Hexabromobenzene
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Sodium hydroxide and metals clorides from salt using polypropylene diaphragm
This is a test diapragm from this topic
https://www.sciencemadness.org/whisper/viewthread.php?tid=16...
About 330 grams of sodium chloride dissolved in 2 liters of water. Solution was poured into a 5 -liter polypropylene container and a diaphragm made
as written in the topic about diaphragms. Cathode solution was diluted to equalize fluid levels
Anode is iron scrap. Cathode stainless steel from the hose from the shower. Voltage 5 volts. Current 1a. At the end of the electrolysis, it fell to
0.8 amperes. Electrolysis time 6 days
Diaphragm was quickly extracted from the electrolyzer to prevent leakage.
Diaphragm was clogged with iron hydroxide, but then washed with acid. This did not have effect on conductivity
Cathode solution was filter and was evaporated to a density of 1.3. About 70 grams of salt fell in the precipitate. 270 ml of alkali solution of about
30% was obtained. About 100 grams of sodium sodium hydroxide total
Anode solution was also filtered and evaporated. In the process of evaporation, hydrolysis and corroding of metal containers occurs. After drying, 230
grams of wet crystals were obtained. Iron chloride 2 is highly polluted by sodium chloride by this results preliminary. Also, iron chloride is
oxidized in the air
Iron chloride 2 has little value, but can be used to prepare iron benzoats and obtaining, for example, acetophenone
Other chlorides can be prompted in the same way. For example, zinc chloride. The method does not require acids and gives a side alkali.
You can also get chlorine
In the process of electrolysis, there were no damage to the diaphragm. This can work for a very long time
[Edited on 6-2-2025 by Hexabromobenzene]
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Hexabromobenzene
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Using a polypropylene diaphragm, about 1 kg of sodium hydroxide, a liter of a zinc chloride with a density of 1.5 and about 1 kg of iron chloride 2,
which is oxidized in the air, was prepared.
A lot of liquid flows through the polypropylene diaphragm. Do electrolysis with the maximum current as much as possible to increase the output and
avoid clogging. Also, do not immerse deep into the solution of the metal anode to reduce the metall dissolution current yield
[Edited on 25-6-2025 by Hexabromobenzene]
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Hexabromobenzene
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Experiments confirm this again
Do not immerse the anode to the full depth. This will lead to the formation of a large amount of sediment. Immerse at minimum possible depth. Use
ammeter. Watch when the current starts to go to the plateau. As the anode destroys and current falls significantly, immerse new parts
These measures will lower current yield of electrochemical destruction of the anode
This is all connected with diffusion ions
Area of the anode should be many times smaller than the area of the cathode
In theory of 1 faraday of the charge (26.801 A·h) decomposes 2 mol sodium chloride(~118gr) in case brine in both anode and cathode chamber
Because when the mol of the charge is flowing, one mol of sodium ions passes into a cathode chamber forming a mole of sodium hydroxide and mol of
chloride ions go into the anode chamber forming another mole of sodium hydroxide in cathode chamber. Sodium and chloride have a charge 1
[Edited on 17-8-2025 by Hexabromobenzene]
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Hexabromobenzene
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Interesting data from
https://beta.iopscience.iop.org/article/10.1149/1.3493888
On the formation of ozone and peracids. I confirm the strong smell of ozone during the electrolysis of sulfuric acid with small-area electrodes
| Quote: |
The potential of the lead anode in the electrolysis of an aqueous Na2 SO4 solution is usually above 2 volts (see below). Therefore, besides the main
process of OH- discharge there may be, according to Le Blanc,13 when the anodic potential is above 1.75 volts, a discharge of SO4 - - ions followed by
the formation of new oxidation products such as persulfates. The presence of any such by-products in the anolyte was determined by us in the following
manner : (a) In the first sample of carefully filtered anolyte we tested qualita- tively for lead and got a negative result b) In the second parallel
sample the content of peroxide com- pounds was determined by the ferric sulfate method. The values found were calculated as persulfuric acid and from
this figure the per cent current loss due to H2S2O8 formation was computed |
On the effects of chloride pollution
| Quote: |
If any chlorine ions are present in the solution, the destruction of lead anodes is markedly increased due to relatively rapid intermediate formation
of PbC12 . The PbC1 2 formation takes place in spite of a higher required potential than the normal oxygen discharge potential, due to a high oxygen
overvoltage together with the depolarizing action in the formation of PbC1 2 . The net chlorine ion discharge potential is less than that for oxygen.
Le Blanc13 reported that in the electrolysis of HC1 no chlorine gas is discharged if the chlorine content of the electrolyte is less than 2.08 g./L.
