Author Topic: Home-made I2  (Read 15969 times)

0 Members and 1 Guest are viewing this topic.

Osmium

  • Guest
Home-made I2
« on: May 27, 1998, 11:09:00 AM »
This is just an idea, and I have no proof that it really works, but hey, go to the library and check it yerself.

First, obtain some NaI or KI. Dissolve it in water.
Second thing we need is a strong oxidising agent, like NOx (nitric acid + Fe wool), Cl2 (acidify bleach, or HCl and permanganate or MnO2), maybe even H2O2 or HNO3, which is bubbled through the iodide solution, or simply add one of the oxidisers to it. I don't know which one works, read and experiment.
This oxidises the iodide to iodine. Extract I2 with suitable solvent or distill I2 away with a stream of air to separate most of the inorganic shit.
Crude I2 is purified by sublimation. To do this, place crude I2 in a crystallizing dish and add some KI. Fill a large round-bottomed flask with cold water and place it onto the glass pot containing the crude I2. Now carefully heat the crude I2. It will evaporate and crystallize on the outside of the flask. Carefully remove it  to obtain quite pure I2.



Nobody interested?

O. checked it himself. It can be done, of course.
Oxidising agents like H2O2 in dil. HCl, Cl2, nitrite/H+, oxygen with NOx catalysis, K2Cr2O7, KMnO4, MnO2, bleach or PbO2(all in acidic soln) can be used.
The iodine is separated from the reaction mixture by (steam) distillation. Solubility of I2 in H2O is low (0.8g/l), all the crystals can be filtered away. Dry them in a desiccator over conc. H2SO4 or CaCl2 and purify by sublimation. Heat with sand bath. To avoid other halogenides as contaminants, especially when using Cl2 or bleach as oxidiser, grind the raw iodine with powdered KI before subliming.

Voila, OTC iodine, in huge amounts and inexpensive

Tlange

  • Guest
Re: Home-made I2
« Reply #1 on: May 28, 1998, 02:52:00 AM »
Brilliant....now if the RP was only as easy to make...hmmm. ;-)

Osmium

  • Guest
Re: Home-made I2
« Reply #2 on: May 28, 1998, 11:52:00 AM »
I'm working on it ;-)

Osmium

  • Guest
Re: Home-made I2
« Reply #3 on: July 01, 1998, 01:41:00 PM »
Hope you'll find it now, jimwig.

jimwig

  • Guest
Re: Home-made I2
« Reply #4 on: October 01, 1998, 02:42:00 AM »
Osmium - I have finally found it after almost ten months of searching all over the globe via the net of course. I can finally quit and take a shower- thank God!!!!!

drone 342

  • Guest
Re: Home-made I2
« Reply #5 on: October 15, 1998, 07:08:00 PM »
Os,

Do you have a work-up method for this now?

-drone #342


300 Spartans

  • Guest
Re: Home-made I2
« Reply #6 on: October 17, 1998, 02:20:00 PM »
try gathering the mushing into a pulp pacific kelp boil the shit out of it till dry then add you oxidizer and acids  aka osium let steep filter then heat placeing a round fish bowl over the top of your containerand as the man said Presto! unlimited and cheap supply of iodone crystals

Osmium

  • Guest
Re: Home-made I2
« Reply #7 on: October 18, 1998, 07:13:00 AM »
Drone: As I said, solubility of I2 in water is low, as long as no excess of I(-) is around. Simply filter it away or extract with organic solvent.
For bromine I recommend distillation of the reaction, or maybe blowing air through the solution and collecting it in a cold trap. In situ preparation of Br2 is probably best for brominations. I don't think extraction of Br2 is a good idea (cough, cough...). Reagent grade KBr from Merck is on its way to my house, and I will try it when I find the time.

drone 342

  • Guest
Re: Home-made I2
« Reply #8 on: October 20, 1998, 10:10:00 PM »
Os,

The extracting works pretty well for Br2 -- just use toluene. The toluene bromine solution is fractionally distilled (with an aspirator), and pure bromine is aquired. The advatntage is that by extracting with a solvent, you can get the volume of for your starting material for your distillation down, but the purity of the final product up. Nothing to it, though I'm definately interested if you have a better method. I look forward to labnotes. 

