I wanted to carry out a polymerization reaction using radical mechanism, so I wanted to recrystallize my initiator AIBN. Can anyone help me with it? Thank you.
When I recrystallized AIBN I would make a supersaturated solution of it using methanol.
1) Heat methanol to 50 deg C
2) Have an amount of AIBN in a separate beaker
3) Will stirring add the hot methanol to the AIBN until it is dissolved
4) Allow the mixture to cool. This should allow for crystals to form
When I recrystallized AIBN I would make a supersaturated solution of it using methanol.
1) Heat methanol to 50 deg C
2) Have an amount of AIBN in a separate beaker
3) Will stirring add the hot methanol to the AIBN until it is dissolved
4) Allow the mixture to cool. This should allow for crystals to form
I recommend you the book "Purification of Laboratory Chemicals" by W.L.F. Armarego and C. Chai. Very useful!
Temperature of crystal. solution below 40 °C:
o:,a'-Azobis(isobutyronitrile) (AIBN) [78-61-1] M 164.2, m 103°(dec). Crystd from
acetone, E2O, CHCl3, aq EtOH or MeOH. Has also been crystd from abs EtOH below 40° in subdued
light. Dried under vacuum at room temp over P205 and stored under vacuum in the dark at
methanol as described above. If not used immediately, store at reduced temperature
The AIBN was purified by recrystallization in methanol. Approximately 5 g of AIBN
were weighed on an analytical balance and transferred to an Erlenmeyer flask with
cover, along with about 200 ml of methanol The mixture was stirred tr,
using a magnetic stirrer for 1 hour at room temperature. in
Then, filtration was performed using filter paper. The undissolved part was
discarded while the filtrate was placed in the refrigerator for 24 hours. There was
New filtration through filter paper, withdrawing now crystals of AIBN
formed at low temperature. AIBN was recrystallized dried in the desiccator
reduced and, after drying, was transferred to a pressure bottle with lid and
stored in the freezer until use.
The original master's thesis can be found on the website:
http://www.lume.ufrgs.br/bitstream/handle/10183/16176/000697955.pdf?sequence=1
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