Folks,

A couple or years ago I published what's become know as the 'dkenny' method.

as good as this method is...

I have been working with another bd maker, Biotom, who has been using, not a formula but a fine tuned knowledge combined with a consistent source of lousy oil. If I remember correctly its normally around 10 KOH. Biotom jump in and add details.

we've been working on combining methods.
It looks like the 0.2 multiplier in my method need improvement..Biotom typically get the titration to 1 to 1.5KOH instead of 3 or so. That was happy with. It looks like the new multiplier should around 0.15 - 0.17.. so the formula would be T-3 * 0.17 or T-3 * 0.15.
same amount of methanol 12% of the oil volume.

the Problem??
back in January my oil supplier sold his business.. I lost my source of bad oil..the worst I've is around 5KOH..

So what I'd like to ask for current BD makers that use acid esterification to validate the new multipler. so I need volunteers..
1. take a batch of your lousy oil that you've had good results using the 0.2 multiplier and use 0.17 insted. please post your results
2. I like to the testing in a range of titrations. ideally KOH. less than 10, 10-14,14-18, and 18 and up.

risks..
the batch might not drop as far, but it might drop futher??
the range for required draining might change? I think it might shift higher, say 16-20, instead of 14-18.


some other differences
Biotom adds acid to oil, mixes then adds methanol. I'll leave this open if anyone wants to try it this way. after the stuff is all mixed he only run the pump for about 20 mintues then turn it off. leaves it over night. remixes after 24 hrs, checks the titration then start with a base/base process. He's also verified that heat is needed. active heat( might be dangerous, remember the pump is off) or sufficient insulation. Again Biotom, add details..

who's game..
I'd like to use the results to update Richdatech site( make-biodiesel.org) and the CBT.
if anyone wants credit..it shall be given in the update..all I ask is after its released you verify that I didn't accidentally forget you.

Thanks for your time

-dkenny

Friends

-I have been using acid esterfication for several years now, as Dave stated I have a steady supply of BAD oil T 8 - 10, and had to learn how to make the best of it. Base/base, plus reprocess plus reprocess and so on just wasn't doing it for me. I read here about the fatta method back in 2005, using 1 - 2 ml of acid per ltr of oil, and although this method works , the results weren't consistant so I still had to reprocess often. I experimented whith differing amouts of acid, heat on, heat off, more methanol, less methanol and so on. So, now I do acid base base every batch, and most recently acid base base base. The latter takes longer but the results are very good.
-for the acid treatment, I found .75 ml/ltr of oil and 15 ltr of methanol. 10% (batch size 150 ltr) this results in a T of .75 - 1.7 in 12 - 14 hrs the lower T if 12% methanol is used. HEAT ON
-I use a HW tank immersion heater controlled by the lower element Tstat. set at 140f.
-I use a ph meter to check T solution, and oil sample If starting ph of sample is 1.5 after Treatment. I've used too much acid and will ultimately use 1 -1.5 gr/ltr more koh. the target ph of the sample for me is 2.5
-some of you my have read my posts about the violent reaction I encountered mixing acid into methanol lucky for me water and baking soda were close at hand! I know people do it this way, but I will never recommend it. I find it much safer to handle a small amount of acid to mix directly into the oil. otherwise, I would have to handle 15ltr of very acidic methanol. why take the risk!!!
-I'm not sure what else I can add here, but will answer any questions posted here Tom

