Brazil Instituto de Química, Universidade Federal da Bahia, Campus de Ondina, Received:

May 9, 199

K.V.Radha, G.Manikandan, Novel Production of Biofuels from Soybean Oil.