Author Topic: Evaporating large aqueous solutions?, no rotovap  (Read 383 times)

overunity33

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Evaporating large aqueous solutions?, no rotovap
« on: February 29, 2012, 06:31:01 PM »
What would you guys do if you had to evaporate a gallon or so of aqueous solution every night?  It can't be boiled off, max temp maybe 40C.  I was thinking of getting a large pressure cooker, stick a heating mat and mag stirrer under it then making a simple distilling column and run a vacuum to it.

The problem is my rotary vane pump runs so hot I can't leave it on 24/7 without active (water)cooling.  You guys have recommendations for a quiet pump that wont overheat and wont be damaged by water vapor? 

Vesp

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Re: Evaporating large aqueous solutions?, no rotovap
« Reply #1 on: February 29, 2012, 08:16:58 PM »
This is a really hard question since I don't think you can really say anything would work until you try it. I like the pressure cooker idea.  I think what you say is good, but I do not know if it the pressure cooker would actually seal. My pressure cooker has a rubber ring that looks like it would only work in one way (pressure on the inside, pushing out.. not the other way) But it is easy enough to try without ruining the pressure cooker -- just connect a vacuum tube to the release valve.

I know aspirators can boil water at room temperature, if the water is colder than room temp. If you were to put it on a magnetic stirrer hotplate, and had the stirrer and heater on, you could probably get it to boil pretty furiously with the agitation and added energy.

The only other possible thing I can think of at the moment, that would perhaps be possible (I bet much less practical and more expensive) would be to do some sort of reverse osmosis?  http://en.wikipedia.org/wiki/Reverse_osmosis#Process

If you had a membrane, and your molecule in the solution could not pass through it, but the water could, you might possibly be able to have something like a very very saturated + non-dissolved solids of Calcium chloride solution in one side suck away some/most of the water leaving a more concentrated solution of your product.

This, say could reduce your amount of water by maybe.. half a gallon? or more? (again I don't think this is practical, just brain storming)

The calcium chloride solution that has more water in it could then be boiled off at a much higher temperature, and  reused... the other remaining solution could possibly would than have to be vacuum dried again, but you'd have less liquid to contend with.

I'd go with your first idea -- and see how that works out.

Perhaps you can just alter your process and make it so you have less than a gallon of solution to evaporate? Probably not...
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pyramid

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Re: Evaporating large aqueous solutions?, no rotovap
« Reply #2 on: February 29, 2012, 08:36:43 PM »
If you have no rotovap then all you can do is the vacuum distillation, use an aspirator or a diaphragm pump. You don't even need a condenser if using aspirator, just let all the vapor go down the sink. Of course doing this every night wastes a hell of alot of water.
So I would use a diaphragm pump, there is not alot else you can do. But I don't know what it is you have to evaporate either.

A PTFE diaphragm pump will work without a trap but you will need to clean it afterwards or let it run. In my experience a pump of this type can run for hours on end without cooling, never heard of needing to cool these. But perhaps I'm doing it wrong.
Now, I don't think they can just run all day long, I doubt any pump can do that without cooling as you mention. Water is and always will be a bitch to remove by distillation.
« Last Edit: February 29, 2012, 08:39:00 PM by pyramid »

Vesp

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Re: Evaporating large aqueous solutions?, no rotovap
« Reply #3 on: February 29, 2012, 08:52:37 PM »
You could also get a water pump + aspirator and recycle the water that is being pumped - but that would only be convenient if you already had such a setup.
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overunity33

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Re: Evaporating large aqueous solutions?, no rotovap
« Reply #4 on: March 01, 2012, 02:15:02 AM »
Thanks guys.

Vesp your osmosis idea is pretty solid for industrial bees that have the need for a trick like that.  Serious lateral thinking...

I would rather not have the water running all the time, the diaphragm pump seems like the best option.

Any advice on diaphragm pumps that can run for a week straight?  Doesn't need to be powerful too at all, like 28inHg or so.  The solution will just be acetic acid or HCl, <15%v/v

Maybe a tiny rotary vane with serious heatsinking would work better?
« Last Edit: March 01, 2012, 02:21:18 AM by overunity33 »

overunity33

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Re: Evaporating large aqueous solutions?, no rotovap
« Reply #5 on: March 01, 2012, 02:16:19 AM »
Might buy some peltier units for the condenser, maybe even a huge heatsink for the pump.

Sedit

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Re: Evaporating large aqueous solutions?, no rotovap
« Reply #6 on: March 01, 2012, 04:33:14 AM »
You have two options in my book, one being if the temperature is not to much of an issue then use an old deep fryer because I have one able to boil off two gallons of water or more in around 20-30 minutes and I now have it rigged up as a powerful steam generator.

