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I tried this post about an hour ago but it didn't work. I think it failed when I tried to load a picture of my still.

Anyway, my still is working.

My still is a barrel with a hot water heater element rated at 4500 watts at 240. The element on mine is wired with 120 volts. The barrel is insulated has a pressure gauge and a safety valve using a hose going into a kitchen pitcher full of water. If the water rises, the pressure is increasing and it's time to turn the heat off. The condenser is a bucket type where the coil of copper tubing (3/8" id) is wound around in the inside of the bucket and pops out the side down at the bottom and forms a spout for the methanol to drain out of and into another bucket. I fill it with ice while distilling.

So far so good. The highest temp I've been able to read with a temp gun is 165 degrees F. It doesn't seem to want to rise any more than that. I'll watch the temp, the safety valve and pressure gauge see how it goes.

The drum was about 2/3 full of byproduct or maybe a little less. It took about 4 hours to get up to temp and for methanol to start dripping out the tube.

Pics are available on the thread titled "Methanol Recovery?" I'm afraid that if I try to upload a pic on this thread it'll lock up again.

I'll be checking this thread frequently over the next few hours so feel free to comment, ask questions or offer suggestions that could help the process.

Thanks,

Wayne


Very funny Scottie, now beam down my clothes.
 
Location: Dansville Michigan Near Lansing | Registered: 17 September 2005Edit or Delete MessageReport This Post
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It's been running for over 12 hours now and I've collected a whooping 2 1/2 gallons.

Of course it took 4 hours before the first drop came out.

Any ideas on how to make it faster/more efficient?

I'm using 3/8" id copper tubing for the condenser. It started out a 20' coil.

Would making it shorter help?

The bucket condenser sets lower than the barrel. Could raising the condenser help?

Someone suggested the 3/8" id tubbing may be too small. This was refering to the amount of pressure required to push the methanol vapor out without causing too much pressure in the still. So far there has been no presure build up at all that I am aware of. At least I can say for sure that the water in my safety valve hasn't risen a bit.

About an hour or two ago I ran the circulation pump because I read somewhere that agitation helps a lot. It not only didn't help it actually stopped the process for a few minutes.

It seems to be having a hard time building temp. It has increased but very little. When the methanol started the side of the barrel at the bottom, adjacent to the heater bung was 165 degrees F measured with a temp gun reading the outside of the steel.

When last checked the same area read 180 degrees F but the top of the barrel read 162 degrees F.

The sides and top of the drum are insulated with paper backed insulation. It's pretty thin stuff, maybe 6" thick or so.

I'm cooling the coil with ice in the bucket. It doesn't seem to matter if it's full of ice or only a little and mostly water.

The liquid methanol just trickls out. It produces maybe a half gallon per hour, if that.

Any help would be greatly appreciated.

Wayne


Very funny Scottie, now beam down my clothes.
 
Location: Dansville Michigan Near Lansing | Registered: 17 September 2005Edit or Delete MessageReport This Post
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Fifteen hours and counting...

Still drippin...

200 degrees F...

Total amount of methanol recovered? FIVE gallons.

Kind of a joke isn't it?

Wayne


Very funny Scottie, now beam down my clothes.
 
Location: Dansville Michigan Near Lansing | Registered: 17 September 2005Edit or Delete MessageReport This Post
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Electricity costs come to what?

$1.50?

Rick
 
Location: The Deep South | Registered: 06 December 2004Edit or Delete MessageReport This Post
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I have no idea what the electricty cost will be. Even if it is only $1.50 thats $1.50 + about $17.00 for ice + at least $50 for the still, condenser, valves and other plumming.

Granted you only pay for the equipment once and I'm sure I can come up with something different than ice for cooling the condenser.

Out of about 36 gallons of glycerin I reclaimed a little less than 6 gallons of methanol. That's a little less than 17% recovery rate.

Unless I can dramatically improve efficincy I'll be forced to just let the methanol evaporate. That is just WAY too much time, effort and expense for very little return.

I'm wide open to ideas to improve the system.

Wayne


Very funny Scottie, now beam down my clothes.
 
Location: Dansville Michigan Near Lansing | Registered: 17 September 2005Edit or Delete MessageReport This Post
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Two questions:

1. How hot was the contents of the pot when you finshed distilling?

2. Was the copper tube past the bucket of water hot warm or cold while distilling?
 
Location: Australia | Registered: 17 July 2001Edit or Delete MessageReport This Post
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I think the temp is the still eventually got up to about 220 degrees F.

