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incomplete reaction? Need help..
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Ive made 3 batches of biodiesel with a freedom fueler processor and both of my first 2 batches turned out great. After the dry wash the fuel was light gold color and could read the paper through a mason jar of it. Those first batches were done with a 1 stage base process. My first batch this year i had oil from the same supplier, Tony Romas, and it titrated the same as my first batches. This time though i tried a 2 stage base-base using 75% methoxide the first go and 25% the second. The fuel appeared the same as the first 2 batches before drywashing but after i drywash the last batch and let it sit again it is no longer clear? Do i have an incomplete reaction? any other factors could cause this? If i have an incomplete reaction and have to re-process how much lye and methanol should i use? Thanks
 
Registered: October 17, 2009Reply With QuoteReport This Post
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Originally posted by Leachman_44:
Ive made 3 batches of biodiesel with a freedom fueler processor and both of my first 2 batches turned out great. After the dry wash the fuel was light gold color and could read the paper through a mason jar of it.

What the fuel looks like says almost nothing about the true quality of it. Kind of like looking at the outside body of a car, it doesn't tell you what condition the car is really in.

Did you perform a 3/27 test or any other quality check?

quote:

Those first batches were done with a 1 stage base process. My first batch this year i had oil from the same supplier, Tony Romas, and it titrated the same as my first batches. This time though i tried a 2 stage base-base using 75% methoxide the first go and 25% the second. The fuel appeared the same as the first 2 batches before drywashing but after i drywash the last batch and let it sit again it is no longer clear? Do i have an incomplete reaction? any other factors could cause this? If i have an incomplete reaction and have to re-process how much lye and methanol should i use? Thanks


You need to do a 3/27 test to make a rough determination of the quality of the fuel.
Cloudiness can be caused by several things including water and temperature as well as others.

Since you said you're using a freedom fueler, my guess is that you've been giving bad directions for making fuel from the beginning.

What does your oil titrate at?
How many grams of catalyst are you using?
What kind of catalyst?
How long did you process for and at what temperature?


I have not yet seen a freedom fueler that can make a quality batch of fuel. They are under powered machines that are supplied with poor quality components and bad instructions.


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Registered: March 09, 2006Reply With QuoteReport This Post
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My oil titrated at a 2 then used a 5.5 base number for Naoh Ended up using 1098g for a 40 gallon batch. My oil is heated to 125F and mixed for 1.5 hours and let the glycerine settle for 4 hours then did the 2nd process with the rest of the methoxide and let it settle overnight. Then heated it again and ran through the drywash for 1.5 hours. The next day it was cloudy again so i tried washing again and same result.
 
Registered: October 17, 2009Reply With QuoteReport This Post
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Originally posted by Murphy:
Since you said you're using a freedom fueler, my guess is that you've been giving bad directions for making fuel from the beginning...
I have not yet seen a freedom fueler that can make a quality batch of fuel. They are under powered machines that are supplied with poor quality components and bad instructions.
This is good information to know. Can you be more detailed in your first hand experience using the Freedom Fueler and which parts of the instructions are bad.

I am kind of in the market for a biodiesel reactor and unbiased reports like yours on the various biodiesel reactors available will help me make a choice.
 
Registered: May 04, 2010Reply With QuoteReport This Post
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Leachman_44,

Here's a few suggestions:
1) Bump up the amount of catalyst you're using.
Depending on how old your Freedom Fueler is, the literature for titrating may still be based on the older base of 3.5.

For your 40 gal of oil, here's the calculation I'd use.
1 Gal = 3.785 liters
40 Gal = 151.4 liters
2+5.5=7.5 grams per liter
151.4 x 7.5 = 1135.5 grams

Depending on the NaOH you're using, you may also need to adjust for purity.
For example, if your NaOH is 90% pure....
5.5/.90 = 6.11

Most NaOH that I buy runs between 95-98% pure.
5.5/.95 = 5.8
5.5/.98 = 5.6

Assuming yours is 95% pure, the new NaOH amount would be:
(5.8 + 2) x 151.4 = 1180.9, or 1181 grams.

2) Check your oil for water content
If you still have a sample of the oil you used for this batch it's pretty easy to do.

Pull a sample of oil used; preferably from near the bottom of the container it's in.
Measure out 30 mL of oil
Heat up a frying pan
Pour in the 30 mL of oil
If it pops, bubbles, hisses, produces steam, then it likely has water.

There's a good video of this test in action here:
http://www.utahbiodieselsupply.../qualitytests.php#1a

If there's water in the oil you process, you'll want to remove it before processing as it can really mess up the process.

3) Do a 3/27 test on the fuel. It will give you an indication of how well reacted the fuel is.
Murphy is dead on with this one. I do it with every batch I make.
If it doesn't pass, I'm able to re-react it before I wash it which can help to reduce emulsions or mess up the dry wash media.

Details on how the test works and what it's looking for are here:
http://www.make-biodiesel.org/...le&id=153&Itemid=186
There's also a video there that illustrates how to do it.

Be sure to make sure your temperature of Biodiesel and methanol you use to do the test is between 68 deg. F to 72 deg. F for an accurate result.

