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Biodiesel => Chemistry and process => Topic started by: theraw on March 05, 2013, 10:37:44 PM

Title: Glycerol from ASM reactions
Post by: theraw on March 05, 2013, 10:37:44 PM
Hi all, I'm hoping the ASM users can help me with this.

I've been reading much about the benefits that come from using ASM so I'm seriously considering giving it a go but I wanted to know if the glycerol it produces sets solid and if it does how quickly does it set. I'm guessing it's a possibility seeing as it's a Sodium based catalyst.

I've been making bio for close to 5 years now and my processor is set up so that the pipework and pump can be 100% drained. This coupled with the fact that I've always used KOH means that I've never had a problem with glycerol setting anywhere and I don't really want to start now!

Thanks in advance for your replies.

Rauri
Title: Re: Glycerol from ASM reactions
Post by: Julian on March 05, 2013, 11:00:34 PM
Welcome to the wiki and forum.

I've only used ASM a few times and on a couple of occasions the entire batch set solid, but that's another story!

The batches that have worked have produced solid glycerine as would NaOH.
Title: Re: Glycerol from ASM reactions
Post by: therecklessengineer on March 06, 2013, 06:02:14 AM
I've done two ASM batches now and the glyc has set into a sort of semi-solid gloopy mess. It'll still pour...just about!

Try it, you won't regret it!
Title: Re: Glycerol from ASM reactions
Post by: RichardP on March 06, 2013, 06:41:05 AM
My glyc from ASM goes thick but not solid. If I put it in the house overnight it's easy enough to pour.
Title: Re: Glycerol from ASM reactions
Post by: Julian on March 06, 2013, 09:44:48 AM
Interesting, when you two get semi solid glycerine, how much methanol has been removed from it?
Title: Re: Glycerol from ASM reactions
Post by: therecklessengineer on March 06, 2013, 09:50:13 AM
Yes, should have mentioned that. The above is the fully methylated variety - none has been removed.
Title: Re: Glycerol from ASM reactions
Post by: Julian on March 06, 2013, 09:55:20 AM
Ah, there's the difference, mine was quite heavily demethed.

Good to know that it's pumpable if not demethed ... I might now have a bash at glycerine washing.
Title: Re: Glycerol from ASM reactions
Post by: BassAddict on March 06, 2013, 06:41:09 PM
My glyc from ASM goes solid even when kept indoors - not rock solid but it is now pumpable and I have to shovel it in the top of the reactor (safely as can be) or mix with hot oil. This is with meth in ready to use for a glyc wash.
Title: Re: Glycerol from ASM reactions
Post by: nigelb on March 06, 2013, 06:54:04 PM
My ASM glyc always goes solid

I drain it into a steel clip complete with valved inlet and vents on the lid and a drain valve on the side

For the glyc wash I put it on the Turk Burner to melt it down..then pump it in.

Nige
Title: Re: Glycerol from ASM reactions
Post by: julesandtash on March 06, 2013, 07:58:01 PM
Mine goes solid too.
I dont demeth at all, just glyc wash the oil then two stage process.
All glyc is drained before any water is added.

Glyc goes completely solid within 24 to 36hrs whatever the feedstock I use.
Title: Re: Glycerol from ASM reactions
Post by: Jamesrl on March 06, 2013, 08:01:16 PM
I did a batch yesterday, the glyc for the wash was two weeks old and had sat in the shed all that time. The only part of the 20ltr that could'nt be used, due to viscosity, was the bottom 2".

After a glyc wash it sets like a brick.

BTW I've recently fitted a special glyc entry point, makes life a piece of pi$$. I can put 20ltr of glyc in as fast or faster than the methoxide.
Title: Re: Glycerol from ASM reactions
Post by: RichardP on March 06, 2013, 08:19:26 PM
BTW I've recently fitted a special glyc entry point, makes life a piece of pi$$. I can put 20ltr of glyc in as fast or faster than the methoxide.

Is it called a 'lid'?
Title: Re: Glycerol from ASM reactions
Post by: K.H on March 06, 2013, 08:47:12 PM
BTW I've recently fitted a special glyc entry point, makes life a piece of pi$$. I can put 20ltr of glyc in as fast or faster than the methoxide.

Is it called a 'lid'?
;D ;D ;D ;D ;D ;D
Title: Re: Glycerol from ASM reactions
Post by: Jamesrl on March 06, 2013, 08:52:54 PM
BTW I've recently fitted a special glyc entry point, makes life a piece of pi$$. I can put 20ltr of glyc in as fast or faster than the methoxide.

Is it called a 'lid'?