Hi there Dave Kenny ---- I would not have contemplated trying the acid method if it were not for you and that other knowlegable chap -Antifuel 1. You might remember me asking you questions about my not particularly good reactions when I first tried the acid method & you suggested it might be water in my oil & so I always heat my 150 ltr 'batch'of oil overnight to 220F.My oil then was 7.5KOH but now it is good oil and titrates at between 1 and 3.5 KOH. I realise I am a total novice and I'm told I don't need to use the acid method with my oil being so good but on seeing an article that the commercial producers in the USA use this method down to 1 titration I thought I'd try it due to my finding that the straight KOH method seemed to vary in the fuel quality and especially the clearing of it.
I based my acid calcs on your .2 maths to arrive at a theroretical 0 KOH after the acid is done. I may well be wrong but I don't titrate after I have processed the acid stage for two hours!!!! I then add the KOH stage as if it is new oil at 8 grms per ltr. I process this last stage for two hours. I maintain heat with two 3 KW immersions in series controlled by a seperate adjustible stat and the temp of the first stage is at 140 deg F throughout. I find the temp stays at above 130 even with the heat off as I find the temp increases when I add the KOH and last half of the meth. I have stuck to the 20% methanol total calc since I started back in August last year and just divide it by 2 in each of the acid then alcali stages. I started trying to 'wash' my fuel with water to start with found it quite a chore and decided to try the dry filtering method and I now have 10 micron & 5 & then 1 micron 10 inch filters fastened together in a 'bank'. If I'm careful to not suck up any glycerol this set of filters has done 350 galls of fuel at least. I found with experience that patience is definately a virtue because if after draining off the black stuff I then heated the fuel to 75C to drive off the 3% meth left in the finished fuel I then left it at least 2 more days before filtering it was clear and filtering could be carried out -however I noticed that there was a little fine brown sediment at the bottom of some of my fuel containers so I wonder if indeed there is some further chemical reaction which has taken place in the finished fuel?? If I'm patient,I ask myself can this fine sediment be avoided if I wait longer before filtering????
In conclusion I feel most grateful & appreciative your help and whilst I realise my method is perhapse not as acurate as you method teachings at least I find it works admirably and I find it not a chore at all in fact I quite look forward to the straightforward way I have now got used to.. Thanks a million and regards from Mick Hall in the UK ----- P.S. -- I wonder does the curry powder and other spice additives which I can smell in my oil -have any thing to do with my excellent reactions ??????? (tongue in cheek)

dkenny, biotom, etal

Would you please state the concentration of the acid used when listing the acid amount?

quote:

Originally posted by Biotom:
. . . I experimented whith differing amouts of acid, . . .

-for the acid treatment, I found .75 ml/ltr of oil and 15 ltr of methanol. . . .

It helps me to understand the differences/similarities in the various mix ratios.
Thanks

Biotom,

I have a lot of questions. DKenny says you get it down to nearly 1 after the acid stage. What was your starting titration again? What is the target? What is the multiplier? How do we convert this from KOH th NaOH? Thanks.

My oil is usually not so bad, but I would try it anyway just to try to get it down to 1.

My acid concentration ranges from 93% to 98%. this does have some effect but not much.

Biotom what's yours?

-dkenny

Since using and remembering the raw formula off the top of my head was too difficult for me, I made a quick reference sheet a long time ago.

Here would be the new one.



The new curve appears below the curve for the old method. I split the difference and used .16 for the .15-.17 mL acid / L oil range suggested. You can see, the difference between the two methods becomes more apparent for higher titration oil.

Oh, the color change in the line represents the point at which a draining step has been suggested. That could change in the lower curve as more experimentation is done, as dkenny mentioned.

Eurocab

my oil T's at between 8 - 10 althought the last oil was realy good, T 7.5
I will post the results of the testing here, testing was done over a 10 day period, one sample kept hot, the other allowed to cool and stay at room temp. On the last day, the cold sample was reheated and tested I'm sure you will find the results interest as dave and I did.

Dave

the acid I purchased is 93% Tom

Ryan P

I like the graf you provided, now we need people with bad oil to varify this. I'm on the hut for higher T oil Tom

The tank full I have sitting at home warm will likely titrate at 9ml, since the batch I made previously from the same tote was 9ml. I'll give it a whirl and see what happens.

this is the result from the first test. note I use 4ml oil in 40 ml IPA


sample 1 (hot)
-start temp 70f
-start ph.............1.3
-add 4ml..............ph7.2
-add 2ml..............ph7.3
-add 4ml..............ph7.5
-add 4ml..............ph7.8
-add 3ml..............ph8.5 Bingo
- acid # = 17 divided by 4 = 4.25
-I don't T the way it is posted on CBT ,I follow T the better way from JTF ( the only good thing I got from that board) this is a surpising result for me , because T is always 1.5-1.7 the only differance was the heat !!!!

