Author Topic: Enhanced gly wash  (Read 1146 times)

Offline mauser

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Enhanced gly wash
« on: December 28, 2023, 03:36:57 PM »
   
     Glad to see this forum still in business, thanks

   So, ive been given 400 lts of reclaimed meth (hydrometer tested to be 93.2 %) and 30 kg of koh.

   I wbd with naoh , b/s , polish with red oak sawdust. Since i use naoh im trying to find ways to incorporate these chems in my process.

   1)  after wbd, drain noah gly into 12lts reclaimed meth with 1.5g koh/lts of oil . Titration of my oil is 2.5

   2)  I plan to start using the no tit process. If i add 4lts to the s1 (18% volume ) with 21lts virgin meth, would that be to much reclaimed to add 

Offline dgs

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Re: Enhanced gly wash
« Reply #1 on: December 29, 2023, 10:15:42 AM »
   
     Glad to see this forum still in business, thanks

   So, ive been given 400 lts of reclaimed meth (hydrometer tested to be 93.2 %) and 30 kg of koh.

   I wbd with naoh , b/s , polish with red oak sawdust. Since i use naoh im trying to find ways to incorporate these chems in my process.

   1)  after wbd, drain noah gly into 12lts reclaimed meth with 1.5g koh/lts of oil . Titration of my oil is 2.5

   2)  I plan to start using the no tit process. If i add 4lts to the s1 (18% volume ) with 21lts virgin meth, would that be to much reclaimed to add

Hi mauser and welcome to the forum.

The enhanced glyc wash method is really to reduce the acid value of high titrating oils, whilst removing any water caused by ffa neutralisation.

Re your point 1 I'm not sure why you would drain your glycerol into your reclaimed methanol. In any case wbd is counter productive. ok, so you reclaim some methanol but most of the value of glycerol is the biodiesel held in it by the soap, wbd won't reclaim this biodiesel. However a glyc wash will recover most of your methanol and the biodiesel.

Re point 2 Based on your figures the mix of reclaimed and virgin methanol will work ok. I have used reclaimed with 1% water content with only a very small reduction in yield.

You could always dry your wet methanol with cement powder ( a bit messy but it does work )
FOC water tests by Sandy brae or Karl Fischer for forum members.

Offline mauser

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Re: Enhanced gly wash
« Reply #2 on: December 29, 2023, 03:38:25 PM »
   
    Hi dgs, Thanks for the reply.

    Regarding point 1,  maybe i didnt explain that well enough. After wbd the noah gly has only residual meth and will solidify in short order.

    My reasoning was to use the 93% reclaimed meth to liquify the naoh gly and ready it for the next batch of oil. This would ( i hope ) remove the water in the 93% meth by migrating it to the gly and yet being able to help neutralize ffa.

    To be clear, the 93% meth i speak of, was given to me and i did not distill it. My wbd distillate is 98% +.

Quote
I have used reclaimed with 1% water content with only a very small reduction in yield.

   What % was the reclaimed that had 1% water content?

   As for wbd being counter productive, to each his own, i have no plans to join the water washing club. Im sure my methods will evolve, but for now, wbd is the donkey im riding to chase windmills

   Cheers

Offline dgs

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Re: Enhanced gly wash
« Reply #3 on: December 29, 2023, 04:29:07 PM »
Hi mauser, ok, I understand now. when you mix your reclaimed with the glycerol, then add as your glyc wash I wonder how much water will be retained by the glycerol or will the water react with the small amount of catalyst in the glycerol and just make more soap. I'm sure you will find out.

BTW, you don't mention a batch size.

The methanol with 1% water was quoted as being a minimum of 97% methanol. I tested the water at 1% (sandy brae) I have no idea of other solvents present.

Just a tip, you will get a good reaction if you use a 50/50 mix of KOH and NaOH. Glyc won't go solid. Split your batch into half (on paper) use your base of each into the same methanol (KOH first, then use the methoxide heat to dissolve the NaOH faster.

Cheers, Dave.
FOC water tests by Sandy brae or Karl Fischer for forum members.

Offline countrypaul

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Re: Enhanced gly wash
« Reply #4 on: January 01, 2024, 11:06:11 AM »
Hi Mauser,

It seems quite wasteful and unneccessary to do a WBD then add methanol back into the glycerol. Droppig the glycerol before demth will save energy (since you are not demething the glycerol) and allow the glycerol (with bio and meth still present) to be used for washing the next batch of oil. The longer that the catalysr and water (both present in the glycerol before demth) are in contact with the bio the more soap will be produced and less catalyst left for the glyc wash.
Are you saving the methanol from your demething?

