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Short introduction to
"How to make Biodiesel"

 

How to make Biodiesel

Biodiesel forms due to a chemical reaction called transesterification, meaning that glycerol in the oil is substituted by an alcohol in the presence of a catalyst. In our case we use Methhanol and NaOH (caustic soda) or KOH (caustic potash). In this "How to" we will do our best to make clear to you how to prepare a good biodiesel. Don't let yourself be put off by our method, though. There are many other ways and tricks to prepare good biodiesel and you can find much about it at the other websites mentioned above.

The 3 ingredients

Oil

The primary ingredient is oil or fat. This will be waste vegetable oil for the average producer at home, which may be collected for free in most restaurants.
One can, of course, grow rapeseed or Jathropa and crush it for oil, as often happens in the United States.

Many US farmers are nowadays self-supporting with regard to energy. They use biodiesel in tractors and other farming machinery and mostly diesel aggregates are used to generate electricity.

 

People who prepare diesel on a larger scale are able to use waste frying fat, fish oil, animal fat and several other kinds of oils. The nice thing about biodiesel is that you can make it out of so many different substances, mostly waste products. There is always something in stock, and even the use of new oil is cost-effective still.

Alcohol

The second ingredient is alcohol. Methanol is mostly used in the application of recycled vegetable oil. When processing new oil, it is often possible to use ethanol, but as ethanol is more difficult to handle, we use methanol here.

We like to point out that methanol is a very dangerous material, as is ethanol. Avoid inhaling and skin and eye contact, always wear gloves suitable for this substance, eye-protection and face-mask and always work in a well-ventilated room.

Katalysator

The last ingredient is the Catalyst. Both KOH (potassium hydroxide, caustic potash) and NaOH (Sodium hydroxide, caustic soda) may be used. The advantage of KOH is that the residual glycerine is much less toxic than when NaOH is used. In that case, it is even possible to process the glycerine into artificial fertilizer. KOH dissolves much more readily in methanol as well. However, an advantage of NaOH is that it is very simply and cheaply to get as a plunger, while it is good to handle. That is why we use it in this manual.

You can always have a go with KOH as well. Take care that you use NaOH with a purity of 96% or higher. KOH of that percentage is rather hard to find, but 92% and 85% will work fine as well. Both NaOH and KOH are very dangerous chemicals. Please take the precautions mentioned above when using these chemicals.

Although biodiesel can be derived from many oils and fats, mostly waste frying oil is used. Restaurants often have to pay for the removal of their waste oils. Therefore it is rather simple to collect oil for free from a restaurant

The most convenient way is to collect it in its original packaging. Oil mostly is supplied in plastic containers. If your supplier is willing to refill these containers with the waste oil you are certain that the oil is not polluted extra by water, dirt and other externally interfering factors. Another option is that you provide the restaurant with a barrel to catch the oil. Obviously, you can spare yourself the trouble and use new vegetable oil. It simply is for sale at supermarkets and wholesalers.

 

Oil quality

The cleaner and newer the oil, the simpler it is to make high quality diesel.

Its colour and transparency tell a lot about oil quality. Light and clear is good; darkand turbid smelly oil is less suitable to produce biodiesel.When you are not sure of the oil quality, it is advisable to make first a small amount of diesel. If this turns out to be good, then you can process the rest of the oil. Our manual may seem to be very simple and in fact making biodiesel is not that difficult. It only becomes tricky when you have oil of lesser quality, like oil with much water. Too much water may interfere with the process, especially when you are using too much of catalyst a kind of gel may form. One way to check your oil for water is by heating about half a liter of oil to a temperature of 50� C. If it starts to bubble/hiss/crack etc. then the oil contains too much water. When you do not see any of these phenomenons at 60� C, there is no reason to remove the water.

