Quote: Originally posted by rockyit98 | for vacuum distillation you don't need a Vacuum pump per se. "vacuum distillation" really means reduce pressure distillation.one time my Vacuum pump
didn't work so i distilled some water by adding water and a stirbar to vacuum distillation apparatuses that can keep a vacuum for days without
giving up.first with no water at the cooling condenser(empty) i cranked the heat full so entire setup will fill with steam and so would escape from
the "vacuum outlet". i attached one way valve so only steam can get out then cut off heat and let the water cooled till about 40C. at this point one
way valve has don it's job and no air is inside only water vapor. turned on stirring (necessary for reduce pressure distillation ) and the cooling
water and slowly up the heat till thermometer showed that water is distilling at 40-50C.
the moral of the story is that you don't need to keep the vacuum pumped running or connected one you created a vacuum in the first place and long a
you don't lose it.
i distilled Glycerol by first heating it up to 110C to remove water and after it cooled down and adding it to a vacuum distillation apparatuses and
pulling a vacuum and closing the valve that between pump and the setup. and heating cooling and most importantly stirring. |
This is very cool! So at what temperature did your Glycerol finally distill over at?
May I ask what was the size/scale/ground glass standard of your setup was?
Did you have any sort of vacuum gauge in line?
I finally acquired a cheap but pretty-damn-close to functional digital manometer, intended for HVAC use, along with one of their nicer pumps. I have
thus far, set up my system :no matter how simple, tightly clamped, greased excessively, minimally, not at all - as soon as the vacuum pump turns off,
(with the rest of the system ultra tightly sealed with gas rated close-off valve) the pressure starts rising. Sometimes super fast, sometimes it
takes a few minutes to rise back up to atmospheric. I can't fathom how I could get it air tight enough to maintain and hold a low vacuum, especially
to later perform a distillation!
I used Propylene Glycol as a standard and determined that my 7CFM fancy HVAC pump distilled PG at a temp that indicated I was at 2mmHG aka 2 torr aka
2000 microns, and my electronic micron gauge was reading it as 900 microns.
I paid $170 USD for the pump, including the digital micron gauge, and several different fittings. This was from a local classified ad.
Note: My A/C Condenser -> repurposed as vacuum pump pulls close to as much vacuum as the HVAC grade pump, without almost no sound, where as HVAC
pump sounds like a robot alien invasion is coming.
Anyone have experience connecting such things in series? Or setting up a 2 step series? Yes the topic is covered in 10000 threads, but I never found
nitty gritty details on connecting pumps in series.
|