Sciencemadness Discussion Board
Not logged in [Login ]
Go To Bottom

Printable Version  
 Pages:  1  2  
Author: Subject: Arkoma attempts 95% azeotropic EtOH
aga
Forum Drunkard
*****




Posts: 7030
Registered: 25-3-2014
Member Is Offline


[*] posted on 15-4-2016 at 10:41


Quote: Originally posted by arkoma  

*Y'all do get the pun, dontcha'?

A Star Redneck.

Er, yeah, ahem, we just didn't like to say er, anything, ahem.

I now got about 450ml near-azeo EtOH.

Also some tripot phos in the oven in a now-broken glass bowl :(

Was OK until i cranked the heat to 220 C.




View user's profile View All Posts By User
macckone
International Hazard
*****




Posts: 2129
Registered: 1-3-2013
Location: Over a mile high
Member Is Offline

Mood: Electrical

[*] posted on 15-4-2016 at 12:55


Use a copper reflux colum like everyone else. Three foot with intercooler will give nice reflux ratios 3 or 4 :1. The length and diameter are very dependent on heat input. You can get over 80% in a single run from mash and azeotropic on a second run after diluting to 50%. Discard the heads and tails. Primary contaminant is acetyal which gives a butter flavor. You can distill water out of vinegar a setup like this with 10:1 reflux ratios. But SS is better for corrossion resistance as acetic acid will corrode copper.
View user's profile View All Posts By User
JJay
International Hazard
*****




Posts: 3440
Registered: 15-10-2015
Member Is Offline


[*] posted on 15-4-2016 at 17:06


I've used water-detecting paste that they sell at automotive stores to check for water in ethanol before (it's typically used for checking to see if you have coolant in your oil or water in your gasoline, etc.). Usually I just check the density (that's what ACS and USP suggest).

http://www.distill.com/specs/UK.html

I think you could add a small amount of anhydrous copper (II) chloride and look for a blue/green color to detect water, but I have not tried this... that might be a fun way to spend my Friday night.
View user's profile View All Posts By User
Corrosive Joeseph
International Hazard
*****




Posts: 914
Registered: 17-5-2015
Location: The Other Place
Member Is Offline

Mood: Cyclic

[*] posted on 22-4-2016 at 05:14


My 300mm stainless tube column packed with a scrubber returned 91% EtOH in one run from my 'moonshine' starting material...........

Testing my 400mm tube soon. More to come....................




Being well adjusted to a sick society is no measure of one's mental health
View user's profile View All Posts By User
arkoma
Redneck Overlord
*******




Posts: 1575
Registered: 3-2-2014
Location: On a Big Blue Marble hurtling through space
Member Is Offline

Mood: ¡socialista!

[*] posted on 22-4-2016 at 06:51


I'm actually NOT drinking it. (Dumbass alert) and after checking my Vogel's (D'uh!!!)(facepalm) CaO, which I have.




Quote:
“Travel is fatal to prejudice, bigotry, and narrow-mindedness, and many of our people need it sorely on these accounts. Broad, wholesome, charitable views of men and things cannot be acquired by vegetating in one little corner of the earth all one’s lifetime.”

and..

“The gentle reader will never, never know what a consummate ass he can become until he goes abroad.”

Mark Twain, The Innocents Abroad

View user's profile View All Posts By User
XeonTheMGPony
International Hazard
*****




Posts: 1594
Registered: 5-1-2016
Member Is Offline

Mood: No Mood

[*] posted on 22-4-2016 at 09:07


*Edit: Clarified statement

Step one: Throw the radio out, it has no place in a lab! Especially when dealing with flammables

Step Two: Hit self very hard with solid object for even thinking of consuming a mind altering substance when working with flammables and setting foot into a lab *(Alcohol consumption + Lab = Darwin award)

Step three: Make a shield around the column but do not directly insulate

Step four: Ditch the oil do as others stated and used distilled water bath (We need very precise temp control here)

Step five: Start with low heat, allow every thing to saturate befor bringing the heat up, the slower you go the higher the purity you get!

