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Author: Subject: Production of Perchlorates by Lead Dioxide and Sulfuric Acid?
Polkem
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shocked.gif posted on 22-6-2024 at 20:47
Production of Perchlorates by Lead Dioxide and Sulfuric Acid?


Topic:
I found a PDF talking about the conversion of chlorates to perchlorates using sulfuric acid and lead dioxide without electrolysis. I obviously found this quite intriguing seeing as many face lots of difficulty through the "conventical" methods of electrolysis with the high costs of electrodes. I am wondering whether if the information here is true, and if so why haven't people talked about this before?

Sources:

Figure 1: Figure 1. "Chlorates and Perchlorates Their Manufacture, Properties and Uses, Prepared by Department of Chemistry and Chemical Engineering Southwest Research Institute" page 149

Figure 2: Figure 2. (patent US2853362A)

I was quite interested in what was stated so i did more research and came across (patent US2853362A), which further explains this process. This can be found online easily, it states it works for all chlorate salts. And seems very easy and straightforward, especially for the amateur chemist.

PDFs:
https://file.io/GmeboVPjGUeP
here is the link that contains both the PDFs, the link expires in a years time.

Figure 2.png - 90kB Figure 1.png - 87kB

Edit: I know of heating up chlorates to high temperatures letting them melt and eventually becoming perchlorates, however this process is different and i am wondering is the mechanisms are as well due to the extra chemicals in this process, and lower heating i believe.
[Edited on 23-6-2024 by 6tom]

[Edited on 23-6-2024 by 6tom]
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[*] posted on 22-6-2024 at 22:21


There are chemical procedures that are not known, tried or widespread among amateurs. This will be one of them. It should also be explained that: The advantage of the PbO2 anode is that (if it does not decompose) it can produce NaClO4 from NaCl in one step. The process described here requires starting material NaClO3, powdered PbO2 (poison) and H2SO4. So the critical chemical here is NaClO3. However, if we have NaClO3, it is possible to use the method of melting NaClO3, which produces NaClO4 + NaCl + residue NaClO3. In one melting step at 280 C. The resulting mixture of salts is ground into a fine powder and dissolved in acetone. NaCl + NaClO3 are insoluble in acetone. NaClO4 is highly soluble in acetone. Crystalline NaClO4 is obtained by separation and evaporation. https://www.youtube.com/watch?v=1Ylt2ZKJlME
So, in the light of the other described methods, the PbO2 + H2SO4 method does not look so amazing and the best.....:cool:





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[*] posted on 22-6-2024 at 22:54


Hello Doctor, Thank you for your reply.

I can see where you're coming from however the reason I found this method so intriguing to me is the scalability. I have easy access to both Lead Dioxide and Sulfuric acid, frankly, I am quite afraid of handling large amounts of molten sodium chlorate and perchlorates, whereas in the method discussed, everything is dealt with in liquid conditions within a beaker, without overly hot conditions.
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[*] posted on 23-6-2024 at 01:37


Yes, liquid conditions at 130 C are sure advantage. And H2SO4 + PbO2 is in a huge amount in any car accumulator. Maybe crystallic acidity in final NaClO4 can be problem. It maybe will require next neutralisation step. Any way, interesting method....:cool:



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