-drone #342


HoneyDream

  • Guest
Re: Home-made I2
« Reply #9 on: July 21, 1999, 08:58:00 AM »
Where can i obtain some I2?  sorry to sound lame, but if i have a question and i cant find it on search, or anywhere else the best i can do is ask..  what exactly is I2, iodine crystals?

pebble

  • Guest
Re: Home-made I2
« Reply #10 on: July 21, 1999, 09:54:00 PM »
I know that there are different ways to make iodine crystals and everybody it seems, has their own way. I have found that this works for me and it's quite easy to do. Here is the synth for making iodine crystal using tincture.
 
   Get a one gallon jar. Pour in 16 1oz. tincture bottles that contain 2% iodine, this is two cups. Then pour in a cup of muratic acid. The add two cups of hydrogen peroxide and then a cup of 70% ribbing alcohol. Shake this up and let it sit for 5 min. Then come back and fill the entire jar with very cold DH2O. Cap it and let it stand for 20 min. (Do not shake this time).

   Then get a couple of coffee filters and filter the liquid along with the iodine crystals. Then pour a little cold DH2O to stablize contents and taks your filters and squeeze out all water and then put your iodine crystal in a jar and you'll pure iodine crystals. It's really that easy. Other methods are also similar and others are just hard and complicated and a bullcarp waste of time. Try it and you'll see just how easy it really is.

Pebble


HoneyDream

  • Guest
Re: Home-made I2
« Reply #11 on: July 21, 1999, 11:17:00 PM »
thank you pebble.  one question about that:

At the end, you said filter the liquid in a
coffe filter, squeeze out the water from the
filters and you have pure iodine crystals.
my question is: are you saying the iodine
crystals will get stuck in the filter? as in
the liquids will go through the filter but
the iodine wont, and so all in your filter is
pure iodine crystals?

thankx.


pebble

  • Guest
Re: Home-made I2
« Reply #12 on: July 22, 1999, 12:37:00 AM »
Yes, just filter and at the bottom of the jar will be the iodine. You'll see it when you pour all the contents out. It will look like mush until you squeeze out all of the water. When you squeeze out all of the water, you'll have iodine crystals that the filters contain. Dump these in a jar. These are also light sensitive, so keep them away from light.

Pebble


Soldier

  • Guest
Re: Home-made I2
« Reply #13 on: July 22, 1999, 03:06:00 AM »
A quick way to test the purity of the Iodine from these methods is, take a small amount of I2 (about the size of the head of a pin or a little larger), put in pyrex dish, and heat in some safe manner. The I2 will sublimate. If the residue left is granular in texture then IODIDES are still present which washing with DH2o should take care of.

------------------
A little revolution...is a good thing. Thomas Jefferson


CHEM GUY

  • Guest
Re: Home-made I2
« Reply #14 on: July 25, 1999, 01:48:00 AM »
drone 342,

Last time I checked elemental halogens reacted with unsaturated carbon bonds with or without light present.

Br2 + C6H5-CH3 --> C6H5Br2-CH3


Merry Crankster

  • Guest
Re: Home-made I2
« Reply #15 on: July 28, 1999, 06:52:00 PM »
while dreaming anothers dream I screwed up but the results were exellent, heres how it whent.

   Dreamer misread h2o2 (hydrogen peroxide right) as dh2o(distilled water, right).