Nah, I don't use a bucket, only a totally sealed GL, y'know, a proper reactor.
Title: Re: Glycerol from ASM reactions
Post by: bertle on March 06, 2013, 08:58:50 PM
Yesterday I loaded my processor with oil, warmed it up and added the liquid glyc from the previous asm batch, using my special glyc inlet port (lid). Mixed it for a while and turned it off to settle. I then got called home early, (processor is at work), before I got time to drain off the glyc.
This morning I opened the drain valve and nothing came out! I now have 20 litres of solid glyc under 180 litres wvo. Bugger!
Title: Re: Glycerol from ASM reactions
Post by: Jamesrl on March 06, 2013, 09:03:41 PM
Yesterday I loaded my processor with oil, warmed it up and added the liquid glyc from the previous asm batch, using my special glyc inlet port (lid). Mixed it for a while and turned it off to settle. I then got called home early, (processor is at work), before I got time to drain off the glyc.
This morning I opened the drain valve and nothing came out! I now have 20 litres of solid glyc under 180 litres wvo. Bugger!

See, that's what happens when y'gotta lid, I don't got one.
Title: Re: Glycerol from ASM reactions
Post by: bertle on March 06, 2013, 09:11:11 PM
It's worse than that I have the capability to isolate the tank and drain down the pipes and pumps, this I also failed to do so all that lot is solid too! Double bugger!
Title: Re: Glycerol from ASM reactions
Post by: theraw on March 06, 2013, 09:13:49 PM
I now have 20 litres of solid glyc under 180 litres wvo.

That's my biggest fear! Anyway, my process is glyc wash, 2 stage no titration and then bubble demeth all on the same day one stage straight after the other so the only time I have the risk of glyc setting solid in the reactor is the bubble demeth as that usually runs overnight whilst there's still heat in the processor. That said the majority of the glyc that drops out from that stage usually drops out within the first couple of hours so I'll just have to make sure that it's drained sooner rather than later.

Thanks so much for all the replies, really appreciate it, it's given me the confidence to give ASM a go!
Title: Re: Glycerol from ASM reactions
Post by: 1958steveflying on March 06, 2013, 09:37:09 PM
It's worse than that I have the capability to isolate the tank and drain down the pipes and pumps, this I also failed to do so all that lot is solid too! Double bugger!

A heat gun (safest) or blow torch gently teased around the pipework will get it flowing, the same with the bottom drain.
Title: Re: Glycerol from ASM reactions
Post by: julianf on March 06, 2013, 09:39:12 PM
I think my reactor would have been past the point of recovery many times without compressed air...

On the next rebuild, im planning on actually adding some injection points.
Title: Re: Glycerol from ASM reactions
Post by: bertle on March 06, 2013, 09:59:25 PM
It's worse than that I have the capability to isolate the tank and drain down the pipes and pumps, this I also failed to do so all that lot is solid too! Double bugger!

A heat gun (safest) or blow torch gently teased around the pipework will get it flowing, the same with the bottom drain.

I was thinking gas axe would warm it up, didn't want to blue my nice stainless pipework though!
Title: Re: Glycerol from ASM reactions
Post by: nigelb on March 06, 2013, 10:01:20 PM
Andrew....that is a real schoolboy error. Best of luck getting that liquid again.

Nige
Title: Re: Glycerol from ASM reactions
Post by: nigelb on March 06, 2013, 10:11:20 PM
From experience I would never let raw glyc settle inside the reactor. I leave glyc in there if there is a 7% water wash in with it. That takes several days to set up but only in the coldest weather.

ASM has it's own set of rules. You just need to know what they are.

Nige
Title: Re: Glycerol from ASM reactions
Post by: Julian on March 06, 2013, 10:24:55 PM
I now, frequently leave demethed glycerine in the processor overnight, by shutting a valve right at the tank outlet and draining all the pipe work.  Haven't yet had a problem.
Title: Re: Glycerol from ASM reactions
Post by: Jamesrl on March 06, 2013, 11:00:44 PM
It's worse than that I have the capability to isolate the tank and drain down the pipes and pumps, this I also failed to do so all that lot is solid too! Double bugger!

If you couldn't drain down your pipework and pumps whilst the reactor is full loaded you ain't built it right.

I can strip off and work on, if needed, ALL or any part of the pipework and pumps.

In anyway there's a VERY simple answer to setting glyc and clear pipes/reactor if you need to leave it over night, I'll give you a little time to work it out before I tell you.

Remember KISS
Title: Re: Glycerol from ASM reactions
Post by: Julian on March 06, 2013, 11:16:48 PM
Sir, Sir, I know Sir .... leave the pump running.
Title: Re: Glycerol from ASM reactions
Post by: Jamesrl on March 06, 2013, 11:34:49 PM
Sir, Sir, I know Sir .... leave the pump running.

