Biodiesel From Used Kitchen Grease or Waste Vegetable Oil

This is how to make your own biodiesel fuel from used cooking oil. The oil -- waste vegetable oil
(WVO), used fryer grease, animal fats, lard -- is often free for the taking. All you need is a few
common chemicals and some equipment you can easily buy or make yourself. The result is a cheap,
clean-burning, non-toxic, renewable, high-quality diesel motor fuel you can use in your car without
modifications.

CAUTION: Wear proper protective gloves, apron, and eye protection and do not inhale any vapors.
Methanol can cause blindness and death, and you don't even have to drink it, it's absorbed through
the skin. Sodium hydroxide can cause severe burns and death. Together these two chemicals form
sodium methoxide. This is an extremely caustic chemical. These are dangerous chemicals -- treat
them as such! Always have a hose running when working with them. The workspace must be
thoroughly ventilated. No children or pets allowed. See Safety for further information.

Making biodiesel

Ingredients

Mixture:
Waste vegetable oil (WVO) -- used cooking oil, fryer grease, animal fats, lard
Methanol (CH3OH) -- 99%+ pure
Sodium hydroxide (NaOH -- caustic soda, lye) -- must be dry

Titration:
Isopropyl alcohol (rubbing alcohol) -- 99%+ pure
Distilled water
Phenolphthalein solution (not more than a year old, kept protected from strong light) -- "Phenol" or
"Phenol Red" from swimming pool or hot tub supply stores may not be the same as
phenolphthalein; it can be used but the directions for use may be different

Washing:
Vinegar
Water

Procedure

1. Filter WVO to remove any food scraps or solid particles.

2. Heat WVO to remove any water content (optional).

3. Perform titration to determine how much catalyst is needed.

 4. Prepare sodium methoxide.

5. Heat WVO, mix in the sodium methoxide while stirring.

6. Allow to settle, remove the glycerine.

7. Wash and dry.

8. Check quality.

This procedure is called transesterification, similar to saponification. Sound familiar?

Saponification is soap making. To make soap you take a transfatty acid or triglyceride (oil or
kitchen grease) and blend it with a solution of sodium hydroxide (NaOH, caustic soda or lye) and
water. This reaction causes the ester chains to separate from the glycerine. These ester chains are
what becomes the soap. They're also called lipids. Their unique characteristic of being attracted to
polar molecules such as water on one end and to non-polar molecules like oil on the other end is
what makes them effective as soap.

In transesterification, lye and methanol are mixed to create sodium methoxide (Na+ CH3O-). When
mixed in with the WVO this strong polar-bonded chemical breaks the transfatty acid into glycerine
and also ester chains (biodiesel), along with some soap if you're not careful (more on that later). The
esters become methyl esters. They would be ethyl esters if reacted with booze (ethanol) instead of
methanol.

Figures 1-3 show these two reactions. The zigzag lines in the triglyceride diagram (Figure 1) are
shorthand for carbon chains. At both ends of each line segment is a carbon atom.

Figure 1

In Figures 2 and 3 these zigzags are shorthanded as R1, 2 and 3.

Figure 2

Figure 3

1. Filtering

Filter the WVO to remove food particles. You may have to warm it up a bit first to get it to run
freely, 95 deg F (35 deg C) should be enough. Use a double layer of cheesecloth in a funnel, or a
restaurant or canteen-type coffee filter.

2. Removing the water

Many people heat the WVO first to remove any water content. Waste oil will probably contain
water, which can slow down the reaction and cause saponification (soap formation). The less water
in the WVO the better.

This is how they do it. Raise the temperature to 212 deg F (100 deg C), hold it there and allow any
water to boil off. Use the mixer to avoid steam pockets forming below the oil and exploding,
splashing hot oil out of the container. Or drain water puddles out from the bottom as they form --
you can save any oil that comes out with the water later.

When boiling slows, raise the temperature to 265 deg F (130 deg C) for 10 minutes. Remove heat
and allow to cool.

You may be lucky and find a regular source of WVO that doesn't need to have the water boiled off,
in which case don't do it -- boiling means extra energy and time. Personally I don't boil off the water
first, I'd rather avoid the extra step in the process and save the energy it uses. But unless you're sure,
it may be better to be on the safe side.
3. Titration

To determine the correct amount of lye required, a titration must be performed on the oil being
transesterified. This is the most difficult step in the process, and the most critical -- make your
titration as accurate as possible.

