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Author: Subject: High Temperature Safe Potassium-Chlorate based Rocket Candy
PHILOU Zrealone
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[*] posted on 11-5-2016 at 05:25


Quote: Originally posted by mysteriusbhoice  
Quote: Originally posted by Chemist_Cup_Noodles  
Wait, why are you using HMTD? At that point you might as well use ATP, it's technically more stable. But to detonate it, seems like you could just use your laser since it's so unstable.

On another note, do you buy or make your KClO3? Have you ever considered throwing it in a perchlorate cell? You can make a GSLD for this somewhat easy. Maybe even make some perchloric acid, and then ammonium perchlorate.

I have never seen sodium citrate used in any SRB's. This is good stuff. But recently I've started using a little bit of sodium metabisulfite in my mixtures of KNO3 and sugar for a little extra kick. I tried it out the other day and it certainly produced quite the burn rate. With a little additional sulfur powder in it too, every time I tried lighting the wet mixture it would ignite a little but it would produce so much gas the torch would get blown out instantly. After burning quite a sizeable amount of this mixture, I noticed extremely little solid remnants, maybe even less than with plain KNO3 sugar mix. I'm off of work today so I'm going to experiment some more.


i make my KClO3 using MMO anodes i bought
and sodium citrate is amazing shiz it accelerates the burn rate

i made a rocket without it and it performed poorly compared to the one with it

now the question is why is it better !!
perhaps its like using sodium benzoate but more acessible

also adding a little starch allows chlorate mixtures to be heated strongly until it carbonizes but if the temp is above 200 celsius it will explode like any mixture heated that strongly

also sodium acetate works but that fuel is DANGEROUS its highly explosive and unstable and any cooking will cause it to detonate it works too well and gives INSANE BURN RATE!!

Any alkaline metal salt of an organic acid will do the job of whistle mix with a chlorate.
But with benzoate, the dead weight of sodium is less and there is more C fuel.
In the case of citric acid, depending on the number of Na atoms, you get more or less dead weight vs fuel; but also more H atoms.
In the case of acetates you get very big dead weight and more volatile combustion products (more H atoms).




PH Z (PHILOU Zrealone)

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PHILOU Zrealone
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[*] posted on 11-5-2016 at 05:29


Quote: Originally posted by Eosin Y  
This is just why I haven't started with energetics yet! 1 out of 100 times, my huge (Sod's Law) batch of potassium acetate-copper perchlorate rocket mix doesn't burn, and I instead end up with no hands and a hole in my ceiling.

If you can get an EPP license, you can get free-flowing Na and K ClO4 from a number of suppliers. I think that, stochiometrically, you would need 65 grams of NaClO4 and 53 grams of 90% One Shot H2SO4 drain cleaner (an excess of 4 grams of NaClO4) to synthesise, in theory, 50 grams of HClO4, which can then be just blunt-force distilled with a Bunsen burner to yield very pure HClO4. Be very careful when you distill, as I think that careless distillation results in Cl2O7, which is not good. I'd recommend these mixes in theory:

CuClO4 - sodium benzoate
NH4ClO4 - sodium benzoate
CoClO4 - sodium acetate

These are just the first things that come to mind. If I can get some distillation apparatus, I might experiment with some of them.

Strange, you registred a little after "a nitrogen rich explosive" has been banned....and you write a bit like him...

Recheck your formulas --> stoechiometry and valences.
Cobalt salt for whistle mix...that would be expensive...

If you use perchlorate, nothing is against use of ammonium salts --> benzoate and acetate for better gas output!

[Edited on 11-5-2016 by PHILOU Zrealone]




PH Z (PHILOU Zrealone)

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Eosin Y
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[*] posted on 11-5-2016 at 05:48


Who's 'a nitrogen rich explosive?' I checked the end of the member list with status to see who he was, but he isn't there? Cobalt salt would be expensive, but interesting.
H2SO4-98g/mol
NaClO4-122g/mol
HClO4-100g/mol
Therefore, given H2SO4+NaClO4=H2+NaSO4+HClO4:
I can use 0.5mol of each reagent with an XS of 0.05mol NaClO4 to get the following:
49g H2SO4 and 67.1 grams NaClO4 to yield exactly 50 grams HClO4.

For the best of both, why not NH4ClO4-Na2C6H6O7 to give both high burn rate and stability?