Not even warm, it's simpler than that and NOTHING is turned on or left running.
Title: Re: Glycerol from ASM reactions
Post by: Julian on March 06, 2013, 11:54:05 PM
Doh, I was sure leaving the pump running while the glycerine was SETTLING would work.
Title: Re: Glycerol from ASM reactions
Post by: bertle on March 07, 2013, 07:41:06 AM
It's worse than that I have the capability to isolate the tank and drain down the pipes and pumps, this I also failed to do so all that lot is solid too! Double bugger!

If you couldn't drain down your pipework and pumps whilst the reactor is full loaded you ain't built it right.

I can strip off and work on, if needed, ALL or any part of the pipework and pumps.


I can isolate everything, I can even take a pump off and keep processing with the other one, I just didn't do it as I was in an unexpected rush. Some things are more important than bio, not many mind you.....
Title: Re: Glycerol from ASM reactions
Post by: Tony on March 07, 2013, 08:18:01 AM
In anyway there's a VERY simple answer to setting glyc and clear pipes/reactor if you need to leave it over night, I'll give you a little time to work it out before I tell you.

Got me curious too.

Use KOH?
Drain the Glyc first?

C'mon pops don't leave us in suspense.
Title: Re: Glycerol from ASM reactions
Post by: Julian on March 07, 2013, 10:19:03 AM
Sir, Sir, I know Sir .... leave the pump running.

Not even warm, it's simpler than that and NOTHING is turned on or left running.

OK, got it now ... turn the processor up-side-down so the glycerine settles and sets at the top, then turn the right way up to drain the bio.
Title: Re: Glycerol from ASM reactions
Post by: Jamesrl on March 07, 2013, 10:22:58 AM
Got me curious too.

Use KOH?
Drain the Glyc first?

I thought we were talking ASM and leaving it WITH the glyc still on board.
Title: Re: Glycerol from ASM reactions
Post by: Jamesrl on March 07, 2013, 10:25:35 AM
Julian, you're getting colder than the Antarctic on a winters day.

It really is simple.
Title: Re: Glycerol from ASM reactions
Post by: Tony on March 07, 2013, 10:30:17 AM
Got me curious too.

Use KOH?
Drain the Glyc first?

I thought we were talking ASM and leaving it WITH the glyc still on board.

Ah, so this doesn't apply to NaOH Methoxide?

You're such a tease.
Title: Re: Glycerol from ASM reactions
Post by: Jamesrl on March 07, 2013, 10:37:50 AM
Got me curious too.

Use KOH?
Drain the Glyc first?

I thought we were talking ASM and leaving it WITH the glyc still on board.

Ah, so this doesn't apply to NaOH Methoxide?


You're such a tease.

KOH makes no difference so yes it will work on catalysts that solidify as the temperature drops.

A clue, though you shouldn't need one, think Sg.

I'm going over to the skunk works now so I'll check out your thoughts later.
Title: Re: Glycerol from ASM reactions
Post by: Tony on March 07, 2013, 11:40:33 AM
Add Methanol or water?
Title: Re: Glycerol from ASM reactions
Post by: thewormman on March 07, 2013, 12:19:07 PM


I'm going over to the skunk works now so I'll check out your thoughts later.

'And the poor man longed to eat from the crumbs of the rich mans table....'

What a tease, you love it don't you Jim... ::)
Title: Re: Glycerol from ASM reactions
Post by: Jamesrl on March 07, 2013, 06:52:16 PM
Add Methanol or water?

You add nothing.
Title: Re: Glycerol from ASM reactions
Post by: Jamesrl on March 07, 2013, 06:54:19 PM


I'm going over to the skunk works now so I'll check out your thoughts later.

'And the poor man longed to eat from the crumbs of the rich mans table....'

What a tease, you love it don't you Jim... ::)

Still no ideas then?

I've used the idea before and it works a treat.
Title: Re: Glycerol from ASM reactions
Post by: Head Womble on March 07, 2013, 07:22:18 PM
Double skinned reactor, add some heat and off you go.
Title: Re: Glycerol from ASM reactions
Post by: Jamesrl on March 07, 2013, 08:20:30 PM
Double skinned reactor, add some heat and off you go.

No, it can be used on any reactor.

Come on, you lot ain't thinking.

Whatever happened to the lateral kind.
Title: Re: Glycerol from ASM reactions
Post by: Head Womble on March 07, 2013, 08:31:11 PM
Don't demeth it ?
Title: Re: Glycerol from ASM reactions
Post by: oakwoodtv on March 07, 2013, 09:59:48 PM
A sealed container connected to the bottom drain of the reactor larger than the volume of the glycerol with
a tap above the glycerol level to drain the bio       
Title: Re: Glycerol from ASM reactions
Post by: RichardP on March 07, 2013, 10:07:28 PM
Probably just a valved suction inlet before the pump, stick the pipe in the glyc, open valve to pump and away it goes.
Title: Re: Glycerol from ASM reactions
Post by: Jamesrl on March 08, 2013, 03:57:05 PM
A sealed container connected to the bottom drain of the reactor larger than the volume of the glycerol with
a tap above the glycerol level to drain the bio       

Give him the money Mable.