IMPORTANT: The lye must be dry -- keep it away from water, store it in an airtight container.

Make up a solution of one gram of lye to one liter of distilled water. Make sure it dissolves
completely. This sample is then used as a reference tester for the titration process. It's important not
to let the sample get contaminated, it can be used for many titrations.

Mix 10 milliliters of isopropyl alcohol in a small container with a 1 milliliter sample of WVO --
make sure it's exactly 1 milliliter. Take the WVO titration sample from the reaction vessel (Figure 5
#1) after it's been warmed up and stirred.

Add to this solution 2 drops of phenolphthalein, an acid-base indicator that's colorless in acid and
red in base.

IMPORTANT: Phenolphthalein has a shelf life of about a year, it is very sensitive to degradation
by light so after a while it will start giving erroneous readings.

Using a graduated eye dropper (with increments marked in tenths of milliliters) or some other
calibrated instrument (from medical supply outlets), while carefully keeping track of the amounts,
drop measured amounts of the lye/water solution a couple of tenths of milliliters at a time into the
WVO/isopropyl/phenolphthalein solution.

Follow each drop with vigorous stirring of the solution. In cold weather the WVO might congeal
and not work so you might need to do the titration in a heated room. If conditions are right
eventually the solution turns pink (magenta), and stays pink for 10 seconds. This is the indicator
color for a pH range of 8-9 (see the photograph in the left column of this page, "Color of titrated
liquid sample when at the correct pH"). It's important to find the exact amount, to just reach this pH
without dropping in too much!

It's a good idea to do this entire process more than once to ensure that your number is correct. I've
found that depending on the type of WVO, how hot it got in the fryer, what was cooked in it and
how long it was used, the amount of lye/water solution needed to titrate it is usually 1.5 to 3
milliliters. You can also use litmus paper or a digital pH tester instead of the phenolphthalein. Try it
with fresh cooking oil from your kitchen too, it should need much less lye to reach pH 8-9.

The calculation

The next step is to determine the amount of lye needed for the reaction. Take the number of
milliliters derived from the titration and multiply by the number of liters of WVO to be
transesterified.

There is one more thing to be included in the calculation. Every liter of neat vegetable oil (fresh --
never been cooked) needs 3.5 grams of lye for the reaction. So for every liter of WVO to be
transesterified add an additional 3.5 grams of lye.

Example: The titration determined that it took 2.4 milliliters to reach pH 8-9 and you'll be
transesterifying 150 liters of oil.

2.4 grams times 150 liters equals 360 grams lye

Plus 3.5 grams times 150 liters equals 525 grams lye

360 + 525 = 885 grams lye

If the titration result was 1.8 milliliters to reach pH 8-9, the final amount of lye needed for the
reaction would be 795 grams.

I've found over time that the number of grams of lye needed per liter of WVO has generally been
between 6 and 7.

Test batches

The first few times you do this process or if you're planning on transesterifying a lot of WVO it is a
good practice to first try out your lye amounts on a 1 liter batch in a kitchen blender. This works
really well and you don't need to heat up the WVO too much, just enough so it will spin well in the
blender. Blenders are very thorough at mixing the ingredients so heating is not as critical.

Start by mixing up the lye and methanol in a blender (one that will never be used for food again).
First make sure the blender and all utensils used are dry. Forming the exothermal sodium methoxide
polar molecule will heat up the blender container a bit. Keep mixing until all the lye has been
dissolved.

Once the sodium methoxide is prepared, add to the blender 1 liter of WVO. Make certain all your
weights and volumes are precise. If you're unsure of the titration result numbers then use 6-6.25
grams of lye per liter of used WVO, or 3.5 grams for fresh vegetable oil. Blender batches need only
be run for about 15-20 minutes for separation to be completed before switching off. The settling
takes some time to complete. The solution can be poured from the blender into another container
right after switching off the blender.

It is good to do a few batches with varying amounts of lye recorded so later when checking results
one can choose the lye quantity that did the best job.

When too much lye is used the result can be a troublesome gel that is tough to do anything with.
(See Glop soap.) When not enough lye is used the reaction does not go far enough so some
unreacted WVO will be mixed with the biodiesel and glycerine. This will form three levels with
biodiesel on top above unreacted WVO with glycerine on the bottom. If there is too much water in
the WVO it will form soaps and settle right above the glycerine forming a fourth level in the
container. This layer is not too easy to separate from the unreacted WVO and glycerine layers.