Another means is if the temperature needs to be kept low is to use a flat baking sheet and placing it on top of a heating pad normally used for ones back or things like that, it works rather well. Keep half of the solution or so covered as it will help in keeping the temperature at a level to sustain rapid evaporation. This is an old trick the alchemist and early chemist used because having it as open as possible sometimes looses more heat then benefit gained from higher surface area.
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salat

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Re: Evaporating large aqueous solutions?, no rotovap
« Reply #7 on: March 01, 2012, 05:59:38 PM »
My husband uses an assortment of fry daddies - they range in size from fry grand daddy which will hold a 3 L flask down to the fry baby which he cut the top off of for small scale stuff.  He redid the wiring so he can connect it to a power controller.  I borrowed the small one the other day and I was able to use it with the power controller he created out of a dimmer switch.

Grapeseed is a very good oil to use - it's smoke point is 216.

He's also used electric woks this way but the fry daddy is better because he can immerse almost the entire flask in the oil to get even heating.

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Vesp

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Re: Evaporating large aqueous solutions?, no rotovap
« Reply #8 on: March 01, 2012, 07:14:34 PM »
" It can't be boiled off, max temp maybe 40C.  "

That is basically a hot summer day - I don't think anything with heat is a good option?
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DopeBee

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Re: Evaporating large aqueous solutions?, no rotovap
« Reply #9 on: March 02, 2012, 12:25:01 AM »
Whenever I need to get rid of large amounts of water (and my desired product doesn't degrade quickly or sublimate quickly) I just buy a dozen or so aluminium turkey trays and set them outside. I'm always surprised at how quickly water evaporates on it's own.

lugh

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Re: Evaporating large aqueous solutions?, no rotovap
« Reply #10 on: March 02, 2012, 01:21:38 AM »
Rotovaps were first fabricated as described in the attached file which has been downloaded hundreds of times from where it was first posted:

http://www.sciencemadness.org/talk/viewthread.php?tid=7128

another method of construction can be found at:

http://www.erowid.org/archive/rhodium/chemistry/equipment/rotavap.html

and further information that LT/ posted on the Hive long ago can be found at:

https://the-collective.ws/forum/index.php?topic=9873.msg153369#msg153369

so there's lots of very useful information available  ;) The end results from the effort applied  8)

« Last Edit: March 02, 2012, 01:54:26 AM by lugh »
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embezzler

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Re: Evaporating large aqueous solutions?, no rotovap
« Reply #11 on: March 11, 2012, 03:31:46 AM »
Low heat, a commercial dehumidifier, a "hood" to stop the dehumidifier taking other water from anywhere else in the environment and a little patience should sort this.

Roto vap would still be a worthy construct for many reasons

More info would guide the swarm
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Goldmember

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Re: Evaporating large aqueous solutions?, no rotovap
« Reply #12 on: March 11, 2012, 03:14:15 PM »
An electric blanket with a lined shallow tray and a fan blowing across the surface.

faust.motion

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Re: Evaporating large aqueous solutions?, no rotovap
« Reply #13 on: August 27, 2012, 12:57:13 PM »
Microwaves are great for this. I've used them in the past to evaporate large quantities of cactus syrup. You don't have to worry about scorching plant fats and the evaporation happens quite quickly, from about 500ml to 150ml in just under 20 minutes.
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no_dream

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Re: Evaporating large aqueous solutions?, no rotovap
« Reply #14 on: October 03, 2012, 12:24:25 PM »
What about using a heated filled column, into which the heated solution is dropped in. The large area should help concentration, the concentrate and vapours fall down to the flask, which is set up for vacuum distillation.

Or just slowly adding the lean mixture to the flask with stirring the same rate water distills off. Evaporating large volumes gives problems like heavy foaming, bumping etc.

I also advocate using fridge pumps. They tolerate water vapor to some extent, change oil frequently. If they go bad, throw away. Recirculating aspirator with cooling is the best, but its noisy and consumes much energy & produces much heat.

fishinabottle

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Re: Evaporating large aqueous solutions?, no rotovap
« Reply #15 on: October 07, 2012, 06:18:52 PM »
Azeotropic distillation with ether for example proceeds at temperatures you look at and can be arranged easiy as continous distillation to remove the water. Other organic solvents will do it too DCM, chloroform to name two inflammale ones. For the recirculation the needed amount is pretty small.

no_dream

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Re: Evaporating large aqueous solutions?, no rotovap
« Reply #16 on: October 10, 2012, 05:49:31 PM »
Im not much believing the azeotropic method is viable, have you tried it? Large ether losses, low efficiency