All distillations are the same I find, precise temp control and taking your time, and ensuring a clean well lit lab with no distractions and a clear head = high purity results!

Only insulate your fractional column if you simply can not get the head temp to the target with slight increase in the heat source, but if this is required drop the heat source down, let the column balance then insulate a fraction, allow to balance and see where you end up befor increasing the heat source again.

If you use ethanol allot it is well well worth building a dedicated unit out of copper, as it cuts down vastly on the time it takes in set up.

[Edited on 22-4-2016 by XeonTheMGPony]
View user's profile View All Posts By User
arkoma
Redneck Overlord
*******




Posts: 1575
Registered: 3-2-2014
Location: On a Big Blue Marble hurtling through space
Member Is Offline

Mood: ¡socialista!

[*] posted on 22-4-2016 at 09:14


Quote: Originally posted by XeonTheMGPony  

If you use ethanol allot it is well well worth building a dedicated unit out of copper, as it cuts down vastly on the time it takes in set up.


No. 250ml will last me a WHILE. I don't drink it. I've considered a 5 gallon still, only $200'ish, but nah. I'd get to thinking that I need to be SELLING the surplus. That would be all bad.

*EDIT* And yes, my notes narrate a "comedy of errors". As in, "Don't do it this way". I'm 52 years old and live alone in a detached home. I also know I can screw up.

I hope though that any younger/reckless/new to the hobby members read carefully and therefore don't have as cavalier an attitude. ;)

[Edited on 4-22-2016 by arkoma]





Quote:
“Travel is fatal to prejudice, bigotry, and narrow-mindedness, and many of our people need it sorely on these accounts. Broad, wholesome, charitable views of men and things cannot be acquired by vegetating in one little corner of the earth all one’s lifetime.”

and..

“The gentle reader will never, never know what a consummate ass he can become until he goes abroad.”

Mark Twain, The Innocents Abroad

View user's profile View All Posts By User
aga
Forum Drunkard
*****




Posts: 7030
Registered: 25-3-2014
Member Is Offline


[*] posted on 22-4-2016 at 09:16


Quote: Originally posted by arkoma  
CaO, which I have.

Let us know how that works out.

I tried it with oven-dried CaO and didn't get much drying of the EtOH at all.




View user's profile View All Posts By User
JJay
International Hazard
*****




Posts: 3440
Registered: 15-10-2015
Member Is Offline


[*] posted on 22-4-2016 at 09:19


Molecular sieves work great for removing the last of the water. They are a little pricey, but you can reuse them.
View user's profile View All Posts By User
XeonTheMGPony
International Hazard
*****




Posts: 1594
Registered: 5-1-2016
Member Is Offline

Mood: No Mood

[*] posted on 22-4-2016 at 09:20


Quote: Originally posted by arkoma  
Quote: Originally posted by XeonTheMGPony  

If you use ethanol allot it is well well worth building a dedicated unit out of copper, as it cuts down vastly on the time it takes in set up.


No. 250ml will last me a WHILE. I don't drink it. I've considered a 5 gallon still, only $200'ish, but nah. I'd get to thinking that I need to be SELLING the surplus. That would be all bad.


I used to use huge volumes as a solvent and for fuel so I had a 56gallon feed still! and the reflux was made out of 3" diameter copper with a thermostatically controlled condenser lol.

and it came out at 90% in large volume. But for you doing small batch work I'd make 1L once you get it all set up right and store it some where cool and dry, to get it right in small scale is a royal pain in the rear, well worth making more then you need as you'll regret not doing so.

But the critical point is there is no rushing it, the slower you go with your temp, the finer the finished product, part of that temp control is having a good tight gradient on your column
View user's profile View All Posts By User
arkoma
Redneck Overlord
*******




Posts: 1575
Registered: 3-2-2014
Location: On a Big Blue Marble hurtling through space
Member Is Offline

Mood: ¡socialista!

[*] posted on 22-4-2016 at 09:22


Quote: Originally posted by aga  

I tried it with oven-dried CaO and didn't get much drying of the EtOH at all.