4. Preparing the sodium methoxide

Generally the amount of methanol needed is 20% of the WVO by mass. The densities of these two
liquids are fairly close so measuring 20% of methanol by volume should be about right. To be
completely sure, measure out a half-liter of both fluids, weigh, and calculate exactly what 20% by
mass is. Different WVOs can have different densities depending on what type of oil it originally
was and how long it was used in the deep fryer.

Example: When transesterifying 100 liters of WVO, use 20 liters of methanol.

The methanol is mixed into a solution with the sodium hydroxide (lye), creating sodium methoxide
in an exothermic reaction (ie it gets warm from bonds forming). Keep all utensils the lye comes in
contact with as dry as possible.

CAUTION:
Treat sodium methoxide with extreme caution! Do not inhale any vapors! If any sodium methoxide
gets splashed on your skin, it will burn you without your feeling it (killing the nerves) -- wash
immediately with lots of water. Always have a hose running when working with sodium methoxide.

Sodium methoxide is also very corrosive to paints. Lye reacts with aluminum, tin and zinc. Use
glass, enamel or stainless steel containers -- stainless steel is best. Used restaurant equipment supply
stores and scrap metal recycling yards are two good places to look for this type of equipment. Braze
on plumbing fittings for drains, etc. where needed.

5. Heating and mixing

Pre-heat WVO reclaimed from a restaurant's waste grease barrel to 120-130 deg F (48-54 deg C).

A propeller or paint stirrer coupled to a 1/2-inch electric drill works fine as a mixer.

Too much agitation causes splashing and bubbles through vortexing and reduces mix efficiency.
There should be a vortex just appearing on the surface. Adjust the speed, or the pitch or size of the
stirrer to get the right effect.

If you want a quieter processor, an electric pump plumbed to form a mixing loop for stirring the
WVO would do a nice job. Mount the pump above the level that glycerine will gel at to prevent
clogging up the pump (see below).

Add the sodium methoxide to the WVO while stirring; stir the mixture for 50 minutes to an hour.
The reaction is often complete in 30 minutes, but longer is better.

The transesterification process separates the methyl esters from the glycerine. The CH3O of the
methanol then caps off the ester chains and OH from the NaOH (lye) stabilizes the glycerine.

6. Settling and separation

Allow the solution to sit and cool for at least eight hours, preferably longer. The methyl esters --
biodiesel -- will be floating on top while the denser glycerine will have congealed on the bottom of
the container forming a hard gelatinous mass (the mixing pump must be mounted above this level).

An alternative method is to allow the reactants to sit for at least an hour after mixing while keeping
the brew above 100 deg F (38 deg C), which keeps the glycerine semi-liquid (it solidifies below 100
deg F). Then carefully decant the biodiesel.
This can be done by draining the reactants out of the bottom of the container through a transparent
hose. The semi-liquid glycerine has a dark brown color; the biodiesel is honey-colored. Keep a
watch on what flows through the sight tube: when the lighter-colored biodiesel appears divert it to a
separate container. If any biodiesel stays with the glycerine it is easy to retrieve it later once the
glycerine has solidified.

If you left the mixture in the tank until the glycerine gelled, reheat the tank just enough to liquify the
glycerine again. Don't stir it! Then decant it out as above.

Figure 4 shows one example of a system for separating two liquids with different densities. This
could make a good pre-filter or be used to separate oils, soap and glycerine/esters goop. Marine/boat
fuel cleaning systems do a good job of filtering.

Figure 4 Figure 5

Figure 5 shows the reaction vessel (#1) where the WVO is mixed (also could be done with a pump)
and heated. Heating is accomplished by (#2) a hotplate, propane-burner, or a diesel stove would
work well.
Figure 6
A proposed alternative using very little electricity is illustrated in Figure 6.
This system would use a furnace-type burner run on reclaimed esters to
heat its reaction vessel. The vessel's stirring action is created by thermo
inversion currents generated by the vessel's external cooling tubes and a
baffled exhaust vent that runs up through its center.

