Alright, not much to say this evening. (Damn, that sounded like applause. . . nah.)

I tried adding a little water to my MnSO4, but Doh! It's soluble in water. That's alright. Boiling doesn't seem to hurt the stuff, so I'll just boil it down, then vacuum filter it through some diatomacious earth.

PP

Great, best of luck!

I've decided to go the MAA route, however with the addition of ammonium sulfate the alum didn't precipitate, I've added so much manganese sulfate that not all of it dissolves in the cell. I was under the impression that the MAA would precipitate, maybe it doesn't need to though. Do you think I just need to add more ammonium sulfate, and then that could possibly get the MAA to precipitate via the common ion effect, or something like that?

Either way, I haven't been able to work on it much since I'm taking some classes that are fairly intense for me, and my wonderful power supply seems to have crapped out. I have another one just like it, and a car-battery charger however.. I'd still like to fix the power supply so its not a waste.

Prepuce, a car battery charger will serve as a great starting point for the power supply.  Some minor changes to it, and you can have a power supply with adjustable current.

Solubility of benz. in H2O is 0.33g / 100 ml.

Sedit, I know you've been doing this reaction with a lot of current, I just don't see how that much power is nearly vaporizing your liquids. I'm not saying that I don't believe you--not at all. It just seems to be working differently for me and I'd like to understand why.

I've seen the thread on SM, and read most of it. I'll probably have to read it another dozen times to pick up all the relevant information. The pictures were very good.

Doucherman, I have an adjustable power supply. I was just mentioning it in case there were others who wanted to try the method. Even if high currents are required, it would be good to have one that could be adjusted and used for other things. I appreciate the suggestion, though.

Here's an update on what I've been doing. I'm kind of torn between the electrolysis method and the KMnO4. Now that I've been through both I'd say they take about the same amount of work. The permanganate procedure takes a shitload of H2SO4 compared to the yields, but I haven't been through the math on the electro. procedure to compare. I'm not sure if the acid from the permanganate can be reused, either.

I made another run at making Mn(SO4)2 by conversion of MnSO4 with KMnO4. I worked out the ratios of the ingredients from the patent, which were given as:

   169   Manganous sulfate      (MnSO4.H2O)
   4780   H2SO4 - 70%      
   108   Potassium permanganate      

(I assumed that these were ratios by weight, but that the 70% H2SO4 was made with 70% H2SO4 and 30% H2O by volume.)

I scaled back the above ratios to give me more workable quantities. Since it was the least amount, I based it on the KMnO4.

   1.56g      MnSO4.H2O      
   44.26g   H2SO4 - 70%      
   1.00g      Potassium permanganate      

Before starting the MnSO4 needs to be converted to MnSO4.H2O. This is done, according to the patent, by drying at 150C. I did this by placing the material in a beaker and stirring with a thermometer until the temperature reached 150C. At that time the powder was nearly white in color.

The MnSo4.H2O is combined with the H2SO4 at a temperature between 40-50C, with "good" stirring. I used a mag stirrer, which had a little trouble because the MnSO4 is not soluble and was gritty at the bottom of the beaker, but it wasn't bad enough to preclude using it.

I did not forget that the KMnO4 had to be added a little at a time, since rushing it may lead to an explosion.

Altogether it took probably 2 hours to complete the process because I was being very careful. The patent says that after adding KMnO4 the mixture will turn red, then brown. Mine at first turned purple from the permanganate and I'm sure that was expected. Then it turned sort of reddish brown, then brown. It was never the red you see when this procedure is done electolytically. This may be because I added the permanganate so slowly. The mixture did end up a deep, dark brown.

In other news, I had a flask of toluene with a bit of whatever it was I made in a previous electro. attempt sitting on the table waiting for me to get around to washing it. I'd been checking it every now and then to see if there was any odor of benzaldehyde, and a couple of times I was able to detect the smell over the odor of the toluene. It doesn't take much benz. to be able to smell it, though. Tonight I opened it again and was surprised to find that there was no longer an odor of toluene at all. It has evidently all converted just sitting there. It wasn't much, but hey, success is success.

PP

I just don't see how that much power is nearly vaporizing your liquids. I'm not saying that I don't believe you--not at all. It just seems to be working differently for me and I'd like to understand why.

My cell was measured at running 120 degrees F IIRC. I have it writted in another threed someware around here. Just a few spec's you can compair againsts yours I am running mine with the powersupply already noted with about 2x2 Pb electrod in solution on either end. The divider is made from a porous flower pot that is about 4in across at the top I believe(ill get better data later since I want to know how much it holds my self).  The electrods are spaced I would have to say atlest 8 inchs to prevent the powersupply from shutting down on safety. I would keep a Plexy glass sheet over all of it to prevent the acid mist from getting out and fouling everything up. I already lost one powersupply to that already.

I will attempt to get better measurements later of the cell. I have plans on making it more stable as well because the outer container was quickly makeshift to allow me more room to prevent the current overflow problem I was having by spacing the electrods.

Heres something that discusses the oxidation of toluene in acetic acid to yeild three products using a graphite cathode. The products are BnO, BnOH and BnOAc. Sadly it is lacking much details so I am going to try to track down the references sited and see if I can get a better idea on there process.

The Mn(SO4)2 produced via KMnO4 would not oxidize toluene as advertised. I let it run for several days just to be sure, and there wasn't even a trace of the odor.

Based on that, I did the electro. oxidation once more. Followed directions exactly, and everything looked and acted as it should. The only problem was that this, too, would not oxidize toluene. Not at all.

I think that the ratios are more important than they might seem. I looked them up but don't have them on hand. I'll post them later, probably tomorrow.

I also believe that getting MnO2 from batteries is no good. There are too many other things mixed in, and we have way to find out what. In another run I mixed MnO2 right from a battery with 50% H2SO4, then added H2O2 a little at a time. This produced a noticeable amount of Cl, even though I didn't put it in the mix. My objective was to follow a procedure for cleaning Mn02 I found on SM. I decided not to go any further once it started making chlorine.

In other news I noticed that WalMart carries concentrated H2SO4 as a drain cleaner. Never saw it there before, but read the label and saw that it contained "virgin" sulfuric acid and IIRC 5 buffers. I'd like to know what buffers are supposed to accomplish iin strong acid used as a drain cleaner. I suspect it's to make it unusable for our purposes.

PP

You are stirring it a bunch as well, right?
The more the better IMO

"Cleans up clear as glass with a bit of H2O2 and a few days though.. Heat and boil down till Fumes and you got some very nice looking acid."

That's a new one on me. How much H2O2 do you use, and for how long? Any details would be appreciated.

It's just used to oxidise the dyes and buffers out.  This is one of those cases where chemists use units of measurements such as "splash" or a "bit" etc.  Just add a splash of H2O2 to a good sized quantity of H2SO4 and let it sit for a couple days.  If the color clears up, then just boil it down until the sulfuric acid starts to give off white fumes from heating.  If it doesn't clear up, add more and repeat.

Sedit, that picture does look good. I'm going to use it on the stuff I have now and see if it will clean up as nicely.

And thanks, Douchermann. Adding a splash here and a healthy shot there is the kind of chemistry I do best. It's good to remember, though, that the splash goes in the beaker and the shot goes in me. Not the other way around.

PP