careysub
International Hazard
Posts: 1339
Registered: 4-8-2014
Location: Coastal Sage Scrub Biome
Member Is Offline
Mood: Lowest quantum state
|
|
Fractionation Insert for West Condenser
I was contemplating what the minimal set of condensers for a home lab might be, if one wanted to do fractional distillation, regular distillation, and
reactions under reflux.
I think the number is two to allow for a reflux with product condensation set-up, but then the question is which two?
The West seems the most versatile (and is inexpensive), and lab guides describe using packing materials (glass beads, tubes, copper padding).
Looking at a 14/20 200 mm West condenser, I am dubious about stuffing random materials into the tube and getting them in and out satisfactorily.
This got me thinking about a single insert piece that could be inserted and retrieved easily. Perhaps with proper design a superior performance might
be achievable.
What I am think of is an all-copper assembly put together with press fits, perhaps consisting of a copper rod inserted through perforated/formed
copper sheet disks (20-40 of them?). The disks could be stamped out from a template.
Question is - what would be a good plate design?
Holes offset from plate to plate?
I notice that Vigreux columns have downward sloping eaves, so snipping into each disk would allow bending leaves/vanes up or down.
Hickman heads have a moat around an aperture, something like this could be stamped out (upraised cup edges?).
You could make a continuous structure out of coiled wire.
[Edited on 4-10-2014 by careysub]
|
|
forgottenpassword
Hazard to Others
Posts: 374
Registered: 12-12-2013
Member Is Offline
Mood: No Mood
|
|
Have you looked at the design of a Dufton column? It is essentially as you suggest -- a solid insert with a continuous coil wrapped around to force
the vapour to the walls. Originally a piece of wire was used, but there are all glass ones sold too. It is a very effective column design.
|
|
careysub
International Hazard
Posts: 1339
Registered: 4-8-2014
Location: Coastal Sage Scrub Biome
Member Is Offline
Mood: Lowest quantum state
|
|
Quote: Originally posted by forgottenpassword | Have you looked at the design of a Dufton column? It is essentially as you suggest -- a solid insert with a continuous coil wrapped around to force
the vapour to the walls. Originally a piece of wire was used, but there are all glass ones sold too. It is a very effective column design.
|
No, I had never heard of these.
It looks like the central cylinder plus coil almost completely fills the condenser tube (enough clearance for removal and insertion). Selecting the
proper rod diameter and wire gauge would allow a close fit.
How much clearance is needed between the condenser tube and central rod (thus dictating the preferred gauges)?
Having the name "Dufton" and Googling, I also found this:
http://www.nsexports.com/fractionating-columns.php
At the bottom is a "Fractionating Columns Rod and Disc Pattern" showing what appears to be a rod with disks strung on it exactly as I described. I
wonder if they are just plain disks, with a small gap for vapor passage?
|
|
forgottenpassword
Hazard to Others
Posts: 374
Registered: 12-12-2013
Member Is Offline
Mood: No Mood
|
|
I would say about 2mm. I have one that I could measure, but it is packed up in a box somewhere. You could probably find a reference giving diameter of
wire to use in an old textbook. It was a widely used design.
The 'disc pattern' column is called an Oldershaw column, I believe -- although there the plates are permanently attached to the wall of the column.
|
|
careysub
International Hazard
Posts: 1339
Registered: 4-8-2014
Location: Coastal Sage Scrub Biome
Member Is Offline
Mood: Lowest quantum state
|
|
Quote: Originally posted by forgottenpassword | I would say about 2mm. I have one that I could measure, but it is packed up in a box somewhere. You could probably find a reference giving diameter of
wire to use in an old textbook. It was a widely used design.
The 'disc pattern' column is called an Oldershaw column, I believe -- although there the plates are permanently attached to the wall of the column.
|
Thanks, knowing the names of things really helps in locating information about them.
Knowing "Oldershaw" I quickly located this report:
http://www.nt.ntnu.no/users/skoge/prost/proceedings/ecce6_se...
describing the construction of an Oldershaw variant.
It uses circular plates strung on a central column with little holes in them (same as my concept), but with "downcomers" a vertical surface attached
to the plate. In this system the plates have an edge gasket to seal them on all but the "downcomer" side.
I would implement this by stamping/cuttting the plates out of thin copper sheet, with a downcomer extension on one side that is bent to create the
downcomer surface. Perforate the central hole, punch little vapor holes, string on a copper rod and you are done.
The spiral design is also interesting. A 14/20 West condenser has a small bore, so a thinner gap might be in order. 14 or 16 gauge copper wire (1.6
and 1.3 mm) should do it. A good implementation would be to use glass tubing (available in all even mm diameters, I think), and secure the wire coil
to the tube by inserting wire ends into the tube ends and melting closed.
[Edited on 5-10-2014 by careysub]
|
|
Magpie
lab constructor
Posts: 5939
Registered: 1-11-2003
Location: USA
Member Is Offline
Mood: Chemistry: the subtle science.
|
|
You might be able to make a Podbielniak column by placing a helical wire against the inside wall. You may have a little trouble finding information
on this design. It is described in Cason & Rapoport's book Laboratory Text in Organic Chemistry, 1950. This book also cites
Podbielniak, Ind. Eng. Chem, Anal Ed, 3, 177, (1931) for column construction.
[Edited on 5-10-2014 by Magpie]
The single most important condition for a successful synthesis is good mixing - Nicodem
|
|
zenosx
Hazard to Others
Posts: 188
Registered: 7-7-2012
Location: East TN / Near Oak Ridge
Member Is Offline
Mood: Awaiting Results....
|
|
It was broken long ago, but when I was much younger my mum got me a condenser/column that had a glass spiral wrapped around a glass rod that could be
inserted into the condenser. There was very little play between the spirals and the sides, and it rested on the three prongs most liebig's have. If I
still had it I would post a photo
A question that sometimes drives me hazy: am I or are the others crazy?
Albert Einstein
|
|