Ch 62 Industrial Chemical Reactions and Processes

EXPERIMENT No. 1: Biofuel Synthesis: Fermentation, Distillation, and Mass Balance

INTRODUCTION:

Biofuel refers most commonly to ethanol-blended gasoline fuels. Ethanol is produced through the
fermentation of carbohydrates by yeast cells. Fermentation is an energy-yielding process that cells carry
out in the absence of oxygen. Although fermentation does not provide much usable energy
for our cells, it is sufficient for yeast cells. Yeast cells produce ethanol and CO 2 as byproducts,
and the ethanol produced can become a valuable energy source. There is much interest in
ethanol as an energy alternative to fossil fuels, which are nonrenewable and contribute
significantly to atmospheric pollution.

Ethanol, which is blended with gasoline (at about 5- 10%) to yield gasohol, has several
advantages over petroleum as an energy source. The presence of an oxygen atom in ethanol
allows gasohol to burn ‘cleaner’ than regular gasoline, with reduced emissions of carbon
monoxide, nitrogen oxides and hydrocarbons. Ethanol, a renewable fuel source, also helps to address
concerns about greenhouse gas emissions (mainly in the form of CO 2).

Fermentation is the breakdown of complex molecules to simpler ones through the action of
some microorganism, such as yeast. Indeed we normally think of fermentation in the
context of beer or wine, but the term also includes the conversion of milk to yogurt or
cheese, the making of bread, and many more. In all of these indicated examples, carbohydrates are being
fermented by yeast. In the case of bread, yeast converts carbohydrates into carbon dioxide gas (CO 2).
The little pockets of CO2 make the bread rise and produce the fluffy consistency that we
associate with bread. Indeed, it is this formation of gas pockets that distinguishes bread
from crackers. For fermentations that produce alcohol, such as wine, carbohydrate is
converted to ethanol and carbon dioxide:
enzymes
C6H12O6 → 2CH3CH2OH + 2CO2

Fermentation continues until the ethanol concentration is high enough to inhibit yeast
growth. This usually happens when the alcohol content is between 10 - 14 %. If you want to
produce a beverage that has greater alcohol content, you must either distill it or fortify it (with alcohol
that resulted from another distillation process). Whiskeys, vodka, and gin are examples of distilled spirits.
Port wine and liqueurs are examples of fortified wines. Distillation is a purification process wherein a
substance is heated to its boiling point, the vapor produced upon boiling is allowed to flow away from the
boiling liquid, and the vapor is cooled to condense it back to the liquid.

OBJECTIVES:

(1) To study the synthesis of ethyl alcohol via fermentation of sucrose.

(2) To purify ethyl alcohol via fractional distillation.
(3) To create a flow chart of the fermentation and purification process and create a mass
balance relationships between the starting materials and product and by-product.

Prepared by: Gilbert Yu and Ronald Fabicon Page 1

PROCEDURES:

I. FERMENTATION

Week 1
1. Add 70 g of sucrose and 300 mL of distilled water to a 500 mL Erlenmeyer
flask with a side arm.
2. While the sugar is dissolving, add 6 g of dry yeast, 60 mL of water, and 0.70 g
of disodium hydrogen phosphate to a 100 mL Erlenmeyer flask.
3. Add a magnetic stir bar and stir on a hot plate with gentle heating (30-35o)
until the ‘solution’ (100 mL flask) takes on a uniformly murky appearance. Remove the stir
bar and pour the yeast solution into the Erlenmeyer flask (500 mL flask) containing the
sugar solution.
4. Weigh the Erlenmeyer flask containing the sugar – yeast mixture. Make sure
the contents are thoroughly mixed by periodically swirling the flask. In order
to ensure the production of ethanol and not acetic acid, the fermentation
must be carried out in the absence of oxygen.
5. Cap the flask with a cork or rubber stopper. Wire a length of rubber tubing to
the side arm of the 500 mL Erlenmeyer flask. Glass tubing (~8 inches long)
should be wired to the other end of the rubber tubing. Insert the glass tubing
into a six-inch test tube that is resting in a large beaker.
6. Add saturated lime water (Ca(OH) 2) to this tube (testtube) to a depth of one inch.
Assuming your apparatus does not have a leak, this configuration will be
airtight. The evolution of carbon dioxide will drive out the residual air that is
in the apparatus, and the test tube bubbler will ensure that no oxygen will
diffuse back into the fermentation flask. The appearance of bubbles, and the
formation of a white precipitate of calcium carbonate, serves as evidence that
a reaction is really taking place.
7. Label your flask and let this apparatus sit on top of the lab bench shelves
undisturbed for one week. Bubbles should appear before you leave the lab. If
they do not, consult your laboratory instructor.
8. Let the fermentation run for at least 5 days.

