Acetone to aid reaction !

[Head Womble]

Ok so it it does prove to be an increase in yield, decrease in gly, this (to me) seems to be the biggest benefit.

Now it's been reported that ASM has a similar effect (some say more bio out than veg in), so with this in mind,
I wonder if the ideal process could well be,
Gly wash to reduce FFA's,
two stage non titration with ASM + acetone (to reduce the amount of catalyst and meth),
WBD to reclaim the acetone and meths (should this be acid titration to reduce HMPE formation, would this effect the meth/acetone purity?),
pump water washing with acetone.

Yes I know it's getting complicated, but if there's a possibility of better conversions with less meth/catalyst used and reduced costs, plus a better yield it could be worth the effort.

Sadly I'm in position to do any testing on this.

[Carrington]

Hi mark
The acid shouldn't distill out with the meth/ acetone so Purity of distillate shouldn't be a problem.
I'm still not sure about wbd I think if there is meth left in Glyc then it would be better to take advantage of it with the Glyc wash.

Yes I think you a right about the effort if we get it right now things could get really easy in the future

[Carrington]

Mark
I have the dry powdered acid , if you want some I will get some down to you

[Head Womble]

So you also see the advantage of this method, I wasn't sure I'd grasped all the information correctly.

[Head Womble]

Mark
I have the dry powdered acid , if you want some I will get some down to you

That would be great mate, I've been waiting for some sulphuric before I can test the WBD with acid.

That said I want to finish the testing on water washing with acetone before I start changing things.

Also I don't use ASM so can't follow up on my thoughts.

[thewormman]

The use of acetone should prevent the meth going into the Glyc  , if this is so then we could definitely use les meth as well as catalyst.
I think this is why we're getting less Glyc as it contains much less meth

Paul

Why do you think this?
There is nothing in the research that says this so could you point me at whatever states this?
Methanol readily dissolves into Glyc Acetone doesn't, Meth and Acetone do not form a compound but stay separate.

Thanks

[Carrington]

The use of acetone should prevent the meth going into the Glyc  , if this is so then we could definitely use les meth as well as catalyst.
I think this is why we're getting less Glyc as it contains much less meth

Paul

Why do you think this?
There is nothing in the research that says this so could you point me at whatever states this?
Methanol readily dissolves into Glyc Acetone doesn't, Meth and Acetone do not form a compound but stay separate.

Thanks

Hi Dave
In the papers that I have I'm sure it list the different cosolvents used and there different properties and the reason that acetone worked better than others (ipa and xylene ) was the it doesn't mix with glycerine but the others do . If you send me your email I will send over the papers I have.

Paul

[Dickjotec]

I have just tested the glyc from yesterday by heating.
Heated with a blowtorch from below.
Fumes given off and surface flames.
Old demethed glyc just boils.
So it sounds like it does have meth in it. It has also not set overnight which also tends to suggest there is meth in it. Next batch I will WBD and see how much comes back.
Dick

[1958steveflying]

The use of acetone should prevent the meth going into the Glyc  , if this is so then we could definitely use les meth as well as catalyst.
I think this is why we're getting less Glyc as it contains much less meth

Paul

Why do you think this?
There is nothing in the research that says this so could you point me at whatever states this?
Methanol readily dissolves into Glyc Acetone doesn't, Meth and Acetone do not form a compound but stay separate.

Thanks

Hi Dave
In the papers that I have I'm sure it list the different cosolvents used and there different properties and the reason that acetone worked better than others (ipa and xylene ) was the it doesn't mix with glycerine but the others do . If you send me your email I will send over the papers I have.

Paul

I think you have just made the point that the Acetone does not mix with the Glycerine Paul, I have not found anything saying the Methanol does not mix with it, have been looking back through since you said.  I will stand corrected though as I can easily misread these days. lol.

[Carrington]

I have just tested the glyc from yesterday by heating.
Heated with a blowtorch from below.
Fumes given off and surface flames.
Old demethed glyc just boils.
So it sounds like it does have meth in it. It has also not set overnight which also tends to suggest there is meth in it. Next batch I will WBD and see how much comes back.
Dick

It may be that it only prevents the meth/Glyc mixing with a higher dose of acetone . When my codeine where's of I will be trying a micro batch using 13% meth and = amount of acetone . Will then test the Glyc

[nathanrobo]

Next batch I will WBD and see how much comes back.
Dick

Is WBD still considered best practice?

[photoman290]

i feel it is important to follow the experimental method  in the paper as closely  as possible otherwise we will get confusing results. ok recovering the acetone at 25 torr might prove a bit difficult, but that doesn't affect the reaction.  once we have established a base line then is the time to experiment with less acetone. being as non of us are trained chemists, as far as i know? it is important if a chemist did come along to present  them with  the same experiment as in the paper.
i know i am struggling with a lack of basic chemistry. if they used 25% acetone there must have been a good reason. if it worked with 10% i am sure that is what they would have used and if they did they would have said.

[Carrington]

Hi all just a quick one
I think I have got something wrong with regards to meth not being consumed by Glyc when acetone is mixed with it
On first reading I understood it that as acetone is immiscible with Glyc the I took it that so would the meth be when mixed with acetone. Lao the few results we have had in defiantly produced less Glyc by about 20% and this amount is what I'd expect to find in the Glyc I use , so I'm sorry to say I put 2n2 together and believed that my assumption was right .

Wormman asked me about this as he couldn't find any info to back this up , so I have go over the papers again (a few times) and he is right ,
Also dick tested his Glyc for meth and it proved positive for meth.

Sorry that I got it wrong and led people to believe a inaccuracies and thanks to Dave for getting me to look over it again

Just proves lots more testing to be done


Paul

[1958steveflying]

i feel it is important to follow the experimental method  in the paper as closely  as possible otherwise we will get confusing results. ok recovering the acetone at 25 torr might prove a bit difficult, but that doesn't affect the reaction.  once we have established a base line then is the time to experiment with less acetone. being as non of us are trained chemists, as far as i know? it is important if a chemist did come along to present  them with  the same experiment as in the paper.
i know i am struggling with a lack of basic chemistry. if they used 25% acetone there must have been a good reason. if it worked with 10% i am sure that is what they would have used and if they did they would have said.

I cant say I am in agreement with you on this, we know it works with the amounts they used, they have written the paper. However for me it is impracticable to use these amounts without the ability to recover the Acetone in a guaranteed re-usable state. We know why and how it works and using as little as 1 litre in a 180 litre batch had positive results based on our usual 2 stage no titration method. My next batch will have more adjustments which will either further improve my previous results or not.

[thewormman]

Paul I will always question things to find a definitive answer if I cannot see it myself, I am not trying to find fault, but just not making assumptions. I think it comes from years of working on things that could injure people if what I did was wrong.

I have also learnt over the years of losing a few jobs that I need to accept I make errors too, so I now accept graciously if they are pointed out to me    that one took a while...

We are all human and I find the best way to get the best results is to crosscheck everything.

Just a quick one
Also in the distillate will be a % of water so not sure how accurate a sg test would be.
I could do a water in oil test but using a meth/water / acertone to see if I can get a accurate water result then do some simple sg test to see how well the calc's work out.
I'm affraid this my be a test for another day

Did you manage to do this test? I really would like to find a way of identifying Meth/Acetone percentages in the distilate. I think if we can find this then a high percentage of the Acetone can be recovered and since it is not actually consumed during the reaction the volume used is academic. We can just use the optimum 25% or whatever is best.

Dave