However, this was based on laboratory experiments, and in com- mercial cells with relatively high anode current densities and effective anode
depolarization the maximum Cl' content will be lower. At a current density of 520 amp./m. 2 and a H2 SO4 concentration in the anolyte of 200 to 300
g./L., the maximum Cl' concentration as deter- mined by us was 0.15 g./L. ; below this concentration no Cl' is dis- charged and there is no serious
corrosion of the anodes such as occurs above this concentration.
The data obtained (Table X) show that : (1) the addition of Sb to
lead in amounts up to 11 per cent does not increase the stability of lead
anodes; at high current densities it even diminishes it; (2) the presence
of Cl' in the electrolyte in amounts higher than of 0.1 g./L. increases
considerably the corrosion loss of the lead anodes ; at high current den-
sities the PbCl2 is not formed fast enough and a certain amount of
chlorine is liberated as gas with the oxygen. Therefore, in the presence
of Cl' the destruction of the lead anodes is greater at low current den-
sities; (3) the best results as to stability and anode corrosion resistance
are obtained with the anodes made of an alloy containing 99 per cent
Pb and 1 per cent Ag 1 |
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clearly_not_atara
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One interesting question in this rxn is what metal should you use for the anode so that you can most easily distill off hydrochloric acid? We know
that some metal chlorides decompose to oxychlorides or hydroxychlorides when dried from aqueous solution. If it is the HCl we are after then we want a
metal that releases HCl to as great an extent as possible at as low of a temperature as possible. For iron (III) chloride we get two-thirds of the
chloride back at 250-300 C, but we are stuck here until around 400 C:
https://link.springer.com/article/10.1007/BF01979262
For zinc chloride we are at 87% at 300 C but water vapor must be present or ZnCl2 will be volatilized (?!):
https://pubs.rsc.org/en/content/articlehtml/2000/pv/c5dt0486...
For aluminum I am not sure.
and for zirconium oxychloride we obtain nearly all of the chlorine at just 200 C in "moist helium" for which I suppose probably another wet atmosphere
could probably be substituted:
https://pubs.acs.org/doi/pdf/10.1021/ic50129a045 (attached)
Zr is a particularly attractive anode for this rxn although the price or difficulty of acquisition may preclude its use.
Attachment: powers1973.pdf (808kB)
This file has been downloaded 81 times
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Hexabromobenzene
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Oops. I was mistaken in the topic by writing the answer above
I believe that metall chlorides themselves valuable. To release hydrochloric acid from them, you will need special equipment. Metals will corrode in
these conditions
On the other hand, a lot of sediment is formed on the walls of the diaphragm, which slowly moves to the anode, the composition of which has not been
studied. Maybe this is oxichlorids?
About of chlorides. Electrolysis on iron anode gives only iron chloride 2 without impurities of iron chloride 3. But it can be oxidized in iron
chloride 3, for example, electrolysis on an inert anode
The precipitate from iron is also formed very hard. Maybe these are oxichlorides?
The hydrate of zinc chloride is quite stable and it can even be completely dried with calcination. Part to decompose into oxichloride
Also falling out components from the alloy. For example micropactricles copper from a zamac alloy or graphite from steel or other components, for
example, from silicon impurities in stell
Large crystals are released from the solution of iron chloride when dried in air. While the solution is noticeably oxidized
A solution of zinc chloride after electrolysis is not crystalized even after several months of evaporation. It can be concentrated even to the density
of 1.6
I have no experience with other chlorides
[Edited on 23-8-2025 by Hexabromobenzene]
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clearly_not_atara
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It would be interesting to see if VCl2 or CrCl2 are produced here. These are reducing agents. Both solutions will be vulnerable to aerobic oxidation.
I think you can dry them by:
- concentrating the solution (or crystallizing the salt hydrate I don't know exactly)
- adding methanol
- drying the methanol selectively somehow (not sure if this is necessary)
- boiling off methanol in inert atmosphere
I know you can make anhydrous FeCl2 like this.