Week 2
1. You should find that the yeast particles have settled out and the liquid is clear. Do not stir this
liquid. Remove the cork or rubber stopper.
2. Weigh the flask containing the fermentation mixture.
3. Carefully decant into a pre-weighed beaker as much clear liquid as you can.
Weigh the beaker again with the clear fermentation mixture.
4. Determine the density of the clear fermented mixture by pipetting 10.00 mLinto a pre-weighed
beaker. Weigh the beaker and its contents and determine the density (g/mL).
5. Determine the alcohol content of the mixture.

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 DISTILLATION (Week 2)
1. Assemble a simple distillation apparatus and distill the clear fermentation
mixture from above. Your distillate receiving flask must be pre-weighed and
immersed in an ice bath throughout the course of the distillation.
2. Continue distillation until the temperature reaches 95oC.
3. Allow the apparatus to cool and discard the pot residue down the drain.
4. Determine the density and total weight of the distillate.
5. Tabulate all of your data.

Determination of % Ethanol (by weight)

1. Determine the density of the clear portion of the fermentation mixture, and
the distillate.
2. Dilute ethanol and water solutions to form (almost) ideal solutions. In ideal
solutions, there is a linear relationship between % alcohol by weight and
density. The following set of data is from ‘Perry’s Chemical Engineers
Handbook, 6th ed. Table 3-110.

Concentration (wt %) and Density of Ethanol-Water Mixtures at 30 oC

Wt % (Ethanol) Density (g/mL) Wt % (Ethanol) Density (g/mL)

0.00 0.9957 80.00 0.8347
5.00 0.9868 85.00 0.8222
10.00 0.9788 88.00 0.8145
15.00 0.9713 91.00 0.8066
20.00 0.9640 94.00 0.7984
25.00 0.9561 97.00 0.7899
30.00 0.9474 100.00 0.7808

3. Generate a plot of Wt% Ethanol vs. Density. Use the equation of the line to determine the %
ethanol in your fermentation mixture. Do the same to determine % alcohol in the distillate. You
might need to use the smaller values (0 to 30% wt) for the mixture and higher values (80 to
100% wt) for the distillate.

QUESTIONS

1. Write the balanced equation for the formation ethanol and carbon dioxide from
the fermentation of sucrose. Based on the amount of sucrose and other
materials used in the experiment and assuming 100% conversion of sucrose to
ethanol, what % by weight of ethanol will the fermentation mixture be?

2. Carbon dioxide is a by-product in this reaction, rather than releasing CO 2 as

an atmospheric pollutant, what can be done with it?

3. Write a balanced equation for the formation of precipitate in test tube

containing calcium hydroxide (lime) solution.

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4. Draw a process flow block diagram (block and arrows) for this experiment.
Include all unit processes and operations, input materials and output materials (include amounts).

5. At the end of the experiment, only the clear portion of the fermentation
mixture was distilled, what can be done with the residue?

6. Were you able to recover all the ethanol produced using simple distillation?
Why?

7. If you had used a lot more sugar in the fermentation flask, could you produce
a 90% alcohol solution WITHOUT DISTILLATION?

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