I figured a thread like this is a good idea. Sedit has one as well, and you guys are more then welcome to create your own.
I've decided to create one since I've been getting back into the lab lately and this might encourage me to do more things.
Recently I attempted making some crude phenol. It was a total failure and I think I ended up with only Salicylic acid and some black carbon like material.
I mixed ~20 grams of NaOH with 18 grams of ASA. The ASA was purified from aspirin w/ denatured alcohol. I ground the two together, mixed them in a flask and heated with a torch. Water came off as the mixture was molten. I continued to heat it and it became solid, white fumes started to come off (which, the phenol should have been in the form of sodium phenolate, so I don't think this should have happened!) and it started to char and turn black in some areas. I decided that it was probably done, and so I dissolved some in water, added an acid and found a very fluffy white substance to form. Heating it was hoping it would melt at the temperature around which phenol would, and it didn't. It remained a solid until I tossed it.
So I've concluded that heating Sodium hydroxide and ASA together doesn't make phenol. I should have added less NaOH, and attempted to distill the phenol that would form. This would likley still lead to significant charring but it should work. I'll try it some other time.
Even more recently, I've broken apart 3-4 (can't remeber) D sized batteries, extracted the MnO2, ground it in a mortar and pestle and then heated with strong sulfuric acid and some sulfur.
The idea was to get MnSO4 with this reaction:
MnO2 + SO2 = MnSO4
H2SO4 + S = H2O + 2 SO2 ( or really, H2SO3 + SO2 but heat decomps the acid)
Also hot sulfuric acid tends to dissolve MnO2 anyways.
This reacted fumed off lots of white smoke, even (if not especially) before the addition of sulfur, and a decent amount of MnO2 seemed to dissolve. I added HCl to see if any was left, and there was a ton. Chlorine gas was evolved, though bubbles were not noted until vigorous stirring. The chlorine formed for a good hour before I decided to put in an air bubbled to encourage the Cl2 to leave the solution. The air bubbler was originally used for fish, or something like that.
The solution is sitting outside, about 1L worth, with the air still bubbling though it. I'll leave it till tomorrow or the next day to boil it a bit more to get some of the HCl, or chlorine out.
MnO2 + 4 HCl = MnCl2 + Cl2 + 2 H2O
Since there is an excess amount of H2SO4 in the solution.. the following occurs..
MnCl2 + H2SO4 = MnSO4 + 2 HCl
The HCl is either going to be reacted with more MnO2, or get kicked out of the solution, especially when I boil it in the next couple of days.
So, soon I should be left with a lot less MnO2, and a bunch of MnSO4 (or other sulfates of Mn) in a solution of sulfuric acid. Likely with carbon at the bottom. The top will just be separated, titrated, and then used for some oxidation thing I have in mind
Soon, I will try a Nickel/Copper extraction from a solution of 25% Ni and 75% Cu - in their Nitrates that I have prepared. (nickels were dissolved in dilute HNO3)
This will be a bit tricky, but I think it can be done, and for me at least, will be useful to be able to get Ni powder fairly cheaply. Ni powder could be used for Hydrogenation itself, electroplating onto materials for hydrogenation, or to get Ni hydroxide/oxide complexes with ammonia (probably forms?) which could be absorbed onto very fine activated, or reactivated carbon, reduced to leave very small Ni powder with a high surface area - again for hydrogenation.. of course.
Any suggestions on the best how to go about these things? or how to make that phenol?
I've decided to create one since I've been getting back into the lab lately and this might encourage me to do more things.
Recently I attempted making some crude phenol. It was a total failure and I think I ended up with only Salicylic acid and some black carbon like material.
I mixed ~20 grams of NaOH with 18 grams of ASA. The ASA was purified from aspirin w/ denatured alcohol. I ground the two together, mixed them in a flask and heated with a torch. Water came off as the mixture was molten. I continued to heat it and it became solid, white fumes started to come off (which, the phenol should have been in the form of sodium phenolate, so I don't think this should have happened!) and it started to char and turn black in some areas. I decided that it was probably done, and so I dissolved some in water, added an acid and found a very fluffy white substance to form. Heating it was hoping it would melt at the temperature around which phenol would, and it didn't. It remained a solid until I tossed it.
So I've concluded that heating Sodium hydroxide and ASA together doesn't make phenol. I should have added less NaOH, and attempted to distill the phenol that would form. This would likley still lead to significant charring but it should work. I'll try it some other time.
Even more recently, I've broken apart 3-4 (can't remeber) D sized batteries, extracted the MnO2, ground it in a mortar and pestle and then heated with strong sulfuric acid and some sulfur.
The idea was to get MnSO4 with this reaction:
MnO2 + SO2 = MnSO4
H2SO4 + S = H2O + 2 SO2 ( or really, H2SO3 + SO2 but heat decomps the acid)
Also hot sulfuric acid tends to dissolve MnO2 anyways.
This reacted fumed off lots of white smoke, even (if not especially) before the addition of sulfur, and a decent amount of MnO2 seemed to dissolve. I added HCl to see if any was left, and there was a ton. Chlorine gas was evolved, though bubbles were not noted until vigorous stirring. The chlorine formed for a good hour before I decided to put in an air bubbled to encourage the Cl2 to leave the solution. The air bubbler was originally used for fish, or something like that.
The solution is sitting outside, about 1L worth, with the air still bubbling though it. I'll leave it till tomorrow or the next day to boil it a bit more to get some of the HCl, or chlorine out.
MnO2 + 4 HCl = MnCl2 + Cl2 + 2 H2O
Since there is an excess amount of H2SO4 in the solution.. the following occurs..
MnCl2 + H2SO4 = MnSO4 + 2 HCl
The HCl is either going to be reacted with more MnO2, or get kicked out of the solution, especially when I boil it in the next couple of days.
So, soon I should be left with a lot less MnO2, and a bunch of MnSO4 (or other sulfates of Mn) in a solution of sulfuric acid. Likely with carbon at the bottom. The top will just be separated, titrated, and then used for some oxidation thing I have in mind
Soon, I will try a Nickel/Copper extraction from a solution of 25% Ni and 75% Cu - in their Nitrates that I have prepared. (nickels were dissolved in dilute HNO3)
This will be a bit tricky, but I think it can be done, and for me at least, will be useful to be able to get Ni powder fairly cheaply. Ni powder could be used for Hydrogenation itself, electroplating onto materials for hydrogenation, or to get Ni hydroxide/oxide complexes with ammonia (probably forms?) which could be absorbed onto very fine activated, or reactivated carbon, reduced to leave very small Ni powder with a high surface area - again for hydrogenation.. of course.
Any suggestions on the best how to go about these things? or how to make that phenol?