Figure 5 also shows a blender (#3) used to mix up the sodium methoxide.
When making 16 liter (5 gal) batches, I use a yard-sale glass blender for the
sodium methoxide solution (and for nothing else!), but I can't fit it all in at
once, so I measure out three separate portions.
Glycerine

The glycerine from WVO is brown and usually turns to a solid below about 100 deg F (38 deg C).
Glycerine from fresh oil often stays a liquid at lower temperatures.

Reclaimed glycerine can be composted after being vented for three weeks to allow residual
methanol to evaporate off or after heating it to 150 deg F (66 deg C) to boil off any methanol
content (the boiling point of methanol is 148.5 deg F, 64.7 deg C). The excess methanol can be
recovered for re-use when boiled off if you run the vapors through a condenser.

Another way of disposing of the glycerine, though a great bit more complicated, would be to
separate its components, mostly methanol, pure glycerine and wax. This is often accomplished by
distilling it, but glycerine has a high boiling point even under high vacuum so this method is
difficult.

The glycerine by-product makes an excellent industrial-type degreaser/soap. One way to purify it is
heat it to 150 deg F (65.5 deg C) to boil off excess methanol, making it safe for skin contact (take
precautions with fumes). Once the glycerine is back to a liquid the impurities sink to the bottom and
the color will become a more uniform dark brown. This can be cut with water leaving it a tan color,
less concentrated and softer and easier to handle when washing hands. Produced this way the
degreaser could be sold in squeeze or pump dispensers.

Other ideas for disposing of the glycerine are breaking it down to usable methane gas, with a
methane digester or, for a much wilder idea, it could be broken down with pyrolisis. Pyrolisis was
used extensively to run cars on firewood in oil-scarce Europe and elsewhere during World War 2.
The processor has a heat source that heats the fuel (wood or glycerine) in an airtight box without
oxygen. This allows the fuel to release its methane while not allowing it to burn. The methane is
trapped in an inflatable storage container or compressed into a tank. This is an area of biodiesel
development that warrants further work.

Soap residue

Suspended in the biodiesel will also be some soapy residues. These are the result of Na+ ions from
the sodium hydroxide (NaOH) reacting with water created when the methanol bonds with the ester
chains along with any other water that was suspended in the WVO.

If the reaction produces more than the usual amount of soap, this happens when lye comes into
contact with water before it has a chance to react with the WVO -- in this case the excess water
should have been boiled off first. (See Step 2, above, Removing the water.)

The part of the process where it's vital to keep all water out of the reaction is when making the
sodium methoxide. Keep the blender and all utensils the lye comes in contact with as dry as
possible. The chances of a good clean splitting of esters from glycerine with little soap by-product
are much better on a warm dry summer day than on a damp winter day.

7. Washing and drying

There is more than one school of thought on getting the biodiesel from this stage to the fuel tank.
One is to let it sit for a while (about a week), allowing the majority of the soap residues to settle
before running the biodiesel through a filtration system then into the vehicle/home fuel tank.

Another method is to wash the soaps out of the fuel with water, one or more times. When washing
biodiesel the first time it's best to add a small amount of acetic acid (vinegar) before adding the
water. The acetic acid brings the pH of the solution closer to neutral because it neutralizes and drops
out any lye suspended in the biodiesel.

Figure 7 shows a simple way of washing using a translucent PVC type container with a valve 3-4
inches from bottom. For 5 gallon batches use those 5-7 gallon buckets found everywhere these days.
If a translucent container can't be found one fabricated with a sight tube (#6) ought to work.

Fill with water until it is halfway between the container's bottom and the valve, then fill up with the
biodiesel to be washed. After a gentle stirring (keep it gentle, you don't want to agitate up soaps)
followed by 12-24 hours of settling, the oil and water will separate, the cleaned oil Figure 7
can be decanted out the valve, leaving the denser soapy water to be drained out the
bottom (#5).

This process might have to be repeated two or three times to remove close to 100%
of soaps. The second and third washings can be done with water alone. After the
third washing any remaining water gets removed by re-heating the oil slowly
(Figure 8), the water and other impurities sink to bottom. The finished product
should be pH 7, checked with litmus paper or with a digital pH tester.

The water from the third wash can be used for the first or second washes for the next batch. The
impurities can be left in the re-heater for the next batch and removed when it accumulates. The
soaps can be concentrated, left-over biodiesel can be decanted out and what's left is Figure 8
a biodegradable soap good for many industrial-type uses (degreasers etc.).

