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Author: Subject: High-energy composite (HEC) propellants
ecos
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[*] posted on 15-5-2016 at 03:09


Thx PHILOU Zrealone for the answer.

this mean adding extra HCL won't harm ; this will make sure no chlorate exists.


Quote:

Then afterwards add some AgClO4 to precipitate Cl(-) as AgCl.


I think this optional step. right?
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[*] posted on 15-5-2016 at 07:11


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.


Quote:

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. :D rust in pièces :P)




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[*] posted on 17-5-2016 at 01:22


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.


you scare me when you write BOIL !! :) :)
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[*] posted on 17-5-2016 at 07:04


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.


you scare me when you write BOIL !! :) :)

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.




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[*] posted on 17-5-2016 at 07:10


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]




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[*] posted on 19-5-2016 at 01:53


hot XClO4 = maybe decomposition
hot XClO4 + organic substance = Hazards :)
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[*] posted on 19-5-2016 at 11:23


Quote: Originally posted by ecos  
hot XClO4 = maybe decomposition
hot XClO4 + organic substance = Hazards :)

First one ... never in solution!
Second one... one would be indeed stupid to do so!




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[*] posted on 28-5-2016 at 04:57


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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[*] posted on 28-5-2016 at 11:10


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...




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[*] posted on 27-6-2016 at 03:26


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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[*] posted on 27-6-2016 at 03:42


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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[*] posted on 28-6-2016 at 00:57


some users on the forum stated that they could produce perchlorate from MMO anodes.
this was misleading
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[*] posted on 28-6-2016 at 07:02


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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[*] posted on 1-7-2016 at 04:58


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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