I think we're talking about different scenarios. Theres a big difference between the standards required by commercial producers and homebrewers. I would recommend resin to anyone making their own biodiesel, but no doubt its not so suitable for purifying quantities on an industrial scale.

Rick, That is exactly what I am shooting for.

Jehu,

I felt like after all this research I had to say my peace on the subject. It's not a cure all. If you guys want to use it, then just know your not likely to meet the full ASTM specs. Flash point and acid number are very difficult to meet when using resins in the homebrew world. If these are not an issue for you then the resins will do you well.

I've said my peace. Go forth and bio.

I am not going to get ultra technical, but just relate my experience.
Aftre reaction I settle in a seperate drum. This can be overnight or a few days. Then it goes to what was my wash tank equipped with a standpipe minus the glyc layer that stayed behind in the first settling tank.
I used to run the BD through a bag filter for a couple hours but have since opted for heat instead. I heat up the BD in this second settling tank until the methanol starts evaporating and then switch drain ports from teh floor drain to the standpipe drain until it cools. I then shut it down and allow it to settle again either overnight or a couple days.
I do not demeth at this time.
The BD is then sent through a lead and lag resin configuration followed by a 2 micron CAT canister type fuel filter.

Now, the evidence:
Of the samples I submitted for GC testing other than those that were water washed and dried were two destined for resin purification.

One sample came from the mix before it went throughthe rsin and the other right after resin from the same flow. Before resin it hit ASTM for free and total glycerine at .240, right on the edge. After resin it recorded a .161, a positive pass. I did not have a full spectrum analysis done.

The tell tale here is the 2 micron CAT can I use as a final filter.

When I was water washing ect these same 2 micron cans were getting clogged on a very regular schedule, and at that time I was running two in series. Yes the resultant biodiesel did pass the same ASTM standard as the former, one at .203 and the other at .109, the lower number being one sample that had frozen and thawed several times over the winter.

I am finding that by heating the biodiesel and then letting it settle before sending it thorugh the resin is leaving me with a layer of gunk on the floor of the second settling tank.
I am still using the same CAT can as a final filter that I started out with this year, so there are no appreciative residuals still in the fuel or it would do what it did previously, clog up and stop allowing flow.

The layman's test of filling a jar and reading newsprint through it has me not only reading newsprint but being able to clearly see across the courtyard like through amber sunglasses, easily able to make out details several meters away.

Even though this is not the recommended optimised way to use resin and will unduly reduce it's overall life it is still well worth it to me in time and energy savings as well as waste water stream elimination.

At a mere 50USgal to the Lb of resin it adds .05/Lt to my pocket costs as opposed to perhaps twice the savings or more. This is a trade off for me, one I am willing to accept given the benefits of using resin over what I considered quite an avant garde water washing method I developped some time ago that was considerably more time efficient than what is still being used today by most people involved in homebased biodiesel production. Resin purification has been a definite step upwards.
I use Purolite PD 206 in twin reverse flow tanks modified for resin retention.

No prob Rick. I know where youre coming from. I'm happy with the convenience and reliability I get from resin compared to water washing. I prefer a cheap and cheerful lower grade fuel that does the job rather than spend a lot of time getting things perfect, but I know thats required in other situations.

Not to whiz on anyone's parade, but the NBB did some random testing awhile back and found that over 50% of all the commercial fascilities it tested were not complying to ASTM standards for B100, so using commercial producers as any sort of quality standard is warping the results from the onset.

What I have noticed is that my cars run better on the fuel I am producing now compared to the previous years. Is the flashpoint a little higher than ASTM ? Probably, but then when it comes to biodiesel it has plenty of room to maneuver in that department already being so off the chart complared to dino diesel.

What if, and that is hypothetical, the flash point of resin purified biodiesel is 200F instead of 320F when water washed and dried ?

So what? It is still well higher than the flash point of dino at 125F which runs just fine in any finicky diesel engine out there. If methanol residuals is the ONLY concern here it is a non starter IMO.

The tractors and cars running on it right now are not exhibiting any sort of awkward behaviour after thousands of litres being put through them.

