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Author: Subject: LL8 from Dr. Liptakov
MineMan
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[*] posted on 22-4-2022 at 19:07


Yah many interests. You kind of high jacked this thread I would recommend posting about the binders else where. I don’t except out of all of the ones available there must be one that is doable.
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[*] posted on 4-5-2022 at 23:56


I have an alternative way of making copper perchlorate and it hinges on the fact that both copper chloride and sodium perchlorate are both highly soluble in ethanol but sodium chloride is not.
I will soon make a video on this.
Btw on preparing copper perchlorate with membranes you must use KClO4 and heat the cell below 80C and above 50C because it would otherwise be very difficult to seperate copper perchlorate from sodium perchlorate
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Laboratory of Liptakov
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[*] posted on 5-5-2022 at 07:24


Great message, thanks...:cool:...I have both compound for attempt.
I am curious.


[Edited on 5-5-2022 by Laboratory of Liptakov]




Safety explosive Alfred Nobel 1867. Safety ecologic detonator Dr. Liptakov 2015, inventor CHP and Lithex
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[*] posted on 5-5-2022 at 08:50


Quote: Originally posted by Laboratory of Liptakov  
Great message, thanks...:cool:...I have both compound for attempt.
I am curious.


[Edited on 5-5-2022 by Laboratory of Liptakov]


sadly as for trying to mix CuCl2 and NaClO4 in ethanol and it forms a complex which is deep green in color and doesnt crash NaCl out probably Na2Cu(ClO4)4 and I used anhydrous ethanol and 99% pure NaClO4 from solvent extraction.


I have also prepared before calcium perchlorate from ethanol, calcium chloride and sodium perchlorate. This can then be reacted with copper sulfate to form calcium sulfate and copper perchlorate.

I wonder if LL8 can work with somewhat purified Cu(ClO4)2 with slight contamination of NaClO4.

If we are talking about slightly contaminated Cu(ClO4)2 then the most incosequential one would be starting with NH4ClO4 in the membrane electrolysis stage as the electrolyte.
the membrane electrolysis with heated KClO4 is probably the only thing left to try.

[Edited on 5-5-2022 by mysteriusbhoice]
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Laboratory of Liptakov
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[*] posted on 5-5-2022 at 10:11


Yes, for example 5% NaClO4 in Cu(ClO4)2 will works sure. (+ hexamine) Neutral Cu(ClO4)2 is problem. Always were problems with acidity in him. (from HClO4 prepared) Preparation neutral Cu(ClO4)2 from NaClO4 + somethig, require exact verifycated method. Not found yet. Exact weights, temperatures, times etc.



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[*] posted on 6-5-2022 at 16:26


LL, any update on increased density? I can give you a mix with large density that will DDT, you already played around with it. It’s very similar to dragons tail. Basically if you do dragons tail and the ratios I suggested a few years ago and add two catalyst it DDTs :) at the density of a paste
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[*] posted on 7-5-2022 at 01:31


Quote: Originally posted by Laboratory of Liptakov  
Yes, for example 5% NaClO4 in Cu(ClO4)2 will works sure. (+ hexamine) Neutral Cu(ClO4)2 is problem. Always were problems with acidity in him. (from HClO4 prepared) Preparation neutral Cu(ClO4)2 from NaClO4 + somethig, require exact verifycated method. Not found yet. Exact weights, temperatures, times etc.


I have done a lot of membrane electrolysis runs to produce Cu(ClO4)2 from NaClO4 and copper sacrificial anode.
it is then left to evaporate and ethanol is added just enuf which doesnt dissolved all of the NaClO4 and isolates somewhat pure Cu(ClO4)2 but to get the weight you have to dry it again..... carefully and find it out with scale.


IMG_20200716_224238.jpg - 2.7MB

the seperation power totally depends on your membrane and setup an in that pic was the old PVC + Sand but I have made better castable membranes for easy setup like the ionomer concrete.
mix of sand + OPC cement + CaSO4 9:3:1 ratio.
The CaSO4 can be substituted for cation exchange resin from the water filtration section of any hardware store.
be sure to grind the cation exchange resin in a blender first.
Anion exchange resin is only for anion permeation IE making H2SO4 and other processes.

Overall the thing which happens here is.
Cu + e = Cu2+ (anode)
NaClO4 + Cu2+ = Cu(ClO4)2 + Na+ (anode side)
Na+ + H2O = NaOH + H+ (cathode side)
H+ +e = H2 (cathode)

overall
NaClO4 + Cu + H2O = NaOH + Cu(ClO4)2 + H2



[Edited on 8-5-2022 by mysteriusbhoice]
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[*] posted on 7-5-2022 at 10:30


That container looks a little mad. But if it works, it's ingenious equipment. Copper sheets, NaClO4, porous ceramic membrane. After all, we are on a science madness. Interesting thanks.

[Edited on 7-5-2022 by Laboratory of Liptakov]




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[*] posted on 8-5-2022 at 03:04


I have seperated out the copper perchlorate from NaClO4 somewhat from this mix as it does form that green complex but it seems to settle out.

IMG_20220508_112402.jpg - 3.4MB

IMG_20220508_145435.jpg - 2.7MB

IMG_20220508_145622.jpg - 3.2MB
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[*] posted on 9-5-2022 at 04:26


NaClO4 is annoying because its hard to seperate Cu(ClO4)2 from NaClO4 using any solvent.
going ahead and using KClO4 membrane heated to 60C and it seems to be working fine.
hopefully I can create a seperable copper chlorate with less contamination with this.

Using NH4ClO4 is really ideal as NH4ClO4 contamination wont be a big issue.
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[*] posted on 9-5-2022 at 07:54


Interesting. Relatively pure neutral Cu(ClO4)2 is not some easy.