 

Titration

Before you are able to process the vegetable oil into biodiesel you have got to know first how much methanol and catalyst you need. As far as methanol is concerned you may always assume about 200-220 ml methanol per litre of oil. The percentage of NaOH is variable. If new vegetable oil is processed, then you will require 5 g per litre of oil to substitute all glycerol by methanol. If waste oil is used then the same amount of catalyst will be required plus a certain amount to neutralize the free fatty acids that are present in the oil. To this end you will have to determine by way of a test, called titration, how many of these free fatty acids (FFAs) are present in your oil.

What do you need?

10 ml isopropyl alcohol, 99%*
Oil (heated to 45� C)
Phenolphtaleine-solution (0,2%-0,4%)*
Catalyst (NaOH, KOH)*
Distilled water
Some glass saucers
Some hypodermic syringes to enable dosing the right amount.*
a pair of scales preferably accurate to 0.1 or 0.01 g.

*These articles will be provided when purchasing a BioKing

The procedure is as follows

Dissolve 1 g of catalyst in 1 litre of distilled water, this solution is the titrant. NaOH is very difficult to dissolve. This can best be done by putting for instance 50 ml distilled water into a transparant bottle, adding the gramme of NaOH, closing the bottle and shaking it as long as it takes to see no visible grains and pouring this back into the distilled water.

This solution is suitable to carry out titrations in the following weeks. In order to reduce the chance of errors, you may consider to dissolve 3 g of catalyst in 3 litres of distilled water. An error of for example 0.2 g has less effect that way than in the case of 1 litre. Cork the botle and keep it well. Take care when weighing the grains of NaOH that you do not leave the packaging open. The grains are very quickly to attract water and will not be fit for use anymore. The photo on the right shows how the grains look when they are subjected to a few minutes of oxygen.

Step 1

Step 2

Step 3

Step 4


Pour 10 ml Isopropyl Alcohol in a glass cup or saucer.

Heat a bit of the oil to be tested to a temperature of 45� C , mix 1 ml of it with the alcohol and mix well, it will get a yellowish colour.

The amount of alcohol does not require much precision, but it is important that you should measure out exactly 1 ml of oil. An old trick is to suck in a bubble of air first into the hypodermic and then the oil, this way you are able to read more precisely.

Add 2-3 drops of PH-indicator solution (phenolphthaleine).

 

Start carefully to add the water with the catalyst, keep swinging the cup. The fluid will colour to a light pink, but will turn yellow again if you keep swinging. When the oil with alcohol remains pink for a period of 30 s, you stop adding the solution. Make a note of how many ml of solution you have used and repeat the whole procedure once or twice in order to make sure you have titrated correctly.

When you have a PH-meter at your disposal you can use it instead of the phenolphtaleine-solution. When the fluid has reached a PH-value of 8.5, then you have added enough NaOH-solution.

That's all !!!!

If you need less than 3 ml of the solution then you most probably have laid your hands on very good oil, 3-6 ml means that the oil is suitable to turn it into biodiesel. 6 ml or more implies a poor quality, but the oil may still be suitable for the production of biodiesel. Take care when titrating that you should use each instrument for only 1 agent. We advise to label all hypodermics, pipettes and other tools in order to avoid mistakes.


Test batch

Irrespective of the titration results, it is advisable to first process one litre of oil, before turning to the production of bigger amounts. Should you have made a mistake somewhere than this will appear now, this way you avoid that you may have to throw away maybe 100+ litres of oil because you made a mistake in titration.

Fortunately, one litre of test diesel is easy to make. You start with heating 1 litre of oil to 45�C, preferably in a jar or bottle that can be corked. In the meanwhile you mix 220 ml of methanol with the amount of catalyst you determined in titration. Put this in a glass jar or bottle that can be corked well. This mix is called methoxide.

 

How much NaOH?
 
In processing new oil you use 5 g of NaOH per litre of oil.

In processing waste oil you take 5 g +1 g for each ml of catalyst solution you needed for titration. If 4 ml solution was needed, for example then you use

5+4=9 g of NaOH

Mix the methoxide until of the catalyst is dissolved. The chemical reaction will make the fluid to get hot. When all grains of NaOH have been dissolved, you carefully add the heated oil. Subsequently you shake or mix it all during 10 to 15 minutes.