Hey guys,

After reading this thread (and then re-reading it again to try to get a better understanding of what's going on), I still have a couple of questions:

First, can someone help me understand the difference between KOH and NaOH for doing the resin purification? I had been reading quite a bit about this over the past few months, but hadn't come across stuff that talked much about the difference. Fabricator indicated that KOH is a fairly different beast than NaOH. I knew some differences, but had planned on using KOH because it left my glycerine in more of a 'liquid' state, allowing me to settle for longer periods of time (possibly several days) without getting a hard layer at the bottom of my reactor/settling tank. When thinking of using the GL Push-Pull, is NaOH better than KOH (especially when considering the idea of resin purification as a last step)? I haven't settled on either type of catalyst, but had assumed I'd go with KOH, to give me the max settling time with the least amount of issues. If it's easier to point to threads that will help me understand, that would be fine also...just trying to learn more.

Second, can someone who is using a CF on finished product help me better understand their workflow? I believe it is:
Filter WVO - Process - Settle (how long?) - demeth (what process? - in using GL's process, I thought this was done in the processor) - Centrifuge - storage/vehicle
Is that about right?

I hadn't looked at the resins as being the panecea to everything, but I was hoping to have a process similar to:
Filter WVO (with CF) - Add Glycerine pre-wash to reduce H20 and Titration - Settle 1 day - Process (with KOH, using GL's PushPull, recovering methanol in the process) - Settle 2-3 days - push through resin @ very slow flow - storage/vehicle.
which I was hoping would give me good clean, ASTM fuel (or fuel of a quality that would run without issues in both of my direct-injection engines). Now I'm wondering if I want to add a CF immediately prior to the resin bed also.

I don't know if it makes any difference, but my current oil source titrates at 1.2 to 1.6 - I've heard that the glycerine pre-wash can bring that down to 10-20% of it's original titration, giving me something in the 0.3 range (no experience to back this up yet though).

Anyway, any help pointing me in the right direction to get answers to my KOH vs NaOH and my 'whats the right workflow' questions would be great. Based on this thread, I will be using resin but watching with a critical eye to see how it benefits me in my particular circumstance. I'll post on my experiences.

Thanks again,
-Scott

Rick,

You have said your peace however almost all of it is what I have been putting on the web for the last 6 months (over and over again).

In fact, the very information you are getting from Purolite has been corroborated by myself. I talk regularly with the person who helps write the presentations papers.

In particularly, we originally dissected this issue of FFA production from Soaps when using the Hydrogen Form PD206; since my research over the last 2.5 years initially indicated the European Macroporous resin in Na+ form was the way to go.

I eventually derived the idea of using the Na+ Marcroporous resin in a lead column and the gel-type PD206 in a lag column to deal with the high FFA content of Used cooking oil and other High FFA feedstocks.

This idea was recently tested by another facility and found to be exactly correct in its initial assumptions:

1) The Na+ form would not remove glycerin and soap as well as the gel-type resins but it could remove the bulk majority with out producing FFA from crude biodiesel containing high ppm soap concentrations.
2) That the gel type resins could then be used on a range of total impurities, well below the level of solubility, resulting in long resin life span and biodiesel purified well below ASTM levels.
3) That the Macroporous resin unlike the gel resin is a much more robust plastic bead - doesn't expand nearly as much as the PD206 resin and can therefore tolerate >20 flushes with methanol with out a loss in performance.
Making its long-term cost go to < 1 cent per lb of resin.

Some time after working all this out; every one learned about the GL 1-day process which took advantage of the simple chemical fact that methyl ester is neither miscible with soap nor glycerin therefore if you remove enough methanol both will naturally fall out of solution -- to some degree depending on methanol content, catalyst and how long a brewer was willing to settle.

So it became apparent that it was now possible for the homebrewer to us either the gel resin or other Hydrogen form resins on biodiesel with impurities at the level of solubility. This gauranteed ASTM fuel or better in the area of total glycerins and soaps -- as Legal Eagle's and ABC's GC analysis have shown.

Now the issue of methanol vs. glycerin and soaps in biodiesel. Although some people choose to run unwashed biodiesel (meaning it still has some free glycerin, dissolved glycerin, soaps and methanol in it primarily); there are some valid concerns when doing this and I would suggest these concerns have a lot to do with choice of catalyst and settling time.
Be that as it may residual soaps and glycerins in higher concentrations have shown to not fully combust (particulary glycerin) and therefore polymerize and form deposits in engines (this is BAD).

Where as, the diliterious effects of an excess methanol concentration (typical for settled biodiesel) on engines is less substantiated. In fact a little excess methanol scrubs out water content and also improves cold weather performance of biodiesel (viscosity and gelling).

