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Manifest
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KClO3 Stoichiometry questions
Hello, I am planning on doing the boil down bleach method however I am unsure whether to make an equally concentrated volume with KCl or to use the
stoichiometric amount in a saturated solution.
(Nurdrage says use equal volume, MrHomeScientist says use stoichiometric amount)
I am unsure whether I am doing this correctly:
First off, the disproportionation:
3 NaClO → 2NaCl + NaClO3
I have 5% bleach and I plan to boil down a litre so 5% of 1000 is 50.
50 grams NaClO = 0.67 moles
So I divide that by 3 = 0.67/ 3= 0.22 moles
0.22388794856 moles to grams = 23.83 grams of NaClO3
Next reaction is
KCl + NaClO3 → NaCl + KClO3
23.83 grams = 0.22
0.22 moles of KCl = 16.69
and 27.43g of Potassium Chlorate produced.
Is this accurate? Because that is pretty shit for a litre of Bleach.
You guys are all jealous of my scales, take the green shades off.
[Edited on 28-4-2014 by Manifest]
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plante1999
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Looks very similar to the pratical results I had obtained in the past. Electrolysis is the way to go.
I never asked for this.
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Manifest
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And that is with 100% efficiency.
Electrolysis is in process. I run it from 9 in the morning from when I wake up to 10 and night, that reminds me...
It's been running for 2 days this way now at 1Amp, 6 volt
When I switch to 12 volts for a second I get 5 Amps.
I figured this would have decreased due to loss of sodium chloride, maybe not.
Anyway, should I keep being patient or how do I know when electrolysis is complete?
How much KCl do I add? Should 50g be sufficient?
[Edited on 27-4-2014 by Manifest]
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plante1999
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Depends on you exact set-up.
Electrolysis should be kept at 3.3 to 5 V for maximum efficiency, over that you degrade your anode more then anything else.
I never asked for this.
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Chemosynthesis
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Not to nag, but it's "Cl" rather than "CL." The latter hurts my eyes.
Edit- thanks. Also, I agree with Plante99; for both chlorate and perchlorate production, electrochemistry is the way to go. I recall some friends of
mine way back using industrial strength reagents to disappointing effect.
[Edited on 27-4-2014 by Chemosynthesis]
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Manifest
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Apologies, that was due to fast typing.I only do it on K̶C̶L̶ KCl
Corrected.
[Edited on 27-4-2014 by Manifest]
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Manifest
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What am I doing wrong with your formula Plante?
As per your PDF
Time(H)= ((171.6/amp)x saltm)x %100
x= ((171.6/1)*1*35 = 6006 hours?
250.25 days? That can't be right.
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plante1999
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EDIT
I made a small mistake.
It appears I made a mistake in the equation I gave!
You should divide by the %. As such 35 become 0.35 and you divide instead of multiplying.
Total run time approx : (171.6/1) x 1 / 0.35 = 490 hours
490/24 = 20 days at 35% efficiency.
[Edited on 27-4-2014 by plante1999]
I never asked for this.
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Manifest
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No, I have got 1 Mole in my cell at a efficiency of 35%
EDIT
Oh, I see.
20 Days straight though, will I get a shit result if I continue until Sunday?
[Edited on 27-4-2014 by Manifest]
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plante1999
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It will need 20 days straight to turn one mol of salt into one mol of chlorate with pH control at 35% efficiency with one amp. By pumping two amp it
would be two time as fast.
I never asked for this.
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Manifest
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Would I not be better to apply 6 amps or would that rip the anode apart?
Should I add acid to bring the PH down?
Would Vinegar work or is it too weak?
[Edited on 27-4-2014 by Manifest]
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plante1999
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Hydrochloric acid is better.
Depends on your anode, mmo will work at 0.2 amp per square cm of surface area. The killer is the voltage, not the amps usually.
I never asked for this.
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S.C. Wack
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Quote: Originally posted by Manifest  | | I am unsure whether to make an equally concentrated volume with KCl or to use the stoichiometric amount in a saturated solution.
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There are situations where double salts can be formed with excess KCl but not here I think.
Calcium hypochlorite is the way to go, if you want lots and want it today.
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Zyklon-A
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Here is some information on chlorate production stoichiometry:
http://www.sciencemadness.org/talk/viewthread.php?tid=28777&...
I agree with S.C. Wack that calcium hypochlorite is the most efficient method if you want it fast - not the cheapest, but the fastest.
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blogfast25
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Were they expensive, your picogram scales? 
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Zyklon-A
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No, I struck a special deal, I got them for free when I bought the Hadron Collider!
[EDIT] Ah, I thought you were talking to me, I used nearly the same figures in the link supplied above.
[Edited on 28-4-2014 by Zyklonb]
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Bert
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Mood: " I think we are all going to die. I think that love is an illusion. We are flawed, my darling".
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Dang, that is one REALY ACCURATE scale there!
Say, can I borrow the Hadron collider on weekends if I pay the power bill?