I attempted to use some of the last bit of liquid I recovered and it made me suspicious that it was water. It didn't really smell like methanol. I sort of had no real smell at all. So rather than take a chance I just used some of the first 5 gallons recovered that was well under 220. It was at about 175 or so for all of that. I left it on while napping for the last 3 hours or so and I think it started to yeild water at the very end. I'm sure of the last gallon there is some methanol there but I'm afraid there is also water.

The copper tubing that pokes out of the bucket remained cold the entired time. Moisure would collect on the outside of the tubing. It was that cold.

Wayne


Very funny Scottie, now beam down my clothes.
 
Location: Dansville Michigan Near Lansing | Registered: 17 September 2005Edit or Delete MessageReport This Post
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Wayne, you said: "About an hour or two ago I ran the circulation pump because I read somewhere that agitation helps a lot. It not only didn't help it actually stopped the process for a few minutes."

I think you were mislead. On first switching on the pump any patches of cooler material in the corners of the drum would have been swept into the bulk and cooled it a little. That would stop the distillation temporarily but have no long term harmful effect. Stirring should allow the methanol to evaporate more readily as it keeps exposing a new surface. It certainly helps to avoid frothing which sometimes causes glycerine to come over with the methanol.

To calculate the recovery it is necessary to know how much oil and methanol you started with. As the outlet of your copper pipe was cool the whole time you did not lose methanol to the atmosphere.

The fact that the pot temp got up to 220 deg F does not mean much. It is the temperature at the highest point in the delivery pipe that counts. If that was at 212 F you would certainly be distilling water, given that the pressure did not rise.

The whole art of distilling and controlling the distillation requires that there be no significant back pressure at the head of the still. If there is pressure the boiling point goes up and the temperature becomes meaningless unless you also know the pressure at the same point as the thermometer. It appears in your case that the rate of heat input was low enough that there was little or no pressure rise. It seems you might be able to use a bit more wattage in your heater or better insulation on your drum to speed up the process.

However you need a thermometer to know what is going on. Ideally you will have a vertical section of 3/4 inch pipe coming up out of the drum with an angle to the condensing tube, and the thermometer bulb is set in the angle. If the temp here goes above 148 F stop distilling.

It is a good idea to collect the methanol in batches as the water content will increase. The water content can be measured easily using a hydrometer, available from home brew shops.
 
Location: Australia | Registered: 17 July 2001Edit or Delete MessageReport This Post
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"It is a good idea to collect the methanol in batches as the water content will increase. The water content can be measured easily using a hydrometer..."[/QUOTE]

I don’t understand where the water would come from if you were distilling methanol from glycerin? Unless, you used the “pre-wash” method and introduced water to your batch before distilling, otherwise there should be no water to worry about.
 
Location: Upstate NY | Registered: 03 September 2005Edit or Delete MessageReport This Post
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There could have been water in the oil to start with and a little is generated when the FFA reacts with the NaOH. Not much of course but Wayne did think water was present. Perhaps his pressure relief device sucked back. Perhaps he used the 5% water/glycerine wash. Who knows. Using a hydrometer allows one to be certain you aren't going to spoil the next batch.
 
Location: Australia | Registered: 17 July 2001Edit or Delete MessageReport This Post
dva
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Wayne,
As it must be starting to get quite cold in your part of the world, how about doing all your condensing out in the open. With an air-cooled condenser coil operating at air temperatures of, say, -5C on a cool evening, you can do away with the ice.
You will naturaly, need to use plenty of insulation to keep the still warm, and insulate up to the bend in the pipe, but not after it.
regards
dva
 
Location: Yorks,England | Registered: 30 June 2001Edit or Delete MessageReport This Post
dva
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Neutral,
re my posting above,
If wayne left his methanol collector vessel out in -5C would this freeze the water content ? If so could he then decant the methanol and dump the unwanted ice ?
regards
dva
 
Location: Yorks,England | Registered: 30 June 2001Edit or Delete MessageReport This Post
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dva,
As methanol is used as a windscreen wash antifreeze, perhaps it would not separate.
 
Location: Perth W.Australia | Registered: 10 August 2001Edit or Delete MessageReport This Post
dva
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Yes, I was wondering about that as I wrote it, but thought that I'd ask anyway. Anybody able to clear this point up ?
regards
dva
 
Location: Yorks,England | Registered: 30 June 2001Edit or Delete MessageReport This Post
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I think Tony is right, I doubt it would seperate. I have noticed on really really cold mornings that the washer solvent will be slushy in the reservoir. In other words, it stays combined even when frozen.

Wayne


Very funny Scottie, now beam down my clothes.
 
Location: Dansville Michigan Near Lansing | Registered: 17 September 2005Edit or Delete MessageReport This Post
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