Lastly residual soaps and glycerins if dissolved in biodiesel due to excess methanol content, will settle out if any methanol evaporates over time; making it more of a filter plugging problem for engines, if stored for any period of time.

In the end, each biodiesel producer needs to look at their desires and the particular parameters of use. Resin purification won't be for everyone.

Producers like Fabricator using a potassium catalyst, have quick turn around time, use used cooking oils, can't determine adequately the methanol content and only desire good usable fuel - aren't necessarily likely candidates.


On the other hand people who settle for 24 hours or more, use a sodium catalyst want to ensure ASTM levels of total glyercins and soap along with other impurities and need better cold weather performance are very strong candidates for using resin purification processes.

GCG

PS please note that the Na+ form GF202 resin had one other important test result - Sodium (Na+) "leeching". The resin needs to be thoroughly flushed and the lag bed becomes even more important because of this.

quote:

Originally posted by handcuff:
Hey guys,


First, can someone help me understand the difference between KOH and NaOH for doing the resin purification? i'liquid' state, allowing me to settle for longer periods of time (possibly several days) without getting a hard layer at the bottom of my reactor/settling tank. When thinking of using the GL Push-Pull, is NaOH better than KOH (especially when considering the idea of resin purification as a last step)?

Second, can someone who is using a CF on finished product help me better understand their workflow? I believe it is:
Filter WVO - Process - Settle (how long?) - demeth (what process? - in using GL's process, I thought this was done in the processor) - Centrifuge - storage/vehicle
Is that about right?

I hadn't looked at the resins as being the panecea to everything, but I was hoping to have a process similar to:
Filter WVO (with CF) - Add Glycerine pre-wash to reduce H20 and Titration - Settle 1 day - Process (with KOH, using GL's PushPull, recovering methanol in the process) - Settle 2-3 days - push through resin @ very slow flow - storage/vehicle.
which I was hoping would give me good clean, ASTM fuel (or fuel of a quality that would run without issues in both of my direct-injection engines). Now I'm wondering if I want to add a CF immediately prior to the resin bed also.

I don't know if it makes any difference, but my current oil source titrates at 1.2 to 1.6 - I've heard that the glycerine pre-wash can bring that down to 10-20% of it's original titration, giving me something in the 0.3 range (no experience to back this up yet though).

Anyway, any help pointing me in the right direction to get answers to my KOH vs NaOH and my 'whats the right workflow' questions would be great.

Thanks again,
-Scott

HC,

KOH just doesn't settle out as readily even after removing methanol so the GL 1-day process doesn't work in 1 day. In terms of resin use it simply slows the process down if your relying on settling out soaps prior to the resin column purification.

If your using the Spinner type or OC20 type CF then Fabricator is the best person to answer this particular question however he isn't using Resin for purification so he may not run in the best order for you.

We currently run our centrifuge prior to removing methanol since we don't want reverse reactions due to the presence of glycerin and catalyst in the same mix minus an excess of methanol. With the spinnner CF you might choose an initial gravity settle for 25 minutes, drop out 97% of the glycerin created, neutralize the catalyst with a very small addition of sulfuric acid, methanol removal/recovery, spinner CF for gunk, ion exchange columns.

For 1.2 - 1.6 are you using KOH as a testing base? Is this reported in terms of FFA or in terms of a total acid number? Either way it is very good oil...

GCG

GCG,

Thanks for the help with the additional information. Given what you are saying, I may end up going with NaOH instead of KOH, since it falls out more readily.

My goal was to give it multiple days to fall out before going on to the next phase (even with GL's process that has it dropping faster). With NaOH, I've heard that this created the risk of it becoming hard in the bottom of the processor and not coming out (or not coming out nearly as easily). Is there a way to prevent this, or is it just a thing where you need to drain it every few hours to keep it from getting too built up?

My titration is 1.2 - 1.6 using KOH. I don't fully understand the difference between checking FFA or total acid number. My guess is it is total acid number, as this is what we were adding to the base number to get to the amount of KOH to add to the batch.

Thanks,
-Scott

[QUOTE]Originally posted by RickDaTech:
I CALL BS!
can someone explain why I'm better off using any one of these ion exchange resins? [QUOTE]

How much BD do you make per year??
What vehicle do you run it in??

Handcuff;
I use NaOH exclusively, always have, and the only time I have had teh glyc harden in a drum is when I left it there over the winter.

The method I am using sees very very little additional glycerine available for dropping out. This is witnessed by the type of scum I am getting on the drum floor.