I had some success with trapping the concentrated very hydrated sodium from this
soap. The way I did this was by pouring the soap onto a stretched cheese cloth and
allowing the water to run through leaving the sodium on the cloth. This is as far as
I've gone with this so far but it seems one could press much of the water from the
sodium then vacuum dessicate this saturated sodium under dry conditions back to a
usable sodium hydroxide.

Transesterified and washed biodiesel will become clearer over time as any
remaining soaps drop out of the solution.

Another idea I have been working with is chilling down the biodiesel thus allowing the soaps to
condense and settle out faster. When the oil gets chilled it seems to speed up the settling of the
residual lye. With a short settling time the oil clears considerably.

Bubble washing

Some experimenters are getting good results with the Idaho bubble washing technique. It takes
longer, but uses less water. They find it very effective, giving a clean, polished product.

Here's how they do it. The bubbles are formed by compressed air passing through an air stone. For a
small installation, buy an aerator at an aquarium shop -- they come in several sizes and cost about
$10 to $40. Sometimes they have a filter attached -- throw it away.

Add about 30 milliliters of vinegar (acetic acid) per 100 liters of biodiesel and then about 50%
water. Then drop in the air stone.

The air stone sinks to the bottom of the tank. When you switch on the aerator, the air bubbles rise
through the biodiesel, carrying a film of water which washes the biodiesel as it passes through. At
the surface, the bubble bursts, leaving a small drop of water which sinks back down through the
biodiesel, washing again.

If the mixture is still cloudy after a couple of hours, add a little more vinegar.

Bubble-wash for 12 hours or longer (up to 24), then drain off the washing water, skim off any wax
floating on top. Repeat the bubble wash two more times; keep the water from the 2nd and 3rd wash
for washing the next batch.

For severe soap formations, first heat the biodiesel/soap mixture to 122 deg F (50 deg C). Add
enough vinegar to bring the pH to slightly below 7. Stir for half an hour, cool and continue with
bubble drying as usual.

See also Bubble washing

8. Quality

The quality of the fuel product can be checked by visually examining it and checking its pH. The pH
of the finished product can be checked with pH paper or a digital tester. It should be neutral (pH 7).
It should look like clear vegetable oil with a light brown tint, similar to filtered apple cider.

There are not supposed to be any films, particles or cloudiness to it. Films would be remaining
soapy residue, re-wash or re-filter it at 5 micron or finer. Cloudiness would be water still in it, re-
heat it. Particles could be anything and indicates the filter is failing.

Any oils will clear up considerably when heated but the test is, when it cools back down is it still
clear? If it is not yet clear then allowing it to settle out for an additional week or two should be
enough to clear it up.

For final filtering it is best to use a marine-type fuel filter -- the ones with a transparent canister so it
is possible to keep an eye on the fuel's clarity. I used to trust when I washed it to just pouring fuel
into the tank through folded cheesecloth in a funnel. After running into an increased number of dirty
fuel filters I've become more careful.

It is important to know also that biodiesel does a great job of cleaning up fossil diesel fuel films
coating the interior parts of any old diesel engine. For this reason, take care to check and change
your vehicle's fuel filters when first switching over to biodiesel. I like putting a small, cheap, clear
or translucent plastic in-line fuel filter right before my vehicle's stock filter. This will prefilter the
fuel before it reaches the vehicle's fuel filter, which is more expensive to replace. This also makes it
easy to see when fuel is flowing and to keep an eye on the condition of the filter.

Limitations

Biodiesel does have some limitations. First it has cold-weather starting problems. Depending on the
type of oil used, around 40 deg F (4-5 deg C) it may start to solidify. One remedy is to mix with a
proportion of fossil diesel. Or try a Racor or Diesel-Therm electric fuel heater. Heated garages are
nice too. Some people report that standard antigelling compounds work fine, others say they're
unpredictable. (Be aware that antigelling agents can be highly toxic.)

Retard the injection timing by 2-3 degrees -- this overcomes some of the effect of biodiesel's higher
cetane number. The engine loses a bit of the extra power you get with biodiesel, but it runs quieter
and the fuel burns cooler, reducing NOx emissions. (See also NOx emissions and biodiesel.)

There can be an increased rate of corrosion of rubber parts in the fuel system over time with 100%
biodiesel. Newer cars do not use rubber parts. Biodiesel has been used in many older motors
without any problems. Viton parts are best, but others are just as good.