I plan to take an Oxy-Acetylene torch to it to dry it. Heating to incandescence oughta do the trick. Vogel says DISTILL over CaO.





Quote:
“Travel is fatal to prejudice, bigotry, and narrow-mindedness, and many of our people need it sorely on these accounts. Broad, wholesome, charitable views of men and things cannot be acquired by vegetating in one little corner of the earth all one’s lifetime.”

and..

“The gentle reader will never, never know what a consummate ass he can become until he goes abroad.”

Mark Twain, The Innocents Abroad

View user's profile View All Posts By User
aga
Forum Drunkard
*****




Posts: 7030
Registered: 25-3-2014
Member Is Offline


[*] posted on 22-4-2016 at 10:17


Who is this Vogel dude ?

Bet it's PHDchemist in disguise ;)

Just kidding.

If it's in Vogel's 3rd, it will probably work if done correctly !

(the 'correctly' part tends to trip me up a lot ...)




View user's profile View All Posts By User
macckone
International Hazard
*****




Posts: 2129
Registered: 1-3-2013
Location: Over a mile high
Member Is Offline

Mood: Electrical

[*] posted on 24-4-2016 at 09:57


You can't oven dry CaO. You need extremely high heat and low carbon dioxide.
View user's profile View All Posts By User
zed
International Hazard
*****




Posts: 2269
Registered: 6-9-2008
Location: Great State of Jefferson, City of Portland
Member Is Offline

Mood: Semi-repentant Sith Lord

[*] posted on 24-4-2016 at 15:40


Well, 95% I can buy at my corner liquor store. Not terribly expensive either.

But, Absolute is a very handy reagent, and harder to come by. Molecular sieves, you say? You have done this?

Lately?



View user's profile View All Posts By User
macckone
International Hazard
*****




Posts: 2129
Registered: 1-3-2013
Location: Over a mile high
Member Is Offline

Mood: Electrical

[*] posted on 24-4-2016 at 19:25


I will stick with my epsom salts and potassium carbonate. You need 3A molecular sieves.
View user's profile View All Posts By User
aga
Forum Drunkard
*****




Posts: 7030
Registered: 25-3-2014
Member Is Offline


[*] posted on 24-4-2016 at 22:48


Quote: Originally posted by macckone  
You can't oven dry CaO. You need extremely high heat and low carbon dioxide

I put mine in an oven at ~ 220 C insead of the furnace.

This may easily explain why it didn't work.


[Edited on 25-4-2016 by aga]




View user's profile View All Posts By User
Eddygp
International Hazard
*****




Posts: 858
Registered: 31-3-2012
Location: University of York, UK
Member Is Offline

Mood: Organometallic

[*] posted on 25-4-2016 at 01:25


I would have added some dry (anhydrous) MgSO4 to the alcohol while distilling, as woelen suggested (CaSO4 is more of a hassle, MgSO4 can be easily removed!).
And yes, careful heating ensures efficiency; anti-bumping granules might be interesting if you really are having those problems - remember, safety is key, especially with hot flammable liquids!




there may be bugs in gfind

[ˌɛdidʒiˈpiː] IPA pronunciation for my Username
View user's profile View All Posts By User
JJay
International Hazard
*****




Posts: 3440
Registered: 15-10-2015
Member Is Offline


[*] posted on 25-4-2016 at 01:54


I'm distilling some right now from 70% through a 30 cm Vigreux on a water bath. It's pretty slow going (approx 100 mL per hour) and might require another distillation to reach 95%.

Edit: From 950 mL of 70% v/v denatured ethanol, approximately 720 mL of distillate dripped over until nothing more came through the Vigreux. I haven't checked, but I already know that the concentration is pretty close to 95%; I could distill it a couple more times, but I'm just going to dehydrate it.



[Edited on 26-4-2016 by JJay]
View user's profile View All Posts By User
arkoma
Redneck Overlord
*******




Posts: 1575
Registered: 3-2-2014
Location: On a Big Blue Marble hurtling through space
Member Is Offline

Mood: ¡socialista!