Rapopart’s Rules for critical commentary:
1. Attempt to re-express your target’s position so clearly, vividly and fairly that your target says: “Thanks, I wish I’d thought of putting it
that way.”
2. List any points of agreement (especially if they are not matters of general or widespread agreement).
3. Mention anything you have learned from your target.
4. Only then are you permitted to say so much as a word of rebuttal or criticism.
Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).
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MrHomeScientist
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In my video I followed the procedure I'd seen elsewhere of combining equal volumes of boiled bleach and KCl solution, but as you mentioned I do think
stoichiometric would have been better. Less water available for the chlorate to dissolve in should lead to better recovery. The only reason I can
think of to have such a huge excess of KCl is maybe some sort of common ion effect further reducing solubility of the chlorate. I need to try this
again with stoichiometric amounts.
I've also now done electrolysis, and it works very well. The bleach method is nice and simple, but if you have the apparatus for electrochemistry
that's the way to go. I've only done one run for 24 hours, so I can't say anything about electrode life, but it went quite smoothly. It's nice to be
able to just set it up and walk away while it does the work for you.
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Zyklon-A
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Electrolysis is the way to go if you want a lot.
Don't use graphite unless you want to waist a lot of time and compromise the purity of the product. I am running a cell with MMO anodes currently,
and I have plenty of MMO if you want to buy some.
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Manifest
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Haha you guys are assholes, I didn't feel like shortening it to two digits because I copy and pasted from the Google calculator.
It's more accurate anyways.
Yes, I know how to round off, Bert.
MrHomeScientist, did you record your electrochemical synthesis? I'd love to see it.
[Edited on 28-4-2014 by Manifest]
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blogfast25
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We're the *ssholes? You don't think using numbers like that makes you look a bit silly?
Oh well...
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MrHomeScientist
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Unfortunately no I did not record it. I did the experiment as a last-ditch, emergency bid to make some chlorate I needed for a demonstration that
weekend. So I really threw it together poorly and had little time to record and edit a video. Now that I know it works, though, I'll definitely
produce a video on it.
I've made a commitment to myself that I'm going to do something in the lab every weekend. This is an effort to increase my YouTube posting
frequency, but it doesn't necessarily mean a new video every week (though I'd love to do that). So far, the first two weekends have been taken up
inventorying every one of my chemicals and developing a more organized and formal storage system. Turns out I have 155 unique chemicals in total!
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Manifest
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assholes in a joking, non serious kind of way, don't take me literally.
I guess it does.
@MrHomeScientist
How much Chlorate did you obtain and what was your electrodes and what voltage and current did you apply?
Is chlorate better/worse/equal to KNO3 for pyrotechnics?
[Edited on 28-4-2014 by Manifest]
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MrHomeScientist
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Here are the stats on my thrown-together chlorate cell.
Anode: MMO mesh
Cathode: Ti mesh
Immersed elecrode area: ~3in2 (~19cm2)
Voltage: 4.8V
Current: 2.55A
Run time: 24 hours
Yield: 28.5g very crude, greyish product
Detailed write-up:
I made a solution of 78.3g KCl in 260mL distilled water. To this I added 0.3g potassium dichromate dissolved in 5mL distilled water. I poured about
210mL of the finished solution into a plastic Chinese take-out container (as I said, thrown together quickly and not intended to last), and acidified
the rest with 0.5mL of 9.5M HCl and set it aside. I cut two slits in the lid of this container for the electrodes, and a small hole in the center to
vent (this was done outside).
I only ended up adding 1mL of the acidified stock solution about halfway into the procedure, because the volume hadn't realy appeared to decrease at
all. I immersed the container in a water bath, and the solution and bath were warm to the touch throughout.
After stopping electrolysis, I capped the container with a new lid and placed it in the fridge. After cooling and filtering off the liquid, I had
28.5g of product. This is extremely crude, and is a greyish-green in color. The grey color came from some powder that spalled off the MMO at the start
of electrolysis, but the mesh doesn't appear degraded at all (it was the first time I had used it). Definitely needs a recrystallization.
I have no experience with pyrotechnics, but I've heard that you should avoid chlorate and use perchlorate instead, due to its decreased sensitivity.
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AJKOER
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While the following disproportionation is widely promulgated:
3 HOCl ----) 2 HCl + HClO3
a commercial patent I have seen (see World Patent W091-03421-1, “High Purity Chloric Acid” , link http://www.google.com/patents/EP0490978A1?cl=en ) appears to imply the following scheme in a closed reaction:
3 HOCl ----) 2 HCl + HClO3
2 HCl + 2 HOCl = 2 Cl2 + 2 H2O
Net:
5 HOCl ----) 2 Cl2 + 2 H2O + HClO3
In other words, there is a possible loss of Hypochlorous acid to Chlorine so more likely around five moles of HOCl is required for each mole of HClO3
in a closed reaction chamber, and not three as is the common unqualified assertion.
[Edited on 29-4-2014 by AJKOER]
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