Leave the oil to rest. In less than an hour already you will see a separation between biodiesel and glycerine.

 

Good or not good?
 

The test has been successful if you see a distinct dividing line between the biodiesel and the glycerine, the amount of glycerine should be about 10% of the total content.

If less than 10% glycerine forms, then you probably have used too little catalyst, carry out a new test with 0.5 � 1 g more of catalyst.

If you see a clear layer of soap between the biodiesel and the glycerine, then you probably have used too much of catalyst. Carry out a new test with 0.5 - 1 g less of catalyst.

If you see lumps in the biodiesel, then you have bad oil or the titration was incorrect. Carry out a new titration and make a new test batch from it. If you see lumps again, then you better should not use this oil.

Leave the biodiesel to rest for 12-24 hours. Dark coloured, somewhat viscous glycerine will have formed at the bottom of the jar, with a distinct dividing line with the pale fluid above it. The colour of biodiesel varies and depends on the type of oil that was used, but is mostly palish yellow. The diesel can be clear, but this is not required per se, it may be very turbid as well. Not to worry. Eventually it will become clear, but there is no reason to wait.

Warning: Methanol, Methoxide (Methanol/catalyst-mix), and NaOH are dangerous chemicals. Before use always read the safety regulations provided and follow the instructions on the packaging. Always work in a well-aired room and always wear personal means of protection, such as a suitable face mask, gloves and face protection when working with these materials

 

To make a whole tank

1 Fill the tank with the amount of vegetable oil desired, up to a maximum of 150 litres.
2 Turn on the heating and wait until the oil has reached the desired temperature of 45� C heeft bereikt. Turn off the heating element. Attention: The heating element must never be turned on when it is not fully submerged in the liquid, this can damage the element!!!!
3 While the oil is heating you can prepare the methoxide, this is as follows:

- Fill the premix-tank with 15 litres of Methanol and the amount of catalyst desired

- Swith a wooden or synthetic object, as long as is needed to dissolve all grains.

4 When the oil has reached the right temperature and the methoxide is ready, you can start mixing. To this end you have to open valves A, C and D and switch on the pump with the button "Pump 1hr". Open the tap (F) on the methoxide-tank. The content will mix gradually with the circulating oil, when the methoxide has run out you can replenish methanol until the amount recommended of 220 ml of methanol per litre of oil has been reached. The oil will be mixed with the methoxide, during 1 hour exactly, the exact time needed for a good and complete reaction.
5 The pump will switch off automatically after one hour.
6 After having letting it rest for 1-2 hours, you may drain the glycerine from the bottom of the tank. Another 8 hours later you may drain the last glycerine from the barrel. The biodiesel is now ready to be washed.

As the BK200 is not equiped with an automatic stiring device, the content of the premix-tank is kept small, this is in order to make the mixing more easy. You will have to pour the remaining methanol during the mixing of the oil with methoxide in the little tank.

 

The washing
 
Washing of the diesel with water is very important for various reasons. Your biodiesel will probably have a high alkaline value, because of the fact that non-used catalyst particles are still in the fluid. By washing the lye will be removed and the biodiesel will become PH-neutral (7). While washing we remove furthermore soap, methanol surplus, solid particles and any other pollution that may happen to be in our diesel. You may think: "Methanol is a good fuel, why do I have to remove it from my biodiesel?" Methanol as such is a good fuel indeed, but surplus methanol may damage your injection-system.