You don't need a valve to return the bio, as the heavier glyc drops in the bio returns back up the same pipe.

To make things easier use 22mm pipe and valve.
Title: Re: Glycerol from ASM reactions
Post by: Head Womble on March 08, 2013, 04:18:53 PM
A gly trap then, I've spoken to Tony about this in the past (his idea not mine).
Title: Re: Glycerol from ASM reactions
Post by: Julian on March 08, 2013, 04:22:04 PM
Oh, that old chestnut.  We were all expecting something novel and exciting based on deep fundamental physics, and we get a bucket with a lid and a pipe ... really!

The idea's been muted many times before, but not for static collection of glycerine that I can remember.  Have you tried using it for collecting glycerine as the reaction progresses?  A bit like real time two stage reaction.
Title: Re: Glycerol from ASM reactions
Post by: Tony on March 08, 2013, 05:12:58 PM
I was going to say keep up Jim but you posted in this thread already

http://www.biopowered.co.uk/forum/index.php/topic,933.msg9245.html

The stainless tank has built in coils which could be used to warm what drops out back to liquid for removal.

Thinking about it I bet the gear pump would do a good job of moving the glyc from the sedimenter to containers for disposal.
Title: Re: Glycerol from ASM reactions
Post by: bertle on March 08, 2013, 09:28:00 PM
A sealed container connected to the bottom drain of the reactor larger than the volume of the glycerol with
a tap above the glycerol level to drain the bio       

Give him the money Mable.

You don't need a valve to return the bio, as the heavier glyc drops in the bio returns back up the same pipe.

To make things easier use 22mm pipe and valve.

I don't get it, how does that get the solid glyc out of my processor?
I got the bio out easily enough, I just opened the valve I put in a couple of inches above the cone and drained it in to some cans.
Title: Re: Glycerol from ASM reactions
Post by: Jamesrl on March 09, 2013, 12:59:07 AM

I don't get it, how does that get the solid glyc out of my processor?
I got the bio out easily enough, I just opened the valve I put in a couple of inches above the cone and drained it in to some cans.

It doesn't BUT it will help you and others should the need to rapidly depart the scene occur again.
Title: Re: Glycerol from ASM reactions
Post by: RichardP on March 09, 2013, 07:12:15 AM
BTW I've recently fitted a special glyc entry point, makes life a piece of pi$$. I can put 20ltr of glyc in as fast or faster than the methoxide.

You've not enlightened us thickos on your lid free glyc injection system yet.
Title: Re: Glycerol from ASM reactions
Post by: bertle on March 09, 2013, 08:11:35 AM

I don't get it, how does that get the solid glyc out of my processor?
I got the bio out easily enough, I just opened the valve I put in a couple of inches above the cone and drained it in to some cans.

It doesn't BUT it will help you and others should the need to rapidly depart the scene occur again.

Ah ok, I have got the pleasure of sorting this out this afternoon, nearly out of fuel and could have done with some in the settling drum by now.
Who would be a bio brewer.......
Title: Re: Glycerol from ASM reactions
Post by: nathanrobo on March 10, 2013, 07:11:12 PM

Hmm... that's why I went back over to KOH
Title: Re: Glycerol from ASM reactions
Post by: Head Womble on March 10, 2013, 07:34:51 PM

I don't get it, how does that get the solid glyc out of my processor?
I got the bio out easily enough, I just opened the valve I put in a couple of inches above the cone and drained it in to some cans.

It doesn't BUT it will help you and others should the need to rapidly depart the scene occur again.

Ah ok, I have got the pleasure of sorting this out this afternoon, nearly out of fuel and could have done with some in the settling drum by now.
Who would be a bio brewer.......

How did you get on ?
Title: Re: Glycerol from ASM reactions
Post by: bertle on March 10, 2013, 08:06:55 PM

I don't get it, how does that get the solid glyc out of my processor?
I got the bio out easily enough, I just opened the valve I put in a couple of inches above the cone and drained it in to some cans.

It doesn't BUT it will help you and others should the need to rapidly depart the scene occur again.

Ah ok, I have got the pleasure of sorting this out this afternoon, nearly out of fuel and could have done with some in the settling drum by now.
Who would be a bio brewer.......

How did you get on ?

Well after a couple of hours getting covered in glyc it is all sorted and reloaded ready to make a batch this week. Once the oil was out it was apparent that the glyc was not totally solid just very thick and a good rodding sorted it out. I had to take the pumps appart and clean them out but could have been worse!