[Edited on 11-5-2016 by Eosin Y]
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[*] posted on 11-5-2016 at 09:00


Quote: Originally posted by Eosin Y  
The other problem is that I don't have a hot plate. I'm setting up a home lab at the moment, and a hot plate is something I can't afford. My method involves high temperature HClO4, but there is no need for separation of H2SO4 and HClO4 as the excess of NaClO4 will see to that. Anyway, I can distill it off and destroy any Cl2O7 with distilled water, before it destroys my glassware.

[Edited on 11-5-2016 by Eosin Y]


Are you saying you plan on distilling HClO4? Keep in mind that HClO4 is kinda like H2SO4, having a high boiling point. But the difference is, HClO4 is a strong oxidiser which when anhydrous can explode if heated. Distillation of HClO4 is usually done under vacuum, do you have a pump?

What I worry might happen: Concentration starts at maybe 50%. Mostly water comes over. Mixture reaches 70%, still mostly water coming over. Mixture goes past 70% while at 200˚C...BOOM!
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[*] posted on 11-5-2016 at 09:16


What exactly is the boiling point of perchloric acid? I was thinking of doing the H2SO4-NaClO4 and then adding lots of water before nuking it at above perchloric acid's boiling point to distill over HClO4-water.
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hissingnoise
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[*] posted on 11-5-2016 at 10:35


Somehow, I don't think perchloric acid is quite ready for you . . .

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[*] posted on 11-5-2016 at 10:54


It's more of a long term project. First thing is to distill some standard acids (drain cleaner H2SO4, nitric acid from KNO3+H2SO4,) then set up a proper lab with decent chemical supplies. Then I will start to move on to perchloric acid and other things.
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[*] posted on 11-5-2016 at 12:06


Quote: Originally posted by Eosin Y  
Who's 'a nitrogen rich explosive?' I checked the end of the member list with status to see who he was, but he isn't there? Cobalt salt would be expensive, but interesting.
H2SO4-98g/mol
NaClO4-122g/mol
HClO4-100g/mol
Therefore, given H2SO4+NaClO4=H2+NaSO4+HClO4:
I can use 0.5mol of each reagent with an XS of 0.05mol NaClO4 to get the following:
49g H2SO4 and 67.1 grams NaClO4 to yield exactly 50 grams HClO4.

For the best of both, why not NH4ClO4-Na2C6H6O7 to give both high burn rate and stability?
...
CuClO4 - sodium benzoate
CoClO4 - sodium acetate

You really write like him...and make the same kind of mistakes...

Cu is bivalent in oxydising media so Cu(II) perchlorate --> Cu(ClO4)2
Co is bivalent or trivalent so Co(II) perchlorate or Co(III) perchlorate are Co(ClO4)2 and Co(ClO4)3

90% H2SO4 and dry NaClO4 will provide you upon boiling 72% HClO4 but the rest in the overheated flask will go as high as 100% HClO4 because Na2SO4 will catch a lot of water as a crystaline salt --> BOOOM

NH4ClO4 is a good idea maybe try with NH4 acetate, NH4 benzoate or NH4 citrate.




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[*] posted on 11-5-2016 at 13:01


Oh right. KClO4 then because it is less hydrophilic. Also, if I used 98% H2SO4 wouldn't I just need to filter it to get perchloric acid (provided I use an XS of KClO4.)
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PHILOU Zrealone
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[*] posted on 13-5-2016 at 06:21


Quote: Originally posted by Eosin Y  
Oh right. KClO4 then because it is less hydrophilic. Also, if I used 98% H2SO4 wouldn't I just need to filter it to get perchloric acid (provided I use an XS of KClO4.)

KClO4 will behave just like NaClO4...the problem is the heating to distillate HClO4...and overheating risk of concentrated HClO4.

98% might do the trick, but don't filter on paper and keep cool --> glass fiber filter paper or fritted glass.
HClO4 72% or over turns paper into a gellous transparent lumps of an explosive stuff.




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[*] posted on 14-5-2016 at 04:00


new proper video on how i make this into a rocket
and a new propellant mixture that has an even higher heat stability!!
https://www.youtube.com/watch?v=BGbFqWckr2U
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[*] posted on 9-4-2017 at 13:37



Has anyone been using this stuff?

There is a patent giving details for a gas producer composition that contains chlorate + starch.




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[*] posted on 10-4-2017 at 03:53


Quote: Originally posted by PHILOU Zrealone  
Quote: Originally posted by Eosin Y  
Oh right. KClO4 then because it is less hydrophilic. Also, if I used 98% H2SO4 wouldn't I just need to filter it to get perchloric acid (provided I use an XS of KClO4.)