The smaller Bio-King� units are supplied with a built-in water-mist system, with it we can wash our diesel effortlessly. It works as follows:

  1. Attach a garden hose to the coupling provided, open the tap and leave it running for 1 hour, this will make about 20 litres of water to "spray" through the mist. The water is heavier than the diesel and takes, while falling down, the pollution with it. 
    Attention: Hot water washes better than cold water and soft water washes better than hard water. 
    In the case of you having problems with the proper washing of your diesel you may consider using hot water and a water softener.
  2. Leave the diesel to rest for at least 1 hour, so that the water can do its job well.
  3. Drain the water at the bottom. Handle things tactfully. If you open the valve completely it will cause an eddy causing the biodiesel to be remixed with the water and this, obviously, will not be your intention.
  4. Repeat this process at least twice before the water leaves the diesel almost clean (PH7). Take care that all water is drained from the processor. You would be well-advised to purchase a PH-meter of PH-indicator paper in order to test your biodiesel.

Now you can pump the diesel from the BioKing into a storage tank or the like, again by means of the pump on the BioKing.

This works as follows: You connect a hose to the hose socket at the filter, open taps A, C and E and start the pump 'Manual'. The biodiesel will now be pumped into your storage tank via the filter. Most remaining water will be extracted from the diesel by the built-in water separator. There will always remain a certain percentage of water in the diesel making it somewhat turbid. It is better to leave the diesel another 2 or 3 days in an open tub, this will make the surplus water to evaporate, this is called drying. You will see your biodiesel getting more clearly. The drying can be accelerated by leaving the biodiesel in the sun to dry or by heating it until a temperature of about 45� C and subsequently letting it cool down in an open tub. If the diesel turns turbid again after cooling down, then this means that the diesel has not been washed properly, wash it again. What you have now is biodiesel, ready for use. You may use it purely in your car or if desired, mix it with �Dinodiesel�. In winter in particular, at low temperatures it may be sensible to mix 20 to 30% of normal diesel with your biodiesel. Biodiesel tends to thicken even more than normal diesel does when it is cold.

One can think of temperatures below -5� C. When you are starting to use biodiesel, it is sensible to begin with a mixture of 20% biodiesel and 80% normal diesel. One of the biodiesel�s good properties is that it cleans your fuel tank and fuel circuit, this makes that small particles will turn up in your fuel system. If you were to start immediately with 100% biodiesel in your car then you will most probably have your fuel system blocked. Therefore, you will have to increase the percentage of biodiesel gradually. This way you can find out at which ratio your car runs best

We hope that we have put you on the right way with this manual in the production of biodiesel. You have seen that it is not difficult and with the help of the BioKing and these instructions you will probably succeed. We cannot guarantee good biodiesel though, this depends completely on your method and the ratio of the ingredients. Previously in this manual we have mentioned a few websites where you can find much on biodiesel. Study these well. There are other methods to produce biodiesel with an apparatus such as the BioKing and these methods may appeal to you more. If you have any questions on the production of biodiesel or the BioKing you can always mail to info@bioking.nl 

We will try and help you as quickly and as well as we can to get you on your way again.

 

How to simple test your biodiesel

 

Test #1 - clarity

Take an approximately 500ml sample of your fuel in a clear container. You should be able to read newsprint through it. If you cannot see through the fuel it's an indication there may still be water, glycerin, monoglycerides or diglycerides in your fuel. You don't want any of these in your finished fuel.

Test #2 - miscibility

Using your 500ml sample, mix in about 1 cup of water. Shake until water mixes with the fuel. Let sit for a few minutes. The fuel should separate from the water and there should be no layer of soap between the two layers. If soap is created, it's an indication further washing is needed. If the fuel does not separate easily, it's an indication of poor quality fuel.

Test #3 - Odor

Smell the fuel, it should have a faint odor of vegetable oil with no alcohol type smell.

Other tests

If your reaction went according to plan, and the biodiesel passed the three tests shown above, you can be confident you have good fuel. However it is possible to run other tests to be sure. You can test the pH of the fuel exactly the way you titrated your original oil. Good biodiesel should have a pH of around 7. You can test the specific gravity of the fuel with a hydrometer, or you can even send the fuel out to a lab and have it tested to see if it meets ASTM D6751 specifications.

 

 

 

 

 

 

 

 

 

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