Author Topic: Oxone or Performic/Peracetic  (Read 5897 times)

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Flip

  • Guest
Out of nowhere with a question
« Reply #20 on: June 11, 2002, 01:27:00 PM »
Hope nobody minds if I pop in from out of nowhere with a question, but.....

What are the potential differences in using ethanol instead of methanol in the oxone route?  Now this probably sounds idiotic but I have a friend who has not experienced much success after switching from smaller methanol reactions to larger ones using ethanol.  He suggested that the differing bp's of the solvents was perhaps to blame, as the exothermic reaction would run too hot. Would the solvent indeed be a factor or is the reaction just very sensitive to scale up?  A friend of mine is ready to abandon this method after recieving only occasional success.  What other factors might be involved in the success of the oxone run?

_flip_@hushmail.com

Chromic

  • Guest
Performic, peracetic and persulfate
« Reply #21 on: June 11, 2002, 01:33:00 PM »
Sorry, I stand corrected. I assumed that since formic acid is a stronger oxidizer than acetic acid, the write up for the performic acid surely couldn't be greater than 5hrs.

Turns out it is, for whatever reason. Might be unnecessary too.

humidbeing

  • Guest
oxone
« Reply #22 on: June 11, 2002, 04:08:00 PM »
Also, swim would like to know the sucsess ratio, for those
that have been trying the oxone route.

CG I miss you sweety, I really do.

pickler

  • Guest
Humid, Pickler uses the oxone on a regular basis ...
« Reply #23 on: June 11, 2002, 05:03:00 PM »
Humid, Pickler uses the oxone on a regular basis and it works fine.

We'll soon find out if I'm a chemist or not!

aznxprophetxtasy

  • Guest
Yes, ethanol can be used...
« Reply #24 on: June 11, 2002, 07:18:00 PM »
Yes, ethanol can be used read the article on rhodiums site thoroghly about oxone. "Oxidation of propenylbenzenes to P2P's using Oxone" by Chromic (THANKS CHROMIC FOR THE WONDERFUL RIGHT UP)

Addendum by Psychokitty...

"Old paper detailing the oxidation of many substances using Oxone hints strongly that ethanol can be used in place of methanol as the solvent in this reaction. Use of isopropanol is also possible. All solvents seem to react to some degree with the Oxone in solution."

SWIM plans to use ethanol of methanol for his oxone run and it should work according to theory....

GOD

  • Guest
why is that?
« Reply #25 on: June 11, 2002, 10:58:00 PM »
pickler-
are there any specific modifications swiy is using for oxone runs?  Swim see's quite a few bee's having difficulties.  In swiys opinion, what is the reason for this? (other than not strong enough vacuum).

when someone asks what the sound of one hand clapping sounds like, you should smack them in the ear.

pickler

  • Guest
The only thing Pickler does is filter the oxone ...
« Reply #26 on: June 11, 2002, 11:16:00 PM »
The only thing Pickler does is filter the oxone to make an oxone solution. That's it. Swim just follows the synth after that!

We'll soon find out if I'm a chemist or not!

chem_123

  • Guest
interchangeable? ethanol and methanol in the oxone
« Reply #27 on: November 01, 2002, 02:14:00 PM »
so, as Flip stated, ethanol can it bee exchanged for methanol? and it seems that it can, then, can the other bee true as well?
methanol bee used instead of ethanol?

                             
                                      Why?

Rhodium

  • Guest
Not for all reactions, but in many instances.
« Reply #28 on: November 01, 2002, 02:38:00 PM »
Not for all reactions, but in many instances.

chem_123

  • Guest
the Al/Hg/MeNO2 amalgam?
« Reply #29 on: November 01, 2002, 02:52:00 PM »
can it bee substituted there? that's the only place that it suggests using it.

500mL ethanol in a flask with 400mg of HgCl2 (669mg of HgI2?), etc.

can 500mL of methanol bee used?

                             
                                      Why?

Rhodium

  • Guest
Yes. HgI2 will take much longer to amalgamate ...
« Reply #30 on: November 01, 2002, 03:37:00 PM »
Yes. HgI2 will take much longer to amalgamate though, as its solubility is so low (regardless of solvent).

terbium

  • Guest
Mercuric iodide from Tincture of Iodine.
« Reply #31 on: November 01, 2002, 05:38:00 PM »
Actually the Merck says that mercuric iodide has very good solubility in alcohol and also the equimolar amount of potassium iodide found in Tincture of Iodine should greatly improve its solubility in water.

Merck Index entry:

  5932.    Mercuric Iodide, Red. 
  Mercury biniodide.  HgI2; mol wt 454.40.  Hg 44.14%, I 55.86%.          Scarlet-red, heavy, odorless, almost tasteless powder; sensitive to light; at 130 deg becomes yellow, and then red on cooling.  Poisonous!  d 6.28.  mp 259 deg.  bp =350 deg and sublimes. Soly in water (25 deg) 0.006 g/100 g.  1 g dissolves in 115 ml alcohol, 20 ml boiling alcohol, about 120 ml ether, about 60 ml acetone, 910 ml chloroform, 75 ml ethyl acetate, 260 ml carbon disulfide, readily in alkali iodides, HgCl2, Na2S2O3; sol
in 230 ml olive oil, 50 ml castor oil.
  Protect from light.
          