1 pint 7% tincture iodine(from feed store)

added to this 3 pints dh20

+ 1/2 cup of muriatic acid(hardwarestore                            stuff cement                                  cleaner)

then said oops that should have been h2o2 insted of dh20.......

so then added 1 pint h202 nothing happening yet. so went to the hive and saw something about bleach and muriatic extraction of Iodine tincture.

so said what the hell and added bleach about 1/2 cup and whalla solution became clear brown color with lotso darke colored cystals floating around in there.

filtered crytals through a few coffee filters  in funnels pressed out extra liquid and air dried an hour or so. Looks like killer Iodine  grey purplish crystle flakes/granules.
dreamed it in Hi/rp reduction at 1 part to 1 part Pephedrine with 1/2 part rp good product 50-60% return.



outlaw

  • Guest
Re: Home-made I2
« Reply #16 on: July 31, 1999, 12:51:00 AM »
Ok I have a friend who has a plastic bag with
containing Organic iodine 40\salt base
ingrredients are ethylenediamine Dihydriodide,salt,artificial color, silicon Dioxide. Also says Salt(NaCI}minimum-87%
maximum-91%. can anyone give advice on what needs to be done to this for clean I2 if anythying. Believe me the search engine has been my life for over a month so if anyone can help Id apreciate it. Happy dreaming to all.

Demented Angel

  • Guest
Re: Home-made I2
« Reply #17 on: November 21, 1999, 10:54:00 AM »
I know this is an old thread, but was wandering around the Hive, came across it, and thought, "Hey, since folks have posted a couple of quick and easy ways to get I2, and since 'How do I get I2?' is a commonly asked question, why dont I go ahead and post a method I came across?"

So here goes.  I came across this method awhile ago, and dreamt that it worked very well.

This was originally posted by cantstanditanymore, and has been rewritten by me because I have misplaced the original document.  Oops! 

DA


Iodine Extraction
-----------------
Originally posted by cantstanditanymore

Ingredients:
   1 pint tincture of iodine (7%)
   3 pints hydrogen peroxide (3%)
   1/2 cup distilled water
   1/2 cup muriatic acid

Other things needed:
   1 gallon jug
   1 set rubber gloves - nothing says cook like iodine stained fingers!
   coffee filters
   more distilled water for rinsing of product

Put tincture, peroxide, acid, and distilled water in your clean gallon jug.  (Note, as with all chem equipment, only clean it with distilled water.)  Cap the jug and shake well.  Set aside for 20 minutes or so.  Go watch an episode of South Park while you wait.  Pour off excess liquid.  Take 2 coffee filters, placing one inside the other, and filter remaining product through the coffee filters.  When filtration is complete, roll up product in filter and squeeze firmly to remove moisture.  Transfer to clean set of coffee filters and rinse crystals with distilled water.   Do this 4 times to clean your product.  Once again, squeeze firmly to remove as much moisture as possible.  Place product on clean, dry filters or in pyrex dish, and set in a dark place to dry.  As soon as is dry, transfer product to dark, airtight container.  Approximate yield, 16 grams.



Demented Angel

  • Guest
Re: Home-made I2
« Reply #18 on: November 21, 1999, 12:21:00 PM »
Oh, one thing I nearly forgot.  Original post told of using pantyhose to filter crystals out.  In my dream I didn't have any hose around so used the coffee filters.  Hose seem like might have worked easier.

DA


Dorian Gray

  • Guest
Re: Home-made I2
« Reply #19 on: November 25, 1999, 11:57:00 PM »
Try this:

1. Dissolve 100g KI or NaI in 300ml 10% HCl
2. Add 100ml H202 (hydrogen peroxide)

As you add the H202, I2 falls out. This can
be filtered off, as it is only slightly soluble in water.
It is a good idea to wash it with some distilled water, as it might still contain some KCl or NaCl.
When I do this in my dreams, I squeeze the filter to get the I2 crystals dry (not completely).
Then it can be purified by resublimation (see above).

reaction mechanism (:-)):

The H2O2 gives off oxygen ions.
These react with the hydrogen ions
from the HCl to form H20. The H202 is now H20, too, since the O left it, because they argued the whole time. Not a very stable relation, that H202.
Now that chlorine ions from the HCl are alone.
But they don't want to be alone. They want to be satified. So they grab the K ions from the KI, since they are stronger than those iodine ions.
Now the iodine ions are alone. And they want to be satisfied, too. So they react with temselves to form I2 :-).

D.G.