[*] posted on 25-4-2016 at 11:05


oh, this is "pricy" alcohol for sure. Not the point.




Quote:
“Travel is fatal to prejudice, bigotry, and narrow-mindedness, and many of our people need it sorely on these accounts. Broad, wholesome, charitable views of men and things cannot be acquired by vegetating in one little corner of the earth all one’s lifetime.”

and..

“The gentle reader will never, never know what a consummate ass he can become until he goes abroad.”

Mark Twain, The Innocents Abroad

View user's profile View All Posts By User
JJay
International Hazard
*****




Posts: 3440
Registered: 15-10-2015
Member Is Offline


[*] posted on 25-4-2016 at 19:44


Oh, right, if anyone wants to pay $100/L for anhydrous ethanol, hit me up :D

[Edited on 26-4-2016 by JJay]
View user's profile View All Posts By User
XeonTheMGPony
International Hazard
*****




Posts: 1594
Registered: 5-1-2016
Member Is Offline

Mood: No Mood

[*] posted on 26-4-2016 at 03:59


Quote: Originally posted by arkoma  
oh, this is "pricy" alcohol for sure. Not the point.


Pure near anhydrous Alcohol is very pricey! Lots of time, energy, material work goes into it on the lab scale.

That is why I do all my high investment synths in larger then needed batches, so when I need it all the work has all ready been don.
View user's profile View All Posts By User
Velzee
National Hazard
****




Posts: 379
Registered: 19-8-2015
Location: New York
Member Is Offline

Mood: Taking it easy

[*] posted on 26-4-2016 at 06:19


Where'd you get that pin, arkoma?

EDIT: Nevermind.

[Edited on 4/26/2016 by Velzee]




Check out the ScienceMadness Wiki: http://www.sciencemadness.org/smwiki/index.php/Main_Page

"All truth passes through three stages. First, it is ridiculed. Second, it is violently opposed. Third, it is accepted as being self-evident."
—Arthur Schopenhauer

"¡Vivá Cristo Rey!"
—Saint José Sánchez del Río
View user's profile View All Posts By User
Chemist_Cup_Noodles
Harmless
*




Posts: 46
Registered: 27-5-2015
Location: Northern VA
Member Is Offline

Mood: Anticipative

[*] posted on 26-4-2016 at 06:38


Hm, dehydrating your alcohols from what I've seen doesn't have to be too pricey. IIRC, you can use magnesium shavings and molecular seives. You might can get magnesium bits for free from a local machinist if you dig around hard enough. And molecular seives can be reusable if you dry them right. So this seems like a good way to go if you can wait a long time.

I found a pretty long JOC Article on drying your solvents that should be of good use: http://ccc.chem.pitt.edu/wipf/Web/Solvent_Drying.pdf




I'll be honest-- We're throwing science at the wall here to see what sticks. No idea what it'll do.
-Cave Johnson, Portal 2
Add yourself to this map of SciMad members! https://zeemaps.com/map?group=388676&add=1
View user's profile Visit user's homepage View All Posts By User
arkoma
Redneck Overlord
*******




Posts: 1575
Registered: 3-2-2014
Location: On a Big Blue Marble hurtling through space
Member Is Offline

Mood: ¡socialista!

[*] posted on 26-4-2016 at 08:16


@chemist_cup_noodles thanx for the paper KOH was never even on my radar.




Quote:
“Travel is fatal to prejudice, bigotry, and narrow-mindedness, and many of our people need it sorely on these accounts. Broad, wholesome, charitable views of men and things cannot be acquired by vegetating in one little corner of the earth all one’s lifetime.”

and..

“The gentle reader will never, never know what a consummate ass he can become until he goes abroad.”

Mark Twain, The Innocents Abroad

View user's profile View All Posts By User
JJay
International Hazard
*****




Posts: 3440
Registered: 15-10-2015
Member Is Offline


[*] posted on 26-4-2016 at 09:33


I wonder how hard it would be to remove ketone denaturants with sodium bisulfite.

I probably shouldn't....
View user's profile View All Posts By User
 Pages:  1  2  

  Go To Top