sample 2(cold)
-start temp 70f
-start ph..............1.5
-add 4ml...............ph8.3
-add 1ml...............ph8.8
-acid # = 5 divide by 4 = 1.25 gr KOH couldn't believe these test reults so I retested both samples and results were unchanged go figure

sample 3 stock oil from heated holding tank
-start T 70f
-start ph..............7
-add 4ml..............7.2
-add 4ml..............7.1
-add 4ml..............7.0
-add 4ml..............7.1
-add 4ml..............7.2
-add 4ml..............7.4
-add 4ml..............7.8
-add 4ml..............8.6
-acid # 32 divide by 4 = 8gr KOH

The following are the results from the last test. 10 days after first sample was Tested

Hot sample
-ph of T solution ......................11.0
-starting ph of hot sample.................1.5
-add 1ml solution...............................ph6.1
-add 1ml solution...............................ph7.6
-add 1ml solution...............................ph8.0
-add 1ml solution...............................ph8.5
Total 4 divided by 4 = 1gr KOH

Cold sample

-starting ph.................................1.5
-add 4ml solution...............................ph7.2
-add 4ml solution...............................ph7.5
-add 4ml solution...............................ph8.1
-add 1ml solution...............................ph8.5
Total 13 divided by 4 = 3.25gr KOH

Cold sample heated for 16 hr
-starting ph..................................1.4
-add 4ml solution...............................ph8
-add 1ml solution...............................ph8.6
Total 5 divided by 4 = 1.25gr KOH

Ryan P

I look forward to your results Tom

Ryan P,

please give it a try..

I'm going to try to keep track of all the results and see what comes out.

then update the doc on how to do acid/base processing.

Thanks

-dkenny

Im in. Ill try using a multiplier of .15
Also, as some know, I get some oil that has contaminants in it, and now wash and dry that particular oil before reacting. Once washed, that oil now goes to a titration of 22, so it should be a good test for the higher ranges.

hooknline,

that would be great to try..just what we're looking for some with 'bad' oil not just lousy.

I know with the 0.2 multiplier we can get this to 3 KOH, but can we do better???

please just run your normal acid stage, titrate then stop..when happens next might change from normal. you might need more methanol only, more acid or both??

-dkenny

ps sure wish I had some bad oil to play with as well. but would need a couple of hundred gallons..I don't working in sample sizes.

batch of oil(250L) with a T of 14KOH in the processor now with 60% methanol and a multiplier of .15. 2 hr mix, then I will check in the am to see what I have
update: 2 hr mix last night, let sit for 12 hrs. Just checked T and it is 7. Starting temp was 130, is 115F right now.
I am mixing for another 2 right now, then I will recheck T
update#2: mixed another 2 hours. Titrated at 1 hr and at 2 hr. 1hr T was 5, 2hr T was 9????? both T's repeated to verify.
Here's what Im wondering. If the creation of water is a side reaction, will the longer it is mixed, and the higher initial T create more water than a shorter mix time and a lower initial T? This would contaminate the available methanol, requiring more methanol in the acid stage for a higher intital T??? Kinda like the chart that Ryan put up, but also correlating to methanol needed as well as acid needed?
update #3: Just added 10% more methanol(3L)for a total of 70%, with 1ml/L acid and mixing some more to see what that gets me. I like experimenting.
update #4: t is now 4 after 1 hr mixing. Will check again in 1 hr\
update # 5: T is now 1.75 Im going to let it run another 1/2 hour and see how low it gets.

This message has been edited. Last edited by: hooknline,

Alright, final T of 1.5 Down from a starting T of 14! Incredible. total of 2.5ml/l and 70% of the methanol instead of 60%. total mix time of 5 hrs, the rest was just time settling and doing its thing, about 13 hrs of no mixing. ending temp 115F. Hope this info helps