4) Increase the mixing time to a full 2 hours
The mixing action in the Freedom Fueler's isn't completely ideal for making Biodiesel so extending the time it mixes can sometimes help.

5) Check the soap content in the Biodiesel
While fuel can be fully reacted (pass a 3/27), it can also be loaded with soap. Biodiesel with lots of soap in it can possibly create the cloudy effect that you indicated.

Here are two tests you can use to check for soap:
A) Shake-Em Up Test (Subjective, not highly accurate, but a good place to start)
- Grab a glass jar (Mason jar, milk jar, etc)
- Fill it half-way full of Biodiesel to be tested
- Fill it the rest of the way with distilled water
- Shake it for about 20-30 seconds
- Allow it to sit for about 45 min to 1 hour
- Look at the water on the bottom
- If the water is hazy & cloudy (like soapy water), you definitely still have soap in the fuel.
- If the water is fairly clear but not quite as clear as the distilled water was, there's a chance it still has soap.
- If the water is as clear as when you put it in, there's a good chance that much of the soap has been removed.

This test is highly subjective to your eye and if distilled water isn't use, it can throw it off. It's a good test though to let you know if you're "close" to getting all the soap out

B) Soap Titration Test
Requires some chemicals, see link below:
http://www.utahbiodieselsupply.../qualitytests.php#4a

Quick version of the test:
Add 10 mL Biodiesel to 100 mL Isopropyl Alcohol
Add 15-20 drops Bromophenol Blue
Add measured amounts of Hydrochloric Acid until it turns yellow
Record the number of milliliters (mL) used
Calculate soap content

Watch the video & you'll see how it's done.

If you find that your fuel still has soap in it, you'll need to continue to wash it.

I've talked to several people that own Freedom Fuelers with the dry wash option. I believe it uses Purolite (the black beads they ship with it).

The canister they ship in my opinion is drastically undersized for the amount of fuel you're trying to dry wash and the flow rate they have you push the fuel through at is way too fast.

One thing you can do is slow the flow of fuel through the canister down significantly (like down to 1/4 as fast as they tell you to go through it).

If the media isn't completely plugged from soap from previous batches, it should help clarify your fuel quite a bit.

So in summary:
1) Check the water content of your oil.
- If it's wet, dry it out before processing it
2) Recalculate your titration, your amount you used was too low
3) Increase the mixing time in your processor to at least 2 hours
4) Perform a 3/27 test on your fuel BEFORE you wash it
- if it fails, consider reprocessing
5) DO NOT attempt to dry wash your fuel if it doesn't pass a 3/27 test. That's a fast way to mess up your dry wash media
6) Slow down the rate of flow by at least 1/4 through your dry wash canisters
7) Perform the Shake-Em Up Test to see if you're getting close to getting all the soaps out. If it's coming out clear, switch over to the Soap Titration Method to identify just how much soap is still left

It's possible to make ASTM quality fuel in a Freedom Fueler, but as Murphy said, to do it you pretty much have to disregard the instructions that ship with the unit. I also recommend performing titrations and calculating the amount of catalyst needed manually instead of relying on their chart. Also, always adjust for your catalyst purity. Doing your own calculations and adjusting for purity will ensure you're adding the right amount.

Here's some simple instructions for how to titrate:
http://www.utahbiodieselsupply.com/titration.php

Murphy has a nice set of instructions as well:
http://www.murphysmachines.com.../how_to_titrate.html

As for the current batch, my gut feel is that it's going to fail a 3/27 and is possibly still loaded with soap.

However, you may just be experiencing some gelling of the fuel depending on what kind of oil you used and what the temperature is where the fuel is being checked. Different kinds of oil can have vastly different gelling properties.

Hope that helps.
-Graydon




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Location: Utah | Registered: October 08, 2004Reply With QuoteReport This Post
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quote:
Originally posted by Leachman_44:
My oil titrated at a 2 then used a 5.5 base number for Naoh Ended up using 1098g for a 40 gallon batch. My oil is heated to 125F and mixed for 1.5 hours and let the glycerine settle for 4 hours then did the 2nd process with the rest of the methoxide and let it settle overnight. Then heated it again and ran through the drywash for 1.5 hours. The next day it was cloudy again so i tried washing again and same result.


What temperature was the fuel when it was clowdy? If you passed 3/27, and went through ion-exchange, then you could be using a higly saturated oil such as lard or hydrogenated oil.

I would NOT use more catalyst unless there is a reason to. If you passed 3/27, there is no reason to.

With more information regarding your process and quality control tests, it would be easier to troubleshoot.
 
Location: CO, CA, KS, or FL | Registered: January 17, 2009Reply With QuoteReport This Post



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Originally posted by HelpingHand:
I would NOT use more catalyst unless there is a reason to. If you passed 3/27, there is no reason to.
I agree with helpinghand. You used about 7.2g NaOH per liter of oil titrating 2. That should give you very high conversion fuel.
If your biodiesel already passes 3/27 and you add extra NaOH you will make LOTS of soap. You could easily end up with 40 gallons of solid soap in your reactor. Not a fun occurrence.

You now need to do a 3/27 test to see where you stand.
 
Location: Southside | Registered: January 12, 2010Reply With QuoteReport This Post
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