I do not leave anything to settle in the reactor, which in my case is a water heater as these do not drain cleanly and have a lip at the outlet port that captures varying amounts of glycerine depending on the type of water heater used. In my case that is a litre or so with more rsiduals dripping out over the next couple days.

So, as soon as the reaction is done I transfer the lot over to a seperate dedicated settling tank(drum) equipped with a standpipe where the glycerine will drop below the standpipe's outlet and then I can transfer glyc-free biodiesel over to the standby tank (former wash tank) also equipped with a standpipe for heating and partial demething before using the standpipe's outlet for transfer into the resin beds finishing it all off with a 2 micron CAT canister type filter for use or storage.

Legal,

I had also heard that KOH was more "forgiving" than NaOH with various oils (and thus, a tad easier for the 'newbie' home brewer). That was something that I heard less frequently than the hardening issue, but those were the two reasons I was going to use KOH.

In retrospect, I will probably use NaOH and let it settle for 2-3 days, while draining out the glycerine every 6-8 hours or so. I think that should allow decent mitigation of all the issues (plus allow me to make soap, which was a concern of mine with KOH).

I'll be settling in the reactor, so I am still somewhat concerned. Won't be able to do any of it until I get my pump (still waiting for David from Biodiesel Systems to deliver the pump I bought a few months ago).

-Scott

quote:

You have said your peace however almost all of it is what I have been putting on the web for the last 6 months (over and over again).

Yes you have been saying all this all along.

[QUOTE]Originally posted by RickDaTech:
I CALL BS!
can someone explain why I'm better off using any one of these ion exchange resins? [QUOTE]

How much BD do you make per year?? What do you run it in???
I Guess NONE!!!!!!!!!!

Originally posted by Jehu:
once the glycerol has been drained a few litres of hot water sprinkled into the batch without mixing and drained off in the morning will remove some of the contaminants and increase resin life.



Jehu, what if this small water bath was done after demeth while the bio was settling out soaps via GL1day?

1. will this be to much water to settle out before sending it on to the resins?

2. would it be better to spray the water while the bio is hot (right after demeth) or wait until its room temp?

3. how long would it take for the water to settle out?



DW

quote:

Originally posted by RickDaTech:
Can someone explain why I'm better off using any one of these ion exchange resins?

• They don't save any time
  
• They add cost
  
• You don't need resins with the GL method
  

Hi Rick
I was glad when resins came out and I would defend them, altho I've moved on from them because of the cost:

"They dont save time" - actually that was one of the big plusses for resins; they saved me loads of time compared to water washing;

"They add cost" - the resin was a bit expensive, but I found water washing was expensive too in terms of the hot water used.

"You dont need resins with the GL method" - thats true, but then you dont need the GL method with resin either.

I combine the GL method with sawdust dry washing and it works as well as water washing and resin, but saves removes much of the labour associated with water washes and removes the expense of resin. But otherwise I'd prefer resin to water washing any day.

PS - Sorry Rick, I mistook this for a new post, but actually it was nsolo who posted and made me think you had just posted.

Jehu,

Did you see my question before your last post?



DW

quote:

Originally posted by hsolo:
Originally posted by Jehu:
once the glycerol has been drained a few litres of hot water sprinkled into the batch without mixing and drained off in the morning will remove some of the contaminants and increase resin life.

Jehu, what if this small water bath was done after demeth while the bio was settling out soaps via GL1day?
1. will this be to much water to settle out before sending it on to the resins?
2. would it be better to spray the water while the bio is hot (right after demeth) or wait until its room temp?
3. how long would it take for the water to settle out?

DW

Sorry Nsolo, I didnt see your post - I thought Rick had posted so I was replying to him

1: the water falls straight to the bottom, and as there is no agitation it doesnt make the biodiesel damp. It extracts a small amount of soap on the way down but most dissolves in the water layer as it sits overnight.
2:Yes its definitely better done right away when the biodiesel is still hot.
3: The water settles out right away, but the idea is to leave it sitting overnight to give the soap time to be absorbed.

Jehu,

thanks, just a few more questions.


1. with a 125L batch, say 2 or 3 liters misted with a windex bottle?

2. do i have to drain after the water settles overnite or can i just leave to settle until im ready to use it ( i have a standpipe to draw from )


im planning to use KOH, so i wanted to test this method against ---

1. circulating until the last bit of meth is gone then settling

2. using a column with red oak sawdust


any other info on this settling wash would be helpful.


thanks, DW