          USE:  In anal. chemistry for preparation of Nessler's Reagent (alkaline mercuric potassium iodide solution).
          THERAP CAT:  Antiseptic (topical).
          THERAP CAT (VET):  Has been used as a topical antiseptic, counterirritant, vesicant.



Baseline Does Not Exist.

madprosr

  • Guest
evil mercury chemists unite!
« Reply #32 on: November 13, 2002, 10:41:00 PM »
Swim tried adding I2 crystals (made from NaI + HCl + H2O2, dried 4h over CaCl2) to elemental Hg. 0.32g I2 was added to 0.25g Hg. It did not turn to a red powder as hellman describes. The substances were mixed with a strip of Al (bad choice...)
It remained a pile of purple I2 crystals with little Hg blobs buried in it.
4h later it looks the same, if anything the pile is more black, the end of the Al strip has turned black and gooey (yuck, why didn't swim use glass).

Swim also put .5g Hg in 30ml of 2% I2, 2.4% NaI, 47% alcohol 4 days ago. Swim has shaken it 2-3x per day but the Hg is very slow to react and dissolve. Annoying, swim wants to amalgamate things!!!

hCiLdOdUeDn

  • Guest
when swim puts the mercury in 2% tincture it ...
« Reply #33 on: November 14, 2002, 01:32:00 PM »
when swim puts the mercury in 2% tincture it actually doesnt seem to dissolve much of the Hg (visibly) but the 15mL of the solution will amalgmate around 25g of foil :)

From my experiments 1g of mercury can make ~100mL of tincture/hg solution which is enough to amalgamate up to 150g of foil.

Sink or SWIM

El_Zorro

  • Guest
So basically you're saying to dissolve as much ...
« Reply #34 on: November 14, 2002, 04:12:00 PM »
So basically you're saying to dissolve as much mercury as possible in 2% tincture, then use 15ml of the resulting liquid in a reaction with 25g of aluminum foil, not 25g of ketone?

Who is that masked man?

hCiLdOdUeDn

  • Guest
Yep! It works perfectly.
« Reply #35 on: November 14, 2002, 05:20:00 PM »
Yep! It works perfectly. First the solution with the alcohol/aluminum/tincture mixture is red then after 15minutes faint bubbling will be noticeable. This is when the color goes clear and then after 45min the aluminium is eaten up and it turns to a grey sludge and bubbling is pretty fast.

Sink or SWIM

El_Zorro

  • Guest
Have you tried it with a larger quantity of Al ...
« Reply #36 on: November 14, 2002, 06:20:00 PM »
Have you tried it with a larger quantity of Al than 25g?

Who is that masked man?

PoohBearium

  • Guest
See also
« Reply #37 on: November 14, 2002, 06:21:00 PM »
This is where it all started (sort of):


All aminations were of the al/hg variety, using methanol as a solvent (isopropanol was never used successfully), with ~.5 gram blobs of hg dropped into I2 tincture, allowed to react for a few days, and then used to amalgamate.
 
~unnilhexium




Post 248601

(unnilhexium: "Re: When substituting GAA for Formic acid...", Chemistry Discourse)


"All aminations were of the al/hg variety, using methanol as a solvent (isopropanol was never used successfully), with ~.5 gram blobs of hg dropped into I2 tincture, allowed to react for a few days, and then used to amalgamate.

Swim recorded an actual amalgamtion time, it took 17 minutes(.5g mercury blob, 30g Al). The basic procedure is to put a plastic dish on the old balance, zero it, and poke at a mercury blob until about .3-.5 grams is weighed out, then dump it into some 2% I2 tincture, the kind you buy at walmart.  I can't verify that HgI2 is formed, but I have successfully amalgamated using this procedure."

~unnilhexium




Post 266225

(PoohBear4Ever: "Re: MM Nitro/Al-Hg variation:  No HgCl2", Methods Discourse)


...ISO-SWIM decided that instead of using HgCl2, he would try Hg(2?)I2 instead(mercury blobs dropped into I2 tincture, ala unnilhexium).  The batch was done at a half scale, 12.5g ketone, 10ml MeNO2 and 13.7g aluminum foil.  The tincture, .24g Hg from a thermometer dropped in a 30ml 3% I2 tincture 1 week earlier, was dissolved in 400ml MeOH, and dumped into a 2L RB flask, to which the aluminum and a 2.5 inch stirbar had already been added.  Amalgamation took approximately 35-40 minutes, and once complete, the ketone/nitro was dripped in.... 

~unnilhexium




Post 263260

(isohuman: "MM Nitro/Al-Hg variation:  No HgCl2", Methods Discourse)

That should answer all you question on HgI2...

PB


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