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Topic: Purifying Organic solvents in Azeotropes  (Read 2950 times)

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Offline HCopeland

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Purifying Organic solvents in Azeotropes
« on: July 10, 2016, 11:35:26 AM »
Hey Everyone, New organic chemist here. Yesterday I started running fractured distillations on Crown Handi-Strip Paint stripper to get DCM. Here is the MSDS data.
40 - 60% METHYLENE CHLORIDE (DCM, Dichloromethane)
25 - 45% METHANOL
15 - 25% TOLUENE           
5  - 15% ACETONE   
0  -  5%  PARAFFIN WAX 
0  -  5%  NONYLPHENOL ETHOXYLATE 

So I have approximately 500mL of distillate from a 1L Batch. My vapor temp peaked at the end around 50C. What should I expect in the distillate and How would I separate it fully to 100% methanol free DCM?

P.S. If have any references it would be awesome to have them. I plan to try to distill 98% Nitric Acid and that information would be useful for that synthesis.

Offline Arkcon

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Re: Purifying Organic solvents in Azeotropes
« Reply #1 on: July 10, 2016, 12:05:34 PM »
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Hey Everyone, New organic chemist here.


Awesome, we're always glad to help a new student.

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Yesterday I started running fractured distillations on Crown Handi-Strip Paint stripper to get DCM. Here is the MSDS data.

Ok, um ... yikes.  Most schools provide solvents for their students.  But  hey, if you think you're up to it, and have the resources (glassware, proper heat source -- that's electric not a flame, and other safety procedures) this is a start.

A quick search doesn't give me any dichloromethane azeotropes.  Maybe you can find some tables in the CRC in nearest university library.  The typical way to separate a binary azeotrope is to use a ternary azeotrope, but again, you'll need to find a comprehensive table.

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P.S. If have any references it would be awesome to have them. I plan to try to distill 98% Nitric Acid and that information would be useful for that synthesis.

OK, urm ...double yikes.  Be real certain you're prepared for this, safety-wise.  Start with reading the properties.

As an example of reading, here's a link to a resource that describes a simpler procedure:  http://www.sciencedirect.com/science/article/pii/S004040390002253X  Maybe a local library will get it for you for you to read.  It supposedly discusses further synthetic uses of the mixed reagent.  You'll want to compare it with your plans, and see if it all makes sense to you.  The more you know, the better off you are.

Hey, I'm not judging.  I just like to shoot straight.  I'm a man of science.

Offline AWK

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Re: Purifying Organic solvents in Azeotropes
« Reply #2 on: July 10, 2016, 02:37:18 PM »
CH2Cl2 forms azeotrope with methanol, bp 37.8 containing 92.7 % of dichlormethane.
AWK

Offline lb2

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Re: Purifying Organic solvents in Azeotropes
« Reply #3 on: July 10, 2016, 04:00:35 PM »
Hi HCopeland,

Welcome to the organic chemistry community!

What you are trying to do is a bit suspicious. I won't inquire about the legitimacy of what you are doing, but it's highly unlikely that any organic chemist, even a "new" one, would ever look into distilling paint stripper to get their hands on some DCM.

In any case, whatever the situation is, since you seem to have quite limited experience I would highly advise against you attempting to distill 98% nitric acid. If you don't know what you are doing, this could result in very serious harm.

Offline orthoformate

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Re: Purifying Organic solvents in Azeotropes
« Reply #4 on: July 11, 2016, 10:17:10 AM »
https://en.wikipedia.org/wiki/Azeotrope

A little research in the area of Azeotropic distillation will help you solve this problem.

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