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Hexabromobenzene
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I prepared more than 2 kg of sodium hydroxide in this way. I can’t understand why even when using 2 identical containers, I get an yields only 30%
by sodium chloride. I cannot exceed this magic number even with an excess of electricity. Maybe the anode container should be larger, since at the end
it is noticeable depletion of the liquid in it is likely due to the formation of metal hydroxide
Perhaps using two and three stages ionization salts like sulfate or phosphate will increase efficiency
I use a voltage of 5 volts and I need about 5 kWh to obtain 1 kg of sodium hydroxide. It's still cheaper than alkali in the store
I can’t use 3 volts in this synthesis due to the fact that I need to reduce anode surface to prevent formation of hydroxide. Perhaps I can reduce
the voltage when preparing chlorine, but inert anodes are needed. I can also use ethanol as a substrate for the disposal of chlorine, but I do not
know what to do with large quantities of dangerous chloroacetaldehyde. Chloral is formed only at high temperatures
This method require a volume of about 20 liters to obtain a significant amount of alkali per launch. As an alternative, you can boil sodium carbonate
and calcium hydroxide, but this method also has disadvantages. You need to evaporate a lot of water and sodium carbonate is more expensive than salt
[Edited on 12-9-2025 by Hexabromobenzene]
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Hexabromobenzene
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Quote: Originally posted by Hexabromobenzene  | Experiments confirm this again
Do not immerse the anode to the full depth. This will lead to the formation of a large amount of sediment. Immerse at minimum possible depth. Use
ammeter. Watch when the current starts to go to the plateau. As the anode destroys and current falls significantly, immerse new parts
These measures will lower current yield of electrochemical destruction of the anode
This is all connected with diffusion ions
Area of the anode should be many times smaller than the area of the cathode
In theory of 1 faraday of the charge (26.801 A·h) decomposes 2 mol sodium chloride(~118gr) in case brine in both anode and cathode chamber
Because when the mol of the charge is flowing, one mol of sodium ions passes into a cathode chamber forming a mole of sodium hydroxide and mol of
chloride ions go into the anode chamber forming another mole of sodium hydroxide in cathode chamber. Sodium and chloride have a charge 1
[Edited on 17-8-2025 by Hexabromobenzene] |
Most likely my conclusions are incorrect. 1 Farad will transfer 0.5 mole of ions from each compartment forming 1 mol of alkali and metal chloride
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Hexabromobenzene
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I've accumulated a lot of iron chloride 2 from electrolysis. Zinc chloride can be used in organic synthesis. Iron chloride 2 is useless. However, I
found that iron chloride 3, when heated to 190°C, yields two-thirds hydrochloric acid and iron oxychloride, which can also be converted to chloride.
[Edited on 4-10-2025 by Hexabromobenzene]
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RU_KLO
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You could use ferric chloride for PCB etching....
Go SAFE, because stupidity and bad Luck exist.
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Hexabromobenzene
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I don't etch circuit boards. I have lots of iron chloride, but I'm always short of acids.
I just tried electrolysis with potassium chloride under similar conditions. The same concentration as sodium chloride and a slow iron anode immersion.
The conductivity doubled.
And this isn't a saturated potassium chloride solution. But I don't want to use strong solutions because of the risk of crystallization.
With an iron anode, the current immediately drops significantly upon slow immersion, unlike with a zinc anode, and I don't know why.
I was also able to evaporate zinc chloride after electrolysis to a density of 1.56 without the chloride crystallizing.
[Edited on 13-10-2025 by Hexabromobenzene]
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bnull
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Mood: preparing copper salts and enjoying it
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You could sell iron(ii) chloride. It is useless for you, so you can sell it relatively cheap.
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Hexabromobenzene
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Sodium chloride electrolysis lasted 7 days(200-300 amp hours), but the yield was still 200-250 grams of sodium hydroxide per 900 grams of salt. I
think 30% is the limit of this process.
However, the alkali yield is much higher than with sodium sulfate electrolysis using a lead anode. This can be explained by the fact that there are no
hydrogen ions in the anode chamber, only iron ions. And iron ions cannot enter the cathode chamber. This is why the resistance of the electrolyzer
increases towards the end. In other words, the neutral layer in the diaphragm acts as an ion-exchange resin.
This also perfectly explains the fact why almost no salt is found in the anode chamber after evaporation.
Also zinc partially penetrates the cathode chamber, likely as zincate. Unlike iron, which is not detected there.
The deposit on the diaphragm walls is magnetite, not iron hydroxide II. Apparently, iron hydroxide II quickly decomposes under these conditions and
forms a dense mass. Other metals form larger deposits and reduce the space available in the anode chamber.
I'm currently experimenting with potassium chloride and potassium sulfate. We'll see what yields they produce.
| Quote: |
You could sell iron(ii) chloride. It is useless for you, so you can sell it relatively cheap. |
It's too expensive for me. I produce chemicals for myself. I don't have any plans to ship it yet.
[Edited on 20-10-2025 by Hexabromobenzene]
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Hexabromobenzene
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Potassium chloride experiment is complete. From 850 grams, 470 ml of hydroxide solution with a density of 1.4 was obtained. Some liquid remained in
the precipitated salt. Given that the molecular weight of potassium hydroxide is higher, the current efficiency is approximately the same NaCl runs.
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