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[*] posted on 9-5-2022 at 12:36


Quote: Originally posted by Laboratory of Liptakov  
Interesting. Relatively pure neutral Cu(ClO4)2 is not some easy.



if you think that is annoying I also get orange copper 1 perchlorate!! :*((( if I let it run for too long.
This weird bright orange precipitate eventually appears coating the anode and settles out and its odd because its energetic!! when mixed with fuel after washing then dry.
edit: after looking at other images of copper 1 oxide, it may perhaps just be that mixed with some perchlorate residue but IDK honestly will have to isolate some of it in the future.
The same happens when making copper chloride where white copper 1 chloride is also made somewhere further along the electrolysis.
This bright orange precipitate looks different from copper 1 oxide which is a more dark brown.

I will keep messing about with membranes to try to get the KClO4 Cu(ClO4)2 mix which I believe I had success with this one since KClO4 settles out in the freezer and is not soluble as much in ethanol or water if its cold.

Problem is I killed my membrane because I decided to run some PbO2 to oxidize copper 1 perchlorates and oxides and yea I let that run too long and perchloric acid fucked up my polymer membrane since the substrate is polyurea cleaning cloth and not fiberglass which explains the ammonia smell in the cathode chamber XD.

I am making an ionomer concrete membrane which hopefully will be better.

[Edited on 9-5-2022 by mysteriusbhoice]
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[*] posted on 21-6-2022 at 12:20


OK... while this is not the CHP thread. I am making good on my promise to start making the stuff for a few CHP synthesis. I spent a month (or almost a month) to make 500 grams of sodium chlorate (of varying purity) and am now trying to turn that chlorate into perchlorate via heat composition. Just as LL did in his video.

In the crucible pictured. I added 60 grams of slighly impure sodium chlorate and it has been on my stovetop at the highest heat for almost 3 hours. The color of the chlorate has become considerably darker, but has not begun to melt or turn into a slurry. I did not wrap anything in aluminium foil. Am I losing too much heat or what?


EDIT: I took a measurement with a candy thermometer (which broke when I tried to cool it down too fast... goodbye mr. candy thermometer!)

It was well above 200 degrees celsius, which is as far as the thermometer will allow (and it continued to go farther). So I know I am getting good heat from there. But maybe not as hot as needed?

ceramic.jpg - 1.6MB

[Edited on 21-6-2022 by ManyInterests]
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[*] posted on 21-6-2022 at 13:40


So I put it back on the heat with it being wrapped like this. I hope it will be hot enough to turn the chlorate into perchlorate.

Ceramic2.jpg - 2.4MB
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[*] posted on 22-6-2022 at 10:06


Good luck. But the cup on hot wires looks a like really science madness....:D



[Edited on 22-6-2022 by Laboratory of Liptakov]




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[*] posted on 22-6-2022 at 17:29


OK, so I have tried to make it hotter by putting another larger pot on top of it. The stuff didnt melt, but it did get RED HOT in the crucible. Would I have some perchlorate there?

Edit: no. I only ended up with 0.2 grams! I need a stronger heat source.

[Edited on 23-6-2022 by ManyInterests]
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[*] posted on 27-6-2022 at 14:29


I think I am going to have to ask for a bit of advice in making perchlorates. No matter my efforts I cannot make it work through thermal decomposition.

Edit: Just after a private message talk with LL. I realize that I should have recrystalized and tried to purify my sodium chlorate before commencing with the heating. While I did order electrodes, I had to order another crucible since my previous one broke. What I will do in the meantime is make more chlorates and purify my entire supply via methanol crystalization and hopefully try again via the propane torch method.

I will need to make sure everything is pure because even using platinum electrodes requires very pure sodium chlorate to work. So it is a must anyway.

Everything should be ready for the next batch of tests in three weeks or so.

[Edited on 28-6-2022 by ManyInterests]
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[*] posted on 30-6-2022 at 10:22


Quote: Originally posted by ManyInterests  


I will need to make sure everything is pure because even using platinum electrodes requires very pure sodium chlorate to work. So it is a must anyway.

Everything should be ready for the next batch of tests in three weeks or so.

[Edited on 28-6-2022 by ManyInterests]


No you do not strictly need superbly purified chlorate to convert it into perchlorate on platinum anode. In fact I have never engaged in any sort of purification activities prior to perchlorate conversion....and even worse I routinely go with Pt straight from chloride to perchlorate in the same cell. Takes a while, but truly the lack of need to babysit and interfere with the process really makes it worth even if the anode lifespan is compromised. I put chloride into the cell.....fire it on and forget for a month...unless the anode dies before full perchlorate conversion I only have to add deionised water to top up once in a while. Or saturated chloride solution if I would like to receive "really thick stuff" in the end.
With electrochemical perchlorate production the key element is to be able to have knowledge and possibility to find or make replacement anodes. Because anything less than a solid brick of Pt is going to be an expendable asset. It will wear out, passivate and disintegrate in a few conversion runs at best. All the monstrously work and time consuming efforts of starting with "purified and chloride free" feedstock are not really going to make a noticeable difference in the end. It may make sense to some degree on an industrial scale, but on tabletop reactor realm it is wasted effort.

The "really thick stuff d=1,6g/cm3" not willing to mix with added water on top of it:
https://www.youtube.com/shorts/d7erWvS6JK0

The "expendable Pt anode" resuming work on the perchlorate conversion after being replaced:
https://www.youtube.com/shorts/37r58o5kB_Y


[Edited on 30-6-2022 by markx]




Exact science is a figment of imagination.......
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