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ecos
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Thx PHILOU Zrealone for the answer.
this mean adding extra HCL won't harm ; this will make sure no chlorate exists.
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Then afterwards add some AgClO4 to precipitate Cl(-) as AgCl. |
I think this optional step. right?
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PHILOU Zrealone
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Quote: Originally posted by ecos  | Thx PHILOU Zrealone for the answer.
this mean adding extra HCL won't harm ; this will make sure no chlorate exists.
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Then afterwards add some AgClO4 to precipitate Cl(-) as AgCl. |
I think this optional step. right? |
Yes optionnal!
You can boil HClO4 under reflux to expell the HCl as a gas...and condense it in a basic media (HCl is terribly corrosive to iron containing aloys,
generating picking and rusting of all metallic pieces into the room ...HCl --> R.I.P.  rust in pièces  )
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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ecos
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It seems I didn't read your comments well
I thought you are talking about NaClO4 not HClO4 !!
I think HClO4 is very sensitive and can explode easily, I would prefer a more safer route if possible !
I hear about many hazards for HClO4
Perchloric acid from wiki :
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Anhydrous perchloric acid is an unstable oily liquid at room temperature
It is a powerful oxidizer when hot, but its aqueous solutions up to approximately 70% by weight at room temperature are generally safe, only showing
strong acid features and no oxidizing properties
Safety :
Given its strong oxidizing properties, perchloric acid is subject to extensive regulations.[12] It is highly reactive with metals (e.g., aluminium)
and organic matter (wood, plastics). On February 20, 1947, in Los Angeles California, 17 people were killed and 150 injured when a bath, consisting of
over 1000 litres of 75% perchloric acid and 25% acetic anhydride by volume, exploded. The plant, 25 other buildings and 40 automobiles were
obliterated and 250 nearby homes were damaged. The bath was being used to electro-polish aluminium furniture. In addition, organic compounds were
added to the overheating bath when an iron rack was replaced with one coated with cellulose acetobutyrate (Tenit-2 plastic). A few minutes later the
bath exploded.[13][14]
Work conducted with perchloric acid must be conducted in fume hoods with a wash-down capability to prevent accumulation of oxidisers in the ductwork.
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you scare me when you write BOIL !! 
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PHILOU Zrealone
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| Quote: Originally posted by ecos | It seems I didn't read your comments well
I thought you are talking about NaClO4 not HClO4 !!
I think HClO4 is very sensitive and can explode easily, I would prefer a more safer route if possible !
I hear about many hazards for HClO4
Perchloric acid from wiki :
| Quote: |
Anhydrous perchloric acid is an unstable oily liquid at room temperature
It is a powerful oxidizer when hot, but its aqueous solutions up to approximately 70% by weight at room temperature are generally safe, only showing
strong acid features and no oxidizing properties
Safety :
Given its strong oxidizing properties, perchloric acid is subject to extensive regulations.[12] It is highly reactive with metals (e.g., aluminium)
and organic matter (wood, plastics). On February 20, 1947, in Los Angeles California, 17 people were killed and 150 injured when a bath, consisting of
over 1000 litres of 75% perchloric acid and 25% acetic anhydride by volume, exploded. The plant, 25 other buildings and 40 automobiles were
obliterated and 250 nearby homes were damaged. The bath was being used to electro-polish aluminium furniture. In addition, organic compounds were
added to the overheating bath when an iron rack was replaced with one coated with cellulose acetobutyrate (Tenit-2 plastic). A few minutes later the
bath exploded.[13][14]
Work conducted with perchloric acid must be conducted in fume hoods with a wash-down capability to prevent accumulation of oxidisers in the ductwork.
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you scare me when you write BOIL !!
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And how would you get close to 100% HClO4 when using saturated HCl (max 35% by weight) knowing that you reflux boil it and that it forms an azeotropic
mix with 72% HClO4?
--> If you are below 72%, you will boil water first and then water + tiny % HClO4 and when 72% reached in the balloon it will distill as a pure
compound azeotropically.
So unless you use a strong dehydratant (H2SO4 conc, oleum, SO3 or P2O5) you will be very strong if you can get above 72% what is safe!
Also boiling with reflux doesn't allow much of the azeotropic mix to escape the balloon...water will and with it most of the HCl that has a strong
affinity for it.
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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PHILOU Zrealone
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You may aswel add a 10% quantity of HCl to a saturated NaClO4 solution; then boil down until all HCl is gone and NaClO4 starts to recrystalize and you
will be left with NaClO4 free of NaClO3 but maybe containing some NaCl.
Then extract the dry solid several times with hot aceton and recrystalize NaClO4 from it... NaCl is much less soluble in aceton than NaClO4 is.
[Edited on 17-5-2016 by PHILOU Zrealone]
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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ecos
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hot XClO4 = maybe decomposition
hot XClO4 + organic substance = Hazards
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PHILOU Zrealone
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First one ... never in solution!
Second one... one would be indeed stupid to do so!
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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ecos
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it seems I have a problem.
the process doesn't work for me.
it seems what i have is chlorate not perchlorate 
I need to leave the cell running longer !
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PHILOU Zrealone
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| Quote: Originally posted by ecos | it seems I have a problem.
the process doesn't work for me.
it seems what i have is chlorate not perchlorate
I need to leave the cell running longer ! |
Or you have to switch to another process than electrochemical for making perchlorates: --> chemical processes!
1°) 30% H2SO4 process --> HClO3 30% is boiled refluxed to 72% HClO4 by disproportionation.
H2SO4 + NaOClO2 --> HOClO2 + NaO-SO2-OH (= NaHSO4)
3 HOClO2 + HOClO2 --> 3 HOClO3 + HCl
But since HCl is formed it destroys in part the HOClO2 formed...
HCl + HOClO2 --> Cl2 + O2 + H2O (beware Cl2 is toxic war gas)
So the process has a yield of approx 50% and can't work with HCl as replacer of H2SO4...
2°) Thermic disproportionation of molten NaClO3 or KClO3
3 NaOClO2 + NaOClO2 --> 3 NaOClO3 + NaCl
The process is viewable on YouTube and requires control of temperature...
Too high and:
NaOClO2 --> NaCl + 3/2 O2(g)
NaOClO3 --> NaCl + 2 O2(g)
Responsible of a reduced yield --> 50-60% because hard to heat and agitate homogeneously molten NaClO3 or KClO3 with solidified NaClO4 or
KClO4...usually the surface of the recipient is hotter than the melt...
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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ecos
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I failed to make perchlorate using MMO anodes !
seems they don't work well !
I have to find lead oxide anode
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Dornier 335A
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MMO anodes are the best for producing chlorate (they are eroded less than platinum anodes!), but it is well known that they are unable to produce any
perchlorate. Platinum or lead dioxide is the way to go.
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ecos
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some users on the forum stated that they could produce perchlorate from MMO anodes.
this was misleading
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hyfalcon
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Nope no perchlorate from MMO, only chlorate. Great for feeding your platinized titanium anode or lead dioxide is SUPPOSED to go from chloride to
chlorate. I still believe I would separate the two processes.
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ecos
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I searched for lead dioxide anodes on the internet but couldn't find any cheap source.
I am busy those days to try to build GSLD setup
any body got one with reasonable cost?
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