[Spencnaz]

Ok,

I got 50 gallons of brown jello, how do I get this stuff outta my reactor now?

I took a test sample last night and let it settle in a jar on my desk last night. When I looked at it, it had the consistency of solidified beef gravy, saponifaction /ubbthreads/images/graemlins/mad.gif

So again, what do I do to get this stuff outta my reactor? Heat it up and hope for the best as I try to suck this goop out?

 

[TDISteve]

I have never had a bad batch so this is pure conjecture but you may need to remove the bottom fitting and blast hot water in. What a mess! If you try to heat it you may burn out the element. I use KOH, no jelly.

 

[Spencnaz]

I think there is one fatal flaw with my process here, no heat. I started the reaction without heat as the elements werent hooked up to power.

My titration amounts were correct (unless my titration was off). I'm off to figure out what happend. /ubbthreads/images/graemlins/confused.gif /ubbthreads/images/graemlins/mad.gif

 

[girlmark]

uh oh. The solution to this is to heat it till it liquifies.


Then you turn off the heat and then drain/pump the warm stuff out. Be aware that it'll have methanol in it so dont' huff it while you're draining.

Looks like you have to hook up your heating elements now.

Mark

 

[Spencnaz]

Well all is not lost. I went over to the reactor today and it was still fluid and flowing.

I put a test sample on the stove and heated it to 140F. Noticed a scummy looking foam coming to the top. I skimmed it off and noticed that the oil clarified but it wasnt see thru.

The stuff in the reactor is still a cappachino (dont know of any other analogy) color and frothy. I pulled another test sample and will wait for it to settle.

I'm going to hold fire here until I can get the water heater again wired to 220V again.

That's the status report for today. I keep thinking that my titration was off somehow, perhaps crosscontamination of lab equipment or something. But the main culprit I believe was the lack of heat.

Next time, test batches.....

 

[girlmark]

did your test sample drop any glycerine after it cooled?

in fact, do you have two layers or not?

Mark

 

[h2odrx]

do i understand you? you did not heat your oil before you added the methox?
thanks

 

[Spencnaz]

Nope, didnt see any discernable layers. It was a homogeneous and straw brown in color.

I did notice that after last night, it had formed a gelatinous mass in the sample jar I took last night.

When I ran the pump again today, the oil mixture was still fluid. I will check the sample container again tomorrow.

I sure hope that I dont have to dump this stuff after I run heat thru this.

 

[girlmark]

take a liter and try to do a re-process to it to fix it.
how much of everything did you use, and did you do a titration, and if so, what were the results?


you probably did one of two things:
1. the reaction didn't go far enough to even make some glycerine

or
2. you've made biodiesel but you made so much soap that you're not seeing any glycerine.



If you have problem #1 above, you can fix it by adding more methanol/lye (they have to be mixed together first). TRy a sample batch by taking a liter of the goo and re-processing with 50 ml methanol and 1 gram lye. You can also do a few of these 1-liter batches and try varying amounts of lye

If you have problem #2 you can't fix that by reprocessing but you might be able to wash a liter (GENTLY) and that might make it further into biodiesel.

First, tell us what ingredients (how much) you used...

Mark

 

[Spencnaz]

Ok here is what my calculations yielded:

50 gallons WVO filtered

11 gallons methanol (about 22% of volume to force the reaction)

1242.7 grams of Lye total

No heat was applied to said components, ambient temperature as indicated on gauges was approximately 80 degrees +/- 5 degrees

My initial titration average was 2.5ml. Initial values of reactants were

10 gallons methanol and 758.5 grams NaOH. After recalculating my error the difference of one gallon of methanol and 484.2g of NaOH was added to give the totals stated at the beginning of this post.

Initial agitation time = 2 hours. I deemed this necessary due to the lack of heat input to the reaction.

Titration of a sample pulled today showed a result of 1mg lye needed (?). This is where I have the biggest question.

There is all the data that I have written down in the logbook in a nutshell.

Is there hidden water in the WVO that is inhibiting this reaction?

 

[Spencnaz]

Any opinion on what happend now that I've given the factors girl_mark?

I'm going to see what it looks like either tonight or Wednesday to see if anything has settled out.

 

[Spencnaz]

Ok I took the sample I have (under 1 liter probably about .75l) and added 20ml of water to and agitated gently (end over end) about 20 times.

It's now a light beige in color and looks like a thin milkshake.

 

[Spencnaz]

Update as of last night (7/13/05). I froze this concoction in the freezer Tuesday night and came home yesterday after a days thawing out to a layer of light brown (beige) liquid underneath a dark beer colored liquid occupying the upper 3/4 of the bottle

Have I broken the emulsion with freezing? Remember that in my earlier post I added water and agitated gently.

Input please.

 

[Spencnaz]

Update Seattle......(cue teletype and important news music)

I got the water heater hooked to power, 220v and turned on the heaters, immediately I could hear the oil bubbling and I switched on the pump. The pump was really clogged with glycerol glop but eventually started working.

I have since drained it to a wash tank and the first layer had the consistency of applesauce but dramatically thinned out as more and more heated oil at 130F came out. The sides of the wash tank were quite warm even after about an hour.

So there's my update, now to the wash process.