FYI Each 40g of NaOH will produce 18g of water just dissolving into methanol if you use a base of 5g/L (NaOH to Oil) and 20% virgin methanol, that is 25g NaOH per L of methanol, producing 11g of water so just over 1% of your mix will be water.

The water present in the methanol does not get used up making soap it merely catalyses the formation of soap using up the NaoH (or KOH), the formation of soap does however produce yet more water.

Daves suggestion to dry your reclaimed methanol using cement is well worthwhile if you have the time as his reccomendation to use both NaOH and KOH to prevent the glycerol quickly going solid.

You don't say whether you are doing a single stage process or two stage, if the latter I would only use virgin methanol for the last  stage as you will have no FFA left so minimisising the water present will allow a faster reaction and less soap formation - possibly using a lower base amount of catalyst for the seond stage.

Offline mauser

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Re: Enhanced gly wash
« Reply #5 on: January 04, 2024, 07:07:33 AM »


     Dgs,

      My batches are 170lt. Ill try the mix of 50/50 naoh/koh but since i bubble and settle im wondering if the koh will inhibit the settling process. Anyway, got to find a way to use it up.

     Could you post a link to the cement filtering of meth ( real world examples dealing in gallons not some test in ml. Btw, im a mason so i deal with some form of cement on a daily basis.

      countrypaul,

     I do save the meth from wbd and use it since it is usually 98%. The reclaimed meth ( 93%) was given to me. Just trying to find a way to use it.

     Im not opposed to evolving into a new method. I single staged for years, using a jrl eductor to a clear pass in 1.5 hours at the most. Holding back the gly from stage one to use as a prewash and demething just the bio after stage 2 is not a problem.

Offline dgs

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Re: Enhanced gly wash
« Reply #6 on: January 07, 2024, 06:49:17 PM »


     Dgs,

      My batches are 170lt. Ill try the mix of 50/50 naoh/koh but since i bubble and settle im wondering if the koh will inhibit the settling process. Anyway, got to find a way to use it up.

     Could you post a link to the cement filtering of meth ( real world examples dealing in gallons not some test in ml. Btw, im a mason so i deal with some form of cement on a daily basis.

      countrypaul,

     I do save the meth from wbd and use it since it is usually 98%. The reclaimed meth ( 93%) was given to me. Just trying to find a way to use it.

     Im not opposed to evolving into a new method. I single staged for years, using a jrl eductor to a clear pass in 1.5 hours at the most. Holding back the gly from stage one to use as a prewash and demething just the bio after stage 2 is not a problem.

Hi mauser, apologies for delay in replying.

The kOH will certainly stop the soaps from settling as fast. The answer being after your settling period to filter  through hardwood chips/shavings/sawdust.

You will have to mix the methanol and cement in a sealed container, 5 or 6 us gallons. Use about 2 lbs of cement to 5 gallons, shake well and let it settle a few mins. do this a few times then leave 2 to 3 days for the cement fines to settle.

Make sure you don't get any of the settled cement into your methoxide otherwise you will produce some calcium soaps that are difficult to remove.

The whole process is messy but it does work well. I've used it a few times but after mixing with KOH, this removes water in methanol, water in the KOH and water produced with making potassium methoxide. You may also be able to do this but I'm not sure of the effect of initially mixing KOH into methanol with a high % of water.
FOC water tests by Sandy brae or Karl Fischer for forum members.

Offline mauser

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Re: Enhanced gly wash
« Reply #7 on: January 08, 2024, 04:51:56 AM »


    Ok, Will give it a go. Do you refer to cement as a general term or a specific type and brand.

    A link to the store and their product would be helpful.

    Here, we have portland cement   https://www.titanamerica.com/uploads/SDSPortlandCement-2020.pdf

    or, mortar (type N)  https://www.titanamerica.com/uploads/SDS%20Types%20S-M-N-StuccoRoofTile-2020.pdf

     Section 3 of each pdf has the ingrediants

Offline dgs

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Re: Enhanced gly wash
« Reply #8 on: January 08, 2024, 09:43:54 AM »
Portland cement is the type to use, however if you have some trade contacts and can get hold if some CaO (quicklime) it works slightly better (more efficient at reacting with water)
FOC water tests by Sandy brae or Karl Fischer for forum members.