Chemical Forums

Please login or register.

Login with username, password and session length

Sponsored links

Pages: [1]   Go Down

Author Topic: Need help on a Nitrogen protected high temperature hydrolysis reaction setup  (Read 2635 times)

0 Members and 1 Guest are viewing this topic.

Grundalizer

  • Full Member
  • ****
  • Mole Snacks: +19/-31
  • Offline Offline
  • Posts: 257

I'm going to be running a high temperature hydrolysis of Iron (III) Chloride in DEG with NaOH.  I will need to reach a temperature of 220C for 30 minutes under nitrogen protection and constant stirring.  I assume the best method of heating will be a heating mantle, but am unsure if a 3 neck round bottom flask is the appropriate piece of glassware to use.  Also, any tips on flow rates of N2?  I'm thinking 1 neck has N2 bleed in, middle is thermometer, and the 3rd neck is left uncovered, or at least has a pressure release valve.  I'm trying to make colloidal nano clusters, and by varying the amount of NaOH I can control their diameter.  I'll also have to reflux for an hour around 190-200C i believe.

Thanks for any help on the glassware setup.

I drew a picture.. let's see if it works
Logged

democanarchis

  • Regular Member
  • ***
  • Mole Snacks: +9/-0
  • Offline Offline
  • Posts: 72

I'd propose the following setup.

3-neck roundbottom with stirrer in mantle as per your illustration.
Neck 1: Temperature probe through septum or thermometer through quickfit adaptor, ensuring it isn't in the path of the stirbar and doesn't touch the sides.
Neck 2 (central): Condenser with air outlet running to schlenk line.
Neck 3: Glass stopper, use for addition.

Assemble as above, except with glass stopper instead of thermometer. Evacuate/refill with N2 3x, Add reagents, repeat. Swap out stopper for thermometer, begin heating. If you do it this way, you will be under a blanket of N2 with no need to have a constant flow which would depress the internal temperature and make heating take longer. Just keep the schlenk line open with just enough N2 flow to be visible in your oil bubbler.
Logged

Grundalizer

  • Full Member
  • ****
  • Mole Snacks: +19/-31
  • Offline Offline
  • Posts: 257

I love you.  Thanks for the reply.  This is the first time I'm going to be doing a reaction like this, and I'm a little nervous and excited.  My research advisor is an Analytical Chemist, so she's iffy on orgo setups.  I'm going to ask our orgo proff too this week, he's been there for 40 something years so I imagine he's had his fair share of this.  I think he was from the day where they washed their hands in benzene and smoked while washing with ether.

I'm going to take a picture tomorrow and upload it with the setup, we do have a schlenk line but it's f&#^$*@ old, but it works because I've used it with the roto vap. 

My only question with not having a continuous flow is...where does the heat (hot air/ hot N2) escape too? 

Quickfit adapter meaning...just the normal glass and rubber septum thermometer holder that keeps it centered?

Also, I can picture the condenser on top, but do the normal water cooling lines go to water? and the top go to Schlenk?  I can't picture that...

thanks for help  +1



Logged
Pages: [1]   Go Up
 

Mitch Andre Garcia's Chemical Forums 2003-Present.

Page created in 0.056 seconds with 24 queries.