KClO4 will behave just like NaClO4...the problem is the heating to distillate HClO4...and overheating risk of concentrated HClO4.

98% might do the trick, but don't filter on paper and keep cool --> glass fiber filter paper or fritted glass.
HClO4 72% or over turns paper into a gellous transparent lumps of an explosive stuff.


I was always told anything over 70% is an explosive hazard in and of itself.
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[*] posted on 10-4-2017 at 05:22


Just a quick question: could barium chloride be used in a chlorate/perchlorate cell? Or the chlorate of barium could be made by the same process as calcium chlorate is made, then the barium chlorate could be decomposed to the perchlorate. An easy-seeming method to relatively pure perchloric acid is the treatment of the barium salt with sulfuric acid to precipitate barium sulfate.

Also, perchloric acid is often distilled under vacuum to avoid the risks of higher temperatures. A reaction that precipitates an insoluble salt is vastly preferred to a distillation.

Edit: The route to calcium chlorate is by bubbling chlorine gas through hot calcium hydroxide, per NileRed's video, the reaction works by generating hypochlorite and then it disproportionates upon heating, giving a mixture of chloride and chlorate. This should be adaptable to Ba(OH)2


[Edited on 11-4-2017 by Elemental Phosphorus]

[Edited on 11-4-2017 by Elemental Phosphorus]
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[*] posted on 10-4-2017 at 05:47




Perchloric acid can be prepared from Barium Perchlorate and Sulphuric acid. Sulphuric acid is slowly added to a solution of Barium Perchlorate until no more Barium Sulphate (insoluble) precipitates. The acid can be concentrated to 70% approx. by boiling until dense white fumes appear.


http://www.sciencemadness.org/talk/viewthread.php?tid=12


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PHILOU Zrealone
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[*] posted on 14-4-2017 at 05:29


Quote: Originally posted by Elemental Phosphorus  
Just a quick question: could barium chloride be used in a chlorate/perchlorate cell? Or the chlorate of barium could be made by the same process as calcium chlorate is made, then the barium chlorate could be decomposed to the perchlorate. An easy-seeming method to relatively pure perchloric acid is the treatment of the barium salt with sulfuric acid to precipitate barium sulfate.

Also, perchloric acid is often distilled under vacuum to avoid the risks of higher temperatures. A reaction that precipitates an insoluble salt is vastly preferred to a distillation.

Edit: The route to calcium chlorate is by bubbling chlorine gas through hot calcium hydroxide, per NileRed's video, the reaction works by generating hypochlorite and then it disproportionates upon heating, giving a mixture of chloride and chlorate. This should be adaptable to Ba(OH)2


[Edited on 11-4-2017 by Elemental Phosphorus]

[Edited on 11-4-2017 by Elemental Phosphorus]

Yes should work but no real benefit over CaO/Ca(OH)2 because BaO, BaCl2, Ba(OH)2 are very toxic...much more expensive and CaSO4 allows for an almost as good precipitation as BaSO4.

Also avoid any risk when setting the HClO4 free from Ba(ClO4)2 or Ca(ClO4)2 from H2SO4 and never do it on dry salt with more than 70% H2SO4 because over 72% HClO4 becomes an hazardous compound...so expect an explosion (because of transcient Cl2O7) from H2SO4 (95% concentrate) and dry salt (btw dry salt hard to get owing to strong hygroscopicity)....

[Edited on 15-4-2017 by PHILOU Zrealone]




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[*] posted on 18-4-2017 at 11:34


I am aware of the explosion risks of higher concentration perchloric acid. You are right that calcium sulfate should give almost as good of a precipitate as barium sulfate, however when dealing with an explosion risk and an unstable compound, there are 3 possibilities for what a dissolved salt could do.

1: In some cases, a metal salt will catalyze decomposition of a unstable compound (like hydrogen peroxide). This is unlikely because HClO4 is more stable than HClO3, HClO2, or HClO.

2: It may have no effect. This is most likely, as the amount of dissolved calcium sulfate would be low anyway.

3:It may sensitize the compound. If this were the case, barium sulfate would be much safer as its solubility is essentially zero. (0.0002448 g/100 mL at 20C)

I think a calcium salt is fine actually. I did not remember the calcium sulfate salt solubility (or never knew it exactly), but I knew barium sulfate is basically completely insoluble.

Also, even 70% sulfuric acid may be too much, as H2SO4 is more hygroscopic than HClO4 (I think). If 70% sulfuric acid were used, care would have to be taken, and acid slowly added to salt, not the other way around.
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